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1. 发明专利

RU2139295C1 METHOD OF PREPARING POLYISOBUTYLENE 未知
公开(公告)号：RU2139295C1
公开(公告)日：1999-10-10
申请号：RU98110169
申请日：1998-05-20
申请人： OTKRYTOE AKTSIONERNOE OBSHCHES , OD SINT KAUCHUKA
发明人： AKSENOV V I , GOLOVINA N A , ZOLOTAREV V L , GRUNIN G N , EZHOVA E A , GRISHCHENKO A I , NESMELOV A I , MURACHEV V B , BYRIKHIN V S , KOLOKOL NIKOV A S
IPC分类号： C08F110/10 , C08F2/06 , C08F4/64 , C08F4/642
摘要： FIELD: chemical industry. SUBSTANCE: polyisobutylene is prepared by polymerization of isobutylene at temperatures ranging from -40 C to +40 C in toluene, in-hexane or isopentane in the presence of catalyst complex preformed from titanium tetrachloride and triisobutyl aluminium at temperatures ranging from -30 C to +30 C at molar ratio from 10 to 0.5 and maintained for 0.1-480 minutes, 0.1- 1.5 mole of titanium compound being used per 100 kg of monomer. EFFECT: narrow molecular weight distribution of polyisobutylene, smaller amounts of catalyst system components and high process rate. 4 ex, 1 tbl

2. 发明专利

RU2130948C1 POLYISOBUTYLENE PRODUCTION PROCESS 未知
公开(公告)号：RU2130948C1
公开(公告)日：1999-05-27
申请号：RU98109358
申请日：1998-05-20
申请人： OTKRYTOE AKTSIONERNOE OBSHCHES , OD SINT KAUCHUKA
发明人： AKSENOV V I , GOLOVINA N A , ZOLOTAREV V L , GRISHCHENKO A I , BYRIKHIN V S , NESMELOV A I , MURACHEV V B
IPC分类号： C08F110/10
摘要： FIELD: polymerization reactions and lubricant additives. SUBSTANCE: polyisobutylene useful as thickening lubricant additive and source for preparing hermetics, glues, and other products is produced by polymerization of isobutylene in hydrocarbon solvents in presence of catalytic system consisting of titanium halides and trialkylaluminum, in particular, triisobutylaluminum. Process is carried out at temperature from -40 to +40 C by way of consecutively adding, to solvent (toluene, xylene, n-hexane, isopentane), isobutylene in amount 10-60 wt %, divinylbenzene in amount 0.1-5.0% based on isobutylene weight, titanium tetrachloride on the basis of 0.005-2.0 mole per 100 kg of monomer, and triisobutylaluminum at Ti/Al molar ratio from 20 to 0.5. EFFECT: reduced consumption of catalytic system components, increased yield of product, and increased its thickening capability with low molecular weight. 5 ex

3. 发明专利

RU2134273C1 METHOD OF PREPARING POLYISOBUTYLENE 未知
公开(公告)号：RU2134273C1
公开(公告)日：1999-08-10
申请号：RU98110162
申请日：1998-05-20
申请人： OTKRYTOE AKTSIONERNOE OBSHCHES , OD SINT KAUCHUKA
发明人： AKSENOV V I , GOLOVINA N A , GRISHCHENKO A I , GRUNIN G N , ZOLOTAREV V L , MURACHEV V B , KOLOKOL NIKOV A S , IVANNIKOV V V , NESMELOV A I , KHLUSTIKOV V I , BYRIKHIN V S
IPC分类号： C08F110/10 , C08F2/06 , C08F4/642
摘要： FIELD: synthetic rubber industry, more particularly, manufacture of addition agents, lubricants, adhesives, mastics and other products. SUBSTANCE: polymerization process is carried out in toluene, n-hexane, isopentane, xylene containing water in amount from 0.0003 to 0.006 wt % at temperatures from -40 C to -80 C by initially introducing isobutylene within 10-50 wt % total amount preformed catalyst complex from titanium tetrachloride, butadiene or isoprene, organoaluminium compound selected from group consisting of wherein are C 4 , C 10-20 radicals hydrocarbon respectively, n is not more than 20 based on titanium, to diene to organoaluminium compound molar ratios from 1:3:1:0 to 1:8:0.05 in amount of 0.1-2.0 moles per 100 kg of monomer with respect to titanium tetrachloride and the remaining pert of isobutylene is then continuously introduced and is polymerized at temperature mentioned above, monomer being added as soon as least 90% conversion is attained at first stage, and process is carried out till 50-80 wt % of polymer is finally present in solution. Method makes it possible to prepare highly reactive low molecular polyisobutylene with predetermined molecular parameters, regulate its unsaturation within wide range and significantly widen range of solvent and organoaluminium compound. EFFECT: more efficient preparation method. 8 ex, 1 tbl

