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A kind of preparation method of bis(2,4-dicumylphenyl) pentaerythritol diphosphite

A technology of pentaerythritol diphosphite and cumylphenyl, which is applied in the field of phosphite antioxidant preparation process, can solve the problems that the product purity is difficult to guarantee, the temperature control requirements are extremely high, and the final use effect of antioxidant 9228 is affected.

Active Publication Date: 2021-05-04
锦州英诺威科技服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires extremely high temperature control, a little carelessness will bring a lot of impurities, and the purity of the product is not easy to guarantee, usually the purity does not exceed 90%.
[0007] The second kind: first generate the intermediate dichloropentaerythritol diphosphite of phosphorus trichloride and pentaerythritol, although high-purity antioxidant 9228 can be synthesized, due to the addition of excessive 2,4-dicumylphenol, resulting in the final The yield is low. According to existing literature reports, the yield generally does not exceed 70%, and there is a large amount of reaction catalyst residue, which affects the final use effect of the antioxidant 9228

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Add 35g of pentaerythritol, 525mg of triethylamine hydrochloride, and 130g of toluene into a reactor equipped with stirring, thermometer, condenser and hydrogen chloride absorption device. Under the condition of mpa, add 74.14g of phosphorus trichloride dropwise for 3.5 hours, then raise the temperature to 45-51°C within 1 hour and keep it for 1 hour, then raise the temperature to 85-90°C within 1.5 hours. °C, vacuum gauge pressure - (0.08-0.09) mpa decompression reaction for 1 hour, stop decompression and fill with nitrogen protection to obtain dichloropentaerythritol diphosphite reaction solution;

[0029] 2) Dissolve 175.87g of 2,4-dicumylphenol in 132g of toluene, raise the temperature to 90-100°C, add the dichloropentaerythritol diphosphite reaction solution obtained in step 1) dropwise to 2,4-dicumylphenol In the toluene solution of base phenol, the dropping time is 2 hours, under vacuum gauge pressure-(0.02-0.03)mpa decompression reflux reaction for 4 hours, f...

Embodiment 2

[0032] 1) Add 35g of pentaerythritol, 420mg of di-n-butylamine hydrochloride, and 123g of toluene in a reactor with stirring, thermometer, condenser and hydrogen chloride absorption device, at reaction temperature -5~-2°C, vacuum gauge pressure-( Under the condition of 0.01-0.02mpa), 75.55g of phosphorus trichloride was added dropwise for 3 hours, then the temperature was raised to 45-51°C within 1 hour and kept for 1 hour, and the temperature was raised to 85-90°C within 1 hour. At 85-90 ° C, vacuum gauge pressure - (0.08-0.09) mpa decompression reaction for 1 hour, stop decompression and fill with nitrogen protection to obtain dichloropentaerythritol diphosphite reaction liquid;

[0033]2) Dissolve 174.18g of 2,4-dicumylphenol in 148g of toluene, raise the temperature to 90-100°C, add the dichloropentaerythritol diphosphite reaction liquid obtained in step 1) dropwise to 2,4-dicumylphenol In the toluene of base phenol, the dropping time is 1.5 hours, under vacuum gauge press...

Embodiment 3

[0035] 1) Add 70g of pentaerythritol, 1.19g of tri-n-butylamine hydrochloride, and 270g of xylene in a reactor with stirring, thermometer, condenser and hydrogen chloride absorption device, at a reaction temperature of 2-5°C, vacuum gauge pressure-( Under the condition of 0.01-0.02mpa), 149g of phosphorus trichloride was added dropwise for 4 hours, then the temperature was raised to 45-51°C within 1.5 hours and kept for 1 hour, and the temperature was raised to 85-90°C within 1.5 hours. 85-90°C, vacuum gauge pressure - (0.08-0.09) mpa decompression reaction for 1 hour, stop decompression and fill with nitrogen protection to obtain dichloropentaerythritol diphosphite reaction liquid;

[0036] 2) Dissolve 355g of 2,4-dicumylphenol in 280g of xylene, raise the temperature to 90-100°C, and add the dichloropentaerythritol diphosphite reaction solution obtained in step 1) dropwise to 2,4-dicumylphenol In the xylene solvent of base phenol, the dropping time is 2.5 hours, under vacuum...

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PUM

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Abstract

The embodiment of the invention discloses a preparation method of bis(2,4-dicumylphenyl)pentaerythritol diphosphite. Add phosphorus trichloride dropwise to pentaerythritol, amine hydrochloride catalyst, and aromatic hydrocarbon solvent at a reaction temperature of 5-10°C and slightly reduced pressure, then raise the temperature to 85-90°C in stages, and react under reduced pressure for 1 hour After stopping the decompression, fill with nitrogen protection to obtain the dichloropentaerythritol diphosphite reaction solution; add the above reaction solution dropwise to the aromatic hydrocarbon solvent of 2,4-dicumylphenol heated to 90-100°C, and depressurize Reflux reaction for 4 hours, feed nitrogen, add mixed amine to adjust the reaction system to be alkaline, cool down to room temperature, and filter to obtain bis(2,4-dicumylphenyl)pentaerythritol diphosphite. The invention finally obtains a high-performance product with high yield, narrow melting range, low acid value and excellent hydrolysis resistance through strict control of reaction conditions, such as temperature, pressure, time, catalyst, feeding sequence and post-treatment.

Description

technical field [0001] The invention relates to the technical field of preparation technology of phosphite antioxidant, in particular to a preparation method of bis(2,4-dicumylphenyl)pentaerythritol diphosphite. Background technique [0002] At room temperature and higher temperature, most polymers will undergo auto-oxidation reactions with varying speeds, which cause plastic yellowing, degradation and strength reduction, that is, plastics have undergone aging effects, and any substance that can inhibit or delay this reaction Can be called antioxidants. The reason for aging is that plastics are oxidatively degraded due to the action of light, oxygen, and heat, and the way to eliminate or alleviate the aging degradation of plastics is to add antioxidants to plastics. Therefore, the use of antioxidants is indispensable in the application of various plastic products such as polypropylene, polyethylene film, high-density polyethylene injection molding products, ABS, polycarbona...

Claims

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Application Information

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IPC IPC(8): C07F9/6574
CPCC07F9/65746
Inventor 田军委李志光朱学亮苏美南刘洋
Owner 锦州英诺威科技服务有限公司
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