Preparation method for polysiloxane with extra high molecular weight

A technology of polyorganosiloxane and ultra-high molecular weight, which is applied in the field of preparation of polyorganosiloxane, which can solve the problems of insufficient stirring, limited molecular weight of polyorganosiloxane, and high requirements, so as to avoid partial crosslinking and Uneven heat transfer, reducing the effect of intermediate processes

Active Publication Date: 2010-03-17
GUANGZHOU TINCI MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation process has the following defects: ①The molecular weight of the prepared polyorganosiloxane is limited, and the molecular weight of the product generally does not exceed 1 million; ②The requirements for the stirring system are high, and the fluidity becomes poor with the increase of the polymer viscosity , leading to insufficient stirring, which in turn causes local overheating and cross-linking; ③The product has a high viscosity and is not easy to unload; ④The volatile content of the product is relatively high, generally greater than 1.0%

Method used

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  • Preparation method for polysiloxane with extra high molecular weight
  • Preparation method for polysiloxane with extra high molecular weight
  • Preparation method for polysiloxane with extra high molecular weight

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 18kg of dimethylcyclosiloxane into a 40L reactor, start the agitator, control the speed at 30 rpm, raise the temperature to 130°C, add 0.18g of potassium siloxanate at constant temperature to catalyze the reaction for 6.0 hours; Then, vacuumize for 4.0 hours, and control the vacuum degree to -0.080MPa; then neutralize with 0.18g of silicon-based phosphate, and raise the temperature to 170°C, pass in nitrogen and continue vacuuming for 6.0 hours; stop heating, stir and cool to room temperature, and then exit material, you can prepare ultra-high molecular weight polydimethylsiloxane.

[0031] Extract above-mentioned polydimethylsiloxane product, adopt Fourier transform infrared spectrometer to test, from figure 2 Visible, in the infrared spectral map 1020cm -1 -1090cm -1 There is an obvious characteristic absorption peak of polydimethylsiloxane.

[0032] Extract ultra-high molecular weight polydimethylsiloxane, adopt Waters 515 gel permeation chromatography system...

Embodiment 2

[0034] Add 18kg of α,ω-dihydroxypolydimethylsiloxane into a 40L reactor, start the stirrer, control the speed at 40 rpm, raise the temperature to 140°C, and add 1.8g of sodium siloxane alkoxide at constant temperature to catalyze React for 5.0 hours; under constant temperature, vacuumize for 3.0 hours, and control the vacuum degree to -0.080MPa; then neutralize with 2.5g phosphoric acid, and raise the temperature to 180°C, feed nitrogen and continue vacuuming for 5.0 hours; stop heating, stir and cool to After discharging at room temperature, ultra-high molecular weight polydimethylsiloxane can be prepared.

Embodiment 3

[0036] Add 18kg of dimethylcyclosiloxane into a 40L reactor, start the agitator, control the speed at 50 rpm, raise the temperature to 150°C, and add 5.0g of cesium siloxanolate at constant temperature to catalyze the reaction for 3.0 hours; at constant temperature Then, vacuumize for 2.0 hours, and control the vacuum degree to -0.090MPa; then use 3.2g of acetic acid to neutralize, and raise the temperature to 170°C, feed nitrogen and continue vacuuming for 4.0 hours; stop heating, stir and cool to room temperature, and discharge, that is Ultra-high molecular weight polydimethylsiloxane can be obtained.

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Abstract

The invention discloses a preparation method for polysiloxane with extra high molecular weight, comprising the steps of (1) adding dimethyl siloxane or alpha, omega-dihydroxy polydimethylsiloxane intoa reactor, stirring, controlling the rotating speed being 30 to 60 revolutions per minute, heating up to 90-160 DEG C., adding catalyzer which occupies 0.001% to 0.1% by weight of raw materials and reacting for 2.0 to 6.0 hours at constant temperature, (2) at constant temperature, vacuum-pumping for 1.0 to 4.0 hours, and controlling the vacuum degree being -0.080 to -0.10 MPa, and (3) adding neutralizing agent which occupies 0 to 0.1% by weight of raw materials, heating up to 170-180 DEG C., introducing nitrogen, vacuum-pumping for 2.0 to 6.0 hours, stopping heating, stirring, discharging after cooling to room temperature to obtain the blocky or granular hydroxyl silicone oil products with extra high molecular weight. The invention can prepare the polysiloxane with molecular weight more than 1000000.

Description

technical field [0001] The invention relates to a preparation method of polyorganosiloxane, in particular to a preparation method of ultrahigh molecular weight polyorganosiloxane. Background technique [0002] The synthesis of polyorganosiloxane mostly adopts a catalytic equilibrium process, and the equipment used is mainly a polymerization kettle. In order to obtain high-molecular-weight polyorganosiloxanes, it is mainly realized in the industry by prolonging the polymerization reaction time and de-lowering time. This preparation process has the following defects: ①The molecular weight of the prepared polyorganosiloxane is limited, and the molecular weight of the product generally does not exceed 1 million; ②The requirements for the stirring system are high, and the fluidity becomes poor with the increase of the polymer viscosity , leading to insufficient stirring, which in turn causes local overheating and cross-linking; ③The product has a high viscosity and is not easy t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/10C08G77/08C08G77/16
Inventor 杨思广张利萍林祥坚张宇王哲唐涛
Owner GUANGZHOU TINCI MATERIALS TECH
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