4. 发明专利

RU2206581C2 METHOD FOR PREPARING BUTADIENE-STYRENE RUBBER 未知
公开(公告)号：RU2206581C2
公开(公告)日：2003-06-20
申请号：RU2001122065
申请日：2001-08-06
申请人： OD SINT KAUCHUKA , EFREMOVSKIJ ZAV AOOT
发明人： AKSENOV V I , GOLOVINA N A , RJAKHOVSKIJ V S , STEPANOVA E V , SOKOLOVA A D , ZIBOROVA V P , BELIKOV V A
IPC分类号： C08F236/10
摘要： FIELD: rubber industry. SUBSTANCE: invention relates to preparing synthetic rubbers, in part, butadiene- styrene rubber of solute polymerization used in production of tires, rubber-technical articles and other fields and can be used in petrochemical industry. Process of copolymerization is carried out for some steps. At the first step n-butyllithium taken as measured 20-60 moles per one ton of monomers and a modifying additive taken among the group including diethylene glycol dimethyl, diethyl, divinyl ester, methyl-, ethyl-, di-tetrahydrofurfuryl ester taken as measured for mole ratio to n-butyllithium in the ranges 0.1-0.8 are added to charge with initial concentration of monomers 10-20 wt.-% in the ratio butadiene : styrene in the range from 85:15 to 60:40 by mass and the polymerization process is carried out up to conversion 95%, not less. At the second step divinylbenzene is added taken as measured for mole ratio to n-butyllithium from 0.1 to 0.6, kept for at least 2 min. At the third step the same charge is fed additionally taken as measured for mass ratio to initial amount in the range from 1: 1 to 6:1 and modified additive taken among the group including potassium tetrahydrofurfurylate, styryl or nonyl, substituted potassium phenolate in toluene solution as measured for mole ratio potassium-lithium from 0.01 to 0.1 and process is carried out up to conversion 95%, not less, at temperature of each step 20-60 C. If necessary, at the fourth step styrene is added taken in the amount 3-15 wt.-% of total amount of comonomers fed to system on the first and third steps and process is carried out repeatedly up to conversion of styrene 95%, not less. Method ensures to obtain butadiene-styrene rubber with preferred content of 1,3-links of static or static-block structure (if styrene is added at the final step), broad index ð and enhanced value of friction coefficient with wet surface. EFFECT: improved preparing method, valuable properties of rubber. 2 cl, 1 tbl, 9 ex

5. 发明专利

RU2200740C1 METHOD OF SYNTHESIS OF BUTADIENE-STYRENE RUBBER 未知
公开(公告)号：RU2200740C1
公开(公告)日：2003-03-20
申请号：RU2001122064
申请日：2001-08-06
申请人： EFREMOVSKIJ ZAV AOOT , OD SINT KAUCHUKA
发明人： AKSENOV V I , GOLOVINA N A , RJAKHOVSKIJ V S , STEPANOVA E V , SOKOLOVA A D , ZIBOROVA V P , BELIKOV V A
IPC分类号： C08F236/10
摘要： FIELD: rubber industry. SUBSTANCE: invention relates to method of synthesis of synthetic rubber, in part, butadiene-styrene rubber of solution polymerization, polymerization used in production of tires, rubber-technical articles (RTA) and other branches and can be used in petrochemical industry. Method involves the application of compound as modifying addition taken among the group comprising the following substances: diethylene glycol dimethyl-, diethyl-, divinylester; methyl-, ethyl-, di-, tetrahydrofurfuryl ester and/or sodium tetrahydrofurfurylate; sodium styryl-, nonyl-substituted phenolate as measured for the mole ratio to n-butyllithium in the range 0.05-0.8. Divinylbenzene is used as a coupling agent taken as measured in the mole ratio from 0.1 to 0.6 to n-butyllithium. These reagents are fed to charge and polymerization process is carried out up to conversion 95%, not less, at temperature 30-80 C. If necessary, up to the conversion attainment 95%, not less, the compound taken among group including tin tetrachloride, tributyltin chloride, dibutyltin dichloride, N-methyl-alpha-pyrrolidone, 4-nitroso-diphenylamine, N-butylpropionaniline, 2-chloro-4,6-bis-(diethylamine)-sym-triazine, 4,4-bis-(dibutylamino)-benzophenone, 4-diethylamino-chlorobenzophenone as measures in the mole ratio to n-butyllithium from 0.1 to 0.8 and kept at the same temperature for 15-60 min and/or petroleum oil taken among the group including netoxol, plastar-20K, PN-6K, stabilplast-62 as 40-50 wt.% solution in hydrocarbon as measured of oil content in rubber in the range 10-30 wt.%. Invention allows to obtain rubber with preferential content of vinyl links, good technological effectiveness in processing, enhanced elasticity indices by spring back in alkylaromatic and other solvents. EFFECT: improved method of synthesis. 3 cl, 1 tbl

