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Preparation method of liquid phosphite antioxidant

A technology of phosphite and triphenyl phosphite, which is applied in the field of antioxidant preparation, can solve the problems of difficult raw material recovery, low raw material utilization rate, long reaction cycle, etc., and achieves easy control of the reaction process and high utilization of raw materials. High efficiency, clear and transparent effect

Inactive Publication Date: 2017-01-04
SHANDONG LINYI SUNNY WEALTH CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The main disadvantage of the traditional process is that the reaction is not easy to control when sodium metal is used as the catalyst, and there are great safety hazards in the storage, transportation and production links; the use of organic solvents such as toluene increases the energy consumption cost and the reaction cycle is longer
The process of Zhejiang Research Institute of Chemical Industry is relatively complicated, the utilization rate of raw materials is low, and more wastes such as waste water are generated; the reaction products are complex, and the recovery of raw materials is difficult, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] In a 250ml four-neck flask equipped with stirring, thermometer, condensing device and HCl gas absorption device, add 72.79g phenol, 0.7g catalyst 1,8-diazabicycloundec-7-ene, start stirring, control The temperature is 20°C, add 29.51g of phosphorus trichloride dropwise under normal pressure, control the rate of addition, drop it in about 30 minutes, and keep the reaction at 35°C for 2h, then slowly raise the temperature to 150°C, and control the vacuum degree- 0.050MPa, continuously extract the generated HCl gas and absorb it with lye. After the first step reaction is completed, cool down to 40°C, add 78.12g of isooctyl alcohol, and add 0.5g of catalyst 1,8-diazabicycloundec-7-ene, and raise the temperature to 155±5°C under normal pressure Keep the reaction for 2h, then start to gradually vacuumize to -0.07MPa, and react for 5h. Start distillation after the reaction is completed. The forward distillation is isooctyl alcohol and phenol respectively. Under the condition ...

Embodiment 2

[0020] In a 250ml four-neck flask equipped with stirring, thermometer, condensing device and HCl gas absorbing device, add 72.79g of phenol and 0.5g of catalyst triethylamine, start stirring, control the temperature at 30°C, and add dropwise 29.51g of triethylamine under normal pressure. Phosphorus chloride, control the dropping rate, drop it in about 45 minutes, keep the reaction at 30°C for 2 hours, then slowly raise the temperature to 150°C, control the vacuum degree -0.070MPa, continuously extract the generated HCl gas, and use lye absorb. After the first step of the reaction, cool down to 40°C, add 78.12g of isooctyl alcohol, and add 0.5g of catalyst triethylamine, raise the temperature to 155±5°C under normal pressure and keep the reaction for 2h, then start to gradually vacuum to -0.07MPa , Reaction 5h. After the reaction is completed, start distillation. The forward distillation is isooctyl alcohol and phenol respectively. Under the condition of temperature of 185-195...

Embodiment 3

[0022] In a 250ml four-neck flask equipped with stirring, thermometer, condensing device and HCl gas absorbing device, add 72.79g of phenol, 0.7g of catalyst N,N-dimethylcyclohexylamine, start stirring, control the temperature at 45°C, and Add 29.51g of phosphorus trichloride dropwise under pressure, control the rate of addition, and drop it in about 45 minutes. After the addition is complete, keep the reaction at 40°C for 1h, then slowly raise the temperature to 150°C, control the vacuum degree -0.040MPa, and continuously pump out to form HCl gas, and absorbed with lye. After the first step of the reaction is completed, cool down to 50°C, add 78.12g of isooctyl alcohol, and add 0.5g of catalyst N,N-dimethylcyclohexylamine, raise the temperature to 160±5°C under normal pressure, keep the reaction for 2h, and then start Gradually evacuate to -0.07MPa, and react for 5h. After the reaction is completed, start distillation. The forward distillation is isooctyl alcohol and phenol ...

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Abstract

The invention relates to a preparation method of liquid phosphite antioxidant. The preparation method includes the steps of firstly, allowing phenol and phosphorus trichloride to have substitution reaction in the presence of catalyst to generate intermediate triphenyl phosphite, wherein the catalyst is amine or amidine with steric hindrance; secondly, allowing the generated intermediate triphenyl phosphite to have transesterification with isooctanol, and distilling and purifying to obtain the liquid diisooctyl phenyl phosphite. The preparation method has the advantages that the preparation method is mild in reaction condition, high in preparation safety coefficient, environmentally friendly, short in reaction cycle and high in product yield, does not need solvents and does not generate waste water and solid wastes, the reaction process can be controlled easily, raw materials can be recycled, and the prepared diisooctyl phenyl phosphite is high in content, low in acid value, clear and transparent in appearance, good in flowability, especially suitable for industrial production, and the like.

Description

technical field [0001] The invention relates to the field of preparation of antioxidants, in particular to a preparation method of liquid phosphite antioxidants. More specifically, the present invention relates to the preparation method of monophenyl diisooctyl phosphite. Background technique [0002] Phenyldiisooctyl phosphite is a liquid phosphite antioxidant with excellent application effect. It has the characteristics of convenient pipeline storage and transportation, convenient metering, and uniform mixing with liquid products. In polymers, phenylenedioctyl phosphite can effectively decompose unstable peroxygen compounds and interrupt the thermo-oxidative aging of polymers. In polyvinyl chloride, phenyl-diisooctyl phosphite can be used as an organic auxiliary heat stabilizer, which has the functions of absorbing HCl, replacing unstable chlorine atoms, adding to conjugated polyene sequences and complexing metal ions. It has no obvious stabilizing effect when used in po...

Claims

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Application Information

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IPC IPC(8): C07F9/145
CPCC07F9/145
Inventor 张珍一付建英
Owner SHANDONG LINYI SUNNY WEALTH CHEM CO LTD