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    • 专利摘要:
    A tackifier system which includes the reaction product of oxirane bearing materials with alkyl phenol novolacs for elastomers of alpha-olefin polymers which are sulfur curable.
    公开号:SU921468A3
    申请号:SU752163180
    申请日:1975-08-12
    公开日:1982-04-15
    发明作者:Майкл Галькиевич Томас；Клэренс Питерсен Кеннет；Линч Салливен Джон
    申请人:Шенектади Кэмиклс,Инк (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to molding compositions, in particular to molding compositions based on elastomers, which contain additives, tackiness agent, as well as conventional targeted additives.  Agents with an adherent stickiness are used in elastomeric mixtures to improve the practical range of properties of elastomers, such as stiffness and stickiness, and are also used to improve adhesion and, in some cases, the cohesion of the elastomeric mixture, and the mixture is necessarily softened or lost. em flexibility.  A known composition containing a chain-chain rubber, a phenolic resin-based adhesive, sticky adhesive and target additives 1 However, this composition has insufficient adhesiveness.  The aim of the invention is to improve the adhesiveness of the mixture.  This aim is achieved in that the composition comprising karbotsepnsda rubber and desired additives as enhancing agent present stickiness comprises prodzst interaction (54) COMPOSITION Corollary alkylphenol novolac with C4-Ci6 in the alkyl radical with epoksnsoderzhaschim compound at a edushkem ratio, weight. h: Carbo-chain rubber Prk uk reacting alkylphenol novolak with C4-Ci6 in an alkylene radical with an epoxy-containing compound. Target additive The proposed reagents are the reaction products of A and B.  A means the radical of the alkanol phenol novolac, B - the radical of an oxirane-containing substance.  The product of the reaction between the alkylphenol novolac and the oxirane-containing substance is further designated A B. for simplicity.  Alkpolnol Novolak get well-known condensation of phenols with aldehydes.  According to the invention, an alkylphenol is used which is a phenol substituted by a hydrocarbon radical (for example alkyl) with 4 to 16 carbon atoms.  Typically, an alkyl mixture 392 titer is located in the para-position of the phenol portion.  Alkylphenols commercially available may contain small amounts of disubstituted alkylphenols, as well as ortho-mono-mixed phenols.  Para-alkylphenols available for sale and containing two. substituted alkylphenols and monosubstituted phenols can be used to prepare pre-racMbtx tackifying agents.  Alkyl substituent of phenol contains 8-12 carbon atoms.  The alkyl substituent of phenol may be unbranched alkyl with 4-16 carbon atoms, and may also include a branched chain, for example, from tert. -alkyls with 4-16 carbon atoms.  Examples for novolaks are para-tert-based novolaks. -butylphenol, para-tert. -oxy phenol, para-nonylphenol, para-dodeshphenol and para-hexadecylphenol.  However, the aldehyde used for the condensation of apylphenol is formaldehyde, however. : it may be fully or partially replaced.  acetaldehyde, acetone, propionaldehyde, isobutyraldehyde, 6jntTBialdehyde or benzaldehyde, as defined by the formula for apk, ilphenol novolaks where R and R are the same or different and are alkyl with 4-16 carbon atoms; and R is the same or different and may mean hydrogen, lower alkyl with 1-4 carbon atoms, aromatic carbon, for example, phenyl or heterocyclic carbon, for example, furyl and, if I am an alkyl group with more than 1 carbon atom, phenyl or heterocycle, B must have been hydrogen.  The condensation of alkylphenol with aldehyde can be carried out by any method known in the art.  In the examples, for example, alkylphenol, for several hours, in the presence of an acid catalyst, in an inert solvent at reflux temperatures is reacted with the aldehyde.  In a preferred process, prior to the addition of the aldehyde to the alkylphenol, the alkylphenol, the acid catalyst and the solvent is heated to reflux temperature and then the aldehyde is added.  Any solvent which is inert under the reaction conditions can be used; however, it is preferable to use a solvent with a solvent.  kip  100 C and more.  