A kind of preparation method of high molecular weight poly(methylethyl-methylvinyl)siloxane

A technology of tetramethyltetravinylcyclotetrasiloxane and tetramethyltetraethylcyclotetrasiloxane, which is applied in the field of polysiloxane preparation, can solve the complex preparation process and the ring-opening rate of comonomers different, harsh reaction conditions, etc., to achieve the effect of simple polymerization process, low glass transition temperature, and controllable molecular weight

Active Publication Date: 2019-01-29
SHANDONG UNIV
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  • Abstract
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Problems solved by technology

[0005] Although the above-prepared polysiloxane has a low glass transition temperature (Tg) and does not crystallize at low temperatures, due to the problem of different ring-opening rates of the comonomers, the reaction conditions required for the preparation of random copolymers are relatively harsh. , the preparation process is complex

Method used

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  • A kind of preparation method of high molecular weight poly(methylethyl-methylvinyl)siloxane
  • A kind of preparation method of high molecular weight poly(methylethyl-methylvinyl)siloxane
  • A kind of preparation method of high molecular weight poly(methylethyl-methylvinyl)siloxane

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Effect test

Embodiment 1

[0028] 200g tetramethyltetraethylcyclotetrasiloxane (D 4 Me,Et ), 0.02g tetramethyltetravinylcyclotetrasiloxane (D 4 Vi ) and 0.169g of octamethyltrisiloxane were added to the 2 In the reactor with conduit and thermometer, dehydrate at 60°C for 2h under reduced pressure, then blow dry nitrogen and raise the temperature to 130°C, add 2.00g of potassium hydroxide silicon alkoxide to start polymerization, and react for 2h. After the polymerization reaction is completed, continue to heat up to 200°C, remove small molecular low boilers in the material under the condition of a vacuum degree of less than or equal to 100Pa, for 1h, cool to room temperature and discharge, and obtain high molecular weight poly(methylethyl) - methylvinyl) siloxane. Measure the vinyl content, molecular weight and its distribution and volatile content of the product, and the results are listed in Table 1; the DSC of high molecular weight poly(methyl ethyl-methyl vinyl)siloxane is listed in figure 1 . ...

Embodiment 2

[0031] 200g tetramethyltetraethylcyclotetrasiloxane (D 4 Me,Et ), 0.293g tetramethyltetravinylcyclotetrasiloxane (D 4 Vi ) and 0.169g of octamethyltrisiloxane were added to the 2In the reactor with conduit and thermometer, dehydrate at 60°C for 2h under reduced pressure, then blow dry nitrogen and raise the temperature to 130°C, add 2.00g of potassium hydroxide silicon alkoxide to start polymerization, and react for 2h. After the polymerization reaction is completed, continue to heat up to 200°C, remove small molecular low boilers in the material under the condition of a vacuum degree of less than or equal to 100Pa, for 1h, cool to room temperature and discharge, and obtain high molecular weight poly(methylethyl) - methylvinyl) siloxane. The vinyl content, molecular weight and its distribution and volatile content of the product were measured, and the results are listed in Table 1.

Embodiment 3

[0033] 200g tetramethyltetraethylcyclotetrasiloxane (D 4 Me,Et ), 20g tetramethyltetravinylcyclotetrasiloxane (D 4 Vi ) and 0.169g of octamethyltrisiloxane were added to the 2 In the reactor with conduit and thermometer, dehydrate at 60°C for 2h under reduced pressure, then blow dry nitrogen and raise the temperature to 130°C, add 2.00g of potassium hydroxide silicon alkoxide to start polymerization, and react for 2h. After the polymerization reaction is completed, continue to heat up to 200°C, remove small molecular low boilers in the material under the condition of a vacuum degree of less than or equal to 100Pa, for 1h, cool to room temperature and discharge, and obtain high molecular weight poly(methylethyl) - methylvinyl) siloxane. The vinyl content, molecular weight and its distribution and volatile content of the product were measured, and the results are listed in Table 1.

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Abstract

The invention relates to a preparation method of high-molecular-weight poly(methyl ethyl-methyl vinyl) siloxane. The method comprises steps as follows: (1) tetramethyl tetraethyl cyclotetrasiloxane, tetramethyl tetravinyl cyclotetrasiloxane and an end capping agent are mixed, a catalyst is added, and the mixture is subjected to a polymerization reaction for 1-4 h at the temperature of 80-180 DEG C; (2) after the polymerization reaction ends, the mixture is heated to 180-220 DEG C, micromolecular low-boiling-point substances in a material are removed in a vacuum state, the material is discharged after being cooled to the room temperature, and high-molecular-weight poly(methyl ethyl-methyl vinyl) siloxane is obtained. The high-molecular-weight poly(methyl ethyl-methyl vinyl) siloxane product is stable, the glass-transition temperature (Tg) is low, crystals are not formed at the low temperature, the polymerization process is simple, no solvent is required, the high-molecular-weight poly(methyl ethyl-methyl vinyl) siloxane can be obtained in shorter reaction time by strictly controlling the reaction condition, the yield is high, the molecular weight is controllable, the aftertreatment is simple, and large-scale production is facilitated.

Description

technical field [0001] The invention belongs to the field of preparation technology of macromolecular compounds, in particular to a preparation method of high molecular weight poly(methylethyl-methylvinyl)siloxane. Background technique [0002] Silicone rubber has many unique and excellent properties, such as high and low temperature resistance, insulation, water repellency, good weather resistance, good air permeability and low compression deformation rate, making it widely used in aerospace, chemical industry, machinery, textile, construction, transportation, medical It has been widely used in medicine, agriculture and other fields. [0003] As an applied material, the use value of rubber lies in its elasticity. However, with the advancement of human science and technology and the deepening of space exploration, especially in ultra-cold-resistant environments such as space exploration, it is necessary to use rubber products that can maintain elasticity and sealing perform...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C08G77/06C08G77/34
CPCC08G77/06C08G77/20C08G77/34
Inventor 冯圣玉高立娟马德鹏
Owner SHANDONG UNIV
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