• 专利附录
  • 专利说明
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  • 优先权
    • 专利摘要:
    The microcapsules have a shell of polyurea which surround a pesticidal active substance which is not miscible with water. The process consists in first dispersing a solution of a polyisocyanate in the pesticide which is sparingly soluble in water in the presence of an anionic dispersant and at least one non-ionic protective colloid and/or a non-ionic surfactant, and subsequently reacting the dispersion with a polyamine. In this manner, stable aqueous suspensions of microcapsules are obtained which can be used as pesticides either directly or after dilution with water.
    公开号:SU1741602A3
    申请号:SU864028125
    申请日:1986-09-12
    公开日:1992-06-15
    发明作者:Вальтер Хэсслин Ханс；Дж.Хопкинсон Майкл
    申请人:Циба-Гейги Аг (Фирма)；
    IPC主号:
    专利说明:

    surfaces in the dispersion, when one of the components necessary to form the capsule wall is dissolved in the dispersed phase, and the other in the continuous phase. This method is carried out in such a way that the solution of the first reactive component necessary for the formation of the capsule wall is first dispersed in a continuous phase and then the solution of the second reactive component is added in a medium that forms a continuous phase. At the same time, it is recommended that organic water is not miscible with water. phases in continuous aqueous phase, use non-ionic protective colloids, like polyvinyl alcohol, gelatin and methylcellulose
    A method of obtaining a suspension of microcapsules with a capsule wall of polyurea containing a germicidal active substance Spb is carried out in such a way that a solution of polymethylene polyphenyl isocyanate in the herbicidal active substance is dispersed in water and the dispersion is immediately afterwards introduced into the reaction of an aqueous polyamine solution. ligninosulfonic acid salts are used as a dispersant.
    A significant disadvantage of the known methods is that the use of dispersing agents after adding the second reactive component leads to a strong increase in viscosity, which greatly reduces the mixability of the mixture. "This is especially manifested when the amount of active substance of the dispersed phase consisting of isocyanate and if appropriate, the solvent is high and is, for example, 50 masD or more. As a result of reduced stirring, the reaction process has a negative effect, and this leads to a slow and incomplete interaction of both reaction components. As a result, the resulting suspension of microcapsules in the aqueous phase contains unreacted polyamine and unreacted polyisocyanato in the capsule. This is undesirable, in particular, when directly using the resulting capsule dispersion.
    The aim of the invention is to increase the concentration of microcapsules in the aqueous dispersion while

    , at
    15
    20
    2U
    M602
    increasing the pesticide capsule content,
    In accordance with the invention c. as dispersing agents, oligomers and polymers are used, as well as polycondensates, which contain a sufficient amount of anionic groups so that their water solubility is ensured. Suitable anionic groups are, for example, sulfo groups or carboxyl groups, and polymers with carboxyl groups can only be used at a higher pH, preferably more than 5. The number of anionic groups per polymer molecule is usually at least 60% of the monomeric units involved in the construction of molecules with oligomers and polymers that contain sulfo groups can be obtained either by polymerization of monomers containing sulfo groups or by sulphonation of the corresponding oligomers s or polymers. Polymers that contain carboxyl groups can be obtained by saponification of polyacrylates or polymethylacrylates, and the degree of saponification should be at least 60%. In particular, sulfonated polymers and condensation products of aromatic sulfonic acids with formaldehyde are suitable as anionic dispersing agents. Typical anionic dispersing agents are:
    A. Salts of polystyrene sulfonic acids, in particular alkali metal, alkaline earth metal salts and ammonium salts, as well as salts of organic amines, which can be obtained by polymerization of styrene sulfonic acids or their salts or by sulfonation of polystyrene and subsequent neutralization with an appropriate base, and in the case of sulfonation of polystyrene, the degree of sulfonation is em at least 60% „
    In “Salts of polyvinyl sulfonic acids, in particular salts of alkali, alkaline earth metals and ammonium, as well as salts of organic amines, which can be obtained by polymerization of vinyl sulfonic acids or their salts.
    C. Salts of condensation products of naphthalene sulfonic acids, in particular naphthalene-2-sulfonic acids, with formaldehyde, in particular with alkali salts, alkalis 30
    35
    40
    4S
    50
    55
    ground metals and ammonium salts, as well as their salts,
    U, Salts of condensation products of naphthalenesulfonic acids with phenolsulfogic acids and formaldehyde, in particular (alkali and alkaline earth metal salts and ammonium salts, as well as salts obtained with organic amines.
    E. Salts of ligninsulfonic acids, in particular sodium, potassium, calcium, or ammonium salts
    Preferred anionic dis (agents of polystyrene sulfonic acid (type A), salts of condensation products of naphthalenesulfonic acid with formaldehyde (type C and especially condensation products of naphthalenesulfonic acid with phenolsulfonic acid and formaldehyde (type U)
    Especially preferred as anionic dispersing agents are condensation products of naphthalenesulfonic acids with phenolsulfonic acids and formaldehyde type D, They can be obtained as follows. Naphthalene at 120-130 ° C is first converted with concentrated sulfuric acid and / or oleum into naphthalene sulphonic acid, phenol is added to the reaction mixture immediately after that, first it is reacted at 120-130 ° C and then the reaction water is separated in vacuum at 150-170 ° C and the reaction product after cooling to 90 is condensed with
    Formaldehyde is then neutralized to pH 6-7, evaporated to dryness and the residue is granulated. In this way, a water-soluble anionic dispersant (dispersant A) is obtained in the form of a granulate with an average weight of 6000-8000.
    When sulphonating naphthalene under these conditions, naphthalene-2-sulfonic acid is preferably formed along with a small amount of naphtha lindisulfonic acid. After the addition of phenol, in particular, during subsequent heating to 150-170 ° C, along with phenolsulfonic acid, sulfones are also formed to a large extent, as 4, V-dehydroxydiphenylsulfone and -hydroxyphenylnaphthalylsulfone Therefore, upon subsequent condensation with formaldehyde, a polymer is obtained, the monomeric components of which cephinecholine / sulfinone are synthesized, and the divine sulfonyl sulfone is further synthesized into 4-V-dehydroxyphenylnaphthalylsulfone. partially bonded
    s
    g
    one}
    to
    25
    7M602 "
    through methylene groups and partially through sulfo groups. When preparing the dispersant A, naphthalene, phenol, sulfuric acid, formaldehyde and the base can be used in the molar
    1: 0.5 to 1: 2 to 2.5: 0.4: 0.8: 2 to 3. The preferred molar ratio of naphthalene: phenol: sulfuric acid: formaldehyde: base is 1: 0.7: 2: 0.5: 2, and sodium hydroxide is preferably used as the base. Beneficial to sulfuric acid
     5 was a mixture of concentrated sulfuric acid and oleum, and the amount of free 80 in oleum is equivalent to at least the amount of water in. , -Q is concentrated sulfuric acid, so that when mixing concentrated sulfuric acid and oleum, at least 100% sulfuric acid is obtained. Formaldehyde is preferably used in the form of an aqueous solution, for example, in the form of a 37% aqueous solution. It is advantageous to carry out the distillate separation of the reaction water at a pressure of 10–50 bar.
