Method for preparing 2-hydroxybenzonitrile from ammonium salicylate as raw material

A technology of o-hydroxybenzonitrile and ammonium salicylate, applied in the preparation of ammonia-carboxylic acid reaction, organic chemistry, etc., can solve the problem of low content of o-hydroxybenzonitrile, low conversion rate of raw materials, many reaction steps, etc. problem, to achieve the effect of easy stirring and mixing, avoiding the sublimation and decomposition of salicylic acid, and less waste

Inactive Publication Date: 2011-09-07
YANCHENG INST OF TECH
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  • Abstract
  • Description
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Problems solved by technology

[0012] An invention of a method for preparing o-hydroxybenzonitrile by using ammonium salicylate as a raw material, mainly to solve the problems of many reaction steps, complicated process and low conversion rate of raw materials in the existing o-hydroxybenzonitrile preparation method and process Problems in product application performance caused by low, large equipment investment or low o-hydroxybenzonitrile content in the product

Method used

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  • Method for preparing 2-hydroxybenzonitrile from ammonium salicylate as raw material
  • Method for preparing 2-hydroxybenzonitrile from ammonium salicylate as raw material

Examples

Experimental program
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Effect test

Embodiment 1

[0020] After 138 grams of salicylic acid are made into slurry with 400 grams of water, feed ammonia or add ammoniacal liquor wherein, stir and make it form homogeneous solution, until the pH of solution is 8.0 and obtain the aqueous solution containing ammonium salicylate; After the ammonium salicylate solid obtained after the aqueous solution of ammonium salt is transferred to the reactor through evaporation concentration, crystallization, filtration or centrifugation, add 90 grams of urea, 97 grams of sulfamic acid and 1 gram of magnesium oxide, aluminum oxide, oxide Calcium, silicon oxide, artificial zeolite in m 氧化镁 :m 氧化铝 :m 氧化钙 :m 氧化硅 :m 人造沸石 =0.0001: 0.005: 0.8: 0.08: 1.0 constitutes a catalyst and 120 grams of o-cresol, p-cresol, ethylene glycol, methyl salicylate, diphenyl ether and dichlorophenol by m o-cresol Base phenol: m 对甲基苯酚 :m 一缩乙二醇 :m 水杨酸甲酯 :m 二苯醚 :m 二 氯苯酚 = 0.0001: 0.006: 0.0008: 9: 0.01: 0.12, stirring to form a mixed material; heating the mixed m...

Embodiment 2

[0022] After 138 grams of salicylic acid are made into slurry with 200 grams of water, feed ammonia or add ammoniacal liquor wherein, stir and make it form homogeneous solution, until the pH of solution is 9.0 and obtain the aqueous solution containing ammonium salicylate; The ammonium salicylate aqueous solution obtained after evaporation concentration, crystallization, filtration or centrifugation is transferred to the reactor after the solid ammonium salicylate, then add 105 grams of urea, 146 grams of sulfamic acid and 2 grams of magnesium oxide, aluminum oxide, oxide Calcium, silicon oxide, artificial zeolite in m 氧化镁 :m 氧化铝 :m 氧化钙 :m 氧 化硅 :m 人造沸石 =0.001: 0.05: 1.8: 0.8: 2.0 constitute the catalyst and 160 grams by m o-cresol, p-cresol, ethylene glycol, methyl salicylate, diphenyl ether and dichlorophenol Base phenol: m 对甲基苯酚 :m 一缩乙二醇 :m 水杨酸甲酯 :m 二 苯醚 :m 二氯苯酚 = 1.0: 0.6: 0.8: 3: 2.0: 6, stirring to form a mixed material; heating the mixed material to make the t...

Embodiment 3

[0024] After 138 grams of salicylic acid are made into slurry with 500 grams of water, feed ammonia or add ammoniacal liquor wherein, stir and make it form homogeneous solution, until the pH of solution is 10.0 and obtain the aqueous solution containing ammonium salicylate; After the ammonium salicylate solid obtained after the aqueous solution of ammonium salt is transferred to the reactor through evaporation concentration, crystallization, filtration or centrifugation, add 120 grams of urea, 194 grams of sulfamic acid and 5 grams of magnesium oxide, aluminum oxide, oxide Calcium, silicon oxide, artificial zeolite in m 氧化镁 :m 氧化铝 :m 氧化钙 :m 氧化硅 :m 人造沸石 =0.01: 0.5: 8: 8: 1.0 constitutes a catalyst and 180 grams of o-cresol, p-cresol, ethylene glycol, methyl salicylate, diphenyl ether and dichlorophenol by m o-cresol Base phenol: m 对甲基苯酚 :m 一缩乙二醇 :m 水杨酸甲酯 :m 二笨醚 :m 二氯苯酚 = 2.0: 0.6: 1.5: 1.9: 5.0: 3.0 of the solvent, stirring to form a mixed material; heating the mixed m...

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Abstract

The invention discloses a method for preparing 2-hydroxybenzonitrile from ammonium salicylate as a raw material, comprising the following steps of: introducing ammonia gas or ammonia water to a salicylic acid slurry until the pH of the solution is 7.5-13.0, then evaporating to obtain ammonium salicylate solid; forming a mixture from the ammonium salicylate solid, urea, sulfamic acid, a catalyst and a solvent, wherein the catalyst is prepared from 0.0001-10 of magnesium oxide, 0.0001-5 of aluminum oxide, 0.0001-8 of calcium oxide, 0.0001-8 of silicon oxide and 0.0001-10 of artificial zeolite, and the solvent is prepared from 0.0001-10 of o-methyl phenol, 0.0001-6 of p-methyl phenol, 0.0001-8 of diethylene glycol, 0.0001-9 of methyl salicylate, 0.0001-10 of diphenyl oxide and 0.0001-12 of dichlorophenol; and after insulating at 150-180 DEG C for 0.5-10.0 hours and insulating at 190-260 DEG C for 0.5-10.0 hours, filtering or centrifuging the material, evaporating to remove the solvent, crystallizing, recrystallizing, and drying to obtain the 2-hydroxybenzonitrile product of which the mass percentage composition is greater than 90%.

Description

technical field [0001] A method for preparing o-hydroxybenzonitrile by using ammonium salicylate as a raw material involved in the present invention is a novel method for preparing fine organic intermediates containing phenolic hydroxyl aromatic nitrile structures in the field of organic intermediate chemistry in the fine chemical industry. Background technique [0002] O-hydroxybenzonitrile, also known as salicylonitrile, 2-hydroxybenzonitrile, o-hydroxybenzonitrile, 2-cyanophenol, cyanonitrile, o-cyanophenol, o-cyanophenol, the molecular formula is C 7 h 5 NO, molecular weight 119.12, CAS registration number 611-20-1. The melting point of o-hydroxybenzonitrile for general industrial products is 95-98°C, the melting point of pure product is 102-102.5°C, and the boiling point is 149°C / 1.9kPa (14mmHg). It has certain water solubility and is not resistant to strong alkali or strong oxidant Stablize. As a pharmaceutical intermediate, o-hydroxybenzonitrile can be used in the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/53C07C253/22
Inventor 蔡照胜许琦李文青
Owner YANCHENG INST OF TECH
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