• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    There is described a process for the in situ preparation of stable dispersions of polyurea and/or polyhydrazodicarboxamides in hydroxyl-containing polyethers. These products are prepared by reacting (1) organic polyisocyanates with (2) primary and/or secondary amino group-containing polyamines and/or hydrazines and/or hydrazides, in a high molecular weight polyether which has at least one hydroxyl group with the components (1), (2) and (3) being passed continuously into a continuous mixer at such a rate that the average residence time (dwell time) in the mixer is less than 10 minutes. The equivalent ratio of components (1) and (2) is between 0.8 and 1.05. The dispersions thus prepared are non-sedimenting and combine a relatively high solids content with a relatively low viscosity. The size of the dispersed particles is usually below 1 mu . Owing to these properties, they are suitable for preparing polyurethane foams.
    公开号:SU741801A3
    申请号:SU752135775
    申请日:1975-06-16
    公开日:1980-06-15
    发明作者:Кениг Клаус；Дитрих Манфред
    申请人:Байер Аг (Фирма)；
    IPC主号:
    专利说明:

    3 .7 polyester dispersions as a starting material for the preparation of polyurethane foams, the particle diameter of the filler should be significantly smaller than the size of the cell wall (20-50 µm). In polyurethane coatings, the particles should also be so small that, with a very thin layer of application, a uniform coating with a smooth surface would be obtained. According to the invention, dispersions with a particle size of less than 1 micron are preferably formed. Such dimensions satisfy technical requirements when applied. The starting materials for carrying out the process of the invention are polyesters having up to 8, preferably 2-6, primary and / or secondary hydroxyl groups, with a molecular weight of 200-16000, preferably 500 to 12000. This type of polyether is prepared in a known manner, by converting the starting compounds with reactive hydrogen atoms with alkylene oxides such as ethylene oxide, propylene, butylene, styrene, tetrahydrofuran or epichlorohydrin, or any mixtures of these alkylene oxides. Many times more preferred are those polyesters that have predominantly primary OH groups. As polyamines, two and / or polybasic, primary and / or secondary, aliphatic, araliphatic, cycloaliphatic and aromatic amines can be used, for example ethylenediamine, 1,2- and 1,3-propylenediamine tetramethylenediamine, hexamethylenediamine, dodecamethylenediamine, trimethyldiamine-1 hexane , F, s-dimethylethylene, 2,2-bisaminopropilmetilamin, higher homologs of ethylenediamine like diethylenetriamine, hrietilentetramin and tetraethylenepentamine, homologues propylenediamine, dipropylenetriamine like, piperazine, N, N -bisaminoetilshsherazin, trio in, 4-Aminobenzylamine, 4-aminofeniletilamin, 1-amino-3, 3,5-trimethyl-5-aminometiltsikloge1 san 4.4 -diaminoditsiklogeksilmetan and -propane, 1,4-diaminoschpslogeksan, feshshendiaminy, naftilendiaminy condensates of anillina and formaldehyde, toluenediamines, bisaminomethylbenzenes and at one or both nitrogen atoms mono-apricified derivatives of the mentioned aromatic amines. Polyamines usually have a molecular weight of 60-10000, preferably 60-1000. Hydrazine and mono or N, N-disubstituted hydrazines could be named as hydrazine, with substituents Ci-Sat being alkyl groups, cyclohexyl groups, or pure pears. Generally, molecular weights of 32-500 are preferably hydrazine itself. As gifazidov Motley would be named hydrazides di- or polybasic carboxylic acids such as carbonic, oxalic, malonic, succinic, adipic, sebacic azelaic, mapeinovoy, fumaric, phthalic, isophthalic, terephthalic, further gidrazinmonokarbonovoy acid esters of di- or polyhydric alcohols and phenols, such as ethanediol, propanediol1, 2, butanediol, 