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Preparation method of salicylamide

A technology of salicylamide and preparation steps, applied in the field of preparation of salicylamide, can solve problems such as a large amount of waste water, low yield, complicated purification process, etc., and achieve the effects of high yield, high product purity, and no variegated appearance.

Inactive Publication Date: 2012-01-04
TAINING SHENGDA INDAL
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  • Abstract
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AI Technical Summary

Problems solved by technology

The salicylic acid ammoniation method is to use salicylic acid as raw material, add ammonia water to aminate under appropriate conditions, the products obtained by this method often have a pink color, and the product refining and purification process is complicated and the yield is low
The methyl salicylate ammonification method mainly uses methyl salicylate as a raw material, adding ammonia water and stirring at 30-40°C for reaction, the reaction solution is cooled and acidified, and salicylamide crystals are precipitated. The disadvantage of this method is that The production process produces a large amount of waste water

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0011] A kind of preparation method of salicylamide, in 1000 liters of stainless steel reactors, add 150 kilograms of methyl salicylate, 420 kilograms of toluene, heat to 40~45 ℃, continue feeding ammonia gas to carry out ammoniation reaction, reaction temperature control At 40-45°C, the reaction pressure is controlled at 0.25-0.35 MPa, stop feeding ammonia after 5 hours of ammoniation reaction, then heat to recover toluene and reaction by-product methanol, cool the remaining material to 20°C, crystallize and centrifuge to obtain water Yangamide, the yield reached 97.8%.

Embodiment 2

[0013] A kind of preparation method of salicylamide, in 1000 liters of stainless steel reactor, add 150 kilograms of methyl salicylate, 450 kilograms of toluene, heat to 40~45 ℃, continue feeding ammonia gas to carry out ammoniation reaction, reaction temperature control At 40-45°C, the reaction pressure is controlled at 0.3-0.35 MPa. Stop feeding ammonia after 5.5 hours of ammoniation reaction, then heat to recover toluene and reaction by-product methanol, cool the remaining material to 25°C, crystallize and centrifuge to obtain water Salicylic amide, the yield reached 98.4%.

Embodiment 3

[0015] A kind of preparation method of salicylamide, in 1000 liters of stainless steel reactor, add 150 kilograms of methyl salicylate, 480 kilograms of toluene, heat to 40~45 ℃, continue feeding ammonia gas to carry out ammoniation reaction, reaction temperature control At 40-45°C, the reaction pressure is controlled at 0.25-0.3 MPa. Stop feeding ammonia gas after 6 hours of ammoniation reaction, then heat to recover toluene and reaction by-product methanol, cool the remaining material to 22°C, crystallize and centrifuge to obtain water Salicylic amide, the yield reached 98.1%.

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Abstract

The invention relates to a preparation method of salicylamide, which comprises the following steps: adding methyl salicylate and methylbenzene in a weight ratio of 1:(2.8-3.2) into a reaction kettle, heating to 40-45 DEG C, and continuously introducing to carry out ammonification reaction, wherein the reaction temperature is controlled at 40-45 DEG C, and the reaction pressure is controlled at 0.25-0.35MPa; and after the reaction is carried out for 5-6 hours, stopping introducing the ammonia gas, heating to recycle the methylbenzene and the reaction byproduct methanol, cooling the residual material to 20-25 DEG C, crystallizing, and centrifugalizing to obtain the salicylamide. The salicylamide prepared by the preparation method provided by the invention has the advantages of high yield, high product purity, and no assorted colors on the appearance; no waste water is generated in the whole production process; both the methylbenzene and the reaction byproduct methanol can be recycled and reused; and thus, the invention provides an environment-friendly production method.

Description

technical field [0001] The invention relates to a preparation method of salicylamide. Background technique [0002] Salicylamide, whose scientific name is 2-hydroxybenzamide, is a very important organic synthesis intermediate and a raw material for the synthesis of many of its important derivatives (such as analgesic and antipyretic drugs, molluscicides, etc.). Widely used in medicine, spices, dyes, rubber additives and many other fields. [0003] At present, the preparation method of salicylamide is mainly ammoniation method, and the ammoniation method mainly includes salicylic acid ammoniation method and methyl salicylate ammoniation method. The salicylic acid ammonification method is to use salicylic acid as raw material, add ammonia water to aminate under appropriate conditions, the product obtained by this method is often pinkish, and the product refining and purification process is complicated and the yield is low. The methyl salicylate ammonification method mainly u...

Claims

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Application Information

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IPC IPC(8): C07C235/60C07C231/02
Inventor 张小兵江戈华卢远勤陈胜林汪家良梁智宏
Owner TAINING SHENGDA INDAL
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