In the examples, xylene is used as a solvent, however, xylene, toluene or any aromatic solvent that is inert under the reaction conditions, for example aromatic hydrocarbons with carbon monoxide, can be used.  kip at least 100 ° C.  The choice of solvent is not critical.  To obtain the product A B, any oxirane reactant is reacted with an alkylphenol.  The equivalent weight of the epoxide of reactive oxirane-containing substances is 5-4000.  The term oxirane encompasses substances containing epoxy groups; therefore, oxirane-containing substances based on MONO-, di-, polyglycidyl ethers, glycidyl esters, glycidyl hydantoins, aliphatic oxirano can be used.  Glycidyl ethers such as oxirane-containing substances derived from bisphenol A, phenolic novolacs, resorcinol, or glycerin can be used.  By glycidyl ethers is meant mono-, da-, and so on.  d.  Oxyran polyglycidyl esters.  Glycidyl ester complexes are also used, for example, tetragischutuphthalic acid diglycidyl ether.  The term glycidyl esters includes mono, di-, and other oxiranes.  d.  Oxyran polyglycidyl esters.  Aliphatic oxiranes, for example propylene oxide, can be used.  The term aliphatic oxyracks includes mono-, di-, poly-aliphatic oxiranes.  Cycloaliphatic oxyrenes, for example oxyrahexenes, are also used.  The term "dicloaliphatic oxiras" includes MONO-, di- and t.  d.  polycycloaliphatic oxiranes.  Glycidyl heterocycles, for example XB-2793, a bifunctional hydantoine epoxy-resin, have the following structure: (i-N cl-dH, V o cjL L o o NJ CHg-c Obviously, the term glycidyl heterocycles encompass di- and polyglycidyl heterocyclic oxiranes.  Aromatic oxiranes, for example styrene, can be used.  Suitable epoxy resins produced from bisphenol A are manufactured by the company Shel Kemnckl Co. Shani under the trade name Epon-resin.  According to the invention, an epon-resin of the epon series 828 - epoi 1009, as well as a zon 812 produced from glycerine can be used.  All the epon resins mentioned are glyphenyl esters of bisphenol A, with the exception of epona 871 and epona 812, which are resins based on aliphatic polyepoxides.  The epoxies of the above zpon-series are similar to each other.  Epon 829, for example, is a biphenol A liquid epoxy resin, which basically has the same physical properties as epon 828.  Epon 829 differs from zpon 828 in the content of a small amount of ethyltriphenyl phosphonium iodine catalyst.  Equiva; The effective weight of the epon resins is approximately 140-4000.  The oxirane-containing glycidyl ethers and esters used in accordance with the invention are well known.  Oxirane-containing ethers are prepared by reacting typical epichlorohydrin with a polyhydric alcohol, chlorohydrin ether being obtained, which is then subjected to base treatment, for example sodium aluminates, to form oxirane groups on the chlorohydrin ether.  Glycidyl ethers include 1,2-epoxy-containing polyesters of polyhydric alcohol, for example, their polyglycidyl ethers, such as diglycidyl ether, ethylene glycod, propylene glycol, glycerin, dipropylene glycol, etc. P.  Other typical ethers of this class include glycidyl ethers of polyhydric alcohols, which have 1.2 times greater epoxy equivalence than 1 .  P.  -HgCi-o-c - (YH After the formation of a phenolic new; however, the latter can be isolated and reacted with an oxirane-containing substance, or can be dispensed with the phenol novolak and subjected to it at the site of a reaction with an oxirane-containing substance during heating to distillation.  .  Alkylphenol new and the hydroxy-containing substance are mixed and distilled at temperatures of about 130-250 ° C at pressures ranging from atmospheric to less than one inch of mercury.  Art.  T is determined.  square  Ring and ball.  The invention covers epoxy ethers, obra; The interaction of diatomic phenols with epichlorohydrin in a silk solution.  Any of the various dihydric phenols can be used to prepare gicidal ethers, including single-core phenols, for example, resorcinol, catechin, hydroquinone, etc.  d. , or multi-core phenols, for example bis- (4-hydroxyphenyl) -2,3-propane (bisphenol); 4,4-dis) xibenzophenone, bis- (4-hydroxyphenyl) -1,1-ethane; bis (4-hydroxyphenyl) 1, 1-isobutane; bis - (4-hydroxyphenyl) -2,2-butane; bis- (4-hydroxy-2-methylphenyl) -2,2-propane; bis (4-hydroxy-2-tr, butylphenyl) -2,2-propane; bis (2-dioxynaphthyl) methane; 1,5-dioxynaphthalene and the like.  d.  