    As a non-ionic protective colloid, ordinary water-soluble polymers should be kept in mind, they say.
    the weight of which, as a rule, is 10,000-200,000. In this case, the average diameter of the formed capsules can be influenced by the molecular weight of the used corresponding water-soluble polymer. Use of lower molecular weight water soluble polymers
    H results in a lower viscosity of the reaction mixture and thus the formation of large capsules, while the use of water-soluble polymers with a higher molecular weight leads to a higher viscosity of the reaction mixture and, thus, K -. the formation of capsules with a smaller diameter. Suitable water-soluble polymers are, for example, polyvinyl alcohol, polyvinyl methyl ether, polyvinyl pyrorolidone, hydroxyethylcellulose, hydroxypropylcellulose, methylcellulose (1.5-2 degree of substitution), acetralcellulose, citrate, acetra, cellulose, citrate, nitrocellulose, citrate, cellulose acetate, methylcellulose (1.5-2). poly (2-hydroxyethyl) methacrylate, poly- 2- (2-hydroxyethoxy) -ethyl- (methacrylate, polyethylene oxide) poly-
    thirty
    45
    50
    55
    71
    oxyethylene 3 and polyallyl alcohol (polyglycidol).
    A preferred non-ionic protective colloid (NLC) is poly vinyl alcohol. Particularly suitable are polyvinyl alcohols with a viscosity of 18 - IO P- (measured in
    % aqueous solution at 20 ° C), which is obtained by saponification of polyvinyl acetate, the degree of saponification being at least 60%, but preferably 80 to 95%. Suitable products of this type are MOWIOL®.
    Nonionic water-soluble polymers and water-soluble polymers with mol. Weight are also used as non-ionic surfactants. less than 20,000, preferably less than 5,000. Particularly suitable nonionic surfactants of this type are the reaction products of ethylene oxide or combined interaction of ethylene oxide and organic oxide with fatty alcohols, alkylphenols, fatty acids, essential fatty acids, polyhydroxy compounds, fatty acid amides and fatty amines. the number of units of ethylene oxide and propylene oxide can vary widely (Typically, the number of units of ethylene oxide or ethylene oxide / propylene oxide lies in the range from 1 to 200, preferably 100 and particularly preferably 8 to 0. Suitable non-ionic surfactants are, for example, the following
    Alkyl polyethylene glycol ether of formula
    KG ° ECH rCHi- ° 1-h, u





    where & is C8-Sgo-alkyl;
    P,
    2-100,
    Products of this type are designated BRJ No ETHJLAN® CD, ETUJLAITD GENA-POL®C, GENAPOU4), GENAPUL®.
    Alkylphenol polyethylene glycol ether of formula I
    € 0 {CH2-CIVOj-H
    m,
    re

     AND 2
    where RЈ is Cg-Sz-nicks;
    35 - 2 - 40.
    Preferred values are octyl and nonyl. Products of this type are commercially known. Antarox (GAF), TRITON X ATLOX® 4991 UCI, ARKOPAl, ETNJLAN®
    K. Phenylethylphenol polyglycol ether of the formula
     AND 2
    sn,
    WI 1
    ryb OolCHj-CHfO H
    tz Jrri2
     AND 2
    3;
    50.
    These products may also be referred to as ethoxylated streliphenols. Products of this type are called DISIJ®125 SOPROPHoAj 8.
    Polyethoxyethyl esters of fatty acids of the formula
    AND 2
    R3 C-OfCH2-CH2-O H
    where R C8-C4g-alkyl or alkenyl; P4 2 - 50. These products, in particular, are derived from lauric acid, oleic acid and stearic acid. In trade, such products are called NONISOL, MJRJ® (J.CI).
    Sorbitan-polyethylene glycol fatty acid ester of the formula
    N O-SNG O-SN-SN-O-Yesng-CIS-O n
    itn
    H2C JCH-CH-CH2-0-C -5-pI
    h
    oicHfCH -o
    h
    CH2-0-C -5- I
    oicHfCH -o H
    where R is Cg-C-alkyl; x, y and z are 1-50, and the sum of x + y + z is 20-150. As an acid residue, R4 should be in the form, in particular,
    residues lauric, stearic, fell mitic and oleic acids. Such products are also referred to as Polisor & and are known as TWEEN® (ICI).
    Triglyceride-polyethyleneglycol ether formula
    ABOUT
    CH2-0-C-R5 | O
    CH-0-C-Re
    ABOUT
    and
    where R5, R6 and R7 residue of the formula
    OtCHfCHfO H iCHj CH CH-CH CHfCHzJsCHj
    /
     where Rg and R independently of each other also mean alkyl or C Cr0-alkenyl and n in 3 - 100. As the acid residue RgCO- and R6CO - with C8-C20-alkyl and Cg-Cgo-alkenyl group especially should be borne in mind residues of lauric, palmitic, stearic and
    ъ
    N o-sn2-dn S o-sn2-sn2) x
    CH3.
    . (CH2-Sh2-O CH-CIS0) uN
    H-to "and wi §2 2 / D / t V / XV l 2 yUf
    CH3) N {CH2tN. CH3
    CH2-CH JyfO-CHjrCH (CH2-CH2-0 (0) in H
    7 where x and y are 2-50, respectively, and the sum x + y is k-100 respectively. Products of this type are known in the trade under the name TERRONIL M TETRONIC® (BASF Wyandotle Corp).
    Alkyl- (polyethylene glycol) -poly-propylene glycol ethers of the formula
    17 160210
    oleic acid. A preferred representative of this type of surfactant is ethoxylated castor oil. Such products are known as EMULSOGEW.
    Polyethyloxyethylamides of fatty acids of the formula
    about
    II
    R0-C-N
    jCHfCHfOjjH
    sngng-on
    where RB is C, gCl-alkyl, C 8 C g o-alkenyl; t, - and - respectively 1-25.
    As the acid residue of Rflbu, preferably lauric, oleic, palmitic and stearic acids should be kept in mind. Products of this type will be reported under the names AMIDOX®, ETNOMShF. N-polyethoxyethylamine formula
    Sngsng% en Cg% ngsng-about 8n
    where Rg is Cg-Cfg-alkyl or, d-alne
    Nile;
    ng - 1 to 15 ° respectively. Especially suitable are products that split off fatty amines such as coconut fatty amine, oleylamine, stearylamine, and animal fatty amine. Such products are known commercially under the name, for example, GENAMIN (Uoechit). K, L, N - tetra (polyethoxypolyproxyethyl) ethylene diamines of the formula
    CH3.;
    . (CH2-Sh2-O CH-CIS0) uN
    / t V / XV l 2 yUf
    N. CH3
    CH

    VOfWfCHrOfe-ECH-CHfO - -fCHrCHrOjjj-H
    1117 H60
    hydrogen;
    -alkyl or St.-Sao-alkenyl5
    respectively 2-200 and n about "10 - 80, and in the sum

    C + n, 0 + n,
    is 15.
    t
    Especially suitable are products of this type that are known in the trade.
    of valence alcohol, respectively, the number of moles of diisocyanate corresponding to the number of hydroxyl groups of the corresponding alcohol is. Thus, several diisocyanate molecules are connected by cutting urethane groups with multivalent alcohol to form 10 POLONIC BASF) and pre-10 molecular polyeocyanates. Particularly Stavla are block copolymers of polyethylene oxide and polypropylene oxide.
    (RF n).
