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2-carboxyethylphenylphisphinic acid flame-proof agent production method

A technology of phosphinic acid and carboxyethylbenzene, which is applied in the production of 2-carboxyethylphenylphosphinic acid flame retardants and the field of preparation of flame retardants, can solve the problem that industrial production cannot be realized and technology is difficult to realize , Long process flow and other issues, to achieve the effect of reducing the release of corrosive toxic gases and smoke, simple process and high melting point

Inactive Publication Date: 2007-04-25
云南泰京化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, both of these two flame retardants need to be oxidized by an oxidant to obtain the target compound, and compared with other flame retardants, the process is long and the cost is high
The flame retardants numbered 1, 3, 5, and 6 are all prepared by adding unsaturated organic acids to phosphorus-containing dibasic acids, and the basic raw materials of flame retardant 3 are o-phenylphenol, phosphorus trichlorid

Method used

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Examples

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Effect test

Embodiment 1

[0055] 1. Synthesis of phenylphosphorous dichloride-DCPP

[0056] (a) press pcl 3 :Alcl 3 : The mol ratio of benzene=1.5: 0.5: 0.8, first pcl 3 Put into the reaction kettle, then put into Alcl 3 , start the mixer, and heat up to reflux at the same time;

[0057] (b) Add the benzene of the above-mentioned ratio dropwise, and control the drop to finish within 4 hours, the temperature is constant at 80° C., and absorb a large amount of HCl gas generated during the dropwise addition with water to obtain a by-product—hydrochloric acid;

[0058] (c) Cool down the reacted material to 60°C, put it into the extraction kettle, and add the complexing agent Nacl with a particle size of 120 objects in the weight ratio of extract: Nacl=5:1 to carry out the first extraction, and the temperature is controlled at 50°C, after stirring for 1 hour, let it stand for 30 minutes, collect the extracted upper layer material liquid, and pump the material liquid into the storage tank;

[0059] (d) ...

Embodiment 2

[0075] 1. Synthesis of phenylphosphorous dichloride-DCPP

[0076] (a) press pcl 3 :Alcl 3 : The mol ratio of benzene=2.5: 1.5: 1.5, first pcl 3 Put into the reaction kettle, then put into Alcl 3 , start the mixer, and heat up to reflux at the same time;

[0077] (b) Add the benzene of the above-mentioned ratio dropwise, and control the drop to finish within 4 hours, the temperature is constant at 80° C., and absorb a large amount of HCl gas generated during the dropwise addition with water to obtain a by-product—hydrochloric acid;

[0078] (c) Cool down the reacted material to 60°C, put it into the extraction kettle, and add the complexing agent Nacl with a particle size of 200 objects in the weight ratio of extract: Nacl=7:1 to carry out the first extraction, and the temperature is controlled at 50°C, after stirring for 1 hour, let it stand for 30 minutes, collect the extracted upper layer material liquid, and pump the material liquid into the storage tank;

[0079] (d) ...

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Abstract

The invention relates to a kind of producing method of 2-carboxyethyl phenyl phosphinic acid fire retardant: the phosphorus trichloride and benzene reacts to synthesize phenyl phosphorus bichloride using the aluminum trichloride as the catalyst. The invention with good retarding quality can not only decrease the heat releasing rate of the material, it can also decrease the releasing amount of the caustic and toxic gas or smoke so that it overcome the shortage of releasing poisonous and harmful gas or smoke when the halogen retardant is burning. The invention has high stability and hydrolysis-resistibility so it can be used to copolymerization fire retarding reshaping. The advantage of the invention includes: increasing the yield of DCPP, acyl chloride and CEPPA; reducing the producing cost to a large extent; solving the problem of environmental pollution caused by the waste residue and liquor in traditional producing method; steady operating procedures, easy to control, reliable product quality as well as distinguished economical and social returns.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant, in particular to a production method of a 2-carboxyethylphenylphosphinic acid flame retardant, and belongs to the technical field of chemical industry. Background technique [0002] In flame retardant products, most of the early flame retardants contained halogens, mainly brominated flame retardants. Halogen flame retardants can delay the burning of polymers in the gas phase and solidified phase, especially in the gas phase, they can interrupt the chain reaction and have a clear flame retardant effect. However, halogen flame retardants will emit harmful gases at high temperatures, and the hydrogen chloride or hydrogen bromide released at the fire scene has fatal suffocation and lethality to the human body. When polybrominated diphenyl ethers are burned, carcinogens such as polybrominated dibenzofurans will be released. It has been confirmed that the harmful gas released from the burn...

Claims

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Application Information

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IPC IPC(8): C09K21/12
Inventor 伍天基王利生
Owner 云南泰京化工有限公司
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