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Preparation method for synthesizing polysiloxane neutralizing agent by using alkaline process

A technology of polysiloxane and terminal siloxane, which is applied to the preparation of alkali-synthesized polysiloxane neutralizer and the preparation field of polysiloxane neutralizer, can solve the problem of inability to obtain end-capped products, neutralization Long time, poor compatibility and other problems, to achieve the effects of easy promotion and industrialization, shortened neutralization time, and simple preparation process

Inactive Publication Date: 2015-03-04
兆舜科技(广东)有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phosphoric acid can be neutralized with basic metal catalysts to form a buffer system, even if it is slightly excessive, it will not significantly affect the stability of polysiloxane, but phosphoric acid still exists in the problem of poor compatibility of polysiloxane as a neutralizing agent, which also leads to The neutralization time is too long; on the other hand, the water contained in phosphoric acid will also participate in the end-capping reaction of polysiloxane to varying degrees, resulting in the inability to obtain the expected end-capping product; Tetrasiloxane reacts with phosphoric acid at 170-180°C to continuously remove the generated water to obtain a silicon-based phosphate mixture, but when low molar mass polysiloxane (or cyclosiloxane) reacts with phosphoric acid, Difficult to trigger at high temperature and difficult to control after triggering

Method used

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  • Preparation method for synthesizing polysiloxane neutralizing agent by using alkaline process
  • Preparation method for synthesizing polysiloxane neutralizing agent by using alkaline process

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 100 parts of phosphoric acid with a mass fraction of 88% and 900 parts of hydroxyl-terminated linear products in the flask, start stirring and heat up at a stirring speed of 220rpm, control the temperature at 110°C to dehydrate until transparent, and dehydrate for 12 minutes to obtain silicon-based phosphoric acid Esters, the viscosity of silicon-based phosphate was measured with a Brookfield viscometer.

[0028] The prepared silicon-based phosphate was neutralized with dimethylsiloxane, and the time required for neutralization was recorded, and 10 mg of dimethylsiloxane was weighed for thermogravimetric testing.

Embodiment 2

[0030] Add 10 parts of phosphoric acid with a mass fraction of 85% and 110 parts of hydroxyl-terminated linear products in the flask, start stirring and heat up at a stirring speed of 200 rpm, control the temperature at 100°C to dehydrate until transparent, and dehydrate for 20 minutes to obtain silyl phosphoric acid Esters, the viscosity of silicon-based phosphate was measured with a Brookfield viscometer.

[0031] The prepared silicon-based phosphate was neutralized with dimethylsiloxane, and the time required for neutralization was recorded, and 10 mg of dimethylsiloxane was weighed for thermogravimetric testing.

Embodiment 3

[0033] Add 100 parts of phosphoric acid with a mass fraction of 98% and 600 parts of hydroxyl-terminated linear products in the flask, start stirring to raise the temperature, the stirring speed is 250rpm, control the temperature at 120°C to dehydrate until transparent, and the dehydration time is 8 minutes to prepare silicon-based phosphoric acid Esters, the viscosity of silicon-based phosphate was measured with a Brookfield viscometer.

[0034] The prepared silicon-based phosphate was neutralized with dimethylsiloxane, and the time required for neutralization was recorded, and 10 mg of dimethylsiloxane was weighed for thermogravimetric testing.

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Abstract

The invention relates to a preparation method for synthesizing a polysiloxane neutralizing agent, and particularly relates to the preparation method for synthesizing the polysiloxane neutralizing agent by using an alkaline process. The neutralizing agent can be used for neutralizing dimethyl siloxane different in viscosity. The preparation method comprises the following detailed steps: adding phosphoric acid and hydroxyl blocked siloxane which has dimethyl siloxane links into a reaction container, stirring and heating, controlling the temperature and dehydrating until the mixture is transparent, wherein silicon-based phosphate with different viscosities can be prepared by regulating the dehydration time. The silicon-based phosphate is used as the neutralizing agent for alkaline-process polymerization, and the neutralization time is shortened by 65%-95% in comparison with the conventional neutralization time; moreover, the preparation method is simple in preparation process, convenient to operate and easy to popularize and industrialize, also has an excellent neutralization effect and can be used for remarkably improving the thermal stability of polysiloxane.

Description

technical field [0001] The invention relates to the field of organosilicon, in particular to a method for preparing a polysiloxane neutralizing agent, in particular to a method for preparing a polysiloxane neutralizing agent synthesized by an alkali method, and the neutralizing agent can be used to neutralize different viscosities Methylsiloxane. Background technique [0002] In 1949, Corning Glass Company of the United States invented the method of polymerizing cyclic or short-chain linear polysiloxanes into high molecular polysiloxanes under the catalysis of basic catalysts. This method is widely used in the synthesis of various polysiloxanes. Commonly used basic catalysts include: sodium hydroxide, potassium hydroxide, cesium hydroxide and lithium hydroxide, and temporary catalysts tetramethylammonium hydroxide, tetra-n-butylphosphorous hydroxide and their silicon alkoxides. Temporary catalysts can be deactivated by thermal decomposition after polymerization, while alkal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/30C08G77/06
Inventor 黄永军刘金明尹邦志黄献文
Owner 兆舜科技(广东)有限公司
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