    Preferred nonionic surfactants are block copolymers of ethylene oxide and propylene oxide (PLURONICb),
    NfN, N, K-tetra (polyethoxy-polypropypoxyethyl) -ethylene diamines (TETKONI CS®), nonylphenol polyglycol ethers with 10-20 ethylene oxide units, alkyl-polyethylene glycol ethers, which are cleaved from the fatty alcohols (GENA-P01), which are separated from the aroma (I-RO), and they are separated by red-glycol ethers (GENA-RO), alkyl-polyethylene glycol ethers, which are cleaved from the fatty alcohols (GENA-RO), and they are separated by redox glycol ethers (GENA-RO), which can be removed from the polyester glycol esters (GENA-PPO), alkyl-polyethylene glycol ethers, which are cleaved from the fatty alcohols (GENA-P01) and alkyl-polyethylene glycol ethers, which are cleaved from the fatty alcohols (GENA-P01), and they are separated by redox polyethylene glycol ethers, which are cleaved from the alcohols (GENA-RO). split off fatty amines (GENAHIN). Particularly preferred non-ionic surfactants are block copoly20
    but a suitable product of this type can be obtained by modifying 3 mol of toluylene diisocyanate with 1 mol of 2-ethylglycerol (1,1-bis15 methylolpropanol) (DESMOUUR). Other suitable products are obtained by the addition of hexamethylene diisocyanate or isophorone diisocyanate to ethylene glycol or glycerol. Preferred polyisocyanates are diphenylmethane-.A-diisocyanate and polymethylene polyphenyl isocyanate. These di-, triisocyanates can be used alone or as a mixture of two or more of these isocyanato
    As polyamines, one should generally understand such compounds that contain two or more amy25.
    ethylene oxide and propylene oxide (PLflRONICi O „
    Polyisocyanates are understood to mean such compounds that contain two or more isocyanate groups in a molecule. Di- and triisocyanates are preferred, and isocyanate groups can be bound to an aliphatic or aromatic basic skeleton. Examples of suitable aliphatic diisocyanates are tetramethylene diisocyanate, pentameti- lendiizotsianat and geksametilendiizo- cyanate Suitable aromatic isocyanates are toluilendiiao- cyanate (TDI, mixture and 2,6-isomers), difenilmetan- -diizotsianat / / MDI, DESMODUtTVL) , polymethylene polyphenyl isocyanate (MONDyi MR, PAPI®, PAPT®135), 2, b, k-diphenyl ether of triisocyanate, 3,3-dimethyl- - diphenyl diisocyanate, 3 3g-dimethoxy- - lendiisocyanate and A, V, 4 -triphenylmethanethriisocyanto To another suitable diisocyanate is isophorone diisocyanate. In addition, adducts of diisocyanates to multivalent alcohols, such as ethylene glycol, glycerin and trimetch tyolol propane, are suitable, and in a molecule of many
    valence alcohol is attached respectively to the number of moles of diisocyanate, corresponding to the number of hydroxyl groups of the corresponding alcohol. Thus, several diisocyanate molecules are bound by the urethane groups of the polyvalent alcohol to form high molecular weight polyeocyanates. Special
    molecular polyeocyanates. Special
    0
    but a suitable product of this type can be obtained by modifying 3 mol of toluylene diisocyanate with 1 mol of 2-ethylglycerol (1,1-bis5 methylolpropanol) (DESMOUUR). Other suitable products are obtained by the addition of hexamethylene diisocyanate or isophorone diisocyanate to ethylene glycol or glycerol. Preferred polyisocyanates are diphenylmethane-.A-diisocyanate and polymethylene polyphenyl isocyanate. These di-, triisocyanates can be used alone or as a mixture of two or more of these isocyanato
    As polyamines, one should generally understand such compounds that contain two or more amine groups in a molecule, and these amino groups can be linked to an aliphatic and aromatic basic skeleton. Suitable aliphatic diamines are, for example, W5
    five
    n - - .-- - .. well. W «| g-g9
    diamines formula. CHj-NH2, where
    0
    n is an integer from 2 to 6. Examples of such diamines include ethylene diamine, propylene-1,3-diamine, tetramethylene diamine, pentamethylene diamine, and hexamethylene diamine.
    Other preferred aliphatic diamines are. polyethylenimines of the formula
    HtN-CH2-CH4-NH n-Hg where-n is the integer 5, the number is 2-5. Examples of such polyethylenimines are diethylene trienemine, triethylene tetramine, tetraethylene pentamine, penta ethylenehexamine.
    Other suitable aliphatic polyamines are dioxaalkane -OC-diamines, such as 1,9-dioxadodecane-1,12-diamine of formula
    0
    HjH-CcHi -O-fCHj CHj NH. Suitable aromatic polyamines are, for example, 1,3-phenylenediamine, 2, -toluylene diamine, k, C-diaminodiphenylmethane, 1,5-diaminonaphthalene, 1,3,5-diaminobenzene, 2,4,6-triaminotoluene, 1, 3,6-triamino-naphtali n, 2,, C-tri-aminodiphenyl ether, 3.5 triamino-.1,2, -triazole and 1, A, 5 8-tetraminoanthraquinone "Those of the polyamines mentioned, which are not soluble or not sufficiently soluble in water; can be used in the form of hydrochloride
    In addition, polyamines are suitable, which, in addition to amino groups, contain sulfo groups or carboxyl groups. Examples of such polyamines are 1, α-phenylenediamine sulfonic acid, 1, α-diaminodiphenyl-2-sulfonic acid or diaminomonocarboxylic acids, such as ornithine and lysine.
    These polyamines can be used alone or as a mixture of two or more polyamines „
    As pesticides that can be prepared in accordance with the invention, it should be borne in mind that they are insoluble in water but stable in it, at room temperature they are liquid i substances or have a melting point of 6 ° C or soluble in an organic solvent that is not miscible with water; inert to isocyanates; have the solubility of the polyis of the mentioned type of cyanates, 8 which are not miscible with quality; These solvents in which pesticides can be dissolved should be in the form of aliphatic and aromatic hydrocarbons, such as hexane, cyclohexane, benzene, toluene, xylene, mineral oils, or kerosene. In addition, cyclohexane, as well as chloride, chloroform, carbon tetrachloride, chlorobenzene, and c-dichlorobenzene. In addition, mixtures of mono- or multiply alkylated aromatic compounds are suitable, such as compounds known in the trade under (SHELLSOL®),
    . According to the invention, pesticidal active substances of various types can be obtained, for example, herbicides, plant growth regulators, insecticides, aericides, nemacides, ectoparasiticides, which have a different chemical structure and can belong to different lassam compounds. Classes of substances,. cotsdzym may belong to flattery-10
    15
    2S
    The cide active substances that can be obtained according to the invention are the following: S-triamines, ureas, haloacetanilides, derivatives of diphenyl ethers, derivatives of fenok-sipropionic acids, dinitroanilines, acylalanines, derivatives of triazole, carbamates, phosphoric acid esters , pyrethroids, esters of benzoic acid, polycyclic halogenohydrocarbons of formamidines .and dihydro-1, 3-diazol-2-ylylene-anilines. The following are examples of the most applicable compounds of these classes of compounds
    S-triazine: atracin. propacin, terbutylacine, ametrine, aziprotrin, desmetrin, dipropatrin, prometrin, 2o terbutrin, sekbumeton, terbumetron
    Urea; chlorbrumeton, chloroxuron, chlorotoluron, fluoromethuron, metobromuron, tiazafluroNO
    Haloacetanilide: dimethachlor,
    metolachlor, pretilachlor, 2-chloro-L1-0-methyl-2 methoxyethyl) acet-2,6-xylidide, alachlor, butachlor, diethylethylethyl, propachlor
    Derivatives of diphenyl ethers:
    bifenox, dichloromethyl, D (-pentin-2-yloxy) -diphenyl ether. Phenoxypropionic derivatives
    Acids: Fluaciphon
    Dinitroanilines: butralin, ethalfluralin, fluchlororalin, isopropalin,
    pendimet, profluralin, trifluralin
    i
    Acylalanines: fluralacyl, metalacyl, benzoylprop-ethyl, flamprop-methyl
    , Triazole derivatives: ataconazh | I, propiconazole, (2, -dichlorfenl) - pent-1-yl -1H-1,2, -triazole, .riadime- von „
    Carbamates: dioxacarb, furathiocarb, aldicarb, benomyl, 2-fluoro-butylphenyl methylcarbamate, ethiofencarb, isoprocarb, propoxur, carbetamide, butylate, di-allat, ERTS, molinat, thiobencarb,.
