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Preparation method of antioxidant tris(2,4-di-tert-butylbenzene) phosphite

A technology of di-tert-butylbenzene and di-tert-butylphenol, which is applied in the field of antioxidant preparation, can solve the problems of low product purity, achieve simple distillation recovery, increase yield, and reduce energy consumption

Active Publication Date: 2021-04-16
RIANLON ZHONGWEI NEW MATERIAL CO LTD +2
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the problem of low product purity caused by by-products in the preparation process of tris (2,4-di-tert-butylphenyl) phosphite, and the recovery and utilization of crystallization mother liquor and 2,4-di-tert-butylphenol, the present invention proposes A preparation method of tris(2,4-di-tert-butylphenyl) phosphite (also known as antioxidant 168)

Method used

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  • Preparation method of antioxidant tris(2,4-di-tert-butylbenzene) phosphite
  • Preparation method of antioxidant tris(2,4-di-tert-butylbenzene) phosphite

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preparation example Construction

[0052] A preparation method of a phosphite antioxidant, further comprising, after the reaction is finished, crystallizing the reaction liquid to obtain purified antioxidant tris(2,4-di-tert-butylphenyl) phosphite; crystallization filtrate After distilling off the crystallization solvent, 2,4-di-tert-butylphenol was recovered and used mechanically. The product obtained by the above preparation method of the present invention can be recycled and utilized after the crystallization solvent is removed by simple distillation. The impact on product quality (mainly purity, acid value and hydrolysis resistance) caused by high-temperature and high-pressure distillation recovery of 2,4-di-tert-butylphenol is avoided.

[0053] The crystallization solvent is a mixed system of lower aliphatic alcohol and reaction solvent, and the lower aliphatic alcohol refers to C 1 -C 8 Alcohol, such as: methanol, ethanol, propanol, isopropanol, etc., the reaction solvent is the remaining solvent in the...

Embodiment 1

[0059] The preparation of embodiment 1 antioxidant 168

[0060] (1) Synthesis reaction: Add 133.0g (0.646mol) of 2,4-di-tert-butylphenol, 200mL of xylene, and 2.29g (0.0226mol) of catalyst triethylamine into a 1000mL four-necked flask, stir and heat up to 50~ 55°C; then start to add 29.6g (0.216mol) of phosphorus trichloride dropwise, control the temperature in the kettle at 50-55°C during the dropwise addition, finish dropping after 3.5h, keep stirring for 1hr after adding dropwise; then slowly raise the temperature to 140-145°C ℃, heat preservation reaction for 4 hours, when there is basically no HCl gas generated in the system, increase the reaction temperature to 145-155 ℃, insert a nitrogen tube, continuously feed nitrogen from the bottom of the four-necked bottle, and use a water pump to control the slight negative pressure of the system at 96-100Kpa, Continue to react for 5 hours, take a sample to detect that the pH value of the reaction solution is 4, and stop the reac...

Embodiment 2

[0062] Example 2 Crystallization Mother Liquor Recovery and Application to Prepare Antioxidant 168

[0063] Crystallization mother liquor treatment: distill the crystallization mother liquor in Example 1 to a liquid phase temperature above 145° C., stop distillation, and keep the still liquid for use.

[0064] (1) Synthetic reaction: the crystallization kettle liquid obtained in Example 1, 133.0g (0.646mol) 2,4-di-tert-butylphenol, 50mL toluene, 2.85g (0.0154mol) catalyst tri-n-butylamine were added to 1000mL In the four-necked bottle, stir and heat up to 80-85°C; then start to drop 29.6g (0.216mol) of phosphorus trichloride, and control the temperature in the kettle to 80-85°C during the dropping process, and finish dropping in 3.5 hours. Stir for 1 hour; then slowly raise the temperature to 120-125°C, and keep the temperature for 3 hours. When there is basically no HCl gas in the system, increase the reaction temperature to 145-155°C, insert a nitrogen tube, and continuously...

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Abstract

The invention relates to a preparation method of an antioxidant tris(2,4-di-tert-butylbenzene) phosphite, which comprises the following steps: reacting 2,4-di-tert-butyl-phenol and phosphorus trichloride used as raw materials at 50-145 DEG C, and removing HCl gas generated in the reaction process; heating a reaction liquid obtained in the previous step until HCl gas is stopped being discharged, increasing the reaction temperature to 145-160 DEG C, controlling the reaction pressure to 90-101.3 kPa, continuing the reaction until the pH value of the reaction liquid reaches 3 or above, and ending the reaction to prepare the antioxidant tris(2,4-di-tert-butylbenzene) phosphite. The method adopts micro-negative pressure and by-products generated by reaction are avoided, so that the purity of the product is improved, and the hydrolysis resistance of the product is improved; and the crystallization mother liquor is simply distilled and recycled and then is reused.

Description

technical field [0001] The invention relates to the field of preparation of antioxidants, in particular to a preparation method of antioxidant tris(2,4-di-tert-butylphenyl) phosphite. Background technique [0002] The main function of antioxidants is to delay or inhibit the oxidation of polymer materials by atmospheric oxygen or ozone during polymerization, storage, transportation, and processing, resulting in impact strength, flexural strength, tensile strength, and elongation. Dramatically reduces chemicals that stop material from aging and extend lifespan. At present, antioxidants are one of the most commonly used and used chemical additives in the manufacturing process of various polymer materials. [0003] Antioxidant 168, chemical name tris(2,4-di-tert-butylphenyl) phosphite (also known as tris(2,4-di-tert-butyl) phosphite), is a widely used phosphorous acid Ester solid auxiliary antioxidant. Such compounds do not exhibit significant activity when they are used alon...

Claims

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Application Information

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IPC IPC(8): C07F9/145
CPCY02P20/52
Inventor 李平熊昌武范小鹏黄维孙东辉孙春光李海平
Owner RIANLON ZHONGWEI NEW MATERIAL CO LTD
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