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Process for preparing resorcinol

A technology for resorcinol and a production process, which is applied in the field of resorcinol production technology, can solve the problems of difficulty in scaling up oxidation and extraction separation engineering, no breakthrough in industrialized production, and high technical requirements, and achieves easy control of process conditions, High product yield and the effect of on-site cleaning of the process

Inactive Publication Date: 2006-09-13
HUIFENG CHEM PLANT WUJIANG CITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The sulfonated alkali fusion method produces a large amount of waste water, which causes heavy pollution and high cost
The m-dicumene oxidative hydrolysis method has very little waste water and waste gas, less pollution, and lower cost, but this method has high technical requirements and is restricted by the raw materials of m-dicumene
Many companies have done a lot of work on the production of resorcinol by m-dicumyl oxidation, but oxidation, extraction, separation, and engineering scale-up are quite difficult, and no breakthrough has been made in industrial production so far.

Method used

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  • Process for preparing resorcinol
  • Process for preparing resorcinol
  • Process for preparing resorcinol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 70g m-phenylenediamine, 160g hydrochloric acid (concentration 30%), and 2000g water into a 5L autoclave equipped with stirring and tetrafluoroethylene lined (heated by electric heating coil). After sealing, heat to 200℃ and control the temperature to 200- Reacted at 220°C for 4 hours. After the reaction, the temperature was lowered to room temperature 30°C, and gas chromatography was used to sample. In the reaction solution: the content of m-phenylenediamine is 17.07%; the content of resorcinol is 58.46%; the content of m-aminophenol is 24.47%. The conversion rate of m-phenylenediamine was 82.93%. Adjust the pH to 1-2 with hydrochloric acid, extract with isopropyl ether, and perform gas chromatography on the extract. The purity of resorcinol is 99.84%.

Embodiment 2

[0027] In a 10L autoclave equipped with stirring and lined with tetrafluoroethylene, heated with a zirconium U-tube heat-conducting oil, add 120g m-phenylenediamine, 260g hydrochloric acid ((concentration 30%), 5000g water, heat with heat-conducting oil after leak test When the temperature reaches 220°C, the temperature is controlled at 220-250°C, the reaction is 6 hours, the temperature is lowered, and the gas chromatography is sampled. In the reaction solution: the content of m-phenylenediamine is 1.16%; the content of resorcinol is 97.38%; the content of m-aminophenol is 1.46%. The conversion rate of phenylenediamine was 98.84%. The pH was adjusted to 1-2 with hydrochloric acid, extracted with n-butanol, and the extract was tested by gas chromatography. The purity of resorcinol was 99.48%. The n-butanol was distilled out, and the residue at the bottom of the distillation flask was reduced. After pressure distillation, 85.6 g of white resorcinol was obtained with a chromatograph...

Embodiment 3

[0029] In a 3000L autoclave lined with tetrafluoroethylene, heated with a zirconium tube heat exchanger, add 40Kg of m-phenylenediamine, 80Kg of hydrochloric acid ((concentration 30%), 1600Kg of water, and heat to 220°C after leak testing. The temperature is controlled at 220-250°C, the reaction is 8 hours, and the temperature is reduced to room temperature. The sample is detected by gas chromatography. In the reaction solution: the content of resorcinol is 98.72%; the content of m-aminophenol is 1.28%. The conversion rate of m-phenylenediamine is 100%. Adjust the pH to 1-2 with hydrochloric acid, extract with n-butanol, recover the solvent and distill under reduced pressure to obtain 34Kg of white resorcinol with a yield of 83.45%.

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Abstract

A process for preparing resorcin features that under the action of acidic catalyst, the lentine is directly hydrolyzed to obtain resorcin and metaaminophenol.

Description

Technical field [0001] The invention relates to a manufacturing process of resorcinol, Background technique [0002] In the prior art, resorcinol is mainly used to prepare resorcinol-formaldehyde resin, as a high-performance adhesive, used in rubber and wood processing industries; resorcinol is also widely used in ultraviolet absorbers, dyes, and barriers. Fuels, medicines, pesticides, explosives, electronic chemicals and other fields. [0003] At present, there are two main production processes for resorcinol: one is the sulfonated alkali melting method using benzene as the raw material; the other is the oxidation method using m-dicumene as the raw material. [0004] 1. Alkali melting method for benzene sulfonation: [0005] [0006] 2. m-dicumyl oxidation method [0007] [0008] The sulfonated alkali fusion method produces a large amount of waste water, which causes heavy pollution and high cost. The m-dicumyl oxidative hydrolysis method has very li...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/05C07C39/08
Inventor 王在军石艳李严王龙官孙振荣
Owner HUIFENG CHEM PLANT WUJIANG CITY
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