A kind of synthetic method of flame retardant intermediate methylphosphonphthalein dichloride

A kind of technology of methyl phosphine, synthesis method

Active Publication Date: 2021-04-27
四川省乐山市华莱利科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] As we all know, sulfonyl chloride is widely used as an oxidizing agent due to its high oxidation efficiency and the easy recycling of the by-product thionyl chloride, but there is no report on the synthesis of methylphosphinephthalein dichloride from the oxidation of methylphosphine dichloride

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  • A kind of synthetic method of flame retardant intermediate methylphosphonphthalein dichloride

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Embodiment 1

[0025] This embodiment proposes a kind of synthetic method of flame retardant intermediate methylphosphonphthalein dichloride, comprising the following steps:

[0026] A. Add sulfuryl chloride in a sealed reactor with condenser, stirring and thermometer, and cool to 0°C in a low-temperature bath;

[0027] B. Slowly add methyl phosphine dichloride to the reaction system, the molar ratio of methyl phosphine dichloride to sulfonyl chloride is 1:0.95, keep the reaction temperature at 15°C by controlling the addition speed, and the dropping time is 1h ;

[0028] C, the addition is completed, then continue to stir and react for 1h at a temperature of 5°C;

[0029] D. After the reaction is complete, the by-product thionyl chloride is distilled out by vacuum distillation, and the fraction at 40-50°C is collected, and the vacuum degree is 20mmHg;

[0030] E. Continue to increase the distillation temperature, distill under reduced pressure to obtain methylphosphinephthalein dichloride...

Embodiment 2

[0034] This embodiment proposes a kind of synthetic method of flame retardant intermediate methylphosphonphthalein dichloride, comprising the following steps:

[0035] A. Add sulfuryl chloride in a sealed reactor with a condenser, stirring and thermometer, and cool to 3°C in a low-temperature bath;

[0036] B. Slowly add methyl phosphine dichloride to the reaction system dropwise, the molar ratio of methyl phosphine dichloride to sulfonyl chloride is 1:1.05, keep the reaction temperature at 20°C by controlling the addition speed, and the dropping time is 3h ;

[0037] C, the addition is completed, then continue to stir and react for 1h at a temperature of 0°C;

[0038] D. After the reaction is complete, the by-product thionyl chloride is distilled out by vacuum distillation, and the fraction at 40-50°C is collected, and the vacuum degree is 25mmHg;

[0039] E. Continue to increase the distillation temperature, obtain methylphosphinephthalein dichloride product by distillatio...

Embodiment 3

[0043] This embodiment proposes a kind of synthetic method of flame retardant intermediate methylphosphonphthalein dichloride, comprising the following steps:

[0044]A. Add sulfuryl chloride in a sealed reactor with a condenser, stirring and thermometer, and cool to 3°C in a low-temperature bath;

[0045] B. Slowly add methyl phosphine dichloride to the reaction system dropwise, the molar ratio of methyl phosphine dichloride to sulfonyl chloride is 1:1, keep the reaction temperature at 17°C by controlling the addition speed, and the dropping time is 2h ;

[0046] C, the addition is complete, then continue to stir and react at a temperature of 20°C for 0.5h;

[0047] D. After the reaction is complete, the by-product thionyl chloride is distilled out by vacuum distillation, and the fraction at 40-50°C is collected, and the vacuum degree is 30mmHg;

[0048] E. Continue to increase the distillation temperature, distill under reduced pressure to obtain methylphosphinephthalein d...

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Abstract

The invention discloses a method for synthesizing flame retardant intermediate methylphosphinephthalein dichloride. Slowly add methyl phosphine dichloride dropwise, keep the reaction temperature at 15-20°C, and the dropwise addition time is 1-3h; C, after the addition is complete, continue to stir and react at a temperature of 0-30°C for 0.5-1h; D, After the reaction is complete, the by-product thionyl chloride is distilled out by vacuum distillation, and the 40-50°C fraction is collected; E, continue to increase the distillation temperature, and the methylphosphinephthalein dichloride product is obtained by vacuum distillation, and the 70-80°C fraction is collected. The invention has mild reaction conditions, simple operation, low cost, no addition and generation of gas, high safety, and easy realization of industrial production, and the purity of the methylphosphinephthalein dichloride product and the by-product thionyl chloride can reach 98%. Above, the reaction yield is above 95%.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing a flame retardant intermediate, methylphosphinephthalein dichloride. Background technique [0002] Methylphosphonophthalein dichloride, also known as dichloromethylphosphine, methylphosphonodichloride, molecular formula CH 3 Cl 2 OP is an important chemical intermediate, which can be used to synthesize phosphorus-based flame retardants and phosphorus-containing Wittig reagents, and can also be used as a bifunctional phosphoramide coupling reagent to prepare phosphorus-containing copolymers with other olefin monomers . It is worth noting that methylphosphonphthalein dichloride plays an important role in the field of new phosphorus flame retardants, especially cyclic phosphate flame retardants, which are used in the fields of polyester fabrics, PC / ABS, PMMA and other materials. There are a wide range of applications. For example, Chinese pat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/42
CPCC07F9/42
Inventor 李舟齐鸿吴狄峰杨露王文刘虎
Owner 四川省乐山市华莱利科技有限公司
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