6. 发明专利

RU2192435C2 METHOD OF PRODUCTION OF PLASTICIZED LOW-VISCOUS POLYBUTADIENE 未知
公开(公告)号：RU2192435C2
公开(公告)日：2002-11-10
申请号：RU2000131002
申请日：2000-12-13
申请人： EFREMOVSKIJ ZAV AOOT , OD SINT KAUCHUKA
发明人： AKSENOV V I , ANTONOVA N G , GOLOVINA N A , SOKOLOVA A D , STEPANOVA E V , PAKHOMOV V A , PAUCHENKO N V , KHAZANOV M I , VILKOVA EH N , KRUPYSHEVA L S , KOLOKOL NIKOV A S , GRUNIN G N
IPC分类号： C08F136/06
摘要： FIELD: organic chemistry, polymers. SUBSTANCE: invention relates to technology of production of plasticized low-viscous polybutaidene. Method of production of plasticized low-viscous polybutadiene involves addition of synthetic additions to high-molecular polybutadiene. Product obtained by polymerization of butadiene in a single reactor is used as high-molecular polybutadiene and n-butyllithium is added to solvent as measured of its mole content in the range from 0.6 to 3.2 mmole/l and then butadiene is fed as measured by its final concentration 15-35 wt.-% and process is carried out at temperature 20-80 C up to conversion 95%, not less. Solution of low-molecular polymer as polybutadiene synthesized by known methods is used as synthetic addition in the presence of catalytic systems n-butyllithium potassium tetrahydrofurfurylate or nickel hydrocarbon-soluble salts, alkylaluminium sesquichloride and N-methyl-alpha-pyrrolidone as measured by mass ratio polybutadiene : addition = from 1:1 to 0.3:1. Invention ensures to obtain low-viscous plasticized polybutadiene with increased conventional tensile strength of vulcanizate based on thereof. Invention can be used in industry of synthetic rubber and product produced for making rubber-technical articles, protective covers, sealing compounds and for other aims. EFFECT: improved method of production, valuable technical properties. 1 tbl, 7 ex

7. 发明专利

RU2148590C1 METHOD OF SYNTHESIS OF POLYISOBUTYLENE 未知
公开(公告)号：RU2148590C1
公开(公告)日：2000-05-10
申请号：RU98110164
申请日：1998-05-26
申请人： OD SINT KAUCHUKA , EFREMOVSKIJ ZAV AOOT , OOO TEKHSINTEZ SK
发明人： AKSENOV V I , GOLOVINA N A , ZOLOTAREV V L , NESMELOV A I , MURACHEV V B , EZHOVA E A , BYRIKHIN V S , GRUNIN G N , KHLUSTIKOV V I
IPC分类号： C08F110/10
摘要： FIELD: organic chemistry, chemical technology. SUBSTANCE: invention relates to isobutylene polymerization and obtained low-molecular polymer is used as the base for succinimide addition agents, hermetic agents, glues, thickening addition agents and many other aims. Invention describes method of synthesis polyisobutylene by polymerization of isobutylene in hydrocarbon solvent in the presence of catalytic system consisting of titanium tetrachloride and triisobutylaluminium at the mole ratio titanium : : aluminium from 0.2 to 20. Titanium tetrachloride is used on the basis of its content 0.1-1.5 moles/100 kg of isobutylene. Fraction of C3-C4,-hydrocarbons containing isobutylene at amount from 20 to 60 wt.-% and water at amount from 0.0005 to 0.004 wt. -% is used as hydrocarbon solvent and polymerization process is carried out at temperature from -20 C to -50 C. Method ensures to synthesize polyisobutylene of molecular mass 35 x 103 Da selectively at narrow molecular-mass distribution. EFFECT: decreased catalyst consumption, decreased cost. 1 tbl

