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Method for synthesizing hydroxylamine salt

A technology of hydroxylamine salt and cyclohexanone oxime, which is applied in the field of preparation of hydroxylamine salt, can solve the problems of low yield of hydroxylamine product, unindustrialization and the like, and achieves the effect of improving atom utilization rate and improving atom utilization rate

Active Publication Date: 2013-11-20
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, hydroxylamine product yield is very low, only about 5%
Because of this, the route has not been industrialized since it was proposed in the 1990s

Method used

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  • Method for synthesizing hydroxylamine salt
  • Method for synthesizing hydroxylamine salt
  • Method for synthesizing hydroxylamine salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Synthesis of cyclohexanone oxime reaction process: Weigh 0.6g of TS-1 molecular sieve and place it in the reactor, then measure 15ml (833.3mmol) of water, 6.4ml (61.6mmol) of cyclohexanone with a content of 99.5% and 25% 10ml of ammonia water (NH 3 The molar mass is 133.6mmol, H 2 O molar weight is 379.2mmol) is added in the reactor; Then, stir, heat up, and reaction liquid is warmed up to 70 ℃ by room temperature, dropwise adds 30% hydrogen peroxide 8ml (H 2 o 2 The molar mass is 79.7mmol, H 2 O molar weight is 351.6mmol), normal pressure reaction 0.25h, reaction finishes. The reaction solution and solid TS-1 catalyst were separated by centrifugation. Toluene was used as the extractant to extract and separate the organic phase in the reaction solution. The content of cyclohexanone oxime in the organic phase was analyzed by gas chromatography. The yield of the intermediate product cyclohexanone oxime was 99.2%. At the same time, the TS-1 catalyst obtained by ce...

Embodiment 2～3

[0034] Same as the operating steps and reaction conditions of the process of preparing hydroxylamine by hydrolysis of cyclohexanone oxime in implementation 1, except that the inorganic acid added in the hydrolysis process is respectively 2ml of concentrated sulfuric acid (H + The molar mass is 71.3mmol, H 2 O molar weight is 10.2mmol), 65% concentrated nitric acid 5ml (H + The molar mass is 72.5mmol, H 2 O molar weight is 136.6mmol), and the finally obtained raffinate aqueous phase is respectively hydroxylamine sulfate mother liquor, hydroxylamine nitrate mother liquor. The organic phase was analyzed by gas chromatography, and the yield of hydroxylamine was quantitatively calculated. The experimental results are shown in Table 2.

[0035] Table 2 Influence of the type of inorganic acid on the hydrolysis reaction of cyclohexanone oxime to produce hydroxylamine

[0036] Example

Embodiment 4

[0038] The operation steps and reaction conditions are the same as in Example 1, except that in the process of producing hydroxylamine by hydrolysis of cyclohexanone oxime, the addition of concentrated hydrochloric acid is changed to 0.5ml (H + The molar mass is 5.9mmol, H 2 O molar weight is 21.3mmol). The organic phase was analyzed by gas chromatography, and the yield of cyclohexanone oxime in the reaction process (1) and the yield of hydroxylamine in the reaction process (2) were quantitatively calculated. The experimental results are shown in Table 3.

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Abstract

The invention relates to a preparation method of hydroxylamine salt, which adopts a hydroxylamine synthesis assembly process. The preparation method comprises the following steps: (1) preparation of cyclohexanone-oxime: carrying out one-step synthesis on ammonia water, oxydol and cyclohexanone by using a titanium silicon molecular sieve as a catalyst and water as a reaction medium to obtain the cyclohexanone-oxime; and (2) synthesis of hydroxylamine: carrying out acidic hydrolysis on the cyclohexanone-oxime to generate he hydroxylamine salt and byproduct cyclohexanone, wherein the generated cyclohexanone can be used as a raw material to reenter the green assembly process and participate in the reaction (1). The invention has the advantages of high atom utilization ratio and high yield of the hydroxylamine salt product, the raw material cyclohexanone (oxime) can be recycled, and the titanium silicon molecular sieve catalyst is reusable, thereby saving the production cost.

Description

technical field [0001] The invention relates to a preparation method of hydroxylamine salt, specifically a process for synthesizing hydroxylamine with ammonia water and hydrogen peroxide as raw materials by means of mutual conversion between cyclohexanone and cyclohexanone oxime, belonging to the technical field of fine chemical products . Background technique [0002] Hydroxylamine is also called pine, and its molecular formula is NH 2 OH, which is a colorless, odorless, deliquescent white flake or needle crystal (Chemical Abstracts, 2004 (4): 41-43). Hydroxylamine is easily soluble in water and methanol, and its monomer is extremely unstable. Therefore, in the process of production and use, hydroxylamine often exists in the form of salt. At present, the main hydroxylamine salts include hydroxylamine sulfate, hydroxylamine hydrochloride and hydroxylamine nitrate. Hydroxylamine salt is an important chemical raw material, which has a wide range of uses in the synthesis of...

Claims

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Application Information

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IPC IPC(8): C01B21/14C07C49/403C07C45/42
CPCY02P20/584
Inventor 王延吉张东升徐元媛金常青张广林薛伟王淑芳赵新强
Owner HEBEI UNIV OF TECH
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