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Method for preparing salt of hydroxylamine by using 'coupling' technique of reactive extraction

A hydroxylamine salt and reaction technology, applied in the field of preparing hydroxylamine salt, can solve the problems of unstable product quality, complicated process route, long process flow and the like, and achieve the effects of realizing large-scale industrial production, simple process process and few by-products

Inactive Publication Date: 2007-12-26
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The above-mentioned methods generally have complex process routes, long process flow, unstable product quality, troublesome post-processing, and low yields.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A. Measure 250mL of tri-n-butylamine with a purity greater than 95% and place it in a 2L conical flask with a graduated cylinder, then add 750mL of isoamyl alcohol with a purity greater than 95% into the conical flask as a diluent to prepare the main The volume fraction of the extractant is 25%, and the volume fraction of the diluent is 75% of the mixed organic extract phase solution.

[0032] B. Slowly pour concentrated sulfuric acid with a mass content of 95% to 99% into a 2L beaker filled with deionized water, and stir with a glass rod at the same time to rapidly dissipate the heat generated, and prepare a 1L molar concentration of 0.300mol· L -1 Sulfuric acid aqueous solution, use the AR2140 type electronic analytical balance to accurately weigh the hydroxylamine hydrochloride crystals with a purity greater than 99%, add it to the sulfuric acid aqueous solution to prepare a reaction solution, and the concentration of hydroxylamine hydrochloride in the reaction solut...

Embodiment 2

[0036]A. according to the method for embodiment 1, it is 50% that the main extractant volume fraction is prepared into, and the mixed organic extraction phase solution that diluent volume fraction is 50%.

[0037] B. Prepare 1L molar concentration of 1.200mol L -1 Aqueous sulfuric acid solution, add accurately weighed hydroxylamine hydrochloride crystals to the aqueous sulfuric acid solution to prepare hydroxylamine hydrochloride with a concentration of 0.802mol L -1 the reaction solution.

[0038] C. according to the method for embodiment 1, the mixed extraction agent that has configured and reaction liquid are placed in the reactor that has stirring device in 3L, at 25 ℃, reacted for 20 minutes to obtain hydroxylamine sulfate mother liquor.

[0039] D. Using ion chromatography to analyze SO in the mother liquor of hydroxylamine sulfate 4 2- ions and Cl - ion concentration, the mass concentration of hydroxylamine sulfate obtained in the mother liquor is 82.35g L -1 , the...

Embodiment 3

[0041] A. according to the method for embodiment 1, be prepared into main extractant volume fraction and be 30%, diluent volume fraction is the mixed organic extraction phase solution of 70%.

[0042] B. Prepare 1L with a molar concentration of 2.00mol·L -1 Aqueous sulfuric acid solution, add accurately weighed hydroxylamine hydrochloride crystals to the aqueous sulfuric acid solution to prepare hydroxylamine hydrochloride concentration of 3.50mol L -1 the reaction solution.

[0043] C. according to the method for embodiment 1, the mixed extraction agent that has configured and reaction liquid are placed in the reactor that has stirring device in 3L, at 25 ℃, reacted for 20 minutes to obtain hydroxylamine sulfate mother liquor.

[0044] D. Using ion chromatography to analyze SO in the mother liquor of hydroxylamine sulfate 4 2- ions and Cl - ion concentration, the mass concentration of hydroxylamine sulfate obtained in the mother liquor is 113.56g L -1 , the conversion ra...

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Abstract

This invention provides a method for preparing hydroxylamine salt by reaction-extraction 'coupled' technique. The method utilizes hydroxylamine hydrochloride and HNO3, H2SO4 or H3PO4 as the reactants to prepare hydroxylamine nitrate, hydroxylamine sulfate or hydroxylamine phosphate. During the reaction, a mixture of amide and diluting agent is utilized as the extraction phase to extract byproduct HCl generated during the reaction to obtain high-concentration hydroxylamine salt mother liquor. Then multi-stage cross-flow or vacuum distillation is performed to obtain concentrated hydroxylamine salt solution or crystal. During the reaction, byproduct inorganic acid can be extracted into the organic phase, which can reduce the amount of inorganic acid in aqueous phase, and break the previous thermodynamic equilibrium limit so that the reaction advances toward the positive reaction direction, and the yield is increased. The method has such advantages as simple process, few buproducts and easy operation, and is suitable for industrialization production.

Description

Technical field: [0001] The invention relates to a method for preparing hydroxylamine salt by using reaction-extraction "coupling" technology, which belongs to the technical field of fine chemical products. Background technique: [0002] Hydroxylamine salt is a fine chemical product with a wide range of uses. Hydroxylamine sulfate and hydroxylamine phosphate are mainly used in the production of caprolactam, and also have important uses in the production of pesticides and medicines; hydroxylamine nitrate is mainly used in the treatment of spent nuclear materials and liquid propellants. [0003] At present, the methods for preparing hydroxylamine sulfate mainly include NO reduction method, acetone oximation method, calcium oxide method, hydrolysis method and so on. The methods for preparing hydroxylamine nitrate mainly include catalytic reduction method, ion exchange method, electrodialysis method, precipitation method, neutralization method, electrolysis method, double decom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/14
Inventor 任钟旗张卫东刘光虎陈星群
Owner BEIJING UNIV OF CHEM TECH
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