A kind of method of synthesizing sulfur-containing bisphenol compound antioxidant

A technology for phenolic compounds and antioxidants, which is applied in the field of optimizing the synthesis of sulfur-containing bisphenolic compound antioxidants, can solve the problems of increased solvent recycling, decreased volume production capacity, decreased utilization rate of reactors, etc., and is convenient for industrialization. The effect of production, reduction of recycling times, and low production cost

Active Publication Date: 2014-10-29
山东正鑫新能源有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its weak point is: when 80~85% high-concentration ethanol aqueous solution is reaction solvent, the solubility of reaction mother liquor to methylene-4426-S product is bigger, carries out solid-liquid separation under normal temperature, and some products dissolve in reaction solution In this process, the reaction solution needs to be cooled to 3~6°C through a freezing process to effectively crystallize the product from the reaction solution and then separate it; in addition, the technology of CN102617424A is to complete the methylene-4426-S product in the synthesis reactor At the same time, the recrystallization process of the methylene-4426-S product in 80-85% high-concentration ethanol aqueous solution is completed. Therefore, the amount of solvent used in the process parameters of the design raw material ratio is relatively large. The usual solvent The amount of addition is 2,6-phenol: 80~85% ethanol aqueous solution (mass ratio) = 1:8.0~10.0, due to the increase in the amount of reaction solvent, the circulation of the recovered solvent increases, and the energy consumption increases; the volume of the same reactor produces Decreased capacity and reduced reactor utilization

Method used

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  • A kind of method of synthesizing sulfur-containing bisphenol compound antioxidant

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Effect test

Embodiment 1

[0030] In the GST-2 type stainless steel autoclave with magnetic stirring, 103g of raw material 2,6-di-tert-butylphenol, 9.78g of crystallization nucleating agent (60~90# 7.72g, polyethylene glycol 2.06g) were sequentially added , 30.0g of paraformaldehyde, 709g of 62% ethanol aqueous solution, 40g of 70% sodium hydrosulfide, after nitrogen replacement, start stirring and heating, fully mix the reaction raw materials in the kettle, when the temperature rises to 50~53°C, stop heating, The heat preservation reaction was carried out for 40 minutes, and the reaction was completed. Cool down to 20~30°C, filter, separate the reaction mother liquor, and collect; the separated solid product is washed with 55~75% ethanol aqueous solution to obtain the white crystal methylene-4426-S antioxidant product, purity: 98.8%, Melting point: 142.0~143.5°C, yield 97.6%.

Embodiment 2

[0032] In the GST-2 type stainless steel autoclave with magnetic stirring, 103g of raw material 2,6-di-tert-butylphenol, 9.78g of crystallization nucleating agent (60~90# 7.72g, polyethylene glycol 2.06g) were sequentially added , 28.5g of paraformaldehyde, 709g of 62% ethanol aqueous solution, 40g of 70% sodium hydrosulfide, after nitrogen replacement, start stirring and heating, fully mix the reaction raw materials in the kettle, when the temperature rises to 50~53°C, stop heating, The heat preservation reaction was carried out for 40 minutes, and the reaction was completed. Cool down to 20~30°C, filter, separate the reaction mother liquor, and collect; the separated solid product is washed with 55~75% ethanol aqueous solution to obtain the white crystal methylene-4426-S antioxidant product, purity: 99.1%, Melting point: 142.6~144.1°C, yield 97.8%.

Embodiment 3

[0034] In the GST-2 type stainless steel autoclave with magnetic stirring, 103g of raw material 2,6-di-tert-butylphenol, 7.21g of crystallization nucleating agent (5.15g of n-hexane, 2.06g of polyethylene glycol) were added successively. Formaldehyde 31.5g, 55% ethanol aqueous solution 618g, 70% sodium hydrosulfide 36g, after nitrogen replacement, start stirring and heating, fully mix the reaction raw materials in the kettle, when the temperature rises to 54~56°C, stop heating, keep warm for 60 minutes, the reaction is over. Cool down to 20~30°C, filter, separate the reaction mother liquor, and collect; the separated solid product is washed with 55~75% ethanol aqueous solution to obtain the white crystal methylene-4426-S antioxidant product, purity: 98.6%, Melting point: 142.5~144.1°C, yield 96.9%.

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Abstract

The invention discloses a method for synthesizing a sulfur-containing bisphenol compound antioxidant and belongs to the technical field of antioxidants. The method comprises the steps as follows: adopting 55-65% of ethanol water solution as a reaction solvent and 2,6-di-tert-butylphenol, paraformaldehyde and sodium hydrosulfide as reaction raw materials, adding a crystallization nucleating agent, carrying out thio-condensation reaction in a closed reaction kettle, and preparing a methylene-4426-S product as the antioxidant. A reaction mother solution obtained after reaction can be recycled as a reaction solvent. The crystallization nucleating agent has the effect of a phase-transfer catalyst, which is favorable for reaction of oil-soluble materials and water-soluble materials and increment of the yield. The method has the characteristics of simple production process, high product yield, low production cost, good quality and convenience for industrial production.

Description

technical field [0001] The invention relates to a technical method for optimizing and synthesizing a sulfur-containing bisphenol compound antioxidant product, and belongs to the technical field of antioxidants. Background technique [0002] Methylidene-4426-S is a sulfur-containing bisphenol compound antioxidant product, mainly used for synthetic rubber, polyolefin plastics and other polymer materials, as well as lubricants, fuel oil and other oil products. Sulfur-containing bisphenol Compound antioxidant products specifically refer to the following formula (I): [0003] [0004] (I) [0005] (I) Chemical name: bis(3,5-di-tert-butyl-4-hydroxybenzyl) sulfide, (referred to as methylene-4426-S). [0006] The method of synthesizing methylene-4426-S products in the past technology uses 2,6-tert-butylphenol (referred to as 2,6-phenol), 36% formaldehyde aqueous solution, and sodium sulfide as raw materials, and carries out thiocondensation reaction in ethanol aqueous solution...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C323/16C07C319/14
Inventor 杜飞马龙陆网军
Owner 山东正鑫新能源有限公司
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