Refining method of 2,4-ditertiary butylphenol

A technology of di-tert-butylphenol and refining method, which is applied in the fields of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., and can solve problems affecting product quality, generation of impurities, difficulty in storage, etc.

Inactive Publication Date: 2005-05-04
BC P INC CHINA NAT PETROLEUM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using isobutene as an alkylating agent is its traditional preparation method (such as JP02221236, etc.), and using isobutene as an alkylating agent has the following disadvantages: isobutene is easy to volatilize, is difficult to store, and is easy to cause losses during transportation; isobutene is prone to polymerization in the reaction process , generating impurities and affecting product quality
However, when using this process to rectify the alkylation liquid, it is found that 2.4-di-tert-butylphenol is deenified and converted into p-tert-butylphenol, so that the 2.4-di-tert-butylphenol product with higher purity cannot be obtained.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] A distillation device with a tower kettle volume of 3000 ml was charged with 2,100 g of an alkylation liquid that was reacted with phenol by using MTBE as an alkylating agent, using a strong acid cation exchange resin (D72) as an acid catalyst, and reacting with phenol. Among them, the content of 2,4-di-tert-butylphenol is 70.56%, the content of p-tert-butylphenol is 21.55%, the content of 2,4,6-tri-tert-butylphenol is 5.07%, and the others are 2%. Add 3g of sodium phenate, control the absolute pressure at the top of the tower at 30mmHg, and simply distill. After 3 hours, all the alkylation liquid was distilled out. Sampling and analysis showed that the content of 2.4-di-tert-butylphenol was 73.65%, the content of p-tert-butylphenol was 22.35%, the content of 2.4.6-tri-tert-butylphenol was 1.46%, and the others were 2.54. %, and then add the distillate to a rectification device with a column volume of 3000 ml and a theoretical plate number of 26. After refluxing at the top ...

Embodiment 2

[0015] In a distillation device with a tower kettle volume of 3000 ml, 2100 g of an alkylation liquid that reacts with phenol with MTBE as an alkylating agent and activated clay as an acid catalyst is added. Among them, the content of 2.4-di-tert-butylphenol is 72.56%, the content of p-tert-butylphenol is 20.26%, the content of 2.4.6-tri-tert-butylphenol is 5.13%, and the others are 2.05%. Add 4g of sodium carbonate, control the absolute pressure at the top of the tower at 30mmHg, and simply distill. After 3 hours, all the alkylation liquid was distilled out. Sampling and analysis showed that the content of 2.4-di-tert-butylphenol was 75.56%, the content of p-tert-butylphenol was 21.35%, the content of 2.4.6-tri-tert-butylphenol was 1.06%, and the others were 2.03. %, and then add the distillate to a rectification device with a column volume of 3000ml and a theoretical plate number of 26. After refluxing for 24 hours at an absolute pressure of 10mmHg at the top of the tower, the p...

Embodiment 3

[0019] Add 2600g of alkylating liquid with MTBE as the alkylating agent and strong acid cation exchange resin (D72) as the acid catalyst in the distillation device with a tower kettle volume of 3000ml. Among them, the content of 2.4-di-tert-butylphenol is 72.35%, the content of p-tert-butylphenol is 18.55%, the content of 2.4.6-tri-tert-butylphenol is 5.57%, and the others are 3.53%. Add 2g of sodium hydroxide, control the absolute pressure at the top of the tower at 30mmHg, and simply distill. After 3 hours, all the alkylation liquid was distilled out. Sampling and analysis showed that the content of 2.4-di-tert-butylphenol was 76.75%, the content of p-tert-butylphenol was 20.35%, the content of 2.4.6-tri-tert-butylphenol was 1.36%, and the others were 1.54. %, and then add the distillate to a rectification device with a column volume of 3000 ml and a theoretical plate number of 26. After refluxing at the top of the tower at an absolute pressure of 10mmHg for 24 hours, sampling a...

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Abstract

The present invention relates to a kind of refining method that adopts methyl tert-butyl ether (MTBE) as alkylating agent to react with phenol to synthesize 2.4-di-tert-butyl phenol. Alkaline substances are added to the liquid for neutralization, and after simple distillation, rectification and purification are carried out to solve the problems of difficult conversion and low yield due to the de-ene reaction that occurs in the batch rectification process.

Description

Technical field [0001] The invention relates to a method for refining 2.4-di-tert-butyl phenol, in particular to a method that uses methyl tert-butyl ether (MTBE) as an alkylating agent and an acid catalyst to react with phenol to synthesize 2.4-di-tert-butyl phenol The refining method. Background technique [0002] 2.4-Di-tert-butylphenol is an antioxidant for aviation gasoline, low-efficiency stabilizer for natural rubber and synthetic rubber, heat stabilizer for polyolefin and high-efficiency polystyrene. It can be used to prepare new phenolic resins, coatings, adhesives and pesticides. . In the field of polymer additives, 2.4-di-tert-butyl phenol is the raw material for synthetic antioxidant 168, antioxidant 626, ultraviolet absorber UV-326 and UV-327. Using isobutylene as an alkylating agent is its traditional preparation method (such as JP02221236, etc.). Using isobutylene as an alkylating agent has the following disadvantages: isobutylene is easy to volatilize, is difficul...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/06C07C37/74C07C39/06
Inventor 赵义军初荣敏赖燕萍邓廷昌温金萍
Owner BC P INC CHINA NAT PETROLEUM CORP
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