The molecular weight and chain length of the resulting ether can be varied by changing the ratio of epichlorohydrin to two other polyhydric alcohols.  Epoxy glycidyl esters can be obtained by reacting epichlorohydrin with organic acids or their salts, by reacting glycerol with acid chlorides or by directly reacting the carboxyl group in the presence of a catalyst.  As indicated, aliphatic epoxy compounds can also be used as reactants with alkylphenol novolacs to form AB product.  Aliphatic epoxides may contain 3-12 carbon atoms.  Under aliphatic zoksidami understand epoxy derivatives of olefins.  Olefin may contain alkyl or aryl.  alternates.  The aliphatic epoxides of the invention include propylene oxide and epbn 871.  In addition, aliphatic epoxy resins may be used.  An example of cycloaliphatic resins is a left diglycidyl ester based tetrahydrophic resin, for example, SU-182 araldite or SU-178 araldite with chemical structure O CI - O - IHg According to the invention, alkyl phenol novolacs are reacted with 1-38 wt. % oxirane-containing substances.  Usually 5-20 weight. % oxirane-containing substances are reacted with alkphenol novolacs.  Best results are achieved if 812 weight is taken. % oxirane-containing substances for reacting with alkylphenolic substances.  When the content of epoxy resins 5-20 wt. % based on the amount of phenol, the preferred molar ratio of formaldehyde for resins based on, for example, octyl-, nonyl-, or dodecylphenol is 0.60-1.2 (formaldehyde / phenol).  It is important that the target product be appropriately compatible with the elastomer compound. The formaldehyde content in novolacs may vary depending on the following factors: the nature of the alkylphenol (the higher the chain of alkyl substituted by phenol, the greater the amount of formaldehyde needed to reach the desired melting point); on the ratio of alkylphenol-formaldehyde-based resin to epoxy resin (the greater the amount of epoxy resin, the higher m.  square  the obtained resin, with adhesive tack; and on the molecular weight of the epoxy resin, and the optimal amount of formaldehyde in the tackifying resin based on Epon 828 may be different from the amount in the resin on the basis of Zona 1009.  AB product is primarily a thermoplastic substance.  During the preparation of the AB product, the oxirane-containing substance forms cross-links, however, in such a small size that the nature of AB, remains mostly thermoplastic.  Esterification of phenolic groups also leads to a decrease in hydrophilic properties, which is why the reagents offered have better tackiness under conditions with a high moisture content.  The product AB is checked for relative completion of the reaction between the hydroxy-containing substance and novolac.  The equivalent weight of the epoxide is determined.  Equivalent weight of epoxide in reagents is 775 and more, preferably 2000 is at least 4000 or more, for example, 20,000 or even 100,000 or more, preferably equivalent epoxy weight is 20,000-100,000, t. e.  the residual content of the zipoxide is almost 0.  Can adjust t.  square  (using the device Ring and Ball), regulating the physical conditions under which the alkylphenol novolacs and oxirane-containing substances are jointly distilled to produce the product AB.  The distillation temperature is 160-220 ° C under a vacuum of 10-25 inches.  By adjusting the distillation temperatures get products with t.  square  (definition by the device Ring and ball) 60160 ° C.  AB products with t.  square  60-110 ° C are preferably used as rubber glue.  The products of the reagent and between oxirane-containing substances and alkylphenol novolacs are excellent tackifying agents for different elastomers.  Elastomers are understood to be solid under normal conditions alpha-olefinic hydrocarbon, halohydrocarbon and hydrocarbonacrylonitrile polymers containing unsaturation for sulfur vulcanization.  Consequently, the term “elastomers” includes natural and synthetic Cossacks.  