1,2, -1,3 and -1,4, hexanediol, diethylene glycol, triethylene glycol, tetraztilen glycol, dnpropylene glycol, tripropylene glycol and hydroquinone, as well as amides of hydrazine monocarboxylic acid (semicarbazides), for example, with the above di- and polyamines. Hydrazides generally have a molecular weight of 90-10000, preferably 90-3000, and particularly preferably 90-1000. The mentioned amines and hydrazines are used in this case in the form of aqueous solutions. Aliphatic, aliphatic, araliphatic, aromatic, and heterocyclic polyisocyanates, such as ethylene diisodianate, 1,4-tetramethylene diisocyanate, 1,6-hexamethylenediisocyanate, 1,12-dodedecanediisocyanate, cyclobutane-i-mer, i-cyclotetra diisocyanate, 1,12-dodedecanediisocyanate, 1-tetramethylene diisocyanate, 1, 2-hexamethylenediisocyanate, 1,12-dodedecanediisocyanate, cyclobutane-i-tetramethylenediisocyanate, 1,12-dodedecanediisocyanate, cyclobutane-3, i-tetramethylenediisocyanate, 1, 2-dodecanediisocyanate, 1-tetramethylene diisocyanate; 13- and 1,4-diisocyanate, as well as any mixtures of these isomers, 1-isocyanato-3, 3,5-trnmetsh1-5-anhydroxymethylcyclohexane, 2,4- and 2,6-hexahydrotoluene diisocyanate, as well as any mixtures of these isomers , hexahydro1, 3- and / or -1,4 - fenne diisocyanate, pergisite o-2, 4- and / or -4,4-diphenylmethane diisocyanate, 1,3- and 1,4-phenylene diisocyanate, 2,4- and 2,6-toluene diisocyanate, as well as any mixtures of these isomers, diphenylmethane-2, 4- and / or -4,4-diisocyanate, naphthalene-1,5-diisocyanate, trifenchemmethan-4,44 -triisocyanate, polyphenyl-polymethylene polyiso-. cyanate, which is obtained by analyzing the formal system having acylated urea groups, polyisocyanates having biuret groups, polyisocyanates obtained by the reaction of telomeres ation, polyisocyanates having ester groups as the conversion products of these isocyanates with acetals containing polymeric fatty acid residues. It is also possible to use the isocyanates resulting from the technical preparation, which have isocyanate groups of distillation residues, in this case dissolved in one or several of the polyisocyanates mentioned. Further, it is possible to use any mixtures of the mentioned polyisocyanates.
    Particularly preferred are, as a rule the technically readily accessible poliizooaianaty, for example 2,4- and 2,6-tolu1ten, 1iizotsianat, as well as any mixtures of these isomers STDI) polifenil-polimetile shol fflzotsianaty obtained by aniline - formaldehyde condensation and subsequent fosgenirovaki (crude MDI) and polyisocyanates having carbodiimide, urethane, allophanate, homocyanurate, urinary, or biuret groups (modified polyisocyanates)
    The method of the invention also allows the partial or exclusive use of the relevant amine, hydrazine or hydrazide soocyanates, the functionality of which is more than 2. The transformation of such highly functional compounds in polyesters containing hydroxyl groups according to the invention does not result in solid or not very high reaction products, a leads to highly dispersive low viscosity dispersions.
    The polyadducts obtained according to the invention, dispersed in hydroxyl-containing polyesters, can also be modified by the frequent conjugation of monofunctional isocyanates, amines, hydrazine derivatives or ammonia.
    For example, it is possible to determine the average molecular weight of polyadducts by introducing such functional compounds. When alkanolamines are used with primary or secondary amino groups, it is possible to synthesize polyureas and polyurea poly (polyurea) polyhydrazodicarbonamides, which have free hydroxyl groups. It is also possible to introduce other groups, such as ether, extended aliphatic residues, tertiary amino groups, active double bonds, etc., if suitably substituted mono- or diamines or isocyanates are used together.