    tri-allat, vernolat. Phosphoric esters: piperfos, anilofos, butamiphos, azamethifos, chlorophenviphos, dichlorophos, diazinon, methidathion, azinphos-fetil, aerofos-ethyl, chlorpyrifos, chlorothiophos, crototoxyphos, cyanophos, cytophysophosph, cytophose, ethyl, chloropyrifos, chlorothiophos, crotoxyphos, cyanophos, cytophose, cytophose, ethyl. , disulfoton, etrimphos, famfur, flusulfofion, flut i
    0
    five
    0
    five
    0
    five
    1517 & 02
    thion, phonophos, formotion, heptenophos,
    isophenos, isoxathion, maltion, methofolan1, mevinphos, frost, oximeteton-megil oxydephros, parathion, foxim, pyrimiphos-methyl, lrofenophos, prolaphos, propenthanphos, prothiofos, quinalphos, sulprofos, fefeosfef, fefefos, protifethos, prothiofos, quinalphos, sulfophos, fefeosfef, promethanophos, prothiofos, quinalphos, sulfofos methyl , phenamipos, azafos, 8-benzyl-o, o-diisoprolylphosphorothioate, edinfos, pyrazo-for
    Pyrethroids: allethrin, bioallethrin biosmetrin, cyhalothrin, cypermethrin deltamethrin, fenpropathrin, phenealers flucitrinates, fluvalinates, permatrin, pyrethrins, ravmetrin, tetrametrin, tralometryNO
    Esters of benzoic acid: bromopropyl, chlorobenzylate, chloropropylate.
    Polycyclic halogenated hydrocarbons: aldria, endosulfan.
    form of mussel: chlordimeform.
    Dihydro-1, 3-thiazol-2-ylylen-alinines: N- (2,3-dihydro-3 methyl-1,3-thia sol-2-ylidene) -2, -xylidine.
    Other compounds: methoprene, kinoprene; flupropimorph, tridemorph; bromoxynil; crimidine bupirimana; Setslcidim, chlorfenprop methyl; carboxy; butobiobates, amitrac; Dicofol; oxadiazon; prokhloraz, propargits; di amba; camphor; chlorfenzon,
    Irocapsules can contain pesticidal active substances as self-contained compounds, as well as a combination of two or more pesticidal active substances.
    The method of producing microcapsules is advantageously carried out in such a way that an anionic dispersant and a non-ionic protective colloid and / or a non-ionic surfactant are first dissolved in water and immediately after this is added a solution of one or more polyisocyanates of the mentioned type in one or more active substances or in a solution of one or more of these active substances in a water-immiscible solvent and vigorously stirred until a homogeneous suspension is obtained. Then, with further stirring, one or more polyamines of the type are added and the mixture is stirred until the polyamine is fully reacted with the isocyanate. Polyamines are preferably added as an aqueous solution.
    sixteen
    five
    0
    five
    The method can be carried out at room temperature or at a slightly elevated temperature. Suitable temperatures range from 10 ° C to 75 ° C. It is preferable to carry out the method in the temperature range from 20 to 5 ° C.
    The reaction time of the polyisocyanate with the polyamine is typically 2-30 minutes. The appropriate degree of interaction and the end of the reaction can be established by titration of the free amine present in the aqueous phase.
    The components necessary for the formation of the capsule walls can usually be used in an amount of 2.5 to 30 wt.%, Preferably 5 to 20 wt.%, Based on the material that is encapsulated, and the encapsulating material can consist of the active substance. or a mixture of two or more active substances, or from a solution of the active substance or a mixture of two or more active substances in a water-immiscible solvent. The number of components used in a particular case, necessary for the formation of a capsule wall, depends primarily on the wall thickness of the capsule formed and, moreover, on the size of the capsule,
    According to the invention, aqueous dispersions of microcapsules can be obtained which contain in a liter 100 to 700 g of microcapsules. Preferably they contain in the resulting dispersion 00 to 600 g of microcapsules in a liter. Dispersion microcapsules are immediately ready for consumption. However, they can be stabilized for transportation and storage of various additives, for example, additives of surfactants, thickeners, antifoams and antifreezes.
    However, it is also possible to separate the microcapsules by filtration or centrifugation and either dry or transfer the dispersion again. The microcapsules isolated from the dispersion and dried are a flowing powder that can be stored for almost unlimited time.
    As a result of the simultaneous use of an anionic dispersant and a non-iniogenic protective colloid and / or a non-ionic surfactant already during dispersion
    0
    S
    0
    five
    the solution of the polyisocyanate in the pesticidal active substance decreases a strong viscosity increase, which occurs, in particular, when using a single anionic dispersant. As a result, not only the carrying out of the process is facilitated, but a more rapid and complete interaction of the polyisocyanate and the polyamine is achieved, thereby preventing the formation of by-products. The reduction in viscosity of the reaction mixture results, in addition, with the same shear force (Scherkrafc), to obtain a finer dispersion and thus a decrease in the diameter of the resulting capsules. The capsule emulsions obtained in accordance with the invention are stable and do not show for a long time. the formation of serum or sediment. The resulting dispersions of microcapsules show a suitable choice of the type and amount of anionic and non-anionic dispersant with thixotropic properties and therefore they can be transferred shaking or mixing in a fluid state
    The examples indicate the trade names used and other designations for the following products: izaeophos (0,0-diethyl-0- | (5 chloro-1-isopropyl-1,2-triazol-3 yl) -tyophosphate; propicanazole (1- [2- (2, -dichlorophenyl-4-propyl-1,3-dioxolan-2-ylmethyl] -1-4-1, 2,4-triazole; N-chloro-cetyl-K- (2-methoxy) -1-methylethyl) -2,6-dimethyl-aniline; chlorfenvinphos (0,0-diethyl- 0- / 2-chloro-1- (2,4-dichlorophenyl) -vinyl / phosphate, H-chloroacetyl-H- (2-methoxy-1-methylethyl) -2,6-dimethylaniline; methanol (H-chloroacetyl-I- (2-methoxy-1-methylethyl) -2-ethyl-b-methylaniline; diazinon (0.0- diethyl-0- (2-isopropyl-methylpyrimidine- -yl) - t iofosfat; furatiocards (butyl-2,3 dihydro-212 dimethylbenzofura n-7-yl-N, N -dimethyl-N, H -thiodicarbamate); N- (2,3-dihydro-3-methyl-1, 3-thiazole-2-ylidene) xylidine; profenophos (0-ethyl-0- (2-chloro-bromophenyl) -Y-propylthiophosphate) | MDI-diphenylmethane-diisocyanate. GID-hexamethylenediamine.