By elastomers, we mean styrene-butadiene rubber, natural rubber, ethylene propylene, non-conjugated polyene, for example, an unconjugated diene (a mixture of ethylene, propylene and a diene), butyl, rubber grades and chlorobutyl-based, for example, cis-isoprene polymer, polybutadiene, polychloroplide polymetra, polychloropropylmacene and polychlorofluoropropyl alcohol. and acrylonitrile.  Halohydrocarbon polymers are understood to mean halogenated hydrocarbon polymers, which include chlorobutyl rubbers, as well as polychloroprene.  Hydrocarbon-acrylonitrile elastomers are understood to mean copolymers of acrylonitrile and one or more olefans, for example copolymers of butadiene and acrylonitrile, and elasto-black triple polymers of acrylonitrile. butadiene and styrene.  Suitable elastomers are, for example, polyolefin polymers, for example butyl rubber (i.e.  e.  copolymers of isobutylene with a small amount of diolefin, for example isobutylene-butadiene (98.5: 1.5) or isobutylene / isoprene).  Typically, olefin polymers are solids with a molecular weight of 10,000,000 or even higher.  Ethylene-propylene-diene rubber usually contains, they say. %: ethylene 30-70 (preferred ° 50-60); Propylene 65-20 (preferably 35-54 and) Unconjugated popiolefin 1-15, (preferably 3-5).  Typically, the polyolefin does not exceed 10 mol. %  Each of ethylene and propylene can be 5 to 95 mol. % mixture.  Unconjugated sexes are suitable for the invention; 1lefins, including aliphatic nesopr.  Polyene hydrocarbons and cycloaliphatic nonconjugated polyene hydrocarbons and cycloaliphatic nonconjugated polyenohydrocarbons, such as endocyclic diene 1.  Specific examples of suitable non-conjugated polyolefins include pentadiene, 4; hexadien-1,4; dicyclopentadiene; methylcyclopentadiene dimer; cyclododecatriene; cyclooctadiene-1,5; 5-methylene-2-norbonene; 5-ethylidene-2-norbornene.  Specific examples of suitable ternary polymers are pb leins containing, mol. % ethylene 55; propylene 40-42 and dicyclopentadiene 3-5, ternary Enge polymers, for example ERP-404 Enge and Enge 3509, containing, they say. %: ethylene is about 55; propylene 41 and 5-methylene-2-norbornene 4, a ternary polymer But or, containing, they say. %: ethylene 55, propylene 40 and 5 hexadiene-1,4.  Another suitable terpolymer is Dutrel, which contains, say, mol. % ethylene 50; propylene 47 and 1,5-cyclooctadiene 3.  Reagents that impart stickiness can be used in the above elastomers as reagents for tire, rubber, and rubber compounds that require stickiness in the unvulcanized state.  Examples of rubber products requiring tackiness in the unvulcanized state are tires, tapes and sleeves.  It is known that elastomer and carbon black should adhere well to each other in order for the mixture to have good bond strength in a non-vulcanized and vulcanized state. A high concentration of carbon black improves the aging resistance of vulcanized mixed products.  A typical sulfur vulcanization system can include (as well as the proposed: mixtures of elastomer and tackifier) metal oxide, accelerator and volcano-activator.  nizatsiya and sulfur.  Usually use no more than 2 hours of sulfur - for 100 hours.  elastomer.  At concentrations of 3-10 wt.  h  metal oxide for 100 hours  by weight, the copolymer achieves a satisfactory degree and state of vulcanization.  In addition to use in lath and frame mixtures for tires, tapes and sleeves, a mixture of tackifying agent and elastomer can also be used in rubber adhesives containing styrene-butadiene, natural, ethylene-propylene-diene, butyl and chlorobutyl rubber as a solution , and also in the form of an emulsion.  Example 1  Getting resin.  1258 g of dodecylphenod, 150 g of xylene and g of toluene-succinic acid are fed to a three-neck flask with a capacity of 5 liters, equipped with a stirrer, a thermometer and a condenser.  The temperature is raised to 100 ° C and then 430 g for 37% of non-inhibited formaldehyde is added over about 20 minutes.  After the addition of formaldehyde, the reaction is maintained for 4 hours at reflux temperatures.  Then, 850 g of xylene and 500 g of water are added to the reaction mixture, after which 7 g of 50% sodium hydroxide solution is added, which brings the pH of the reaction mixture to 4-5.  The mixture was stirred at 100 ° C for 30 minutes, the aqueous layer was separated and decanted.  Then, for 30 minutes at 100 ° C, the resin was rinsed with 1000 g of water, the aqueous layer was decanted again and the resin was distilled at 180 ° C under a vacuum of 25 inches.  