    Monofunctional compounds can be used according to the invention in an amount of up to 40 mst.%, Preferably up to 25 mol.% (Calculated on total isocyanate, respectively amine, hydrazine or hydrazide).
    Suitable monofunctional isocyanates include, for example, alkyl isocyanates such as methyl, ethyl, isopropyl, izobz gal-, hexyl, lauryl and stearilizotsianat, hlorgeksilizotsianat, cyclohexyl isocyanate, phenyl isocyanate, tolyl isocyanate, 4-chlorophenyl isocyanate and isocyanate diizoproshshfenil.
    As monoamines, for example, alkyl and dialkimines with alkyl groups, cycloaliphatic amines can be mentioned.
    Schlclohexclamine and homologues, aniline and N-alkylanilines, as well as replacing anilograms, alkanolamines like ethylamine, diethanolamine, propanolamine, dipropanolamine, b-tanolamine, and dibutanolone psh, as well as diethanolamine, as well as diethanolamine, as well as diethanolamine, as well as dibutanolamine, and propanolamine; an amino group, such as N, N-AHMeTiui3TtffleHAnaNmH and K-methylcryptine. As monofunction x hydrazshroizydnyh and. Dradovds are taken into account, for example, MD-dialkylhydrazish 1, gvdrazida monocarboxylic acids, esters of gadrazinmonocarboxylic acids and monofunctional alcohols or phenols, as well as semicarbazvdy, as nafimer, methyl,, past, butylparts, as well as semicarbazvdy, as nafimer, methyl,, stitched, butylphenols, as well as semikarbazvdy, as nafimer,. -, phenyl- and tsnkoheksil / semikarbazid.
    According to the invention, in d; isomer serving as an inapplicable, dispersing modifier with 1 paliether, I have a trimer, attachment plans for excess di- and / or polyisocyanates, and: azanes higher to mono- and / or bifushtsionalyshyshm gvdroksilpoljfiram by heart = i) i 3004000, which were released from non-translucent free HsoniiaiaiaTa using thin-film 1H chromatography. But also in this case, such isocyanate prepolymers can be converted with an excess of free isocyanate to allophanate isocyanates. It becomes possible to convert the adducts that contain the final isociapate groups with excess diacines or hydrazine into polyesters that have amino or semicarbazide endgroups.
    According to the invention, polyesters having a good a shredder can also be used as dispersing agents.
    Finally, hydroxyl polyethers can also be converted with phosgene to chloroformate esters and then hydrated with excess diamine or hydrazine. As already mentioned, polyesters which are liip are preferred. at the end of the chain are NCO- or MH2-grouping.
    The molecular weight of the polyadducts dispersed in the polyester is determined by the quantitative ratio between the polyamine, hydrazine (respectively, hydrazide) on the one hand, and the half-social with the other (in this case with the monofunctional compounds used. It is especially preferable to introduce hydroxyl groups into the polyester) , approximately equivalent amounts of isociaates and H-functional junctions. It is also possible to work with a small excess of isocyanate (about 5%), but then products with a higher viscosity are obtained, since an excess of polyisocyanate reacts with
    polyester. When working with an amine, hydrazine or hydrazide, they can be used in greater excess, and polyadducts with reactive end groups and limited molecular weight are obtained. In general, the NCO- / NH ratio is maintained between 0.80-1.05, preferably 0.90-1.02.
    The concentration of polyads on polyester carrying hydroxyl groups can vary widely, but typically between 1-35% by weight, preferably 3-30% by weight. The amount of dispersed polyadjupeate required for foams with optimal properties is 10 wt.%
    According to the invention, it is possible to directly pour off 10% of the dispersions. However, for economic reasons, it is preferable to obtain the dispersions as high as possible with a high polyadduct content (20-30% by weight) and then dilute it with any polyester to the desired concentration.