8. 发明专利

RU2127276C1 METHOD OF POLYISOBUTYLENE SYNTHESIS 未知
公开(公告)号：RU2127276C1
公开(公告)日：1999-03-10
申请号：RU97104379
申请日：1997-03-20
申请人： HSINTEZ SK , OBSHCHESTVO S OGRANICHENNOJ OT , OTKRYTOE AKTSIONERNOE OBSHCHES
发明人： AKSENOV V I , GOLOVINA N A , GRISHCHENKO A I , ZOLOTAREV V L , SAZYKIN V V , GOL BERG I P , KHLUSTIKOV V I , RJAKHOVSKIJ V S , GRUNIN G N , KOLOKOL NIKOV A S , BYRIKHIN V S , MURACHEV V B , NESMELOV A I
IPC分类号： C07F5/06
摘要： FIELD: organic chemistry, polymers, chemical technology. SUBSTANCE: invention relates to a method of isobutylene polymerization. Method involves the use of triisobutylaluminium as a source of trialkylaluminium and process is carried out in toluene, n-hexane, isopentane containing water at the range from 0.0005 to 0.004 wt.-% at (-40 C)-(+40 C). Process involves the successive addition of isobutylene at its concentration in solvent 10-60 wt. -%, titanium tetrachloride as measured 0.05-1.5 mole/100 kg monomer and/or triisobutylaluminium at mole ratio titanium : aluminium = 0.5-10. The end product is used for production of sealing agents and glues, thickening addition agents and for other aims. EFFECT: decreased consumption of catalyst, increased rate of polymerization in an inert solvent. 4 ex

9. 发明专利

RU2109754C1 LOW-MOLECULAR POLYISOBUTYLENE PRODUCTION PROCESS 未知
公开(公告)号：RU2109754C1
公开(公告)日：1998-04-27
申请号：RU95117345
申请日：1995-10-11
申请人： TOVARISHCHESTVO S OGRANICHENNO , OTKRYTOE AKTSIONERNOE OBSHCHES
发明人： AKSENOV V I , GOLOVINA N A , GRISHCHENKO A I , GRUNIN G N , GOL BERG I P , KHLUSTIKOV V I , RJAKHOVSKIJ V S , KOLOKOL NIKOV A S , BOBROVSKIJ N A , ZOLOTAREV V L , MURACHEV V B , NESMELOV A I , BYRIKHIN V S , SAZYKIN V V
IPC分类号： C08F110/10
摘要： FIELD: polymer production. SUBSTANCE: invention relates to producing polyisobutylene useful as thickening additive for industrial oils and for preparing viscous lubricants, adhesives, hermetics, and other. Polymerization is carried out in solvent constituting mixture of toluene and diisobutylene at weight ratio from 20:1 to 1:20 and at temperature from 30 to +60 C by way of successively introducing isobutylene into solvent to maintain its content within the range 10 to 60 wt % and titanium tetrachloride to its content 0.05 to 1.0 mol per 100 kg of monomer, after which reaction mixture is aged for at least 2 min and then supplemented by triisobutylaluminum. The latter is added in a mixture containing 3 to 50 mol % diisobutylaluminum hydride and/or 5 to 25 mol % tetraisobutylalumoxan. Titanium to aluminum molar ratio ranges from 0.5 to 100. Process enables producing low-molecular polyisobutylene with narrow molecular-mass distribution requiring reduced commercial catalytic system components intakes. Yield of polymer is quantitative and molecular mass of polymer is controllable within wide limits. EFFECT: enhanced process efficiency. 1 tble

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