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Process for synthesis of polysiloxane

A technology of polysiloxane and synthesis method, which is applied in the field of polysiloxane synthesis, can solve problems such as high reaction temperature, long process flow, and difficult control, and achieve narrow molecular weight distribution, lower reaction temperature, and shorter reaction time. Effect

Active Publication Date: 2006-09-27
GUANGZHOU GBS HIGH TECH & IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the method is carried out in two steps, the product quality is unstable and difficult to control.
In addition, this synthesis method adopts ordinary heating method, usually the reaction speed is slow, the process flow is long, and the reaction temperature is high, and the temperature is not easy to control, resulting in low production efficiency and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Add 100g octamethylcyclotetrasiloxane (D 4 ), 0.02g of catalyst potassium hydroxide (KOH), 0.04ml of water, after stirring for 5min at 20°C, place the reactor in the microwave reaction field, open the microwave reaction device, and after reacting for 80min, add 0.025g of phosphoric acid to terminate the reaction. Measured under 520W microwave power, the viscosity of the polymer product is 205000mpa s, the number average molecular weight M n 21.6×10 4 , weight average molecular weight M W 32.4×10 4 , molecular weight distribution M W / M n It is 1.50, the monomer residue is 2.3%, and the product is transparent.

Embodiment 2

[0013] In the reactor with reflux condenser, add 100g dimethylsiloxane mixed ring body (DMC) (wherein the content of hexamethylcyclotrisiloxane is 1%, and the content of octamethylcyclotetrasiloxane is 85%) , the content of decamethylcyclopentasiloxane is 12% and other rings), 0.03g catalyst sodium hydroxide (NaOH), 0.02ml water, the reactor is placed in a microwave reaction field with a power of 1000W, at 25°C After stirring for 2 minutes, turn on the microwave reaction device, and after 60 minutes of reaction, add 0.04 g of sulfuric acid to terminate the reaction, and obtain transparent polysiloxane with a number average molecular weight of M n 14.6×10 4 , weight average molecular weight M W 17.4×10 4 , the residual monomer content was 4.3%.

Embodiment 3

[0015] Add 100g octamethylcyclotetrasiloxane (D 4 ), 0.04g catalyst tetramethylammonium hydroxide ((CH 3 ) 4 NOH), 0.05ml of water, after stirring at 23°C for 5min, the reactor was placed in the microwave reaction field, and the microwave reaction device was turned on with a power of 600W. After 120min of reaction, 0.06g of phosphoric acid was added to terminate the reaction to obtain the polymer product poly The siloxane has a viscosity of 172000mpa.s, a residual monomer content of 5.1%, and the product is transparent.

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Abstract

The invention discloses a process for synthesis of polysiloxane which comprises the steps of charging reactant, catalyst and water, agitating at normal temperature, reacting in the microwave reaction field for 60-120 min, and charging terminating substance, the constituents include (by weight portions) reactant 100 parts, catalyst 0.01-0.05 part, water 0.01-0.1 part, and terminating substance 0.01-0.1 part.

Description

technical field [0001] The invention belongs to the technical field of microwave synthesis, in particular to a method for synthesizing polysiloxane. Background technique [0002] Polysiloxane is a polymer synthetic material with Si-O bond as the main chain and organic groups directly connected to silicon atoms. It has many excellent physical and chemical properties, so it is widely used in electronic appliances, chemical industry, metallurgy, construction, aerospace It is widely used in many fields such as aviation and medical materials. [0003] Ring-opening polymerization using cyclosiloxane as a monomer is a commonly used method for synthesizing polysiloxane. During the polymerization process, because the alkali catalyst used in the ring-opening polymerization of cyclosiloxane is sensitive to water, under normal conditions, a small amount of water will inhibit the reaction. At present, the batch two-step process is mainly used, that is, cyclosil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06
Inventor 王跃林何慧刘莉贾德民陈献新
Owner GUANGZHOU GBS HIGH TECH & IND
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