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Catalyst for synthesis salicylamide and its preparation method and application

A technology of salicylamide and catalyst, which is applied to solid catalyst, preparation method and application field, and achieves the effects of mild reaction conditions, simple preparation method and high catalytic activity

Inactive Publication Date: 2007-10-17
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After searching, we did not find any report on using a catalyst to catalyze the synthesis of salicylamide from urea and phenol

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The content of CaO in the catalyst is 10% (wt), and that of ZnO is 90% (wt). Ca(NO 3 ) 2 solution, the molar concentration of 0.3M Zn(NO 3 ) 2 solution, and 10% (volume content) ammonia solution; under continuous stirring, the above solution was slowly added dropwise to the beaker at the same time, the temperature was controlled at 50°C, and the pH of the precipitate was 8.5. After the precipitation is complete, it is aged for 3 hours, and washed repeatedly with distilled water until neutral; the washed precipitate is dried at 90°C, and then placed in a horse-boiling furnace and roasted at 350°C for 6 hours to obtain the catalyst. Urea and phenol are joined in the reactor of 100ml by 1: 1 by molar ratio, catalyst consumption is 0.5% (wt) of urea and phenol total consumption, reaction temperature 100 ℃, reaction time is 12h, gained product is diluted through methanol, After centrifugation, the supernatant was collected and analyzed by high performance liquid chromato...

Embodiment 2

[0021] The content of CaO in the catalyst is 15% (wt), and that of ZnO is 85% (wt). Ca(NO 3 ) 2 solution, the molar concentration of 0.15M Zn(NO 3 ) 2 solution, and 15% (volume content) ammonia solution; under continuous heating and stirring, the above solution was slowly added dropwise to the beaker at the same time, the temperature was controlled at 30°C, and the pH of the precipitate was 10. After the precipitation is complete, it is aged for 1 hour, and washed repeatedly with distilled water until neutral; the washed precipitate is dried at 105°C, and then placed in a horse-boiler furnace at 550°C for 2 hours to prepare the catalyst. Urea and phenol are joined in the reactor of 100ml with molar ratio of 1: 10, catalyst consumption is 30% (wt) of the total consumption of urea and phenol, 250 ℃ of reaction temperature, the reaction time is 10h, and the gained product is diluted through methanol, After centrifugation, the supernatant was collected and analyzed by high per...

Embodiment 3

[0023] The content of CaO in the catalyst is 15% (wt), and that of ZnO is 85% (wt). Ca(NO 3 ) 2 solution, the molar concentration of 0.2M Zn(NO 3 ) 2 solution, and 15% (volume content) ammonia solution; under continuous heating and stirring, the above solution was slowly added dropwise to the beaker at the same time, the temperature was controlled at 30°C, and the pH of the precipitate was 10. After the precipitation is complete, it is aged for 1 hour, and washed repeatedly with distilled water until neutral; the washed precipitate is dried at 105°C, and then placed in a horse-boiler furnace at 550°C for 2 hours to prepare the catalyst. Add urea and phenol into a 100ml reactor in a molar ratio of 1:50, the amount of catalyst used is 30% (wt) of the total amount of urea and phenol, the reaction temperature is 200°C, and the reaction time is 10h. The resulting product is diluted with methanol and centrifuged After separation, the supernatant was taken and analyzed by high pe...

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PUM

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Abstract

Disclosed is a catalyst of synthetic salicylamide, which has mass percent compositions of 10.0-30.0% calcium oxide and 70.0-90.0% zinc oxide. The catalyst is prepared by a precipitation method. The synthetic salicylamide is formed by adding carbamide and phenol having mol ratio of 1:1-1:50, and adding 0.5-30% catalyst, based on total weight of the reactant, into a reaction vessel; rising temperature of the reaction vessel to 100-250 DEG C., in a condition of agitating, to react for 2-24 hours; and removing the catalyst by diluting and centrifugal settling. The invention has advantages of cheap reaction material easy to get, simple preparing method of the catalyst, high selectivity of salicylamide and mild reaction condition.

Description

technical field [0001] The invention belongs to a solid catalyst, its preparation method and application, in particular to a solid catalyst for synthesizing salicylamide with urea and phenol, its preparation method and application. Background technique [0002] Salicylamide (salicylamide, structural formula is 2-(HO)C 6 h 4 CONH 2 ) scientific name is 2-Hydroxylbenzamide (2-Hydroxylbenzamide), which is a very important intermediate in organic synthesis and is used for the synthesis of many important derivatives (such as molluscicide nifesamide, analgesic and antipyretic drug o Ethoxybenzamide, etc.) are widely used in medicine, spices, dyes, rubber additives and many other fields. At the same time, salicylamide is also an antipyretic and analgesic that is widely accepted and used in large quantities. It is used for fever, headache, neuralgia, arthralgia and active rheumatism, etc., and has a very good therapeutic effect. After searching, we did not find any report on usi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/06B01J23/02C07C235/34C07C231/10
Inventor 孙予罕魏伟彭伟才赵宁肖福魁赵文波李军平王秀芝
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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