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Preparation method of novel silicane fire retardant

A flame retardant and silane technology, which is applied in the field of preparation of new silane flame retardants, can solve the problems of high preparation cost, endanger the health of operators, product residues, etc. The effect of unaffected performance and moderate reaction temperature

Inactive Publication Date: 2015-11-11
SHANGHAI PUYANG NEW MATERIAL TECH CO LTD
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Problems solved by technology

[0002] At present, in the synthesis process of the existing silane flame retardants, the active reaction raw materials used are phosphorus-containing compounds. The health of the personnel, and the preparation method is complex and the preparation cost is relatively high; in addition, the final product of the preparation method is a mixture that is not easy to separate, which will contain product residues of unknown components, which will affect the final performance of silane flame retardants. Performance, such as adverse effects on thermal stability, water absorption, mechanical properties, oxidation resistance, etc. of silane flame retardants

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  • Preparation method of novel silicane fire retardant

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[0015] The preparation method of silane flame retardant of the present invention comprises the following steps:

[0016] 1) Using siloxane as a raw material, dissolve siloxane in an organic solvent, add potassium hydroxide catalyst, stir evenly, heat and reflux for 15-30 minutes to obtain a sodium complex;

[0017] 2) After cooling slightly, add phosphorus trichloride to replace, and then reflux for 25-40 minutes to convert the sodium complex into a phosphorus complex;

[0018] 3) After cooling, filter, concentrate the filtrate, and then cool to -5°C, white crystals are formed;

[0019] 4) Rinse the white crystals obtained in step 3) with methanol, and then dry them in a vacuum oven at room temperature for 0.6-1.5 hours to obtain the silane flame retardant.

[0020] Wherein, the weight fraction of each component is: 10-36 parts of siloxane, 0.06-6.8 parts of organic solvent, 5-16 parts of potassium hydroxide, and 0.02-1.7 parts of phosphorus trichloride. The siloxanes are vi...

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Abstract

The invention relates to a preparation method of novel silicane fire retardant. The method includes the following steps of firstly, dissolving siloxane in organic solvent with the siloxane as raw materials, adding a potassium hydroxide catalyst, and conducting heating reflux for 15-30 minutes after the mixture is stirred to be uniform so that sodium complex can be obtained; secondly, adding phosphorus trichloride for substitution after the phosphorus trichloride is slightly cooled, conducting reflux again for 25-40 minutes, and converting the phosphorus trichloride into phosphorus complex; thirdly, conducting filtering after cooling, cooling filtrate to -5 DEG C after the filtrate is concentrated, and generating white crystals; fourthly, flushing the white crystals obtained in the third step through methyl alcohol, placing the white crystals in a room-temperature vacuum oven to be dried for 0.6-1.5 hours, and obtaining the silicane fire retardant. Compared with the prior art, the reaction condition is gentle, the reaction temperature is moderate, the obtained finished product can be quite easily separated from a reaction system, the flame retardant property and the oxidation resistance can be effectively improved, and meanwhile the mechanics performance, the insulating performance and the heat resistance are not influenced.

Description

[technical field] [0001] The invention relates to the technical field of flame retardants, in particular to a preparation method of a novel silane flame retardant. [Background technique] [0002] At present, in the synthesis process of the existing silane flame retardants, the active reaction raw materials used are phosphorus-containing compounds. The health of the personnel, and the preparation method is complex and the preparation cost is relatively high; in addition, the final product of the preparation method is a mixture that is not easy to separate, which will contain product residues of unknown components, which will affect the final performance of silane flame retardants. Use performance, such as thermal stability, water absorption, mechanical properties, anti-oxidation properties, etc. of silane flame retardants have adverse effects. Therefore, it will be of great significance to provide a method for preparing a silane flame retardant that can reduce the negative i...

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Application Information

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IPC IPC(8): C09K21/12C07F9/06
Inventor 刘雪杏
Owner SHANGHAI PUYANG NEW MATERIAL TECH CO LTD
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