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Recovery method for byproduct, p-chlorobenzoic acid, during production of p-chlorobenzaldehyde

A technology of p-chlorobenzaldehyde and p-chlorobenzoic acid, which is applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carboxylic acid compounds, etc., can solve the problem of reducing the purity of p-chlorobenzoic acid, increasing industrial costs, and unfavorable Reuse and other issues to achieve the effect of low recycling cost, good quality and simple recycling process

Active Publication Date: 2018-12-18
江苏超跃化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But when this process is applied to the recovery of by-product p-chlorobenzoic acid in the production process of p-chlorobenzaldehyde, it is found that p-chlorobenzaldehyde is slightly soluble in water, and the p-chlorobenzoic acid extracted with hot water contains more than 1% p-chlorobenzoic acid. Chlorobenzaldehyde reduces the purity of p-chlorobenzoic acid, which is not conducive to its reuse
In addition, the purification process is complicated again, which increases its industrial cost

Method used

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  • Recovery method for byproduct, p-chlorobenzoic acid, during production of p-chlorobenzaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Pump 5000 L of washing water from the production of p-chlorobenzaldehyde into the enamel reaction kettle, add 10 kg of potassium permanganate, raise the temperature to 60 ± 5 °C for 2 h, and let it settle for 1 h to remove the mechanical impurities and Organic insoluble matter; use negative pressure to extract 3200 L of the solution into another enamel reaction kettle, add 640 kg of toluene, and add 290 L of industrial hydrochloric acid (31%) dropwise. At this time, the pH of the solution is 6 ~ 7, and stir well 1 ~ 1.5h, all the p-chlorobenzoic acid in the solution is precipitated, and when the temperature rises to 70 ± 5 ℃, the p-chlorobenzoic acid is completely dissolved in toluene, and the layers are separated after standing, and the liquid in the water layer is transported to the waste water tank, and then sent to the sewage treatment Station, the organic layer was cooled to normal temperature; the organic layer was cooled with refrigerated brine and started to stir...

Embodiment 2

[0030] Pump 5000 L of washing water from the production of p-chlorobenzaldehyde into an enamel reaction kettle, add 15 kg of hydrogen peroxide, heat up to 60±5°C for 2 h of oxidation, let it settle for 1 h, and remove mechanical impurities and organic insolubles in the lower layer ; Extract 3200 L of the solution in another enamel reaction kettle with negative pressure, add 640 kg of toluene, and add 290 L of industrial hydrochloric acid (31%) dropwise. After 1.5 hours, all the p-chlorobenzoic acid in the solution was precipitated, and when the temperature was raised to 70±5°C, the p-chlorobenzoic acid was completely dissolved in toluene, allowed to stand for stratification, and the liquid in the water layer was transported to the waste water tank, and then sent to the sewage treatment station. Cool the organic layer to room temperature; cool the organic layer with refrigerated brine and start stirring, and continue stirring for 1 h when the temperature drops to 0 °C, all p-chl...

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Abstract

The invention relates to a recovery method for byproduct, p-chlorobenzoic acid, during production of p-chlorobenzaldehyde, wherein the method includes oxidization, crude processing, fine processing and drying processes. By means of the method, the p-chlorobenzoic acid, recycled from washing water during the production of p-chlorobenzaldehyde, is high in purity and is low in content of p-chlorobenzaldehyde. The method is simple in process and low in recovery cost, and is free of environmental pollution. In addition, methylbenzene used in the recovery process can be recycled, so that the methodsatisfies the idea of green chemistry.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for recovering by-product p-chlorobenzoic acid in the production process of p-chlorobenzaldehyde. Background technique [0002] p-Chlorobenzoic acid is a kind of drug intermediate that can be developed mainly, and can be used in the production of organic chemical raw materials and pesticides. It is also a drug intermediate variety, which can be used in the synthesis of non-steroidal anti-inflammatory and analgesic drugs, dye synthesis, and analytical reagents. p-Chlorobenzoic acid is the intermediate of the fungicide dimethomorph, the rodenticide, coumatethin and the insecticide bifenthrin; it can also be used as a standard sample for the determination of carbon, hydrogen and chlorine in organic trace analysis. [0003] The preparation of p-chlorobenzoic acid is generally based on easily available p-chlorotoluene as a raw material. The synthesis methods includ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/285C07C51/16C07C51/42C07C51/43C07C51/48C07C63/70
CPCC07C51/16C07C51/285C07C51/42C07C51/43C07C51/48C07C63/70
Inventor 薛宝安任坚跃刘林佳
Owner 江苏超跃化学有限公司
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