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A kind of high swelling resistance fluorosilicone raw rubber and preparation method thereof

A technology of fluorosilicone raw rubber and swelling properties, which is applied in the field of high anti-swellable fluorosilicone raw rubber and its preparation, can solve the problem of increasing the cost of fluorine-containing polysiloxane macromolecular polymers, insufficient anti-swelling, siloxane To solve the problems of high price of cyclic compounds, achieve excellent mechanical properties and thermal stability, avoid adverse effects, and have good swelling resistance

Active Publication Date: 2019-07-12
广州源海新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation of fluorine-containing polysiloxane macromolecular polymers by ring-opening polymerization of siloxane rings containing long-chain fluoroalkyl groups is described in Yutaka Furukawa.Journal of Applied Polymer Science, 2001, vol.82, 3333-334 and Document A.E.Shamaev.Russian Chemical Bulletin, International Edition, 2004, vol.53 (No.10): 2229-2232 all has the report, yet the siloxane macromolecular polymer containing the long-chain fluoroalkyl group prepared by the document method is in Insufficient in anti-swelling
In addition, the price of siloxane ring compounds containing long-chain fluoroalkyl groups is relatively high, which also pushes up the cost of obtained fluorine-containing polysiloxane macromolecular polymers

Method used

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  • A kind of high swelling resistance fluorosilicone raw rubber and preparation method thereof
  • A kind of high swelling resistance fluorosilicone raw rubber and preparation method thereof
  • A kind of high swelling resistance fluorosilicone raw rubber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] First, 50 parts by mass of siloxane tricyclic compounds containing long-chain fluoroalkyl groups (Si(CH 3 )(CH 2 CH 2 CF 2 CF 2 CF 2 CF 3 )O) 3 And 45 parts by mass of trifluoropropyl-containing siloxane ring compound D 3 Add F into the three-necked flask, stir and heat to 80°C, dehydrate under reduced pressure for 1.5h; then cool down to the reaction temperature of 65°C, add 4.9 parts by mass of vinyl-containing siloxane ring compound D 3 Vi, 0.1 parts by mass of blocking agent Vi 2 Carry out ring-opening polymerization reaction with 0.1 mass part of acidic catalyst fuming sulfuric acid, and the reaction time is 20h; When the material viscosity reaches a predetermined value, stop the reaction, wash the crude product with water to neutrality, and remove low boilers in the crude product under reduced pressure , get high anti-swelling fluorosilicone raw rubber.

Embodiment 2

[0043] First, 10 parts by mass of siloxane tricyclic compounds containing long-chain fluoroalkyl groups (Si(CH 3 )(CH 2 CH 2 CF 2 CF 2 CF 2 CF 3 )O) 3 And 88 parts by mass of trifluoropropyl-containing siloxane ring compound D 3 Add F into the three-necked flask, stir and heat to 140°C, dehydrate under reduced pressure for 0.5h; then cool down to the reaction temperature of 110°C, add 1.95 parts by mass of vinyl-containing siloxane ring compound D 3 Vi, 0.05 parts by mass of blocking agent Vi 4 and 0.04 parts by mass of acidic catalyst oleum to carry out ring-opening polymerization reaction, the reaction time is 8h; when the viscosity of the material reaches a predetermined value, stop the reaction, wash the crude product with water to neutrality, and remove the low boilers in the crude product under reduced pressure , get high anti-swelling fluorosilicone raw rubber.

Embodiment 3

[0045] First, 90 parts by mass of siloxane tricyclic compounds containing long-chain fluoroalkyl groups (Si(CH 3 )(CH 2 CH 2 CF 2 CF 2 CF 2 CF 3 )O) 3 , 8 parts by mass of trifluoropropyl-containing siloxane ring compound D 4 F and 1 mass part non-fluorine-containing double bond-containing siloxane ring compound D 4 Add it into a three-necked flask, stir and heat to 120°C, dehydrate under reduced pressure for 1 hour; then cool down to the reaction temperature of 90°C, add 0.95 parts by mass of vinyl-containing siloxane ring compound D 4 Vi, 0.05 parts by mass of blocking agent Vi 2 Carry out ring-opening polymerization reaction with 1 mass part of acid catalyst fuming sulfuric acid, and the reaction time is 15h; When the viscosity of the material reaches a predetermined value, stop the reaction, wash the crude product with water to neutrality, and remove the low boilers in the crude product under reduced pressure , get high anti-swelling fluorosilicone raw rubber.

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Abstract

The invention discloses fluorosilicone gum with high anti-swelling property, and a preparation method thereof. Per 100 parts by mass of gum comprise the following components in parts by mass: 10 to 90 parts of a long-chain fluoroalkyl-containing siloxane tricyclic compound, 8 to 88 parts of a trifluoropropyl-containing siloxane cyclic compound, 0.5 to 10 parts of a vinyl-containing siloxane cyclic compound, 0 to 8 parts of a siloxane cyclic compound not containing fluorine and double bonds and 0.02 to 0.2 part of an end-capping reagent, wherein the long-chain fluoroalkyl-containing siloxane tricyclic compound can be shown as a formula (Si(CH3)(Rf)O)3, Rf can be shown as a formula -(CH2)mCnF2n+1, n is an integer of 3 to 8, and m is 2 or 3. The fluorosilicone gum with high anti-swelling property, provided by the invention, has high crosslinkable density, has excellent solvent resistance after sulfurization crosslinking, and reduces the cost.

Description

technical field [0001] The invention relates to the technical field of fluorosilicone raw rubber, in particular to a highly anti-swelling fluorosilicone raw rubber and a preparation method thereof. Background technique [0002] Fluorosilicone rubber, also known as γ-trifluoropropylmethylpolysiloxane, generally introduces 0.2% to 0.4% vinyl siloxane copolymerization modification into the molecular chain; it is a colorless, transparent, high-viscosity plastic linear polymer The compound, the main chain is composed of silicon and oxygen atoms, the side groups connected to silicon are methyl, vinyl and trifluoropropyl, and the molecular weight is between 500,000 and 800,000. With various additives, it can be mixed into homogeneous rubber. Under the action of organic peroxide, it can be vulcanized into various elastic rubber products. In addition to the characteristics of general silicone rubber, it also has good resistance to aviation fuel oil, hydraulic oil, engine oil, chemi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/24
CPCC08G77/24C08G77/80
Inventor 向德轩胡扬剑林红卫张再兴李元祥汤艳
Owner 广州源海新材料科技有限公司
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