    The reaction compounds are fed to the flow mixer at room temperature. When the agitator is turned on and as a result of heat generation during the reaction of psiaddition, which is formed depending on the amount of the filler, the reaction temperature increases by 50-150 ° C. However, it is advisable to maintain the temperature (in this case by cooling the baffles below 110 ° C, so that when the water evaporates no bubbles would form. If pyrazine is used, decompose} hydrazine should not be exceeded.
    A distinctive feature of the invention is that the reaction of polyacryeds of polyisocyanates and polyamines, gvdrazines or hydrazides is carried out in continuous flow mixers with energetic mixing with an average residence time of less than 10, preferably less than 3 minutes.
    The time of homogenization or dispersion should be a maximum of 10% of the average residence time in equipment G; to achieve intensive mixing of the components. According to the invention it is possible, but not necessary, to include in series two or more flow mixers.
    For flow mixers, static mixers with fixed structures are adapted to dynamic mixers with moving structures according to rotor / stator principle. They can in this case be heated or cooled.
    When using anhydrous amines, hydrazines and hydrazides, no further processing is required at the end of the reaction for the addition of gas. For the production of aqueous amines (for example, aqueous solutions of ethylenediamine
    or hydrazine hydrate) it is advisable to remove the water from the dispersion in a vacuum.
    The invention should work in such a way that all three components (polyester, H-component and polyisocyanate) from separate containers are supplied through metering pumps to a flow mixer, where most of the polypropagation reaction is intensively mixed and simultaneously flows. But it is also possible to combine the amine compound (component 2) with the polystyrene (component 3) before entering the npoTOtfflOMy mixer. The reacted product enters the receiver, where it is additionally mixed for complete reaction shutdown (in this case, when heated to 50-150 ° C). In the case of the use of aqueous amines, it is desirable to remove the whole product from water in a vacuum.
    Dispersions, crawled by the described method, during or after the reaction can be mixed with additives such as activators, stabilizers, water, blowing agents, fire-fighting agents, dye pastes, etc.
    Dispersions produced according to the invention can be processed, for example, into soft, hard and rigid polyurethane foam 1 & 1 with such improved properties as tensile strength and rigidity. Moreover, polyhydrazodicarbonamide dispersion foams are characterized by a high degree of
    whiteness Dispersions are also suitable for producing, for example, elastomers, films and polyurethane-based coatings.
    The method according to the invention is explained in detail with the following graphs (if not marked, parts should be understood as weight parts, and percentage data as weight%).
    The abbreviations used in the examples for polyesters have the following meanings: Polyether A. Polyether made of propylene oxide and ethylene oxide with an OH number of 34 and a content of primary OH groups of 80% obtained by reacting trimethylol with propane.
    Polyester B. As polyester A, with a OH number of 35 and a content of primary OH groups, 70%.
    Polyether B. Polyether obtained from the reaction on glycerol with propylene oxide and ethylene oxide with an OH number of 56 and a primary content: OH groups of 50%.
    Polyester G. Like polyester A, with a OH number of 28 and a primary OH content of 80%.
    Polyether D. Obtained: by reaction to trimethylolpropane, polyester from alkali oxide and ethylene oxide with OH number 49 and mainly secondary OH groups.
