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Catalyst composition for synthesizing 3-tert-butyl-4-hydroxyanisole from p-hydroxyanisole and its application

A technology of p-hydroxyanisole and hydroxyanisole, which is applied in the field of anisole preparation, can solve the problems of complex process, high energy consumption, and huge usage, and achieve the effect of mild operating conditions, low energy consumption, and simple equipment

Active Publication Date: 2022-06-17
BROTHER ENTERPRISES HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The separation method for the first synthesis method is currently mainly recrystallization method, such as: ①The reactant is extracted with benzene, washed with water, benzene is distilled under reduced pressure, and recrystallized from petroleum ether (ja01611a079) ②The reactant is dissolved in pentane, 5% Washing with sodium hydroxide, batch extraction acidification recrystallization (US2459540A) ③ reactant washing, 5-8% sodium hydroxide washing, vacuum distillation, recrystallization (CN108238857A) etc., this method flow process is complicated, and solvent introduces many kinds And the usage is huge, and the whole process produces a lot of waste water
In addition, according to the material characteristics, direct rectification can also be tried, but this method has high energy consumption and is prone to side reactions, and 3-BHA and 2-BHA are isomers with close boiling points, so it is difficult to obtain high purity by direct rectification 3-BHA products

Method used

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  • Catalyst composition for synthesizing 3-tert-butyl-4-hydroxyanisole from p-hydroxyanisole and its application
  • Catalyst composition for synthesizing 3-tert-butyl-4-hydroxyanisole from p-hydroxyanisole and its application
  • Catalyst composition for synthesizing 3-tert-butyl-4-hydroxyanisole from p-hydroxyanisole and its application

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Effect test

Embodiment 1

[0041] A catalyst composition for synthesizing 3-tert-butyl-4-hydroxyanisole from p-hydroxyanisole, the catalyst composition is composed of a main catalyst, a co-catalyst I and a co-catalyst II:

[0042] The main catalyst is a strong acid cation exchange resin, Amberlyst-15 (dry state, hydrogen type);

[0043] Cocatalyst I is 4A molecular sieve;

[0044] Cocatalyst II is HND-34.

[0045] Wherein, the weight ratio of main catalyst, auxiliary catalyst I, and auxiliary catalyst II is 5:20:0.2.

Embodiment 2

[0047] A catalyst composition for synthesizing 3-tert-butyl-4-hydroxyanisole from p-hydroxyanisole, specifically the same as in Example 1, the difference is: the weight ratio of main catalyst, auxiliary catalyst I, auxiliary catalyst II It is 5:40:0.3.

Embodiment 3

[0049] A method for synthesizing 3-tert-butyl-4-hydroxyanisole, the method adopts a catalyst composition to carry out a synthesis reaction, and the steps are:

[0050] S1, to the raw material p-hydroxyanisole and tert-butanol, add the main catalyst and the auxiliary catalyst I according to the formula, mix and stir at a temperature of 40-60 ° C, and control the reaction time at 10h-12h (the conversion rate reaches maximum, about 30-35%),

[0051] S2. Add cocatalyst II to the reaction system obtained in S1 until the reaction ends, and control the temperature of the reaction system at this stage within the range of 40-50°C.

[0052] Based on 100 g of p-hydroxyanisole, the weight ratio of main catalyst: auxiliary catalyst I: auxiliary catalyst II is 5: (20-40): (0.2-0.3). The main catalyst is a strong acid cation exchange resin, Amberlyst-15 (dry state, hydrogen type); the auxiliary catalyst I is 4A molecular sieve; the auxiliary catalyst II is HND-34.

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Abstract

The invention relates to a catalyst composition for synthesizing 3-tert-butyl-4-hydroxyanisole from p-hydroxyanisole and its application. A catalyst composition for synthesizing 3-tert-butyl-4-hydroxyanisole from p-hydroxyanisole, the catalyst composition is composed of a main catalyst, a cocatalyst I and a cocatalyst II: the main catalyst is a strongly acidic cation exchange The resin has an acidity H0 in the range of -4 to -14, cocatalyst I is a silicon-aluminum molecular sieve or a silicon boron molecular sieve, and cocatalyst II is a solid superacid catalyst, and the acidity H0 is in the range of -16 to -10; wherein, the main catalyst , The weight ratio of cocatalyst I and cocatalyst II is (0.1~5):(10~50):(0.1~1). The catalyst composition used for synthesizing 3-tert-butyl-4-hydroxyanisole from p-hydroxyanisole according to the present invention, when in use, firstly add the main catalyst and the co-catalyst I, and then add the co-catalyst II after the reaction is complete.

Description

technical field [0001] The invention relates to a preparation method of anisole, in particular to a catalyst composition for synthesizing 3-tert-butyl-4-hydroxyanisole from p-hydroxyanisole and its application, belonging to the technical field of green chemical industry. Background technique [0002] 3-tert-Butyl-4-hydroxyanisole: also known as 4-hydroxy-3-tert-butyl-anisole, 3-BHA, English name: 3-tert-Butyl-4-hydroxyanisole, its structural formula is : [0003] Butyl hydroxyanisole, also known as tert-butyl-4-hydroxyanisole, butyl anisole, referred to as BHA, white or slightly yellow waxy crystalline powder, is a commonly used antioxidant, widely used in food, Feed, oil, cosmetics and other fields. It is generally an isomeric mixture of 3-butylhydroxyanisole (3-BHA) and 2-butylhydroxyanisole (2-BHA), wherein the antioxidant effect of 3-BHA is 1.5~ 2 times, helps to improve the antioxidant properties of products by increasing the content of 3-BHA. [0004] According t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/08C07C43/23C07C41/30C07C41/40C07C41/42
CPCB01J31/08C07C41/30C07C41/40C07C41/42B01J2231/4205C07C43/23
Inventor 高海燕潘炎烽王灿汪铠周中平
Owner BROTHER ENTERPRISES HLDG CO LTD