    Dispersant A is a naphthalene sulfonic acid condensate / fe-t of nolsulfonic acid and formaldehyde.


    25
    This mixture is an anionic dispersant.
    The experiments were carried out using a high shear mixer to obtain an OR with the active component in water. With a lower mixing speed, use the usual four-lobed.
    10 agitator.
    Example 1. g of diazinon (of technical quality) is mixed with 12.4 IDE Э This mixture is added to a stirred solution of 1.6 g of sodium ninsulfonate lig15 in 45 g of deionized water at 19,500 rpm. The suspension obtained in this way. after 1 min, the speed of mixing is reduced and 5.1 g of a 40% aqueous solution of HYDA is added to the content, stirring is continued at low speed.
    1min after adding GIDA the mixture cannot be mixed more, through
    2min it can not be drained and through
    5 minutes the mixture hardens and becomes like a clot.
    Example 2. 99 g of diaeinone (technical quality) are mixed
    30 with 12.4 g of IDEA. This mixture is added to a stirred solution of 1.6 g of Pluronic F 08 and sodium boron ligninsulfonate 1, b at a rotation speed of 15,000 rpm. The resulting such
    jj, the dispersion can be mixed. After 1 min, the speed of unmixing is reduced and 5.1 g of a 0% aqueous solution of HIDA is added to the contents; Stirring continue
    40 eat at low speed. The dispersion thus obtained has a constant low viscosity. Through
    The 3d viscosity is measured and is found to be 1000 mPa.s,
    45 Crisis (for comparison). 99.4 g of diazinon (technical grade) are mixed with 7.8 IDN. This mixture is added to a stirred solution of 1.6 g of dispersant B in 45 g of
    50 ionized water at speed
    10,000 rpm The dispersion thus obtained has a low " viscosity. After 1 min, the stirring rate is reduced and 55 g of a 40% aqueous solution of GIDA is added to the contents. Stirring is continued at low speed. Immediately after adding the TNDA, the suspension thickens and after 2 minutes it cannot be reapplied.
    stir up, and after 5 minutes it can not be drained,
    Example. g of diaz | non (technical grade) is mixed with 7.8 g of IDN. This mixture is added to a stirred solution of 1.6 g of Pluronic F 108 and 1.6 g of dispersant A at 10,000 rpm. The mixture thus obtained has a low viscosity After 1 min, the mixing rate is reduced and a 3.25 40% aqueous solution of HMDA is added to the contents. Stirring is continued at low speed. The suspension thus obtained has a low viscosity. After 60–90 min, a slight thickening effect is observed (viscosity 00–1000 mPe-s)
    The viscosity measured after 2 hours is 1000 Mnavc o
    EXAMPLE 5 (for comparison), 82.8 metolachlor (technical grade) is mixed with 1.6 g MDI. This mixture is added to a mixed solution of 1.6 g disperser A in 5, U g of deionized water with 1U600 about „/ / min.
    The dispersion obtained in this way has a low viscosity. After a minute, the mixing speed is reduced and 6.1 g of a 0% aqueous solution of HMDA is added to the contents. Stirring is still continued at a low speed.
    The suspension immediately becomes viscous and turns into a clot. After 3 min the mixture cannot be mixed more.
    Example 6 82.8 g of metolachlor (technical grade) is mixed with 1A, 6 g IDN This mixture is added to a stirred solution of 1.6 g Pluronic F 108 and 1.6 g disperser in kk, 3 g deionized water at 15,000 vol. / min The dispersion obtained in this way has a low viscosity. After 1 minute, the stirring rate is reduced and 6.1 g of a 40% aqueous solution of HMDA is added to the contents. The suspension thus obtained has a constant low viscosity, which after 2 hours is 370 mPa.s
    PRI me R 7 (according to prototype 82.8 metolachlor (technical grade) is mixed with 25.1 g MDI. This mixture is added to the stirred solution 1 (6 g sodium ligninsulfonate in
    1602
    20
    35.7 g of deionized water at a rotation speed of 19800 rpm. The dispersion obtained in this way is
    in vkoy. After 1 min, the stirring rate is reduced and 10.1 g of a + 0% -% aqueous HMDA aqueous solution is added to the contents. Stirring is still continued at low speed. Dispersion
    it can be stirred for 15 seconds, after 30 seconds it thickens, after 1 minute it mixes weakly and after 2 minutes it cannot be mixed. After 5 minutes the mixture turns
    into a clot
    Example 8 82.8 g of metolachlor (technical grade) is mixed with 25.1 g MDIS. This mixture is added to a stirred solution of 1.6 g Pluronic F8 and 1.6 g sodium ligninsulfonate in 3.1 g deionized water at a rotation speed of I80t) 0 rev / min. The dispersion obtained in this way is viscous. After 1 min the mixing speed is reduced and 10, g of 40% aqueous solution of HMDA is added to the contents. The dispersion obtained in this way has a low viscosity, and OK
    mix after 3, 10 and 20 minutes. The viscosity measured after 5 days is 1680 mPa-s.
    The average diameter of the obtained microcapsules, the content of diazinon or metolachlor, the polymer content and external signs and the behavior of the mixtures are presented in the table.
    . Example In a 2 liter Beherovsky vessel, a solution of ZbO g of M-chloroacetyl-M- (t-methyl-2-methoxyethyl) -2,6-dimethylaniline is dispersed and
    70.8 g of diphenylmethane-, -diisocyanate in 353 g of SHELLSOL AB when using a high-speed mixer in solution. 15 g of dispersant A and 15 g of MowIOL 18 - 88 (in the form of a 10% aqueous solution) in ZbO g of water at 27 - 33 ° C. After about 1 minute, 30.8 g of hexamethylenediamine (in the form of an aqueous solution ), and the temperature rises to about 0 ° C. After adding hexametchlenediamine, stirring is continued.
    leave slowly for another hour, while the temperature of the reaction mixture drops to room temperature. The resulting dispersion is stabilized.
    21
    by adding 15 g of PIURONIC®F-108. A microcapsule dispersion is obtained with a capsule diameter of 2-20 mm and 50 сP. The content of the active substance in the dispersion is 25%,%. Polymer content per active substance 28.3.
    Example 100 A solution of 37.3 g of diphenylmethane-4,4-diisocyanate in 480 g of metolachlor is dispersed using a speed mixer in a solution of 7j3 g of dispersant A and 7, -5 g of MOwIOL®40- 88 (as a 10% aqueous solution) in 232.5 g of water


    at the same time, the temperature rises by 3-5 ° C. Immediately after this, 16.4 g of hexamethylenediamine (in the form of a 40% aqueous aqueous solution) are added with further stirring, while the temperature rises another 8-12 ° C. After the addition of hexamethylenediamine, continue A dispersion cooled to room temperature for 1 hour is stabilized with 8.7 g of PIURONIC F108. A thin liquid storage-stable capsule dispersion is obtained with a capsule size of 2-30 / s, viscosity 75 with an active substance content of 5 wt D and a polymer content calculated on an active substance of 11.2% by weight,
    Example 11 “In a 2-liter Beheher vessel, solution is dispersed.
