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A kind of method that utilizes salicylic acid residue to decompose and recover sodium phenolate

A technology of salicylic acid and sodium phenolate, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of high cracking temperature and low yield of phenol

Active Publication Date: 2021-08-06
QINGDAO UNIV OF SCI & TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In patent CN103073394A, the residue is heated and cracked in a cracking furnace, and purified by distillation to obtain phenol, but the cracking temperature is high (450-550°C), and the yield of phenol is low (about 30%)

Method used

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  • A kind of method that utilizes salicylic acid residue to decompose and recover sodium phenolate
  • A kind of method that utilizes salicylic acid residue to decompose and recover sodium phenolate
  • A kind of method that utilizes salicylic acid residue to decompose and recover sodium phenolate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The mass composition of salicylic acid residues: 32.3% of water, 48.1% of salicylic acid, 10.6% of 4-hydroxyisophthalic acid, 0.8% of p-hydroxybenzoic acid, 8.2% of inorganic salts and other components.

[0033] Add 5000kg of reaction medium water (S1) in the reactor 1. After starting the stirring, add 2000kg of salicylic acid residue (S2), and the ratio of residue to water is 0.4:1. Seal the feeding port, after the nitrogen replacement is qualified, close the pressure regulating valve 3 on the exhaust line, start heating the material in the reactor 1, set the reaction temperature to 180°C (at this temperature, the saturated vapor pressure of water is 1.02MPa), and the condenser 2 To cool the water, open the washing water pump 5 to feed the washing tower 4 with washing water (S9), and the washing water is recycled. When the pressure rises to 1.3MPa, the opening pressure regulating valve 3 is set to automatic, and the pressure setting value is 1.3MPa. The reaction exha...

Embodiment 2

[0035] Salicylic acid residue quality composition, the proportioning of residue and water is the same as Example 1. The reaction temperature is set at 200° C. (the saturated vapor pressure of water at this temperature is 1.55 MPa), and the reaction pressure set value is 1.8 MPa. After 150 minutes of reaction, the exhaust gas was reduced, the pressure regulating valve 3 was automatically closed, and the reaction was completed. Other operations are the same as Example 1. This reaction obtains 7200kg of sodium phenate solution, the sodium phenate content of sampling analysis is 13.1%, and the calculated phenol yield is 98.2%.

Embodiment 3

[0037] The salicylic acid residue quality composition is the same as Example 1. The ratio of residue to water is 0.3:1, 1500kg and 5000kg respectively. The reaction temperature is set at 210° C. (the saturated vapor pressure of water at this temperature is 1.91 MPa), and the reaction pressure is set at 2.3 MPa. After 70 minutes of reaction, the exhaust gas was reduced, the pressure regulating valve 3 was automatically closed, and the reaction was completed. Add about 550kg of 50% sodium hydroxide solution (S3), the pH is 12.6, and then add 20kg of activated carbon (S4). Other operations are the same as Example 1. This reaction obtains about 6700kg of sodium phenate solution, and the sodium phenate content of sampling analysis is 10.5%, and the calculated phenol yield is 97.9%.

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Abstract

The invention discloses a method for decomposing and recovering sodium phenolate by utilizing salicylic acid residue, comprising the following steps: adding water into a reaction kettle, starting stirring, and then adding solid salicylic acid residue; controlling the pressure in the reaction kettle, heating the reaction kettle When the material reaches 160-220°C, the reaction exhaust gas enters the condenser for condensation, and the phenol and water in it are condensed and refluxed into the reactor. Use water; after the reaction is completed, the pressure is released and cooled, and sodium hydroxide is added to the reaction kettle to control the pH value to be 12-13; finally, activated carbon is added to the reaction kettle, adsorbed and decolorized, and filtered to obtain a sodium phenolate solution. The method disclosed in the invention enables the salicylic acid residue to be recycled, only generates a small amount of activated carbon solid waste, has little impact on the environment, and belongs to an environment-friendly treatment process.

Description

technical field [0001] The invention relates to a process for treating salicylic acid residues, in particular to a method for recovering sodium phenate by decomposing salicylic acid residues. Background technique [0002] Salicylic acid is an important pharmaceutical and chemical raw material. Salicylic acid is mainly produced by the Kolbe-Schmitt method (abbreviated as Ke method) in the industry. The raw materials are phenol, carbon dioxide, sodium hydroxide, sulfuric acid, etc. The products mainly include two specifications of industrial grade salicylic acid and sublimated salicylic acid. Industrial grade salicylic acid is produced by vacuum sublimation, and it is mainly used as a pharmaceutical raw material. After the sublimation of industrial grade salicylic acid, about 5% brown residue is produced, and its main components are 4-hydroxyphthalic acid, salicylic acid, salicylic acid isomers, inorganic salts, etc. [0003] Most of the components in the salicylic acid resi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/66C07C39/235C07C37/50C07C39/04
CPCC07C37/50C07C37/66C07C39/235C07C39/04
Inventor 岳金彩郑世清赵彦恒葛纪军夏丙堃吴孝好
Owner QINGDAO UNIV OF SCI & TECH
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