Clean production method of 2,4-di-tert-butylphenol

A di-tert-butylphenol, clean production technology, applied in the production of bulk chemicals, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of multi-industrial waste residue, poor selectivity, and inability to reuse

Pending Publication Date: 2020-05-29
SHANDONG LINYI SUNNY WEALTH CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most manufacturers in industrial production use activated clay as a catalyst for 2,4 alkylation reaction. Although activated clay has high activity, low price and low production cost, it cannot be reused and produces more industrial waste residue, and activated clay is harmful to The selectivity of the 2,4 alkylation rea

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 150 grams of phenol, 3 grams of molecular sieve catalyst (La 2 o 3 , CeO 2 The mass fractions are 5%, 5% respectively) into a 500ml four-necked flask, and the temperature is raised to 90°C for nitrogen displacement, and the isobutylene gas is started to flow to the bottom of the bottle. During the reaction, the temperature is maintained at 90-100°C, and the liquid After 4 hours of reaction, the flow of olefin was stopped, and the isobutylene tank was weighed, and the amount of olefin was calculated to be 195 grams. Analysis by gas chromatography showed that the conversion rate of phenol was 99.82%, 2, 4-di-tert-butylphenol selectivity 79.23%;

[0042] After the catalyst was recovered, 0.03 g of new catalyst was added and reacted again under the same conditions. The results showed that the conversion rate of phenol was 99.80%, and the selectivity of 2,4-di-tert-butylphenol was 78.93%;

[0043] The reaction result of the third use: the conversion rate of phenol is 99.8...

Embodiment 2

[0049] 150 grams of phenol, 3 grams of molecular sieve catalyst (La 2 o 3 , CeO 2 The mass fractions are 5%, 7% respectively) into a 500ml four-necked flask, and the temperature is raised to 100°C for nitrogen replacement, and the isobutylene gas is started to flow to the bottom of the bottle. During the reaction, the temperature is maintained at 100-120°C, and the liquid After 4 hours of reaction, the flow of olefin was stopped, and the isobutylene tank was weighed, and the amount of olefin was calculated to be 200 grams. Analysis by gas chromatography showed that the conversion rate of phenol was 99.90%, 2, 4-di-tert-butylphenol selectivity 77.63%;

[0050] After the catalyst was recovered, 0.05 g of new catalyst was added and reacted again under the same conditions. The results showed that the conversion rate of phenol was 99.85%, and the selectivity of 2,4-di-tert-butylphenol was 78.86%;

[0051] The reaction result of the third use: the conversion rate of phenol is 99....

Embodiment 3

[0054] 150 grams of phenol, 3 grams of molecular sieve catalyst (La 2 o 3 , CeO 2 The mass fractions are 7%, 7% respectively) into a 500ml four-necked flask, and the temperature is raised to 120°C for nitrogen replacement, and the isobutylene gas is started to flow to the bottom of the bottle. During the reaction, the temperature is kept at 120-130°C, and the liquid After 4 hours of reaction, the flow of olefin was stopped, and the isobutylene tank was weighed, and the amount of olefin was calculated to be 195 grams. Analysis by gas chromatography showed that the conversion rate of phenol was 99.22%, 2, 4-di-tert-butylphenol selectivity 77.29%;

[0055] After the catalyst was recovered, 0.04 g of new catalyst was added and reacted again under the same conditions. The results showed that the conversion rate of phenol was 99.83%, and the selectivity of 2,4-di-tert-butylphenol was 78.93%;

[0056] The reaction result of the third use: the conversion rate of phenol is 99.83%, a...

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PUM

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Abstract

The invention provides a clean production method of 2,4-di-tert-butylphenol, wherein the clean production method comprises the steps: A) mixing phenol and a catalyst, stirring, heating, adding isobutene, and carrying out a reaction to obtain 2,4-di-tert-butylphenol, wherein the catalyst is a transition metal oxide doped molecular sieve, the transition metal oxide is La2O3 and CeO2, the molecular sieve is an X-type molecular sieve and/or a Y-type molecular sieve, and the mass fraction of the transition metal oxide in the catalyst is 6-20%; and B) mixing the used catalyst with a new catalyst, adding phenol and isobutene, carrying out a reaction again, repeating for several times, extracting and recovering the catalyst by using an organic solvent, and then drying and calcining to finish regeneration and recycling of the catalyst. The molecular sieve catalyst doped with the transition metal is used for alkylation reaction of phenol and isobutene, the catalytic activity is high, byproductsgenerated by reaction of a target product and isobutene molecules can be reduced, and the reaction selectivity is improved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a clean production method of 2,4-di-tert-butylphenol. Background technique [0002] 2.4-Di-tert-butylphenol is an antioxidant for aviation gasoline, a low-efficiency stabilizer for natural rubber and synthetic rubber, a heat stabilizer for polyolefins and high-efficiency polystyrene, and can be used to prepare new phenolic resins, coatings, adhesives and pesticides . In the field of polymer additives, 2.4-di-tert-butylphenol is a raw material for synthesizing antioxidant 168, antioxidant 626, ultraviolet absorbers UV-326 and UV-327, etc. [0003] The production of 2,4-di-tert-butylphenol generally adopts isobutylene or methyl tert-butyl ether as an alkylating agent, and uses heteropolyacids, activated clay, strongly acidic cation exchange resins, etc. as catalysts (CN02125506, CN1935763A). At present, most manufacturers in industrial production use activat...

Claims

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Application Information

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IPC IPC(8): C07C37/14C07C39/06B01J29/90B01J38/52B01J38/02
CPCC07C37/14B01J29/90B01J38/52B01J38/02C07C39/06Y02P20/584Y02P20/52
Inventor 赵南郭德宝赵振莹彭修娜孙聚涛
Owner SHANDONG LINYI SUNNY WEALTH CHEM CO LTD
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