    87g of diphenylmethane-4,4 -diisocyanate in 1080 g of diazinon when using a high-speed mixer in a solution of 9.0 g of a dispersant. A and 9.0 g MOWIOL 18 88 (in the form of a 10% aqueous solution in 392 g of water. Approximately
     38 g of hexa-methylene dimine (in the form of a 40% aqueous solution) are added in 1 minute, while the temperature rises by 5-8 ° C. Stir for another 1 h and the resulting capsule is stabilized by adding a solution of 29 g of GENAMIN T 100 to 80 g of water, A stable capsule dispersion is obtained-- JQ in which the average size of the capsules
    with a viscosity of 700–1200 cP and an average particle size of 2–5 L | m. The content of the active substance is 58.3 weightD and the polymer content is 11.6 weightD calculated on the active substance.
    The ratio of the MOWIOL disperser is 18 - 88 with a practically remaining stable quality of the disperser formed.
    5 - 20 / them, the content of the active substance in the dispersion is 15.9 weight ,. and the polymer content, based on an active substance of 51.3 wtD,
    Example 14. In a Beherovu vessel at room temperature, a solution of 8.5 g of diphenylmethane-4, -4-diisocyanate per 100 g of profofos and at a rate of
    220
    0
    five
    Persia microcapsules can vary in the range from 1: 3.
    Example: 8.1 g of diphenylmethane-4,4-diisocyanate in 100 g of furatiocarb is dispersed using a high-speed stirrer in a solution of 1.5 g of AI dispersant 1.5 g of MOWIOL 18 - 88 as 10 aqueous solution) in 55 g of water at 50 ° C. With further stirring, 3.5 g of hexamethylenediamine (as a 40% aqueous solution) is added to the dispersion, while the temperature of the mixture is
    5 rises by about 3 ° C. After the addition of hexamethylenediamine, the mixture is kept stirring for another 1 hour, while the resulting microcapsule suspension is cooled to room temperature. After adding tO g of GENAMIN T 100, a thin-liquid, storage-safe microcapsule suspension is obtained. The average size of the capsules is 2-50 / CM, the viscosity is 250 cP, the content of the active substance is 50.6% by weight, the content of the polymer is 11.6% per active substance.
    Example 13. A solution of 6.3 g of diphenylmethane-4, 4-diisocyanate and 2k g of AND- (2,3-dihydro-3-methyl-1,3, triazole-2-ylidene) -3.4 xylidine in 47.2 g of SHELLSOL AB using a high-speed mixer in a solution of 0.83 g of dispersant A and 0.83 g of HOWIOL 40 - 88 (as a 10% aqueous solution) in 58 g of water at room temperature. Immediately after this, 6.8 g of hexamethylenediamine (in the form of a 40% aqueous solution) is added, while the temperature rises by about. After the addition of hexamethylenediamine, stirring is continued for 1 hour, while the resulting capsule dispersion is cooled to room temperature. A good flowable dispersion of microcapsules with a viscosity of 150-300 cP is obtained,
    0
    five
    five
    in which the average size of the capsules
    5 - 20 / them, the content of the active substance in the dispersion is 15.9 weight ,. and the content of the polymer in the calculation of the active substance 51.3 weightD,
    Example 14. A solution of 8.5 g of diphenylmethane-4, -4-diisocyanate is dispersed in 100 g of prophylaxis in a Beherovo vessel at room temperature and when using a high-speed
    }
    one
    mixers in solution} g of dispersant A and 1 g of MOWIOL 18 - 88 in 70 g of water. Immediately thereafter, with further stirring, 3.7 g of hemeamethylenediamine (in the form of a 40% aqueous solution) are added and stirring is continued for 1 hour. A stable dispersion of microcapsules with a good suspectability and viscosity of about 100 cP is obtained. The average value of microcapsules is 5 15 / Um, the content of the active substance is 50.5%, the polymer content per active substance is 12.2 wt.% „
    Example 15 - A solution of 19.7 g of diphenylmethane h, h-diisocyanate in 80 g of isazophos is dispersed using a high-speed mixer at room temperature in a solution of 8 g of dispersant A and 0.8 g of MOWIOL 18 - 88 hh, 2 g of water then Then dispersions 8.6 g of hexamethylenediamine (in the form of an HO% aqueous solution) are added, and the temperature rises by about 10 ° C. The mixture is stirred for another 30 minutes at room temperature. A stable dispersion of microcapsules is obtained with a content of 35% w / w of polyurea, based on the amount of active substance used. The content of the active substance in the dispersion is h5 wD, | viscosity 280 cp, capsule size 5
    L p and me R 16. A mixture of 8.1 g of diphenylmethane-4,4-diisocyanate, 80 g of propiconazole and 15, g of xylene is dispersed with vigorous stirring in a solution of 1.6 g of dispersant A, 0.8 g of MOWIOL 18 - 88 and 0.8 g of PLURONIC F 108 No. 58.6 g of water at room temperature. Then g of hexamethylenediamine (in the form of a 40% aqueous solution) is added and stirring is continued for another 1 h. A liquid stable aqueous dispersion of microcapsules is obtained. average capsule diameter 2 - 3 / UM. The content of the active substance dispersion 46 weight. The viscosity is 100 cps, the polymer content is 14.3 wt.% And based on the active substance.
    PRI me R 17. A solution of 42.5 g (xylene and 44.5 g of diphenylmethane-h, 4-diisocyanate in 4O g of propiconazole is dispersed under intensive pe-1, mixing at room temperature in a solution of 20 g of dispersant A and 8 g
    1741602
    24
    I LUKuNiC V 100, 6 g of water. After that, 18.4 g of hexamethylenediamine (in the form of 40% aqueous
    solution), while the temperature rises by about 10 ° C. The mixture is continued to stir until it is cooled to room temperature. A stable liquid microcapsule dispersion is obtained with an average microcapsule of 3-5 LI and an active substance content of 54% by weight. A viscosity of 170 cps and a polymer content of 13.1% by weight, calculated on the active
    5 substance.
    Example 18. A solution of 75, g of diphenylmethane-, k -diisocyanate in 463.7 g of metolachlor with vigorous stirring at room temperature is dispersed in a solution of 15 g of sodium salt of polystyrenesulfonic acid and 10 g of rLURONIC F 108 in 328 g of water o Then add 32.8 g of hexamethylenediamine as a 40% aqueous solution), and the temperature rises by about 15 ° C. The mixture is continued to be stirred until it cools to room temperature. A micro0 capsule dispersion is obtained with an average capsule size.
    I- 2fUM, viscosity 30 сП, content of active substance
    and a polymer content of 23.5% by weight of the active substance.
    PRI me R 1u. A solution of 8.1 g of diphenylmethane-4, h-diisocyanate in 1UO g of metolachlor under vigorous stirring at room temperature is dispersed in a solution of 1.5 g of sodium salt of polystyrene sulfonic acid and 1.5 g of HOWIOL chO — 88 in 76.6 g of water. Immediately after this, 3.5 g of hexamethylenediamine (in the form of a hO% aqueous solution) are added, while
    The temperature rises by about 10 ° C. The mixture is kept stirring for 1 hour. A stable dispersion of microcapsules is obtained with an average capsule size of 1 - 2 / cm, viscosity
    0 330 сП, content of active substance 51,5 weight and polymer content
    IIB c b weight of the active substance, EXAMPLE 20 Solution b, 5 g diphenylmethane-h, 4-diisocyanate in 80 g metolachlor with vigorous stirring at room temperature dispersed in solution i, 6 g disperser Ai 1, b g GENAPOL®C - 200 in Sg of water. After that, add 2.7
    five
    0
    five
    2517 P602
    hexamethylenediamine {in the form of CHO-nogo
    26
    aqueous solution), while the temperature rises to 37 ° C. The mixture is continued to stir until it is cooled to room temperature. A microcapsule dispersion is obtained with a viscosity of 150 cp, an average capsule size of 5-6 Mm, an active substance content of 51 wt.% And a polymer content of 11.5 wt.% Based on the weight of the active substance. The dispersion is separated; spontaneously upon dilution with water .