    权利要求:
    Claims (2)
    [1]
    Polyester E. Linear polypropylene glycol (OH number 56) with secondary OH groups. Polyether J. Linear polypryupylene glycol modified with P) HY at the end with ethylene oxide (OH number 28, about 80% of the primary OH groups). Polyester 3. Obtained by reacting trimethylol polyethylene oxide (he is 550). Example 1. Two successively included mixers with shigami (chambers capacity 1.5 l, respectively 0.5 l, speed 1500 rpm) continuously, at room temperature 800 g of polyester 169 g of mixture are introduced every minute: 80% 2 , 4- and 20% of 2,6-toluene diiso cyanate to 49 g of hydrayingoid. Three components separately from each other are fed directly into the mixing zone of the 1st spiked agitator. In this case, the polyester from the collector is transported through a gear pump, while both liquid components from separate collectors are fed through piston metering pumps. In the spiked mixers, an exothermic polyaddition reaction occurs. With the aid of cooling the stirrers, the reaction temperature is set at 100-105 ° C. After about 2 minutes of being in the apparatus, from the second mixer, the white dispersion is almost completely reacted. The dispersion is transferred to a receiving vessel, where it is kept under stirring at 8 ° -100 ° C. Then, after additional mixing, it is distilled off under vacuum with water evolved by hydrazine hydrate. A stable, white, 20% fine 1% dispersion is obtained with an OH number of 22.5, a viscosity of 3700 cps / 25 ° C and a pH of 8.3. After dilution with polyester G to a polyhydrazodicarbonamide content of 10% by weight, the viscosity of the dispersion is 1900 cP / 25 ° C (OH number 25.2). Comparative Example 1a In 45 kg of polyester D, after adding 1.225 kg of hydrazine hydrate with an intensive stirring in the autoclave at room temperature, a mixture of 80% of 2,4- and 20% of 2,6-toluene diisocyanate is added in half an hour. During the precipitation of polyhydrazodicarbonamide, the temperature was poured to 55 ° C. After stirring for one hour, the water was removed under vacuum at 1 ° C. A white, 10% dispersion is obtained with a OH number of 25D, a viscosity of 19,000 cP / 25 ° C and a pH of 83 Example 2. The method of operation is similar to Example 1. 800 g of polyester A, 169 are metered into the first spiked mixer for 1 minute. g of a mixture of 80% 2,4- and 20% 2,6-toluene diisocyanate and 49 g of hydrazine hydrate. After distillation of the water, a stable, white, fine, 20% dispersion is obtained with a OH number of 27, a viscosity of 3300 cP / 25 ° C and a pH of 8.2. After dilution with polyester A to 10% by weight of filler, the viscosity is 1600 cP / 25 ° C (OH number is 30.5). Comparative example 2a (known to method 1 JO The experiment was carried out according to example la. 45 kg of polyelectric A and 1.225 kg of hydroxyzinhydrate were loaded and 4.225 kg of a mixture of 80% 2.4 and 20% of 2,6-toluene diisocyanate were added within 30 minutes. After one hour of stirring and evaporation of water, a 10% dispersion is obtained with a OH number of 30.5, a viscosity of 17500 cP / 25 ° C and a pH of 8.2 Example 3. The method of operation is the same as example 1, but input is every minute into the spiked mixer. t 1600 g of polyester B, 338 g., a mixture of 80% 2,4- and 20% 2,6-toluylene -1O1 isocyanate and 98 g of hydrazine hydrate, stay in a mixer for 1 min. After the water has been distilled off the floor a stable, white, finely dispersed, 20% dispersion with an OH number of 28, a viscosity of 2900 cP / 25 ° C and a pH of 8.1 is taken in. After diluting the polyether B to 10% filler viscosity of 1500 cP / 25 ° C (OH -Number 31.5). Example 4. The experiment was carried out as in Example 1, but every minute 800 g of polyester B, 169 g of a mixture of 80% 2.4 and 20% of 2,6-toluene diisocyanate and 49 were introduced into both spiked mixers. g hydrazine hydrate: The