At a distillation temperature of about 180 ° C, 15 g of epona 829 is added and distillation in the distillation apparatus continues to 220 ° C.  under a vacuum of 25 inches.  The mixture was held at 220 ° C for 1 hour and poured into a vessel for cooling.  Output about 1327 g with t.  square  (determined by the device ring and ball) 97 ° C.  In the following examples, t.  square  also determined by the device ring and ball.  Epon 829 is a bis-phenol A liquid epoxy resin with an equivalent weight of zpoxide 193-203 and a viscosity of 3000070000 centipoise.  Example 2  In a five-liter flask, supplied analogously to example 1, is fed, g: Daudet. qsh1phenol1258 Xylene150 For 30% non-inhibited formaldehyde430 Toluenesulfonic acid14 Aerosol FROM (di-2-ethylhexyl sodium-sulfos5ascinate) 2 Bring back to reflux and hold for 3 hours, then add 850 g of xylene, 1000 g of water and 7 g 50 % sodium hydroxide solution by stirring the reaction mixture.  The resin layer was allowed to settle for 30 minutes, the aqueous layer was decanted and the resin was distilled at 160 ° C under a vacuum of 10 inches.  Then through the dropping funnel, slowly add.  120 g epona 829.  The vacuum of the system is increased to 20 inches, the temperature is adjusted to and maintained at it until it is.  square  resin will not reach 93 C.  The resin is poured into a cooling vessel (1427 g).  Example 3  The operation is carried out in the same manner as for Example 1, using the following reactants, g: Dodecylphenol 1258 Kyolol 150 At 37% non-inhibited formaldehyde 430 Toluene sulfonic acid21 Xylene 1200 Water 1500 50% sodium hydroxide solution.  9 Araldite SU-182100 Work analogously to example 2, get 464 g of resin with t.  square  98 ° C.  Araldite SU-182 is a cycloaliphatic epoxy resin, in particular, a resin based on tetrahydrotalic acid diglycidyl ester.  Example 4  Use the following substances, g:.  Nonylpheno1060 Xylene150 37% non-inhibited formaldehyde430 Toluenesulfonic acid14 Xylene850 Water1500 Epone 829250 These substances are treated according to Example 2, a sufficient amount of 11-50% sodium hydroxide sodium is added to bring the pH to 5-8.  Target product has t.  square  114 C.  Exit 1300  Example 5  The following substances are used, g: Dodecylphenol1258 Xylene 150 At 37% non-inhibited formaldehyde 430 Toluenesulfonic acid21 Xylene 1200 Water. 1500 Styrene Oxide120 A sufficient amount of 50% sodium hydroxide solution is added to bring the pH of the reaction mixture to about 4-5.  These substances are treated as in Example 2, except that styrene oxide is added dropwise at 115 ° C, maintained for 10 minutes and distilled at 220 ° C.  T.  95 ° C.  Out 1461  Example 6  The following substances are used: g: Dodecylphenol 1258 Xylene150 37% non-inhibited formaldehyde430 Toluenesulfonic acid21 Xylene 1200 Water1500 Propylene oxide480 Add sufficient volume of 50% sodium hydroxide solution to bring the pH of the reaction mixture to about 5-7.  The above substances are treated according to Example 2, except that propylene oxide is added, which is kept at 110 ° C for 1 hour before the transition.  square  88 ° C, yield 1322  Preparation of intermediate for examples 7, 8 and 9.  The following substances are used, g: Para-tert, octylphenol (A) 3090 Concentrated sulfuric acid (B) 30 Diisobutylene (C) 588 37% non-inhibited formaldehyde (D) 1442 Xylene (D) 2800 Water (E) 1500 50% a solution of sodium hydroxide (YAO40 Substances A and B are fed to a pot for canns of a resin with a capacity of 71/2 gallons with a reverse refrigeration unit.  Heat Up To substance B is added over a period of 1 hour and the mixture is boiled under reflux for 6 hours.  Alkyl phenol is cooled to 212 ° C for 3/4 h. Adds substance G.  The mixture is boiled under reflux for 2 hours, then substances D and E are added, and the mixture is stirred at 90 ° C for 30 minutes.  Add substance L and continue to stir for an additional 30 minutes. Then stop the mixing and decant the aqueous layer.  The resin is distilled at 149 ° C and a resin with a tonne is obtained.  PC.  100 ° C.  Intermediate5g product is designated as resin G.  PRI me R 7.  