    EXAMPLE 21 The experiment was carried out as in Example 13, but using instead of GENAPOI C - 200 ANTARU CO 710o. When adding hexamethylenediamine, the temperature rises by 6 ° C. A dispersion of microcapsules with a viscosity of 880 cP and an average capsule size is obtained 5 | CMP which, when diluted with water, spontaneously separates. The content in the dispersion. The active substance is 51 wt.% And the polymer is 11.5 by weight of the active substance.
    II p and mep 22. Conducted experience, as in example 13, but used instead
     Si
    GENAPOIrC-200 ethoxylated dinonylphenol with 150 units of ethylene oxide. After adding hexamethylenediamine, the temperature rises by 5 ° C. A microcapsule dispersion is obtained with a viscosity of 65 cP and an average capsule size of L / m, which spontaneously separates upon dilution with water. The content of the active substance 51. Weight ",% and the polymer content of 11.5 wt.% By weight of the active substance.
    EXAMPLE 23 The experiment was carried out as in the DZ example, but used instead of GENAPOL® C-2UO PLURONI (T-85. A dispersion of microcapsules is obtained with a viscosity of 30 cP and an average value of capsules dilution with water spontaneously separates the content of the active substance M by weight, polymer 11.5% by weight by weight of the active substance. Example 2h.
    ten
    15
    20
    EXAMPLE 25 The experiment was carried out as in Example 13, however, instead of GENAPOIP, c-20 TETRONldtyo was used. When hexamethylenediamine is added, the temperature rises by 5 ° C. A dispersion of microcapsules with a viscosity of 500 cP and an average capsule size of 5 (UM, which spontaneously separates upon dilution with water, is obtained. The active substance content is 51% by weight and the polymer content is 11.5% by weight of the active substance.
    EXAMPLE 26 A solution of 75, g of diphenylmethane-4,1 -diisocyanate in 63.7 g of metolachlor at room temperature with vigorous stirring is dispersed in a solution of 15 g of dispersant A and 10 g of LICE% 108 in ZOCH g of water. Then 32.8 g of hexamethylenediamine (in the form of a 0% aqueous solution) are added, and the temperature rises by about 15 ° C. The mixture continues to stir
    25 to cool to room temperature. A microcapsule dispersion with a viscosity of 60 cP and an average capsule size, with an active substance content of 6.3 wt. and a polymer content of 23.3 e,% of. weight of active substance
    Example 27. A solution of 35.5 g of polymethylene polyphenyl isocyanate MONUUR R Mobay Chemical Company in g of metolachlor is dispersed in a 1.5-liter Beherovsky vessel at room temperature with a high-speed stirrer in a solution of 20 g of TAhOBP SN, 10 g of PLURONIC% 108 and 50 g of ethylene glycol in, 5 g of water. The mixture is stirred for 2 minutes while the temperature rises to 3-15 ° C. After this, 15.5 hexamethylenediamine (in the form of a 0% aqueous solution) is added to the dispersion, while the temperature rises another 7 to 12 ° C. The resulting microcapsule dispersion is kept stirring for another 1 hour and then adding hydrochloric acid
    40
    in example 13, however, a pH value of 7 is used instead. After adding
    VM A 11 VI ttlf 11Т Т Til / ЬЫ r 4Kj4 /% М. JW. „, G„
    GENAPOL® C-200 PLURONIC5 - 42. The resulting dispersion is initially fluid, but within 2 hours it thickens to a viscosity of 1600 centipoise. Dispersion can be easily shaken. The average size of the capsules is 3.5 - 4 / them. The content of the active substance is 51% by weight and the polymer content is 11.5% by weight of the active substance.
    55
    19.5 g of 3, 55% xantam dispersion (polysaccharide) is obtained a storage-stable dispersion of microcapsules with a viscosity of 200 - 500 cP. The diameter of the capsules is, depending on the stirring speed, A -. The content of the active substance is 7.3% by weight and the polymer content is 11% by weight of the weight of the active substance.
    26
    0
    five
    0
    EXAMPLE 25 The experiment was carried out as in Example 13, however, instead of GENAPOIP, c-20 TETRONldtyo was used. When hexamethylenediamine is added, the temperature rises by 5 ° C. A dispersion of microcapsules with a viscosity of 500 cP and an average capsule size of 5 (UM, which spontaneously separates upon dilution with water, is obtained. The active substance content is 51% by weight and the polymer content is 11.5% by weight of the active substance.
    EXAMPLE 26 A solution of 75, g of diphenylmethane-4,1 -diisocyanate in 63.7 g of metolachlor at room temperature with vigorous stirring is dispersed in a solution of 15 g of dispersant A and 10 g of LICE% 108 in ZOCH g of water. Then 32.8 g of hexamethylenediamine (in the form of a 0% aqueous solution) are added, and the temperature rises by about 15 ° C. The mixture continues to stir
    5 to cool to room temperature. A microcapsule dispersion with a viscosity of 60 cP and an average capsule size, with an active substance content of 6.3 wt. and the content of the polymer 23.3 ees,% from. weight of active substance
    Example 27. A solution of 35.5 g of polymethylene polyphenyl isocyanate MONUUR R Mobay Chemical Company in g of metolachlor is dispersed in a 1.5-liter Beherovsky vessel at room temperature with a high-speed stirrer in a solution of 20 g of TAhOBP SN, 10 g of PLURONIC% 108 and 50 g of ethylene glycol in, 5 g of water. The mixture is stirred for 2 minutes while the temperature rises to 3-15 ° C. After that, 15.5 hexamethylenediamine (in the form of a 0% aqueous solution) is added to the dispersion, while the temperature rises another 7 to 12 ° C. The resulting microcapsule dispersion is kept stirring for another 1 hour and then adding hydrochloric acid 5
    0
    . „, G„
    19.5 g of 3, 55% xantam dispersion (polysaccharide) is obtained a storage-stable dispersion of microcapsules with a viscosity of 200 - 500 cP. The diameter of the capsules is, depending on the stirring speed, A -. The content of the active substance is 7.3% by weight and the polymer content is 11% by weight of the weight of the active substance.
    EXAMPLE 28 A solution of 39 g of polymethylene polyphenyl isocyanate (RARPF135) in 511 g of isazophosphate is dispersed in a 1.5-liter Beherovsky vessel at 5 room temperature using a high-speed mixer in a solution of 22 g of XAriOBP SN 11 g of PLURONIL®F 108 and 55 g of ethylene glycol in 372, g of water. The dispersion is stirred for 2 minutes, at the same time the temperature rises by 10-15 ° C. Then S, S g of hexamethylenediamine (in the form of a 40% water thief) is added, while the temperature rises further by 7 - 12 ° C. Continue stirring for another 1 hour and then neutralize with hydrochloric acid to pH 7. After adding 1.5 g of 3 L% Xantam dispersion (polysaccharide) in water, a storage-stable dispersion of microcapsules with a viscosity of 200 to 500 ell is obtained. The average diameter of the capsules consists of s.atatat e depending on the mixing speed 2-8 / UM. The content of the current temperature. A stable, flowable dispersion of microcapsules (viscosity 150 cP) is obtained with an average particle size of 2-3 UM, an active substance content of 51.5% by weight and a substance substance of 13.6 ps per shell of active substance.