temperature of the dispersion leaving the mixer is maintained at 80 ° C by cooling the agitators. After treatment, a stable, white, fine, 20% dispersion is obtained, with a ratio of 45, a viscosity of 1400 cH / 2S ° C to a pH of 7.8. Example 5. The experiment was carried out as in Example 1, but every minute 800 g of polyester A, 148.8 g of a mixture of 2,4- and 2,6-toluene diisocyanate and 67.4 g of a 76% ethylenediamine solution were introduced into both spiked mixers. . After distillation of the water, a stable, white, fine, 20% dispersion is obtained with a OH number of 27, a viscosity of 4600 cU / 25 ° C and a pH of 10.1. After diluting with polyester A to 10% solids, the viscosity is 1730 cP / 25 ° C. Example 6 A dispersion with a different polyhydrazodicarbonamide content was prepared in a conventional foaming unit at maximum polyester loading. In this case, three piston components are introduced into the mixing chamber through the injection nozzles into the mixing chamber of the agitator (chamber volume 159 ml, rotational speed of the agitator with spikes 3500 rpm). After the reaction mixture is in the mixing chamber 2, the dispersing dispersion is additionally stirred in a collector for half an hour of 80 ° C, then it is freed from water in a vacuum. a) Chemically, 5700 g of polyester A, 253.5 g of a mixture of 80% 2.4 and 20% of 2.6-toluene diisocyanate and 73.5 g of hydrazine} hydrate are fed into the mixing chamber using three piston pumps. After additional mixing and boiling water, the finely distributed 5% dispersion is obtained with a OH number of 32, a viscosity of 16 (X) cP / 25 ° C and a pH of 7.7. c) Every year, 5,400 g of polyester A, 507 g of a mixture of toluylanednococyanate and 147 g of hydraznhydrate are fed into the mixing chamber by pumps. After processing, as indicated in a), the finely distributed 10% -new dispersion with an OH number of 30.5, a viscosity of 1900 cP / 25 ° C and a pH of 8.0. c) Every minute, 5,100 g of polyester A, 760, 5 g of a mixture of toluylene diisocyanate and 220.5 g of hydrazneat extract are fed into the mixing chamber. After processing, as indicated in a), a 15% finely distributed dispersion with a OH number of 29, a viscosity of 2450 cP / 25 ° C and a pH of 8D is obtained. e) Every minute, 4800 g of polyester A, 1014 g of a mixture of toluylene diisides and 294 g of gndraeingndrate are fed to the mixing chamber every minute. After processing, as indicated in a), a finely distributed 20% dispersion with an OH number of 27, viscosity 3600 and a pH of 8.1. Example 7. From a piston pump with four necks synchronously through two pump necks every minute for emulsification 400 g of polyester B and 49 g of hydrazine hydrate are fed into the mixer (diameter 6.3 mm, length 290 mm, number of elements 24) at room temperature Two other necks are through a second, equal to the type of mixer, 400 g of polyester B and 169 g of a mixture of 80% 2.4% and 20% by weight of 2, b-tolus1 diisocyanate. Then the mixtures coming out of both of their mixers are fed to the third mixer for good mixing (diameter 6.3 mm, length 152 mm, number of elements 12). Part of the polyaddition reaction is already underway in this mixer. Due to this, the mixture is heated to 60-80 ° C. From the mixer, the dispersion enters the collecting tank, where it is additionally mixed for half an hour, for the end of the reaction under SO-IOO C. Then the dispersion in the vacuum is freed from water. A stable, white, finely-defined, 20% dispersion with OH number 22 is obtained, 5, viscosity 2470 cG 25C and pH 8.1. After diluting with polyester B to 10% by weight, the filament viscosity is 1250 cP / 25 ° C. Example 8. A mixture of 4000 g of polyester 3 m and 245 g of hydrazine hydrate, which are mixed in a pre-mix meigall, is continuously introduced at room temperature into a high-speed center running homogenizer (volume 0.15 l, rpm 3800 rpm). with spikes (chamber volume 0 l), and 845 g of a mixture of 80% 2.4- and 20% 2.6ol T1 diisocyanate. Both components fall separately from each other directly into the mixing zone of the homogenizer. The mixture, due to the beginning polyaddition and high shear forces, is heated. The dispersion, the exit of psh from the apparatus with a temperature of 90 ° C, is transferred to the collection tank, where it is. incubated for 30 minutes at mixing and at 80-100 ° C. After water ottoik, a white, stable, finely distributed 20% dispersion is obtained with an OH-ratio of 495, a viscosity of 3200 cP / 25 ° C and a pH of 8.1. After diluting with polyester 3 to 10% of a solid, the viscosity is 1450 cP / 25 ° C . Example 9. The experiment was carried out as in Example 1, however, they were operated with an excess of hydrazine, before all of the hydrazine hydrate was further emulsified in the polyester. Every minute an emulsion consisting of 800 g of polyester A and 53.7 hydrazine hydrate and 166 g of a mixture of 80,% 2.4 and 20% of 2.6-toluene diisocyanate is introduced into both spiked mixers. After distillation of water, a stable, white, finely distributed, 20% dispersion is obtained with a viscosity of 2880 cP / 25 ° C and a pH of 8.2. After diluting to 10% of solid c) Yu of polyester A, the viscosity is 1450 cll / 2fC. Example 10. The method of operation is as in Example 7. Every minute in one mixer 11, first mixed with 400 g of polyester B and 57 g of dia-yaleriamine, another with 400 g of polyester B and a mixture of 80% of 2,4- and 20% of 2,6-toluene of bisodianate. . Both streams for recirculation enter the third mixer. At the end of the additional mixing, a stable, white, finely distributed 20% dasperse with an OH number of 45, a viscosity of 3250 cP / 25 ° C and a pH of 10 is obtained. After diluting the polyesters B to 10% of a solid, the viscosity is 1300 cP / 25 ° C. Example 11. The experiment was carried out according to Example 1. Every minute, 800 g of polyester A, 45.3 g of hydrazine hydrate and 171 g of a mixture and 80% of the above mixture of toluipeide iisochate and 20% of polyphenylpolymethylene polyisoodanate, obtained by heat transfer from a mixture of 20% of polyester and 20% polypropylene polymethylene polyisoodanate, obtained by heating a mixture of 200% of polyether A, 45.3 g of hydrazine hydrate are added to the spiked agitators. 50% of the shares dv5 b dep 1X. A stable, finely distributed 20% -Hyio dispersion is obtained with a OH number of 27; viscosity 2900 cP / 25 ° C and pH 7.5. After diluting with polyester A to 10% solids, the viscosity is -1450 cC / 25 ° C. Example 12. The experiment was carried out according to Example 7. Every minute, 400 g of polyester Au and 53.5 g of an amine mixture from gadrasihydrate and ethanolamine were mixed in one mixer (molar ratio 9: 2, calculated molecular weight of dispersed particles 2150), in the other there is mixing 400 g of polyester A and 162 g of the above mixture of toluene diisocyanate. Both streams for the reaction enter the third mixer. After distillation of the water, a stable, white, finely distributed, 20% dispersion is obtained with a OH number of 37.6, a viscosity of 2850 cP / 25 ° C and a pH of 9.5. After dilution with polyester A to 10 wt.% Solids, the viscosity is 1500 cps / 25 C. Every minute a 97.7 aniline-formaldehyde condensate solution consisting of 70 wt.% 4,4-diaminodiphenylmethane and 30 wt.% Higher Condensates, 800 g of polyester, and a mixture of 79.8 g of the above toluene diisocyanate with 22.5 g of allophanate with 11.5% NCO-rpynn from 6 m leu of toluene diisocyanate and the first mole of polypropyleneoxide with one OH-group (molar weight 2600). A stable, finely distributed dispersion is obtained with a OH number of 39, a viscosity of 3,500 cP / 25 ° C and a pH of 7.5. After diluting with polyester D to 10 wt.