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Unsaturated epoxidized polysiloxane, preparation method and applications thereof

A technology for epoxidized polysiloxane and hydrogen polysiloxane, which is applied in the field of preparation of epoxidized silicone oil modification, can solve the problem of large amount of epoxidized silicone oil, insufficient conversion rate of silicon-hydrogen, and low-hydrogen silicone oil conversion rate of less than 85%. And other issues

Inactive Publication Date: 2019-02-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Professor Zhang Zhaogui used low-hydrogen silicone oil and allyl glycidyl ether to prepare epoxidized silicone oil. In the low-hydrogen silicone oil / allyl glycidyl ether ratio of 1:1.25 (mol), the addition reaction time reached 5 Under the condition of -6h, the conversion rate of its low hydrogen silicone oil is less than 85%
However, when preparing epoxidized polysiloxane with unsaturated double bonds, there are also problems of insufficient silicon hydrogen conversion rate and a large amount of active silicon hydrogen.

Method used

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  • Unsaturated epoxidized polysiloxane, preparation method and applications thereof
  • Unsaturated epoxidized polysiloxane, preparation method and applications thereof
  • Unsaturated epoxidized polysiloxane, preparation method and applications thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0082] Add 100g of anhydrous vinyl polydimethylhydrogensiloxane (viscosity of 15000mPa·s, vinyl content of 0.56mol%, hydrogen content of 0.02%) into a dried 500mL four-necked flask, and dry over molecular sieves 100mL of anhydrous toluene, high-purity nitrogen was introduced to drive away the air in the bottle and protect the reaction system, 2.5mL of 0.1wt% chloroplatinic acid toluene solution was added dropwise, the temperature was controlled at 50 °C, and 2.9g of allyl glycidol Add the ether into the separatory funnel and drop it into the reaction solution within 1 h, stir and react at this temperature for 5.5 h, after the reaction is over, add 100 mL of ion-free water to wash the reaction solution for 15 min, then separate the water phase at room temperature, Then vacuum removed low boilers, solvent and unreacted allyl glycidyl ether at about 90° C. to obtain light yellow transparent liquid, and the residual active hydrogen content in the product was measured to be 3.0 mmol...

Embodiment 2

[0086] Add 100 g of anhydrous vinyl polymethylvinyl hydrogen-containing siloxane (viscosity of 18000 mPa·s, vinyl content of 0.98 mol%, hydrogen content of 0.04 mol%) into a dried 500 mL four-necked flask, molecular sieve Dried anhydrous toluene 100mL, control the temperature at about 50°C. Add 4.4mL of 0.1wt% chloroplatinic acid toluene solution dropwise, feed high-purity nitrogen to drive away the air in the bottle and protect the reaction system, control the temperature at 65°C, and then Add 5.3g of allyl glycidyl ether into the separatory funnel and drop it into the reaction solution within 2h, stir and react at this temperature for 8h, after the reaction is over, add 100mL of ion-free water to wash the reaction solution for 15min, and then in The water phase was separated at room temperature, and then the low boilers, solvent and unreacted allyl glycidyl ether were removed in vacuum at about 120°C to obtain a light yellow transparent liquid, and the residual active hydroge...

Embodiment 3

[0089] Add 100g of vinyl-terminated polydiethylhydrosiloxane (viscosity of 58000mPa·s, vinyl content of 0.85mol%, hydrogen content of 0.08%), molecular sieve-dried non- Water toluene 100mL, feed high-purity nitrogen to drive away the air in the bottle and protect the reaction system, add dropwise 0.1wt% chloroplatinic acid toluene solution 4.2mL, control the temperature at 85 °C, and then add 11g of 1,2-epoxy- Add 4-vinylcyclohexane into the separatory funnel and drop it into the reaction solution within 1.5h, stir and react at this temperature for 5.5h, after the reaction is over, add 100mL deionized water to wash the reaction solution for 15min, and then The water phase was separated at room temperature, and the low boilers, solvent and unreacted 1,2-epoxy-4-vinylcyclohexane were removed in vacuum at about 150°C to obtain a light yellow transparent liquid. As a result, the residual active hydrogen content in the pale yellow transparent liquid product was 12 mmol%.

[0090] ...

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Abstract

The present invention relates to an unsaturated epoxidized polysiloxane, a preparation method and applications thereof, wherein the unsaturated epoxidized polysiloxane modifies a polybutadiene-styreneactive lithium polymer. According to the present invention, the unsaturated epoxidized polysiloxane contains an unsaturated double bond and a plurality of epoxy groups having high activity, does nothave active silicon-hydrogen bond, and can efficiently carrying out coupling or end capping reaction on an epoxy group and the terminal active lithium of a styrene-butadiene random copolymer to obtaina polyfunctionalized solution polymerized styrene-butadiene rubber, wherein the tire tread vulcanized rubber has low dynamic heat generation and the rolling resistance decrease rate is more than 28%by using the polyfunctionalized SSBR raw rubber as the radial semi-steel tire tread rubber. According to the present invention, whether the silicon-hydrogen addition reaction or the ammonia esterification reaction of the residual silicon-hydrogen and isocyanate is the homogeneous reaction, the preparation method is simple, the reaction is easy to control, and the method is suitable for industrialproduction.

Description

technical field [0001] The invention belongs to the field of preparation of modified epoxidized silicone oil, in particular to a kind of unsaturated epoxidized polysiloxane and its preparation method and the application of the polysiloxane to polybutadiene-styrene random active lithium Polymers were modified to prepare multifunctional SSBR. Background technique [0002] Functionalized SSBR is usually obtained by reacting a butadiene-styrene random copolymer capable of reacting with active lithium. For example, JP2009 287 020A introduces that in the presence of ditetrahydrofurfuryl propane and butyllithium, butadiene Polyethylene and styrene are polymerized in cyclohexane and modified with 3-N,N-bis(trimethylsilyl)aminopropyl(methyl)diethoxysilane. This method belongs to Coupled type, the polar nitrogen atom is also in the middle segment of the polymer. Such as David F.Lawson, Uniontown etc. US5616704A Solubilized cnionic polymerization inttiators described the use of secon...

Claims

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Application Information

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IPC IPC(8): C08G77/388C08G77/442
CPCC08G77/388C08G77/442
Inventor 张建国将文英张书会陈移娇姚谅
Owner CHINA PETROLEUM & CHEM CORP
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