The following substances are used: g: Resin D (A) 500 Xylene (B) 200 Epon 1009 (C) 75 For distillation, a five-liter flask is taken, in which substances A and B are fed, heating to 130 ° C, substance B is added.  Continue the distillation, heat to 190 ° C, then work under vacuum (23 inches), the distillation is carried out at 180 ° C.  T.  square  84 ° C, yield 563 g  Epon.  1009 is a bisphenol A diglycidyl ether epoxy resin with an equivalent weight of 2500-4000 epoxide, which is manufactured by the Shel Chemical Company, a resin manufacturing department.  Example 8  Use substances g: Resin D (A) 500 Xylene (B) 200 DEN-438 (C) 75 Work according to example 7.  Get the resin with t.  square  97 ° C.  DEN-438 is an epoxidized polyglycidyl ether of phenol-formaldehyde novolak with an equivalent weight of epoxide of 176-181 and a viscosity of 35,000 to 70,000 cP at 53 ° C, manufactured by Dow Chemical Company, Midland Michigan, USA.  Example 9  Use of the substance, g: Resin (A). 500 Xylene (B) 200 Epone 828 (C) 75 Worked according to Example 7.  Get the resin with t.  square  97 ° C.  Epon 828 is a bisphenol A based epoxy resin with an equivalent weight of epoxy 185-192 and a viscosity of 10,000-16,000 cP, Example 10.  Use substances g: Dodeylphenol1258. 150 Aqueous formaldehyde (37%) 430 Toluene sulphonic acid14.  Water 1000
    Triethanolamine22
    Epon 828100
    Analogously to Example 2, the product of the reaction of epone 828 and the product of condensation of dodecylphenol / formaldehyde was prepared using the indicated substances. Exit 1237 g, so pl. 97 ° Example 11, substances are used, g: Para-tert.-octylphenol. 950
    Xylene355
    Water formaldehyde (37%) 254
    From acid 6,5
    Epon 829120
    According to Example 2, a reaction product of epone 829 and a condensation product of octylphenol / formaldehyde is prepared using these substances. Obtain 1072 g of resin with so pl. 100 ° C.Y
    Example 12. Use of substances, g: dodecylphenol5032
    Xylene 600
    Water formaldehyde (37%) 1720
     Toluenesulfonic acid84
    Water5000
    Water sodium hydroxide (50%) 28 Epon 829500
    According to Example 2, the product of the reaction of epon 829 and the product of condensation of dodecylfeiol / formaldehyde is prepared using yi substances. The resin yield 6432 g and so on. Pl. 93 ° C.
    Y 2 f-Wii2) u-e-o-ciH2-f (° 4J-CH3 oo NZS-CHLAraldit SU-178 is produced by
    Ciba-Geigy.
    Example 15. The following are used.
    substances, g:
    Para-tert.-octylphenol708
    Xylene265
    Water formaldehyde: (37%) 248 Oxalic acid 5.0.
    Aerosol OT0,2
    HV-279360 resin
    According to example 2 prepared 1yu product
    reaction of resin XB-2793 and product cowdens
    octylphenol / formaldehyde
    specified substances. Output this pitch 798 g
    and so on 105 ° C.
    The resin XB-2793 is a liquid gadanto
    epoxy resin.
    Example 16. The following are used.
    substances, g:
    Para-tert.-octylphenol708
    Xylene
    Water formaldehyde (37%) 248
    Oxalic acid 5.0
    Example 13. The substances are used, Mr. Part-tert.-octiphenol950
    Xylene355
    Water formaldehyde (37%) 254
    Oxalic acid6,5
    Epon 81286
    According to Example 2, the product of the reaction of zpon 812 and the condensation product of octylphenol / formaldehyde is prepared using these substances. The output of resin 1072
    m.p. 102 ° C .;
    Epon 812 is a glycerin based epoxy resin with an equivalent weight of epoxide of 150-170 and a viscosity of 12000-20000. PRI me R 14. Use substances, g Para-tert.-octylphenol708
    Xylene265
    Water formaldehyde (37%) .248
    Oxalic acid 5.0
    Aerosol FROM .0,2
    Araldit SU-17860
    According to Example 2, the product of the reaction of araldnt SU-178 and the condensation product octylphenol / formaldehyde was prepared using the indicated substances. The resin yield is 768 g and so on. Pl. 118 ° C
    Araldite SU-178 is a cycloaliphatic epoxy resin having the following structural formula:
    Aeruzole FROM 2.0
    HV-281860 pitch
    According to Example 2, a reaction product of a resin 2818 and a condensation product of octylphenol / formaldehyde is prepared using these substances. The output of the resin is 771 g and t, nn. 127 XB-2818 Resin is a highly viscous, three-function epoxy resin on
    gidaitoin based.
