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Preparation method of narrow molecular weight distribution polysiloxane

A technology of narrow molecular weight distribution and polysiloxane, which is applied in the field of preparation of narrow molecular weight distribution polysiloxane and narrow molecular weight distribution polysiloxane, which can solve the problems of wide molecular weight distribution and achieve adjustable reaction temperature and short reaction time. controllable effect

Active Publication Date: 2014-08-13
陕西翱翔天宇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] In order to solve the problem of wide molecular weight distribution of existing polysiloxanes, the present invention provides a preparation method of polysiloxanes with narrow molecular weight distributions to obtain extremely narrow polysiloxanes with molecular weight distribution (Mw / Mn≤1.2), And the molecular weight is adjustable from 3000 to 30000

Method used

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  • Preparation method of narrow molecular weight distribution polysiloxane
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  • Preparation method of narrow molecular weight distribution polysiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The preparation method of the narrow molecular weight distribution polysiloxane in the embodiment of the present invention, its step is: add VD to the ampule bottle of 20ml 3 Monomer 1.6ml solvent monomer, then add 1.4ml of freshly distilled tetrahydrofuran, stir for about 20min, keep the temperature in an ice-water bath at a constant temperature, add 0.46ml of n-butyllithium solution, and after the predetermined reaction time is reached, precipitate out the polymer with anhydrous ice methanol things.

[0021] figure 1 It is the FT-IR spectrum of the narrow molecular weight distribution polysiloxane in Example 1 of the present invention. figure 2 It is the NMR image of the narrow molecular weight distribution polysiloxane in Example 1 of the present invention. image 3 The curve marked as 1 is the GPC / RI diagram of the narrow molecular weight distribution polysiloxane in the examples of the present invention. Figure 4 The curve marked as 1 in the middle is the GPC / ...

Embodiment 2

[0024] The preparation method of the narrow molecular weight distribution polysiloxane in the embodiment of the present invention, its step is: add VD to the ampule bottle of 20ml 3 Monomer 1.6ml solvent monomer, then add 1.4ml freshly distilled tetrahydrofuran, stir for about 20min, keep the temperature in an ice-water bath at a constant temperature, add 0.31ml of n-butyllithium solution, after the predetermined reaction time is reached, precipitate out the polymer with anhydrous ice methanol things.

[0025] image 3 The curve marked as 2 is the GPC / R1 graph of the narrow molecular weight distribution polysiloxane in the examples of the present invention. Figure 4 The curve marked as 2 in the middle is the GPC / LS chart of the narrow molecular weight distribution polysiloxane in the embodiment of the present invention.

[0026] After testing, the prepared polysiloxane has a molecular weight of 10000 and a distribution of 1.06.

Embodiment 3

[0028] The preparation method of the narrow molecular weight distribution polysiloxane in the embodiment of the present invention, its step is: add VD to the ampule bottle of 20ml 3 Monomer 1.6ml solvent monomer, then add 1.4ml freshly distilled tetrahydrofuran, stir for about 20min, keep the temperature in an ice-water bath at a constant temperature, add 0.25ml of n-butyllithium solution, after the predetermined reaction time is reached, precipitate out the polymer with anhydrous ice methanol thing.

[0029] image 3 The curve marked as 3 is the GPC / RI diagram of the narrow molecular weight distribution polysiloxane in the examples of the present invention. Figure 4 The curve marked as 3 is the GPC / LS chart of the narrow molecular weight distribution polysiloxane in the examples of the present invention.

[0030] After testing, the molecular weight of the prepared polysiloxane was 15000, and the distribution was 1.09.

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Abstract

The invention relates to a preparation method of narrow molecular weight distribution polysiloxane. The method is characterized in that extremely narrow molecular weight distribution (Mw / Mn is not greater than 1.2) with the adjustable molecular weight of 3000-30000 is prepared through ring-opening polymerization by changing a feeding ratio of 1,3,5-trivinyl-1,3,5-trimethylcyclotrisiloxane (VD3) to an anionic initiator, adjusting the reaction time and the reaction temperature, controlling the monomer conversion rate and combining the advantages of anionic ring-opening polymerization. The preparation method concretely comprises the following steps: adding 0.5-2.0ml of a solvent monomer VD3 monomer to a 20ml ampule, adding 1.4ml of new distilled tetrahydrofuran, stirring for about 20-30min, allowing the temperature to be constant in an ice water bath, adding 0.1-0.6ml of an n-butyl lithium solution, and precipitating a polymer by using anhydrous cold methanol a predetermined reaction time later. The method is characterized by adjustable monomer-to-initiator feeding ratio, adjustable reaction temperature and controllable reaction time in the anionic ring-opening polymerization process, so extremely narrow molecular weight distribution and adjustable molecular weight polysiloxane can be obtained by controlling the monomer conversion rate.

Description

technical field [0001] The present invention relates to a polysiloxane, especially a narrow molecular weight distribution polysiloxane, and also relates to a preparation method of the narrow molecular weight distribution polysiloxane. Background technique [0002] Polysiloxane is used as the base material for the production of high temperature vulcanized silicone rubber (HTV), and is mixed with crosslinking agent, reinforcing agent, colorant, structure control agent, anti-aging agent, etc. to prepare high temperature vulcanized silicone rubber raw rubber; Vinyl silicone oil is used to make liquid silicone rubber, which is the main material for injection thermoforming silicone rubber; vinyl silicone oil reacts with polyurethane, acrylic and other organic materials to make it with better performance (weather resistance, aging resistance, UV resistance) , enhanced toughness, etc.) new materials (such as coatings are important raw materials for the production of various coatings...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/06
Inventor 孔杰周冬凌君骆春佳于震黄勇
Owner 陕西翱翔天宇新材料科技有限公司
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