Method for preparing free hydroxylamine

A technology of free hydroxylamine and tert-butanol, which is applied in the direction of hydroxylamine, nitrogen and non-metallic compounds, can solve the problems of complex reaction process, many by-products, and low yield of hydroxylamine, and achieve simple reaction process, mild reaction conditions, and hydroxylamine The effect of high yield

Active Publication Date: 2013-07-10
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of these processes are: the process is long, the reaction process is complicated, and there are many by-products. Some processes need to use strong acids such as hydrochloric acid. These processes are environmentally unfriendly processes.
The disadvantages of this process are: the amount of ammonia is large, the yield of hydroxylamine is low, and hydroxylamine is easily decomposed to generate nitrogen oxides, nitrogen or nitrate, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a. Preparation of reaction system

[0022] Ti-MOR titanium silicon molecular sieve is used as a catalyst, tert-butanol aqueous solution and ammonia with a mass concentration of 28% are stirred and mixed in a reactor at a weight ratio of 1:50:120 to form a reaction system. The tert-butanol aqueous solution is tert-butanol and Pure water is mixed at a weight ratio of 1:5.

[0023] b, the synthetic reaction of free hydroxylamine

[0024] Heat the above reaction system, when the temperature of the reactor rises to 40°C, add hydrogen peroxide with a mass concentration of 5% to the reaction system dropwise or at one time, the mass ratio of hydrogen peroxide to catalyst is 6:1, and the dropwise addition time For 20 minutes, the reaction was continued for 10 minutes after the dropwise addition was completed, and the pressure of the reaction system was normal pressure.

[0025] c, the extraction of free hydroxylamine

[0026] After the above reaction was finished, the catalys...

Embodiment 2

[0028] a. Preparation of reaction system

[0029] TS-1 titanium silicon molecular sieve is used as catalyst, tert-butanol aqueous solution and ammonia with a mass concentration of 28% are stirred and mixed in the reactor at a weight ratio of 1:50:100 to form a reaction system. The tert-butanol aqueous solution is tert-butanol and Pure water is mixed at a weight ratio of 1:5.

[0030] b, the synthetic reaction of free hydroxylamine

[0031] Heat the above reaction system, when the temperature of the reactor rises to 50°C, add hydrogen peroxide with a mass concentration of 5% to the reaction system dropwise or at one time, the mass ratio of hydrogen peroxide to catalyst is 5:1, and the time for dropping For 25 minutes, the reaction was continued for 10 minutes after the dropwise addition was completed, and the pressure of the reaction system was normal pressure.

[0032] c, the extraction of free hydroxylamine

[0033] After the above reaction was finished, the catalyst in th...

Embodiment 3

[0035] a. Preparation of reaction system

[0036] Ti-MWW titanium-silicon molecular sieve is used as catalyst, tert-butanol aqueous solution and 28% ammonia are stirred and mixed in the reactor at a weight ratio of 1:25:120 to form a reaction system. The tert-butanol aqueous solution is tert-butanol and Pure water is mixed at a weight ratio of 1:5.

[0037] b, the synthetic reaction of free hydroxylamine

[0038] Heat the above reaction system, when the temperature of the reactor rises to 40°C, add hydrogen peroxide with a mass concentration of 5% to the reaction system dropwise or at one time, the mass ratio of hydrogen peroxide to catalyst is 4:1, and the time for dropping For 20 minutes, the reaction was continued for 10 minutes after the dropwise addition was completed, and the pressure of the reaction system was normal pressure.

[0039] c, the extraction of free hydroxylamine

[0040] After the above reaction was finished, the catalyst in the reaction system was filte...

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PUM

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Abstract

The invention discloses a method for preparing free hydroxylamine. The method is characterized by comprising the steps of mixing hydrogen peroxide and water solution of ammonia and tertiary butanol under the catalysis effect of a titanium-silicon molecular sieve, and then synthetizing free hydroxylamine solution of which the mass concentration is 0.15-10% by one step, wherein the weight ratio of the titanium-silicon molecular sieve to the tertiary butanol water solution to the ammonia to the hydrogen peroxide is 1 to (20-170) to (6-600) to (3-10). Compared with the prior art, the method has the advantages of mild reaction condition, high hydroxylamine yield, and simple reaction process; hydroxyl ammonium salt is not formed; the method is friendly to the environment and easy to achieve large-scale industrial production; the pollution to the environment is reduced; and green chemical development is facilitated.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to a preparation method of free hydroxylamine. Background technique [0002] Hydroxylamine is a reducing agent in organic synthesis, which condenses with carbonyl compounds to form oximes. The molecular formula of hydroxylamine is NH2OH, which can be regarded as a derivative formed by replacing a proton in NH3 with a hydroxyl group. It is an unstable white crystal at room temperature, easy to deliquescence, and often exists in the form of aqueous solution. Hydroxylamine has two isomers, cis and trans, trans in the solid state, and a mixture of cis and trans in the gaseous state. At present, there are three main methods for the preparation of hydroxylamine: the first method is to thermally decompose certain hydroxylamine compounds; the second method is to react hydroxylamine hydrochloride with alcohol; the third method is to react nitrite and sulfur dioxide. The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/14
Inventor 吴鹏徐乐吴静丁姜宏黄仕杰杨玉林吴海虹
Owner EAST CHINA NORMAL UNIV
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