    I;
    Resins obtained according to Examples 1-13 are tested for stickiness in elastomer mixtures x i-iv. In blending everything; the components, with the exception of the resin, are rolled on two rollers for rubber production to produce a masterbatch. All substances are rolled for 4-6 minutes at 79 C. Depending on the apparatus, etc., some changes of these conditions are also possible, for example, treatment for minutes at 37-121 C.
    The resin with a tackifying agent is added to the rubber mix as the last g component and the mixture is expanded to about 1/4 inch thick. Mixture 1. Content of substances, weight. h .: Sunlol 170868,75 Smoked shield 50 On F-soot (furnace soot, which has high wear resistance) 65 Zircosol 424016: 5 Zinc oxide3.0 Stearic acid 1.0, Neozon D. 1.0 Santocure 1.2 Diphenylguanidine 0.3 Sulfur 2.0 Resin 3.0 Sinpol 1708 is a 37 + 1/2 wt.% Oil-filled styrene butadiene elatomer produced by Texas-US Chemical Company. Zirkozol 4240 - naphthenic oil, produced by the firm San Oil Company. Neozone D is N-phenyl-beta-naphthylamine, manufactured by E.I. Dupot Santokur, is M-cyclohexim1-2-benz thiazole sulfenamide, manufactured by Monsanto. Mixture II. Content of substances, weight. including: Flax 306100. On F-soot, (furnace soot, implying high wear resistance) 80 Sandex 79040 Zinc Oxide 5 Stearic Acid Sulfur 2 2-mercatobenzothiazole 0.5 Tetra-methylthiuram Monosulfide1, 5 Resin6 Rolled is ethylene-Npropylene-diene-esoprene tri poly-poly poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly-poly, poly, poly, poly, tri, poly role, is the ethylene-nepropylene-diene esoprene tri-poly poly tetramethylentiram, 5 resins; Uni l.Chemical Comp Rolen 306 has the following physical properties: Mooney viscosity 90; specific weight 0,865; The integer number is 10, the non-criticality of the ternary polymer completes the polymer chain. Sandex 790 is an aromatic carbon hydrogen oil produced by the firm San Oil Company. Mixture III. Content of substances, parts: NT-1068100 F-soot (furnace soot, which provides high durability) 60 Flexon 84510 Zinc oxide 5 Stearic acid 1 16, Sulfur..1 2,2-Benzothiazish1 Disulfide 0.75 Smola4 NT-1068 is chlorinated isobutene-isoprene elastomer produced by Exxon Irma. NT-1068 chlorobutyl rubber has the following physical properties: Mooney viscosity 50-60, specific gravity 0.92, and average molecular weight 350000-400000. Flexon 845 is a paraffin oil asle produced by Gambol Oil Refining Company. Mixture, iv. Content of substances, parts: Butyl 218-100 F-soot (kiln soot, which provides high wear resistance) 60 Flexon 84510 Zinc oxide 5 Stearic acid 1 Sera1 2,2-Benzothiazyl disulfide 0.75 Resin 4 Butyl 218 is an isobutylene-isoprene elastomer Exxon. The resin with a tackifying agent, as the last component, is added to the rubber mixture, then the mixture is rolled out in thicknesses of about 1/4 inch, after which the mixture is cut into 3/8 inch strips and formed into 1/2 X 1.4 X 8 strips inches The molding conditions are as follows: 2000 psi pressure for 5 minutes with cooling to 24 ° C. The molded strips are then cut into 1-1 / 4 d4 oyma segments and at various intervals tested for tackiness with a contact surface for 5 seconds. The strips are then stripped with a stickiness tester. The test device is capable of varying contact and separation pressures. The time needed for the separation is measured (the longer the separation time, the looser tackiness). Elastomeric strips are exposed to environmental conditions and relative humidity conditions of 95% at 32 ° C for a total of 96 hours. At successive time intervals, samples are taken for 96 hours and tested for tackiness as indicated below. Resins prepared according to examples 1-12 are used in mixtures l-IV. In tab. 1 shows a mixture of 1 using 3 g of each resin obtained in Examples 1-12; in tab. 3 and 4 - a mixture of 11c using 6 g of each resin obtained in examples 1, 2, 6, 10, 11 and 12; in tab. 7 and 8 - a mixture of 111
    17 92146818
    with the use of 4 g of each obtained in - when-reagents, add ntsnh stickiness, obtained
    measures 11-12 resin; in tab. 5 and 6 are a mixture of examples 1-12.
