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Process for preparing solid superacid catalysts used for synthesis butyl p-hydroxybenzoate

A technology of butyl hydroxybenzoate and solid super acid, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of low catalyst activity, large three-waste emissions, and high consumption, and achieve high activity and selectivity, low production cost and simple process

Inactive Publication Date: 2007-11-28
HUAIYIN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the invention is to: provide the preparation method of the solid superacid catalyst of synthesizing butyl p-hydroxybenzoate, adopt the solid superacid catalyst that this preparation method obtains to replace sulfuric acid and be used for synthesizing butyl p-hydroxybenzoate, solve existing catalyst activity Low consumption, high consumption, high cost, serious corrosion, large discharge of three wastes, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Ti(SO) with a mass percentage of 20% at room temperature 4 ) 2 Attapulgite was added to the solution, and the amount of attapulgite added was Ti(SO 4 ) 2 8%, soak for 0.5h, add NH dropwise while stirring 3 .H 2 O, adjust the pH value of the mixture to 6, age for 6h, filter with suction, wash, dry at 378K for 12h, grind to ≤200 mesh, use 0.1mol.L -1 H 2 SO 4 Solution according to 10ml.g -1 Immerse for 5 minutes, dry at 378K for 1 hour, grind to ≤200 mesh, and roast at 623K for 3 hours in an air atmosphere to obtain a solid superacid catalyst and store it in a desiccator.

[0018] Catalyzed synthesis of butyl p-hydroxybenzoate: take by weighing 1.3g of 3% catalyst of the total mass of the reactant, take by weighing 13.8g p-hydroxybenzoic acid, measure 37ml butanol and join in the three-necked flask, insert the thermometer on the three-necked flask, Reflux condenser, water separator, time from the beginning of reflux, the reaction temperature is 120-135°C, the cata...

Embodiment 2

[0020] Add attapulgite to the solution with a mass percentage of 24% at room temperature, and the amount of attapulgite added is Ti(SO 4 ) 2 10%, soak for 0.5h, add NH dropwise while stirring 3 .H 2 O, adjust the pH value of the mixture to 7, age for 9h, filter with suction, wash, dry at 383K for 14h, grind to ≤200 mesh, use 0.4mol.L -1 H 2 SO 4 Solution according to 13ml.g -1 Immerse in the ratio of 8min, dry at 383K for 1h, grind to ≤200 mesh, and roast at 673K ​​in air atmosphere for 3h to obtain a solid superacid catalyst and store it in a desiccator.

[0021] Catalytic synthesis of butyl p-hydroxybenzoate: the esterification reaction was carried out according to the method of Example 1, and the reaction yield was 94.2%.

Embodiment 3

[0023] At room temperature, the Ti(SO 4 ) 2 Attapulgite was added to the solution, and the amount of attapulgite added was Ti(SO 4 ) 2 11%, soak for 0.5h, add NH dropwise while stirring 3 .H 2 O, adjust the pH value of the mixture to 8, age for 12h, filter with suction, wash, dry at 383K for 16h, grind to ≤200 mesh, use 0.6mol.L -1 H 2 SO 4 Solution according to 17ml.g -1 Immerse in the ratio of 12min, dry at 393K for 1h, grind to ≤200 mesh, and roast at 723K in air atmosphere for 3h to obtain a solid superacid catalyst and store it in a desiccator.

[0024] Catalytic synthesis of butyl p-hydroxybenzoate: the esterification reaction was carried out according to the method of Example 1, and the reaction yield was 94.3%.

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Abstract

The present invention discloses preparation process of butyl p-hydroxybenzoate as solid super acidic catalyst. The preparation process includes the following steps: adding attapulgite clay into 20.0-45.0 wt% concentration Ti(SO4)2 solution, with the amount of attapulgite clay being 8-16 wt% of Ti(SO4)2, and soaking to obtain suspension; regulating the pH value of the suspension to 6-10 with NH3.H2O, ageing for 6-24 hr, suction filtering, washing, drying at 378-383 K for 12-24 hr, grinding to below 200 mesh to obtain white powder; soaking the white powder in 0.1-1.51 mol / l concentration H2SO4 solution for 5-25 min, filtering, washing, drying at 378-393 K for 1 hr, grinding to below 200 mesh to obtain white powder; and roasting in air atmosphere at 623-873 K to activate for 3 hr to obtain the solid super acidic catalyst. The solid super acidic catalyst has high activity, high selectivity, long service life, low production cost and other advantages.

Description

technical field [0001] The invention relates to a preparation method of a catalyst, in particular to a preparation method of a solid superacid catalyst for synthesizing butyl p-hydroxybenzoate. Background technique [0002] Compared with traditional benzoic acid and its sodium salt and sorbic acid preservatives, butyl p-hydroxybenzoate, also known as butylparaben, has a stable antiseptic effect and is not easy to change with the change of pH value. It is one of the food preservatives that our country will focus on developing at present and in the future. [0003] The traditional esterification synthesis of butyl p-hydroxybenzoate uses sulfuric acid as a catalyst. It is cheap and highly active, so it is widely used in industry. However, the disadvantages of using sulfuric acid catalyst cannot be ignored: it corrodes the equipment seriously, discharges a large amount of three wastes, and the post-treatment is complicated. Products become darker, so their limitations become i...

Claims

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Application Information

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IPC IPC(8): B01J27/053C07C69/78B01J21/16B01J21/06
Inventor 钱运华金叶玲陈静胡涛谭立强
Owner HUAIYIN INSTITUTE OF TECHNOLOGY
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