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Synthesis process of p-tert-butylbenzoic acid

A technology of p-tert-butyl benzoic acid and tert-butyl benzoic acid, which is applied in the field of synthesis technology of p-tert-butyl benzoic acid, can solve the problems of unfavorable catalyst recycling, post-treatment of equipment corrosion, poor chromaticity and the like, and achieves Elimination of corrosion and complex post-processing, low production costs, and reduced chroma effects

Inactive Publication Date: 2021-07-09
天津鼎晟新化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the color of the product obtained by this method is not good. Although the amount of acetic acid is controlled, it is not conducive to the recycling of the catalyst, and there are still corrosion problems.
[0003] At present, it is urgent to solve the problems of equipment corrosion and post-treatment complexity caused by the existence of bromide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0029] Step 1, obtaining a supported composite catalyst; the preparation method of the supported catalyst comprises the following steps:

[0030] The first step is to dry the silica gel at 160°C for 2 hours to remove the adsorbed moisture and volatile substances, and set aside;

[0031] Preferably, the surface area of ​​the silica gel is 30-550m 2 / g, more preferably the surface area of ​​silica gel is 50-500m 2 / g, most preferably the surface area of ​​the silica gel is 100-400m 2 / g;

[0032] The pore volume of silica gel is 0.5-3.0ml / g, more preferably the pore volume of silica gel is 0.5-2.5ml / g, most preferably the pore volume of silica gel is 0.8-2.0ml / g;

[0033] The average particle size of silica gel is 0.5-300 μm. , the average particle diameter of the silica gel is more preferably 1-200 μm, and most preferably the average particle diameter of the silica gel is 10-100 μm.

[0034] In the second step, cobalt acetate and sodium bromide are configured in a molar ra...

Embodiment 1

[0042] 1. Preparation of supported composite catalyst: first dry the silica gel at 160°C for 2 hours, remove the adsorbed moisture and volatile substances, and set aside; in the second step, mix cobalt acetate and sodium bromide in a molar ratio of 1:3, and use Ionized water is configured as a mixed solution, and the silica gel is added to form a sol under stirring conditions, and the silica gel can be impregnated with the same volume of the mixed solution of cobalt acetate and sodium bromide; the sol is left to stand at room temperature for 24 hours , then dried the sol at 160°C, activated at 290°C for 5h, and finally activated at 500°C for 6h to obtain a supported composite catalyst.

[0043] 2. Synthetic reaction of p-tert-butylbenzoic acid: add p-tert-butyltoluene, titanium zeolite and supported catalyst into the reaction kettle, feed a gas mixture containing 90% oxygen and other inert gases, at a temperature of 150°C , The reaction time was 36h, and the crude product of p...

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PUM

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Abstract

The invention provides a synthesis process of p-tert-butylbenzoic acid. The synthesis process comprises the following steps: step 1, preparing a supported composite catalyst; step 2, adding the supported composite catalyst obtained in the step 1 and p-tert-butyltoluene into a reaction kettle, and introducing oxygen to obtain a p-tert-butylbenzoic acid crude product; step 3, cooling and crystallizing the p-tert-butylbenzoic acid crude product obtained in the step 2, performing centrifugal spin-drying, and washing with p-tert-butyltoluene to obtain a centrifugal crude product; and step 4, adding the crude product of tert-butylbenzoic acid obtained in the step 3 into toluene, heating and dissolving, then adding activated carbon and diatomite for decoloration, and then cooling, crystallizing and centrifuging to obtain a refined product of p-tert-butylbenzoic acid. The method has the beneficial effects that the high-quality product can be obtained by simply washing the crude product with water, and the oxidation conversion rate is increased.

Description

technical field [0001] The invention relates to the field of preparation of p-tert-butylbenzoic acid, more specifically to a synthesis process of p-tert-butylbenzoic acid. Background technique [0002] The demand for output of p-tert-butylbenzoic acid products increases year by year. In the prior art, it is intended to obtain pure products by controlling the content of bromine and water. In this method, the content of acetic acid in the medium is low, and the catalyst is recycled, so that the process is simplified, and the content of bromine Lowering also reduces acetic acid corrosion. However, the chroma of the product obtained by this method is not good. Although the amount of acetic acid is controlled, it is not conducive to the recovery and utilization of the catalyst, and there are still corrosion problems. [0003] At present, it is urgent to solve the problems of equipment corrosion and post-treatment complexity caused by the existence of bromide. Contents of the i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/265C07C51/43C07C51/47C07C63/04B01J31/22
CPCC07C51/265C07C51/43C07C51/47B01J31/2226B01J2531/845B01J2531/0213B01J2231/70
Inventor 任荣
Owner 天津鼎晟新化科技有限公司