Preparation method of phosphorus-silicon compound

A compound, phosphor-silicon technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of low product yield, difficult realization, harsh reaction conditions, etc. The effect of high yield, low cost and simple process

Inactive Publication Date: 2011-06-01
中国中化股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned preparation method has the following disadvantages: 1. the reaction conditions are harsh, and the polymerization reaction needs to be carried out under a high vacuum of 0.1-0.15mmHg, which is difficult to realize industrially; 3 days; 3. The yield of the product is not high. According to

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

Example 1 Preparation method of phosphorous silicon compound A1

The reaction equation is as follows, where n=6:

In a 500ml three-necked flask equipped with stirring, high-efficiency reflux condenser and thermometer, 221.2g (1.714mol) of dimethyldichlorosilane and 248.2g (2mol) of dimethyl methylphosphonate were added at room temperature and under nitrogen protection. The reaction process was controlled by the following gradual heating method: 30-35°C for 5 hours, 1 hour to 90°C for 2 hours, 0.5 hour to 120°C for 6 hours, 0.5 hour to 190°C for 2 hours. At this time, no more chloromethane gas escaped, and the reaction was completed.

Cool down to below 120°C and discharge. A colorless viscous liquid is obtained, which solidifies into a solid at room temperature, weighs 292 grams, and has a yield of about 98% (calculated based on dimethyl methylphosphonate). It is a phosphorous silicon compound A1.

Freezing point: 30℃

Elemental analysis: carbon 25.2%, oxygen 33.6%, phosphorus 2...

Example Embodiment

Example 2 Preparation method of phosphorus silicon compound A2

The reaction equation is as follows, where n=40:

In a 500ml three-necked flask equipped with stirring, high-efficiency reflux condenser and thermometer, 258.1 g (2 moles) of dimethyldichlorosilane and 248.2 g (2 moles) of dimethyl methylphosphonate were added at room temperature and under nitrogen protection. The reaction process is controlled by the following gradual heating method: 30-35°C for 5 hours, 1 hour to 90°C for 2 hours, 0.5 hour to 120°C for 2 hours, 0.5 hour to 220°C for 20 hours. At this time, no more chloromethane gas escaped, and the reaction was completed.

Cool down to 120°C and discharge. A colorless viscous liquid is obtained, which solidifies into a solid at room temperature, weighs 297 grams, and has a yield of about 98% (calculated based on dimethyl methylphosphonate). It is a phosphorus silicon compound A2.

Freezing point: 30℃

Elemental analysis: carbon 24.6%, oxygen 32.8%, phosphorus 21.0...

Example Embodiment

Example 3 Preparation method of phosphorus silicon compound A3

The reaction equation is as follows, where n=1500:

In a 500ml three-necked flask equipped with stirring, high-efficiency reflux condenser and thermometer, 258.1 g (2 moles) of dimethyldichlorosilane and 248.2 g (2 moles) of dimethyl methylphosphonate were added at room temperature and under nitrogen protection. The reaction process is controlled by the following gradual heating method: 30-35°C for 5 hours, 1 hour to 90°C for 2 hours, 0.5 hour to 120°C for 2 hours, 0.5 hour to 220°C for 20 hours. At this time, no more chloromethane gas escaped, and the reaction was completed.

Cool down to 150°C and discharge. A colorless viscous liquid is obtained, which solidifies into a solid at room temperature, weighs 301 grams, and has a yield of about 99% (calculated based on dimethyl methylphosphonate). It is a phosphorous silicon compound A3.

Freezing point: 30℃

Elemental analysis: carbon 23.7%, oxygen 31.6%, phosphorus 2...

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Abstract

The invention discloses a preparation method of a phosphorus-silicon compound which is shown in the general formula (1) disclosed in the specification. The method comprises: phosphate and chlorosilane are utilized to be subjected to direct polycondensation at the atmospheric pressure in one step so as to obtain the target product with high yield. By adjusting the molar ratio of the phosphate to the chlorosilane, the degree of polymerization of the product can be controlled. The phosphorus-silicon compound can be used as a fire retardant and used in macromolecular materials such as plastics and rubbers. In the formula (1), R1 represents C1-C4 alkyl; R2 represents C1-C4 alkyl, C1-C4 alkoxy or H; R3 represents C1-C4 alkyl or aryl; and n represents an integer within a range of 2-2000.

Description

technical field The invention belongs to the field of organic synthesis and relates to the preparation of functional polymer auxiliary chemicals. Specifically relates to a preparation method of a phosphorus silicon compound. Background technique Phosphorus-silicon compound is a P-O-Si type copolymer compound. On the main chain, phosphorus and silicon are separated by oxygen elements. The structure is shown in the general formula (1): Where: R 1 Each independently represents C 1 -C 4 Alkyl; R 2 Each independently represents C 1 -C 4 Alkyl, C 1 -C 4 Alkoxy or H; R 3 Each independently represents the same or different C 1 ~C 4 Alkyl or aryl; n represents an integer from 2 to 2000. As flame retardants, the above compounds can be widely used in polycarbonate, PC / ABS, PET, nylon and other polymer materials. The method for preparing the phosphorus silicon compound shown in general formula (1) in the prior art is disclosed in Phosphorus, Sulfur, and Silicon, 1992, ...

Claims

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Application Information

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IPC IPC(8): C07F9/40C08G77/30C08G79/04
Inventor 魏峰刘冬雪刘博徐龙鹤李建华姚齐
Owner 中国中化股份有限公司
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