Preparation method of functionalized terminal group polysiloxane

A technology of hydroxyl-terminated polysiloxane and polysiloxane, which is applied in the field of polysiloxane synthesis, can solve problems such as high energy consumption, unstable product quality, and difficult control of the reaction process, and achieve low energy consumption and good performance. Industrial application prospects, production of more controllable effects

Inactive Publication Date: 2014-09-10
石振东
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction process of these methods is not easy to control, the product quality is unstable, and the energy consumption is large at the same time.
In addition, the large-scale synthesis of various types of functionalized polysiloxanes has not been reported yet.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] An amino polysiloxane, its raw materials and dosage are as follows: D43 mol, sodium hydroxide 0.1 mol, deionized water 0.3 mol, ethylenediamine 0.3 mol, and γ-aminopropyl triethoxysilane 1 mol.

[0040] The preparation method includes the following steps: adding D4 and sodium hydroxide to the reactor, stirring at 60°C for 1 h, then adding deionized water and ethylenediamine, keeping the temperature at 60°C and stirring and reacting for 1 h to obtain hydroxyl polysilicon Add γ-aminopropyltriethoxysilane and keep stirring at 60℃ for 4 hours to obtain a viscous, clear and transparent liquid. The liquid is neutralized by acid solution, filtered, and vacuumed to obtain aminopolysiloxane. alkyl.

Embodiment 2

[0042] An amino polysiloxane, its raw materials and dosage are: D4 3 mol, sodium hydroxide 0.25 mol, deionized water 0.05 mol, 3,3'-diaminodipropylamine 0.4 mol, γ-aminopropyltrimethyl 0.1 mol of oxysilane.

[0043] The preparation method includes the following steps: add D4 and sodium hydroxide into the reactor, stir at 80°C for 0.5 h, then add deionized water, 3,3'-diaminodipropylamine, keep stirring at 80°C After reacting for 1 h, hydroxypolysiloxane is obtained, then γ-aminopropyltrimethoxysilane is added, and the reaction is kept at 80°C while stirring for 5 h. A viscous, clear and transparent liquid is obtained. The liquid is neutralized by acid solution, filtered, and pumped. Vacuum to obtain amino polysiloxane.

Embodiment 3

[0045] An amino polysiloxane whose raw materials and dosage are: D3 3 mol, sodium hydroxide 0.1 mol, deionized water 0.006 mol, ethylene diamine 0.2 mol, and γ-aminopropyl triethoxysilane 0.012 mol.

[0046] The preparation method includes the following steps: adding D3 and sodium hydroxide to the reactor, stirring at 40°C for 2 h, then adding deionized water and ethylenediamine, keeping the temperature at 40°C and stirring and reacting for 5 min to obtain hydroxyl polysilicon Oxyane, then add γ-aminopropyltriethoxysilane, keep at 40℃ and keep stirring for 3 hours to obtain a viscous, clear and transparent liquid. The liquid is neutralized by acid solution, filtered, and vacuumed to obtain aminopolysiloxane alkyl.

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PUM

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Abstract

The invention discloses a preparation method of functionalized terminal polysiloxane, including the preparation method of hydroxyl terminal polysiloxane, the steps are as follows: stirring and reacting methylcyclosiloxane, alkali, water and amine; Neutralize acid, filter or wash with water until neutral, then vacuumize. The preparation method of the functionalized polysiloxane with non-hydroxyl functionalized end group, the steps are as follows: stirring and reacting methylcyclosiloxane, alkali, water and amine; adding silane coupling agent and stirring reaction; And, filter, vacuumize. The raw materials used in the present invention are all conventional materials, the reaction conditions are mild, neither high temperature nor inert gas protection is needed, the reaction safety is good, and the cost is greatly saved at the same time. The preparation method of the present invention has simple reaction device, simple and easy reaction process, easy realization, high efficiency, short preparation time, low energy consumption and low cost.

Description

technical field [0001] The invention relates to the synthesis of polysiloxane, in particular to a preparation method of functionalized terminal polysiloxane. Background technique [0002] Polyorganosiloxane molecules have the following characteristics: (1) good electrical insulation, flame retardancy, and weather resistance; (2) ideal physiological and chemical inertness, non-toxic, and non-polluting ecological environment; (3) glass transition temperature Low temperature, high resistance, good low temperature performance, low high temperature rheology; (4) easy spreading film forming, defoaming, hydrophobicity and lubricity caused by low surface tension. It can form block copolymers with other polymer materials, such as the use of polyorganosiloxane emulsion for padding of fabrics, which can not only effectively isolate fibers, avoid direct contact between fibers, but also improve the friction coefficient of the fiber surface Reduced, so that the fibers are easy to slide a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/16C08G77/26C08G77/20C08G77/28C08G77/08
Inventor 石振东
Owner 石振东
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