    PRI me R 31 A solution of 8 g of diphenylmethane-1, α-diisocyanate in 1080 g of diazinon with vigorous stirring at room temperature is dispersed in the solution “I, 0 g of dispersant A, 3, ShushLb - 88 (in the form of 10% - water solution) and 6.0 g PLURONLA 108 in No. 6 g of water. After that, 37.9 g of hexamethylenediamine (in the form of a 0% aqueous solution) are added, and the temperature rises by 3–5 ° C. The resulting liquid dispersion of microcapsules with an average capsule size of 1.5–2, L1m has viscosity 250 - 600 cP. She is
    The weight of the substance is 7.5% by weight, containing 25% of the active substance, 10% by weight of the polymer and 10% by weight of the active substance by the south of the substance.
    . Example 29 "A solution of 20, k g of dichloromethane and 7.5 g of diphenylmethane-, dy eocyanate in 80 g of M-chloroacetyl-N (1-methyl-2-methoxyethyl) -2,6-dimethylamine with vigorous stirring
    at room temperature dispersed in solution 1.8 g of dispersant
    AI 1.8 g PLURONIL% t08 in 66.3 g. 35
    and the weight "% of the substance of the capsule shell to the weight of the active substance,
    权利要求:
    Claims (1)
    [1]
    30 claims
    The method of obtaining an aqueous dispersion of microcapsules with a capsule wall of polyurea and a core of a water-immiscible pesticide by dispersing a solution of a polyisocyanate in a pesticide in water, introducing an aqueous solution of a polyamine and mixing until a microcapsule aqueous dispersion is obtained,
    dy After that, 3.1 g of hexamethylenediamine (in the form of an Ao% solution) are added, and the temperature rises by about 10 ° C. A stable, flowable dispersion of microcapsules is obtained with an average capsule size of 2 - C / UM and a content of 43 weight% “%” Viscosity 40 cP and polymer content 13.3 wD by weight of active substance
    EXAMPLE 30 A solution of 18 g of diphenylmethane-, -diisocyanate in 96 g of chlorofenvinphos with vigorous stirring, dispersed at room temperature in a solution of 1.6 g of dispersant Au and 1.6 g of PLURONIC® F 108 in 50.5 g water. After that, 7 g of hexamethylenediamine (in the form of a 0% aqueous solution) are added, and the temperature rises by 20-30 ° C. The mixture is kept stirring to cool to room temperature. A stable, flowable dispersion of microcapsules (viscosity 150 cP) is obtained with an average particle size of 2-3 UM, an active substance content of 51.5% by weight and a substance substance of 13.6 ps per shell of active substance.
    PRI me R 31 A solution of 8 g of diphenylmethane-1, α-diisocyanate in 1080 g of diazinon with vigorous stirring at room temperature is dispersed in the solution “I, 0 g of dispersant A, 3, ShushLb - 88 (in the form of 10% - water solution) and 6.0 g PLURONLA 108 in No. 6 g of water. After that, 37.9 g of hexamethylenediamine (in the form of a 0% aqueous solution) are added, and the temperature rises by 3–5 ° C. The resulting liquid dispersion of microcapsules with an average capsule size of 1.5–2, L1m has viscosity 250 - 600 cps. She is
    CONTAINS b, b wt.% active substance
    and the weight "% of the substance of the capsule shell to the weight of the active substance,
    Invention Formula
    five
    0
    five
    0
    five
    The method of obtaining an aqueous dispersion of microcapsules with a capsule wall of polyurea and a core of a water-immiscible pesticide by dispersing in water a solution of a polyisocyanate in a pesticide, introducing an aqueous solution of a polyamine and mixing until a microcapsule aqueous dispersion is obtained,
    that, in order to increase the concentration of microcapsules in the aqueous dispersion while simultaneously increasing the pesticide content in the capsule, dispersion and mixing are carried out in the presence of an anionic dispersant selected from the group consisting of naphthalene sulfonic acid condensation salt with formaldehyde, naphthalene sulfonic acid condensation product with phenolsulfate acid and formaldehyde, a salt of polystyrene sulfonic acid, and a non-ionic protective colloid mol. 10,000–200,000, namely polyvinyl alcohol of viscosity 18–0 D, and / or with a non-ionic surfactant selected from the group including
    the product of the interaction of ethylene oxide and propylene oxide with fatty alcohols, alkyl phenol, fatty acids, amides of fatty acids and fatty amines, a block copolymer of ethylene oxide and pylenoxide with mol, m „1600 and H, N, N, N, N - tetraethylenediamine, nonylphenol polyglycol ether , ethoxylated fatty alcohol, with mass
    en 58
    58
    58
    58
    15
    15
    Lignin su 'Fonat
    Ligninsulfonate /
    Pluronic v
    108
    Disper- Yu
    gator
    BUT.
    Dispersant
    A / Plurontc
    F 103 10
    2.1
    2.0
    4.7
    2
    Dis- 20 Pergator A
    5.0
    Dis- 20 pergeator A / / Plu- ronic F 108
    2.0
    the ratio of anionic dispersant and non-ionic protective colloid and / or non-ionic surfactant is from 1: 1 to 1:10, while polyisocyanate and polyamine take in an amount of 10 - 35% by weight of the pesticide, and water in an amount of 30 - 50% from the total amount of dispersion of microcapsules.
    Yu |
    W s- Slightly Upeka stir-stirring shima
    D. low viscosity
    In h, ka Slabopremeshi- Nepiraema remeshimaya
    Constant viscosity
    Low
    2.9
    Weakly Rene- Repeatable
    Mesh-shivaeva-. ma
    ma
    D. low viscosity
    In relation to the active substance
    Table continuation
    类似技术:
    公开号 | 公开日 | 专利标题
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    同族专利:
    公开号 | 公开日
    IL80009D0|1986-12-31|
    DE3685920D1|1992-08-13|
    JPH0764682B2|1995-07-12|
    IL80009A|1989-12-15|
    CA1292678C|1991-12-03|
    EP0214936B1|1992-07-08|
    EP0214936A3|1989-08-02|
    AU6264386A|1987-03-19|
    AT77916T|1992-07-15|
    AU588913B2|1989-09-28|
    US4938797A|1990-07-03|
    ZA866953B|1988-04-27|
    EP0214936A2|1987-03-18|
    JPS6267003A|1987-03-26|
    UA13387A|1997-02-28|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US77608085A| true| 1985-09-13|1985-09-13|LV930552A| LV5193A3|1985-09-13|1993-06-11|Attenuation to obtain microcapsule water dispersion|
    LTRP1282A| LT2611B|1985-09-13|1993-09-29|THE WAY OF RECOVERY OF WATER DISPERSIONS WITH MICROCAPSULES|
    MD94-0059A| MD16C2|1985-09-13|1994-01-17|The method of obtaining hidrodispersion of microcapsules|
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