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Vinyl polysiloxane as well as preparation method and application thereof

A technology of vinyl polysiloxane and base cyclosiloxane, applied in directions without pigment coating, etc., can solve problems such as affecting the yield of vinyl polysiloxane, achieve molecular weight and easy control, low production cost, Highly reactive effect

Inactive Publication Date: 2018-05-15
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI +4
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[Li En, Chen Haiping, Miao Gang, Meiping, Yu Liming. Preparation of low-viscosity methyl silicone oil and vinyl silicone oil with alkali catalysts [J]. Silicone Materials, 2013, (6): 441~443]; comparative experiments were done , DMC is reacted at a constant temperature of 110°C, 120°C, and 130°C, and the conversion rate of the product is only about 60%, which seriously affects the yield of vinyl polysiloxane

Method used

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  • Vinyl polysiloxane as well as preparation method and application thereof
  • Vinyl polysiloxane as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A preparation method of vinyl polysiloxane, comprising the following steps:

[0038]Put 19.6g of DMC (Hubei New Sihai Chemical Co., Ltd.) and 5.2g of tetramethyltetravinylcyclotetrasiloxane (Bailingwei) in a reaction vessel, raise the temperature to 80°C, stir and evacuate to -0.09MPa, and dehydrate for 1h , to obtain a dehydrated monomer mixture; add 1.82g of divinyltetramethyldisiloxane to the dehydrated monomer mixture, and heat up to 100°C; add 0.49g of temporary catalyst tetramethylammonium hydroxide, and heat up to 110°C, Heat preservation reaction for 1 hour; raise the temperature to 120°C, heat preservation reaction for 3 hours; heat up to 130°C, heat preservation reaction for 1 hour to obtain the reaction product; heat the reaction product to 180°C to decompose the catalyst, vacuum -0.09MPa nitrogen, until there is no fraction distillation Go out, obtain colorless and transparent product vinyl polysiloxane. The conversion rate of the monomer in this example is...

Embodiment 2

[0040] A preparation method of vinyl polysiloxane, comprising the following steps:

[0041] Put 27g of DMC (Hubei New Sihai Chemical Co., Ltd.) and 6.2g of tetramethyltetravinylcyclotetrasiloxane in a three-necked flask, raise the temperature to 80°C, stir and evacuate to -0.09MPa, and dehydrate for 1h to obtain a dehydrated single monomer mixture; add 3.6g of divinyltetramethyldisiloxane to the dehydrated monomer mixture, and heat up to 100°C; add 0.56g of temporary catalyst tetramethylammonium hydroxide, heat up to 110°C, and keep warm for 1h; Raise the temperature to 120°C, heat-retain for 3 hours; raise the temperature to 130°C, heat-retain for 1 hour, and obtain the reaction product; heat the reaction product to 180°C, decompose the catalyst, vacuumize -0.09MPa and blow nitrogen until no fraction distills out to obtain Colorless transparent product vinyl polysiloxane. The conversion rate of the monomer in this example is 91.2%.

Embodiment 3

[0043] A preparation method of vinyl polysiloxane, comprising the following steps:

[0044] Put 19.6g of DMC (Hubei New Sihai Chemical Co., Ltd.) and 5.2g of tetramethyltetravinyl cyclotetrasiloxane in a three-necked flask, raise the temperature to 80°C, stir and evacuate to -0.09MPa, and dehydrate for 1 hour to obtain dehydrated Monomer mixture; add 1.82g of divinyltetramethyldisiloxane to the dehydrated monomer mixture, heat up to 90°C; add 0.49g of temporary catalyst tetramethylammonium hydroxide, heat up to 110°C, keep warm for 1h Raise the temperature to 120°C and keep it warm for 3 hours; raise the temperature to 130°C and keep it warm for 1 hour to obtain the reaction product; raise the temperature of the reaction product to 180°C to decompose the catalyst, vacuumize -0.09MPa and blow nitrogen until no fraction distills out. A colorless and transparent product vinyl polysiloxane was obtained. The conversion rate of the monomer in this example is 88%.

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Abstract

The invention belongs to the technical field of polysiloxane, and discloses vinyl polysiloxane as well as a preparation method and application thereof. The method comprises the following steps: (1) mixing 100 to 200 parts of DMC (dimethylcyclosiloxane) with 20 to 60 parts of methyl vinyl cyclosiloxane, and performing vacuum dewatering treatment to obtain a dewatered mixed monomer; (2) mixing the dewatered mixed monomer with 1 to 20 parts of an end-capping reagent, heating to 100 to 110 DEG C, adding 0.1 to 5 parts of a temporary catalyst, heating to 110 to 115 DEG C, performing heat preservation reaction for 1 to 3 hours, heating to 120 to 125 DEG C, performing heat preservation reaction for 3 to 5 hours, and continuously heating to 130 to 135 DEG C for reaction for 1 to 3 hours, so as toobtain a reaction product; (3) performing subsequent treatment on the reaction product, so as to obtain the vinyl polysiloxane, wherein the part is weight part. The method disclosed by the invention is simple, low in cost and high in monomer conversion rate, and is applied to synthesis and modification of silicone rubber and silicon resin and preparation of a releasing agent.

Description

technical field [0001] The invention belongs to the technical field of polysiloxane, relates to a method for efficiently preparing polysiloxane, in particular to a high-efficiency synthesis method of vinyl polysiloxane and the vinyl polysiloxane prepared by the method, The vinyl polysiloxane is used to prepare release agent products and silicone rubber. technical background [0002] Polysiloxane is based on Si-O-Si as the main chain, and the side chain is connected with organic groups (methyl, phenyl, ethyl, vinyl, etc.). This organic-inorganic structure endows it with excellent chemical stability, high flexibility, excellent high and low temperature resistance, weather resistance, lubricity, and low surface tension. It is widely used in waterproof materials and self-cleaning Materials, housing materials, electronic devices and other fields are the basic materials of common silicone products such as silicone oil, silicone rubber, silicone resin, etc., and have extensive and...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/06D21H19/32C08L83/07
CPCC08G77/06C08G77/20C08L83/04D21H19/32
Inventor 胡继文尚颖超涂园园林树东魏彦龙黄振祝欧明
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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