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Method for preparing resorcin

A technology for resorcinol and m-dichlorobenzene is applied in the field of preparation of resorcinol by hydrolysis, can solve the problems of high requirements for production equipment and high price of m-phenylenediamine, and achieves easy separation and purification and low price , the effect of less by-products

Active Publication Date: 2007-12-26
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantages are: high requirements for production equipment, the material used for the pipes in contact with the materials in the reaction system is one of tantalum, zirconium or their composite materials, and the price of the raw material m-phenylenediamine is also relatively high

Method used

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  • Method for preparing resorcin
  • Method for preparing resorcin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 1L stainless steel autoclave equipped with stirring, add 50g m-dichlorobenzene, 5g sodium hydroxide, 5g sodium carbonate, 2g lanthanum oxide, and 200g water. After leak test, heat to 220℃, control temperature 220~230℃, and react. After 2 hours, the temperature was lowered to below 30°C after the reaction, and gas chromatograph was used for sampling. In the reaction solution: the content of m-dichlorobenzene is 40.42%; the content of resorcinol is 20.01%; the content of m-chlorophenol is 39.57%. The conversion rate of m-dichlorobenzene was 59.58%. The reaction solution was taken out, filtered, adjusted to pH 2 to 3 with hydrochloric acid, and filtered again. The reaction liquid was extracted with a solvent, and the extractant was distilled under reduced pressure to recover the extractant and m-chlorophenol to obtain 10.01 g of resorcinol, and the yield of resorcinol was 27.1%.

Embodiment 2

[0027] In a 1L stainless steel autoclave equipped with stirring, add 60g m-dichlorobenzene, 30g potassium hydroxide, 5g calcium oxide, 3g lanthanum oxide, and 200g water. After the leak test, heat to 250℃, control the temperature at 245~255℃, and react. After 4 hours, the temperature was lowered to below 30°C after the reaction, and gas chromatograph was used for sampling. In the reaction solution: the content of m-dichlorobenzene is 4.15%; the content of resorcinol is 42.23%; the content of m-chlorophenol is 53.62%. The conversion rate of m-dichlorobenzene was 95.85%. The reaction solution was taken out, filtered, adjusted to pH 2 to 3 with hydrochloric acid, and filtered again. The reaction liquid was extracted with a solvent, and the extractant was distilled under reduced pressure to recover the extractant and m-chlorophenol to obtain 25.33 g of resorcinol, and the yield of resorcinol was 57.1%.

Embodiment 3

[0029] In a 1L stainless steel autoclave equipped with stirring, add 80g m-dichlorobenzene, 30g sodium hydroxide, 5g lanthanum oxide, 2g cuprous chloride, and 300g water. After the leak test, heat to 250℃ and control the temperature to 240~260℃. After the reaction was completed for 8 hours, the temperature was lowered to below 30°C after the reaction, and gas chromatography was used for sampling. In the reaction solution: the content of m-dichlorobenzene is 20.7%; the content of resorcinol is 35.34%; the content of m-chlorophenol is 43.96%. The conversion rate of m-dichlorobenzene was 79.3%. The reaction solution was taken out, filtered, adjusted to pH 2 to 3 with hydrochloric acid, and filtered again. The reaction solution was extracted with a solvent, and the extractant was distilled under reduced pressure to recover the extractant and m-chlorophenol to obtain 28.2 g of resorcinol, and the yield of resorcinol was 41.29%.

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Abstract

This invention relates to a method for preparing high-purity resorcinol. The method comprises: adding m-dichlorobenzene and NaOH aqueous solution of a certain concentration into a high-pressure reaction kettle, adding alkaline catalyst, metal oxide, metal halide and phase-transfer catalyst, starting a stirrer, heating to 220-300 deg.C, keeping for 2-8 h to obtain resorcinol, cooling the reaction solution to normal temperature, filtering, adjusting pH value to 2-3 with HCl, filtering again, extracting the reaction solution with a solvent, distilling the extract to recover the solvent and obtain byproduct m-chlorophenol. Resorcinol remains in the column reactor. The method has such advantages as abundant raw materials, high catalyst performance, high product selectivity, and little pollution.

Description

Technical field [0001] The invention relates to a process technology for synthesizing phenolic compounds by a hydrolysis method, in particular to a preparation method for preparing resorcinol by hydrolysis with m-dichlorobenzene as the main raw material. Background technique [0002] Resorcinol is an important fine organic chemical raw material, widely used in agriculture, dyes, coatings, medicine, plastics, rubber, electronic chemicals and other fields. In tires, hoses and tapes, resorcinol-formaldehyde resin is used to impregnate rayon and polyamide fiber cords to increase the adhesion between the cords and rubber. It can also be used as an adhesive for synthetic fibers, wood, metal, ceramics, plastics, etc. Treating steel cord with resorcinol-triaryl cyanurate-formaldehyde resin can improve the adhesion of steel wire to rubber. [0003] The synthesis and production process of resorcinol mainly includes sulfonated alkali fusion method with benzene as raw material and oxidation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/08C07C29/09
Inventor 张跃严生虎刘建武沈介发马锦国
Owner 溧阳常大技术转移中心有限公司
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