One-step synthesis of salicylic acid from phenol and supercritical carbon dioxide

A carbon dioxide and supercritical technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of difficult recovery and recycling of catalysts, complex post-processing, and inability to realize continuous production, etc., to improve selectivity , simple separation, and the effect of simplifying the traditional process

Active Publication Date: 2018-03-23
CHINA PETROLEUM & CHEM CORP
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

This method is simple in process, but the post-treatment is complicated, and the catalyst is difficult to recover and recycle.
[0008] The above-mentioned salicylic acid synthesis methods are all carried out in high-pressure reactors, which belong to indirect or semi-continuous production processes, and continuous production cannot be realized.

Method used

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  • One-step synthesis of salicylic acid from phenol and supercritical carbon dioxide
  • One-step synthesis of salicylic acid from phenol and supercritical carbon dioxide
  • One-step synthesis of salicylic acid from phenol and supercritical carbon dioxide

Examples

Experimental program
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Effect test

preparation example Construction

[0027] Preparation of supported potassium carbonate catalyst:

[0028] In the first step, potassium carbonate is prepared into an aqueous solution with a certain mass fraction; in the second step, the carrier and the binder are uniformly mixed; in the third step, the potassium carbonate solution is added to the mixture of the carrier and the binder, kneaded evenly, and extruded into strips. After the molded catalyst was dried at room temperature for a period of time, it was calcined at 500° C. for 5 hours to obtain a supported potassium carbonate catalyst.

Embodiment 1

[0030] Catalysts with different loadings of potassium carbonate were prepared with activated carbon as the carrier and aluminum gel as the binder. In a fixed-bed tubular reactor, the temperature is 190°C, the pressure is 8Mpa, and the space velocity is 0.3h -1 Under these conditions, salicylic acid was synthesized from phenol and supercritical carbon dioxide, and the effects of different loadings of potassium carbonate on the conversion of phenol and the selectivity of salicylic acid were investigated. The specific results are shown in Table 1.

[0031] Table 1 Effects of different potassium carbonate loadings on phenol conversion and salicylic acid selectivity

[0032]

Embodiment 2

[0034] The load of potassium carbonate was 15%, and the other conditions were the same as in Example 1 to investigate the influence of different carriers on the conversion rate of phenol and the selectivity of salicylic acid. The specific results are shown in Table 2.

[0035] Table 2 Effects of different carriers on the conversion rate of phenol and the selectivity of salicylic acid

[0036]

[0037]

[0038] Salicylic acid synthesis reaction:

[0039] The catalyst prepared by using activated carbon as a carrier with a potassium carbonate load of 15% was packed in a fixed-bed tubular reactor, and phenol and supercritical carbon dioxide passed through the reactor continuously to generate salicylic acid. The effects of different temperatures, pressures and space velocities on the conversion of phenol and the selectivity of salicylic acid were investigated.

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Abstract

The invention relates to a one-step method for synthesizing salicylic acid with phenol and supercritical carbon dioxide, and relates to the technical field of salicylic acid synthesis. According to the method, supported potassium carbonate is adopted as a catalyst, and salicylic acid is synthesized with phenol and supercritical carbon dioxide. According to the invention, supported potassium carbonate is adopted as the catalyst, such that the product can be easily separated from the catalyst. A traditional process flow is simplified, and pickling and washing processes in the traditional processes are eliminated, such that the method is a green and clean production process. With the method, phenol conversion rate and salicylic acid selectivity are improved, and continuous production is realized. With the method, the phenol conversion rate can reach 100%, and the salicylic acid selectivity is up to 99.3%.

Description

technical field [0001] The invention relates to a method for synthesizing salicylic acid in one step from phenol and supercritical carbon dioxide, belonging to the technical field of salicylic acid synthesis. Background technique [0002] Salicylic acid, also known as o-hydroxybenzoic acid, is an important intermediate in the fields of medicine, dyes, and chemical preparations. In the pharmaceutical industry, salicylic acid is mainly used in the production of Zhitongling, diuretic, aspirin (acetylsalicylic acid) and other drugs; in the dye industry, salicylic acid is used in the preparation of mordant pure yellow, direct brown 3GN, acid chromium Huang et al.; Salicylic acid can also be used as rubber vulcanization retarder and disinfection preservative. [0003] The known synthetic method of salicylic acid is all to use phenol as raw material, first react with sodium hydroxide solution to form sodium phenate, then pass into carbon dioxide under normal pressure or medium pre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C65/10C07C51/15
CPCY02P20/54
Inventor 王申军马瑞杰菅秀君贾庆龙
Owner CHINA PETROLEUM & CHEM CORP
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