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Method for preparing tri-(2, 4-di-tertiary butyl phenyl) phosphite ester antioxidant

A technology of di-tert-butyl phenyl and di-tert-butyl phenol, applied in the field of preparing tri-phosphite, can solve the problems of high price, increased production cost of antioxidant 168, difficulty and the like, and achieves low price and good catalysis Activity, the effect of reducing production costs

Inactive Publication Date: 2015-07-01
ANQING FULLTIME CHEM INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] When Wang Weijie and others selected 4-dimethylaminopyridine (DMAP) as the catalyst, a yield of 95% could be obtained, much higher than the yield of 80.5% when using N,N-dimethylformamide (DMF) as the catalyst , but the price of DMAP is more expensive than DMF, and the production cost of antioxidant 168 will increase, which has certain difficulties in practical application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 24g of 2,4-di-tert-butylphenol, 15mL of toluene, and 0.10g of ethanolamine to a 250mL three-necked flask equipped with a constant pressure dropping funnel and a thermometer, raise the temperature to 60°C, and slowly add 5ml containing 4.5gPCl dropwise within 60min. 3 The toluene solution, after the dropwise addition, was kept at this temperature for 4 hours, then the temperature was raised to 130° C., and the reaction was carried out at this temperature for 4 hours. The reaction solvent was removed by distillation under reduced pressure to obtain a crude product of tris-(2,4-di-tert-butylphenyl)phosphite. Add 30ml of methanol, stir vigorously for about 3 hours, filter, and dry the obtained solid sample to obtain a white powder product with a yield of 85.1%.

Embodiment 2

[0020] Add 22g of 2,4-di-tert-butylphenol, 15mL of xylene, and 0.12g of diethanolamine to a 250mL three-neck flask equipped with a constant-pressure dropping funnel and a thermometer, raise the temperature to 25°C, and directly add 5ml containing 4.5g of PCl 3 The xylene solution was reacted at 25°C for 4h, heated to 100°C, and reacted at this temperature for 4h. The reaction solvent was removed by distillation under reduced pressure to obtain a crude product of tris-(2,4-di-tert-butylphenyl)phosphite. Add 30 ml of ethanol, stir vigorously for about 1 h, filter, and dry the obtained solid sample to obtain a white powder product with a yield of 76.2%.

Embodiment 3

[0022] Add 21g of 2,4-di-tert-butylphenol, 15mL of chlorobenzene, and 0.2g of triethanolamine to a 250mL three-necked flask equipped with a constant-pressure dropping funnel and a thermometer, raise the temperature to 40°C, and slowly add 5ml containing 4.5g of PCl 3 Chlorobenzene solution, reacted at 40°C for 3h, raised the temperature to 120°C, and reacted at this temperature for 3h. The reaction solvent was removed by distillation under reduced pressure to obtain a crude product of tris-(2,4-di-tert-butylphenyl)phosphite. Add 30 ml of propanol, stir vigorously for about 2 hours, filter, and dry the obtained solid sample to obtain a white powder product with a yield of 83.8%.

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PUM

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Abstract

The invention relates to a method for preparing a tri-(2, 4-di-tertiary butyl phenyl) phosphite ester antioxidant. The method comprises the following steps: by taking 2, 4-di-tertiary phenol and phosphorus trichloride as raw materials and an aromatic compound as a reaction solvent, carrying out reaction at 25-60 DEG C under the action of ethanol amine catalysts; then raising the temperature to 100-130 DEG C and reacting for 1-4 hours at the temperature; distilling at a reduced pressure, removing the reaction solvent, and adding lower alcohol as a solvent to crystallize; and severely stirring for a certain time, and filtering to obtain tri-(2, 4-di-tertiary butyl phenyl) phosphite ester.

Description

technical field [0001] The invention relates to a method for preparing tri-(2,4-di-tert-butylphenyl) phosphite, which belongs to the field of fine chemical industry. Background technique [0002] Antioxidant 168, whose chemical name is tri-(2,4-di-tert-butylphenyl) phosphite, is a very commonly used phosphite antioxidant with good high temperature resistance, low volatility, It has the advantages of non-toxicity and excellent anti-oxidation effect. It is often used as an auxiliary antioxidant in combination with phenolic antioxidants and applied to plastics, rubber and other products. [0003] At present, the vast majority of tri-(2,4-di-tert-butylphenyl)phosphite is prepared by using phosphorus trichloride and 2,4-di-tert-butylphenol as raw materials, and is synthesized under the action of an alkaline catalyst. . [0004] The patent of DE2950694 reported that in the reaction system of toluene and aqueous sodium hydroxide solution, at a temperature of 25-30 ° C, with phosp...

Claims

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Application Information

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IPC IPC(8): C07F9/145
Inventor 周沛方岩雄王东方萍
Owner ANQING FULLTIME CHEM INDAL
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