    IV using 4 g of each obtained in table. 1 shows measured orders
    in examples 11-12 resin. the stickiness of the mixture .1 under the conditions ("" {Jacques yeah
    In tab. 1-8 shows the results of measuring-5 of the medium with the use of 50 g of contact weight and.
    The Scientific Research Institute of Tackiness of Mixtures 1-IV with the application of 500 g of separating weight.
    Table 1
     The time required for dividing. SP-1068 is a trade in resin, para-tert-phenol-formaldehyde, produced in Table. Table 2 shows the tackiness values of blend 1 after aging at 95% o-adhesive at Chemicals, Inc. moisture with 500 g of base weight and 500 g of separating weight.
    52
    100+
    table 2
    60
    67
    70
    95
    lOOt
    100+
    21
    70
    12
    R-1068 (known)
    10 In table. 4 representations of the size of glucoethism mixture 11 after aging at 95% ratio 25
    90
    27
    90
    ten
    70
    eleven
    52
    12
    R-1068
    17 (known) In table. 5 shows the values of glucose m 55 mixture IV, measured under the conditions of ambient22
    921468 Continuation of table 3
    82
    83
    22
    eleven
    100+
    80
    100+
    39
    53
    45
    80
    99
    90
    81
    83
    100+
    61
    50
    77
    13 of dry moisture with a SOQ g of compact weight and 200 g of separating weight. Table4 of the shreds shakes 500 g of the contact weight and 500 g of the reciprocating weight.
    74
    eleven
    85
    12
    R-1068 (known)
    28
    In tab. 6 shows the values of the stickiness of the mixture IV by sending aging at 32 ° C and 95%
    91
    12
    R-1068 (known)
    50
    In tab. 7 shows the stickiness values of the mixture ill, measured under ambient conditions
    AND
    12
    R-1068 (known)
    In tab. S shows the values of stickiness of the mixture 111 after aging at 32 ° C and 95%
    Table 5
    00+
    100+
    100+
    100+
    52
     50
    relative humidity using 500 g of contact weight g of separating weight.
    Table 6
    100+
    95
    27
    50
    using 500 g of contact weight and 500 g of separation weight.
    Table 7
    86
    75
    100+
    100+
    100+
    100+
    100+
    26
    51
    25
    relative humidity using 500 g of contact weight and 500 g of separating weight.
    25
    Resin examples
    eleven
    82
    12
    100+
    R-1068 (New) Table. 9 shows the weights of stickiness of the mixture V, measured under the conditions of the surrounding medium (ec of the medium using 1CIOO g of co-weight and Resin о p n {measures 1068 (known)) Table 10 shows the wears of adhesive V after heat accumulation 32 С 95% of shoes Table 11 shows the average stickiness of the mixture 1, measured under conditions of circle 24
    14
    17
    15
    921468
    26 Table 8
    Capacity, s, through-day 2 T 3
    7188
    91
    94
    100+
    20
    30 3S
    38
    41
    thirty
    34
    42 zzizziEi: lOOfItKH100 + 100 + n 200 g separating weight. Mixture V is the same as mixture 11, but instead of six, there are five parts of the resin. gi T ablitsa 9 Adhesiveness, s, through the day of high humidity with the use of 1000 g of compressive weight and 200 g of the total weight. i T a l i c a 10 h “Fedi with the use of 100 g of contact and 200 g of section weight. Table 11
    权利要求:
    Claims (1)
    [1]
    The claims
    Composition containing carbochain rubber, a phenolic resin tackifier and target additives, characterized in that, in order to increase tack, the composition contains, as a tackifier, the reaction product of alkyl phenolic novolak with C 4 -Ci 6 in the alkyl radical with
    I
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    同族专利:
    公开号 | 公开日
    ZA753592B|1976-05-26|
    US4073776A|1978-02-14|
    US4073826A|1978-02-14|
    JPS57151633A|1982-09-18|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US05/544,772|US4073776A|1975-01-28|1975-01-28|Tackifiers for elastomers|
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