Aminomethyl phenyl phosphinic acid and preparation method thereof

A technology of aminomethylphenylphosphinic acid and chloromethylphenylphosphinic acid, which is applied in the field of aminomethylphenylphosphinic acid and its preparation, can solve the problems of single raw material and oxidation into phosphoric acid, and achieve production The process is simple, the amount of addition is small, and the effect is obvious

Inactive Publication Date: 2015-07-01
泰索新材料科技(杭州)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The limitation of this method is that the raw material is single and affected by the strong reducibility of phosphinic acid. Melamine and phosphinic acid must be added at the same time, otherwise, phosphinic acid will be oxidized to phosphoric acid when heated in the air environment.

Method used

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  • Aminomethyl phenyl phosphinic acid and preparation method thereof
  • Aminomethyl phenyl phosphinic acid and preparation method thereof
  • Aminomethyl phenyl phosphinic acid and preparation method thereof

Examples

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Comparison scheme
Effect test

Embodiment 1

[0030] A preparation method of aminomethylphenylphosphinic acid, the synthesis steps are:

[0031] Heat and react hydroxymethylphenylphosphinic acid, thionyl chloride and anisole in a reaction kettle with a molar ratio of 1:1:3, the temperature of the heating reaction is 40°C, the reaction time is 3 hours, and the reaction ends Cool down to 20 DEG C and filter to obtain chloromethylphenylphosphinic acid crystals afterward, and the filter paper used for filtering is a qualitative filter paper with a pore size of 30 to 120 microns;

[0032] Chloromethylphenylphosphinic acid crystals are added to a sodium hydroxide solution with a concentration of 2wt%, and the molar ratio of sodium hydroxide to chloromethylphenylphosphinic acid is 1:1, and ammonia gas, ammonia gas When adding, the reaction pressure is 0.1MPa, and then filter again after reacting for 1 hour. The filter paper used for filtering is a qualitative filter paper with a pore size of 30-120 microns, and is washed with wa...

Embodiment 2

[0034] A preparation method of aminomethylphenylphosphinic acid, the synthesis steps are:

[0035] Heat and react hydroxymethylphenylphosphinic acid, thionyl chloride and diphenyl ether in a reaction kettle with a molar ratio of 1:1:10, the temperature of the heating reaction is 80°C, the reaction time is 6 hours, and the reaction ends Cool down to 30 DEG C and filter to obtain chloromethylphenylphosphinic acid crystals afterward, and the filter paper used for filtering is a qualitative filter paper with a pore size of 30 to 120 microns;

[0036] Chloromethylphenylphosphinic acid crystals are added to a concentration of 50wt% sodium hydroxide solution, the molar ratio of sodium hydroxide to chloromethylphenylphosphinic acid is 1.1:1, feed ammonia, ammonia When adding, the reaction pressure is 0.5MPa, and then filter again after reacting for 8 hours. The filter paper used for filtering is qualitative filter paper with a pore size of 30-120 microns, and is washed with water for ...

Embodiment 3

[0038] A preparation method of aminomethylphenylphosphinic acid, the synthesis steps are:

[0039] The hydroxymethylphenylphosphinic acid, thionyl chloride and chloromethyl ether with a molar ratio of 1:1:5 are heated and reacted in a reaction kettle, the temperature of the heated reaction is 50°C, and the reaction time is 5 hours. After the end, cool down to 25°C and filter to obtain chloromethylphenylphosphinic acid crystals. The filter paper used for filtering is a qualitative filter paper with a pore size of 30 to 120 microns;

[0040]Chloromethylphenylphosphinic acid crystals are added to a concentration of 5wt% sodium hydroxide solution, the mol ratio of sodium hydroxide to chloromethylphenylphosphinic acid is 1.2:1, feed ammonia, ammonia When adding, the reaction pressure is 0.3MPa, and then filter again after reacting for 3 hours. The filter paper used for filtering is qualitative filter paper with a pore size of 30-120 microns, and is washed with water for 5 times unt...

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Abstract

The invention relates to aminomethyl phenyl phosphinic acid and a preparation method thereof, and particularly provides aminomethyl phenyl phosphinic acid prepared by carrying out halogenation reaction and ammonolysis reaction of hydroxymethyl phenyl phosphinic acid successively, and a preparation method thereof. The preparation method disclosed by the invention comprises the following steps: heating and reacting hydroxymethyl phenyl phosphinic acid, sulfoxide chloride and ether in a reaction kettle at a certain mol ratio at first, preparing chloromethyl phenyl phosphinic acid after completing reaction, and carrying out ammonolysis reaction by introducing ammonia gas in a sodium hydroxide solution so as to obtain the aminomethyl phenyl phosphinic acid. The aminomethyl phenyl phosphinic acid disclosed by the invention is high in content, good in fire resistance and high in molecular activity; when the aminomethyl phenyl phosphinic acid is added into other materials, the advantages of being low in addition amount, good in compatibility and fire resistance and the like can be realized; and furthermore, the performance of a fire-resistant material is further improved.

Description

technical field [0001] The invention belongs to the technical field of novel flame retardant materials, and relates to an aminomethylphenylphosphinic acid and a preparation method thereof, in particular to a method for sequentially performing halogenation reaction and ammoniation reaction on hydroxymethylphenylphosphinic acid The prepared aminomethylphenylphosphinic acid and its preparation method. Background technique [0002] With the development of China's synthetic material industry and the continuous expansion of application fields, flame retardants have broad market prospects in various fields such as chemical building materials, electronic appliances, transportation, aerospace, daily furniture, interior decoration, and basic necessities of life. With people's increasing awareness of environmental protection, safety and health, countries around the world have begun to focus on research, development and application of environmentally friendly flame retardants, and have ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C08K5/5313
Inventor 毛惠敏陆炅石建华
Owner 泰索新材料科技(杭州)有限公司
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