% Solid, viscosity 1450 cP / 25 ° C. Example 14. The experience of the example, however, the amine is pre-dissolved in the polyester. A solution of 61.5 g of hexamethylenediamine, 20 g of the product from the conversion of hydrazine and chlorogolic acid ester of monofunctional polypropylene oxide (molecular weight 2000) to 800 g of polyester E, also 117.5 1 -isocyanate-3.5 - Trimetsh-1-5 -isocyanatomethyl shpsloheksana. A stable, white, finely distributed, 20% dispersion is obtained with an OH number of 45, a viscosity of 2400 ° C and a pH of 10. After diluting with polyester E to 10% by weight of a solid, the viscosity is 1200 cP / 25 ° C. Example 15. The experiment is carried out as in Example 7. Every minute in one mixer I mix 350 grams of polystyrene E, 66 grams of hydrazine hydrate and 30 linear polypropylene oxide with a 114 NH2 group in one OH secondary pear (molecular weight 2000), in the other a mixture of 350 g of polyester E and 228 g of the aforementioned mixture of toluylene diisocyanate. Both streams then enter the third mixer for the reaction. After additional mixing and distillation of water, a stable, white, finely distributed 30% dispersion is obtained with a OH number of 39, a viscosity of 2900 cP / 25 ° C and a pH of 8.1. After diluting with polyester E to 10 wt.% Solids, the viscosity is 900 cP / 25 ° C. Claim 1. Stable non-slurry dispersion of polyurethane foam production, including polyurea and / or polyhydrazidecarbonamide and hydroxyl-containing polyester, characterized in that, in order to increase the low-viscosity dispersion, if with a solids content of 10% by weight, the viscosity is up to 2500 cP (25 ° C), as a hydroxyl-containing compound, it contains a polyester with 2-8 hydroxyl rpjTinaMH and with a molecular weight of 200-16000 with the following component ratio, wt%: Polyurea and / or polyhydrazidecarbonamide 10 -. 35 Polyester with 2-8 hydroxyl groups and molecular weight 200-1600065 - 90
    [2]
    2. A method of obtaining a stable non-dementating dispersion according to claim 1, characterized in that the polyisocyanate is reacted with a polyamine and / or hydrazine and / or hydrazide in a solution of a hydruxyl-containing polyester with an equivalent ratio of 0.8: 1: 1 , 05: 1, and the source components are continuously or separately passed into the flow mixture, in which the product coming out of the state mixer is stirred for 1-600 seconds and collected in a collector. Sources of information taken into account during the examination 1. Acceptance for Germany of Germany No. 1260142, class 39v5 22/05, published. 1968 (prototype).
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    US6087440A|2000-07-11|Continuous process for preparing a polyurethane latex
    AU600659B2|1990-08-23|Stable dispersions of polyureas and/or polyhydrazodi- carbonamides in relatively high molecular weight, hydroxyl group containing compounds, process for the production thereof and use thereof for the production of polyurethanes
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    DE2946625C2|1992-08-20|
    同族专利:
    公开号 | 公开日
    IT1035736B|1979-10-20|
    JPS51114497A|1976-10-08|
    NL171592C|1983-04-18|
    FR2305466A1|1976-10-22|
    SE7505598L|1976-09-28|
    BE829123A|1975-11-17|
    DE2513815A1|1976-09-30|
    NL7505666A|1976-09-29|
    NL171592B|1982-11-16|
    DE2513815C3|1979-05-23|
    CH614455A5|1979-11-30|
    ATA371775A|1977-07-15|
    FR2305466B1|1979-03-02|
    CA1068840A|1979-12-25|
    DK218375A|1976-09-28|
    DD118102A5|1976-02-12|
    GB1453258A|1976-10-20|
    LU72484A1|1976-03-17|
    SE414501B|1980-08-04|
    AU8119875A|1976-11-18|
    DE2513815B2|1978-09-14|
    AT342305B|1978-03-28|
    BR7503066A|1976-09-28|
    JPS5216747B2|1977-05-11|
    ES437721A1|1977-03-16|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE19752513815|DE2513815C3|1975-03-27|1975-03-27|Process for the production of stable dispersions|
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