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A composite oxide catalyst for synthesizing salicylamide from urea and phenol, its preparation method and application

A composite oxide, salicylamide technology, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, carboxylic acid amide preparation, etc., can solve the problem of low salicylamide yield and stable catalyst structure problems such as poor performance, to achieve the effect of being conducive to industrialization, easy to operate, and widely used

Inactive Publication Date: 2018-04-24
ZAOZHUANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the shortcomings of the existing urea and phenol synthesis of salicylamide technology, the conversion rate of urea and the yield of salicylamide are low, and the stability of the catalyst structure is poor.

Method used

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  • A composite oxide catalyst for synthesizing salicylamide from urea and phenol, its preparation method and application
  • A composite oxide catalyst for synthesizing salicylamide from urea and phenol, its preparation method and application
  • A composite oxide catalyst for synthesizing salicylamide from urea and phenol, its preparation method and application

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preparation example Construction

[0031] The present invention also provides the preparation method of described catalyst, comprises the following steps:

[0032] In the first step, the nitrate of magnesium nitrate, aluminum nitrate and metal M is pressed by catalyst metal Mg x Al y m z o m The molar composition was dissolved in deionized water at the same time to form a 100 mL solution with a catalyst concentration of 0.2-1.0 mol / L; at the same time, NaOH and Na 2 CO 3 Dissolved in 100 mL of deionized water as a precipitant to prepare a precipitant, in which NaOH and Na 2 CO 3 The amount of the substance is respectively 2 times and 1 / 5 of the sum of the amount of metal nitrate substances;

[0033] In the second step, control the temperature in a water bath at 40-60 o C. Drop the above-mentioned mixed nitrate solution and precipitant into 100 mL deionized water at the same time, stir vigorously, and keep the pH value of the solution at 8-12 at the same time, and the dropwise addition is completed in abo...

Embodiment 1

[0041] Take 0.02mol Mg(NO 3 ) 2 ·6H 2 O, 0.01mol Al(NO 3 ) 3 9H 2 O and 0.002mol Ni(NO 3 ) 2 ·6H 2 O was dissolved in 100 mL of deionized water, and the total concentration of the three metal salts was 0.32 mol / L. At the same time, NaOH and Na 2 CO 3 Dissolve in 100mL deionized water to prepare a precipitant, wherein the concentration of NaOH is 0.64 mol / L, NaOH 2 CO 3 The concentration is 0.064 mol / L, and the water bath controls the temperature at 60 o C. Under vigorous stirring, drop the above mixed salt solution and precipitant into 100 mL deionized water at the same time, keep the pH value of the solution at 9, and complete the dropwise addition in 1 h. After precipitation is complete, 80 o C hydrothermal treatment for 15 h. The mixture after decompression suction filtration water heat treatment is washed with deionized water until the filtrate is neutral, and then the filter cake is o C drying to obtain the precursor of the catalyst. Finally in N 2 Atmosp...

Embodiment 2

[0048] Take 0.03mol Mg(NO 3 ) 2 ·6H 2 O, 0.01mol Al(NO 3 ) 3 9H 2 O and 0.005mol La(NO 3 ) 3 ·6H 2 O was dissolved in 100 mL of deionized water, and the concentration of the metal salt was 0.45 mol / L. At the same time, NaOH and Na 2 CO 3 Dissolve in 100 mL deionized water to prepare the precipitant. Control the temperature in a water bath at 50 o C. Drop the above-mentioned mixed salt solution and precipitant into 100 mL deionized water at the same time, stir vigorously, and keep the pH value of the solution at 10, and the dropwise addition is completed within 1.2 h. After precipitation is complete, the colloid of gained is placed in the crystallization still, at 80 o C hydrothermal treatment for 20 h. The mixture after water heat treatment was filtered under reduced pressure, and washed repeatedly with deionized water until the filtrate was neutral. Then filter cake at 100 o C drying to obtain the precursor of the catalyst, and finally in N 2 atmosphere at 450...

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Abstract

The invention discloses a composite oxide catalyst for compounding salicylamide by urea and phenol, a preparation method and application of the composite oxide catalyst. The preparation method comprises the steps of taking nitrate of various metal as a starting material, taking sodium hydroxide and sodium carbonate as a precipitant, preparing a hydrotalcite-like precursor by adopting a method that coprecipitation is performed first, and then hydro-thermal treatment is performed, performing high-temperature calcination, and obtaining the composite oxide catalyst represented in the following general formula: MgxAlyMzOm, wherein M is one of alkaline-earth metal, transition metal or rare-earth metal. Compared with the prior art, the composite oxide catalyst has the advantages of simple preparation method, large specific surface, high activity and the like. Under the effect of the catalyst, the conversion rate of urea can reach 100 percent, the yield of the salicylamide is greater than 99 percent. Meanwhile, the composite oxide catalyst is easy to separate and recycle, and good in catalytic stability, is free from pollution of environment and production equipment, and can still keep higher catalytic activity without regeneration.

Description

technical field [0001] The invention relates to the technical field of industrial catalysts, in particular to a catalyst for synthesizing salicylamide from urea and phenol, a preparation method and application thereof. Background technique [0002] Salicylamide, also known as 2-hydroxybenzamide, is an important basic chemical raw material. It can be used as an intermediate in the synthesis of fine chemicals such as pharmaceuticals, spices and rubber additives. More importantly, salicylamide is also used as an antipyretic and analgesic, which has significant curative effects in the treatment of fever, headache, neuralgia, arthralgia and rheumatic arthralgia. The traditional method of producing salicylamide mainly contains salicylic acid ammoniation method and methyl salicylate ammoniation method, both of which use phenol as raw material, react with strong base to obtain sodium phenate, and then the latter reacts with CO 2 The action generates sodium salicylate, and then aci...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755B01J23/10B01J21/10B01J23/02B01J37/03B01J37/08C07C231/10C07C235/60
CPCB01J23/002B01J23/04B01J23/10B01J23/755B01J37/03B01J37/086B01J2523/00C07C231/10B01J2523/22B01J2523/24B01J2523/31B01J2523/48B01J2523/3706B01J2523/847C07C235/60
Inventor 王登峰张学兰刘春丽黄薇王峰盛振腾张晓萍
Owner ZAOZHUANG UNIV
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