Preparation method of high-purity solid hydroxylamine sulphate

A technology of hydroxylamine sulfate and high purity is applied in the field of preparation of high-purity solid hydroxylamine sulfate, and can solve the problems of restricting the competitiveness of hydroxylamine sulfate products, low product yield of nitromethane route, complicated process of acetone oxime route, etc. Recyclability, reduced risk of decomposition, optimized effect of vacuum drying conditions

Active Publication Date: 2014-12-10
QUZHOU JUHUA POLYAMIDE FIBER
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  • Claims
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Problems solved by technology

However, the product yield of the nitromethane route is low, there are many types of by-products, and the investment in separation equipment is large; the process of the acetone oxime route is relatively complicated, with many types of raw materials, large unit consumption, and high cost; the production process of the disulfonate hydrolysis method is mature, but It is only suitable for large-scale production in large factories, the investment cost is high, and the yield of other process routes is relatively low. In summary, large investment, many types of raw materials, high cost, low yield, and low product purity relatively restrict high-purity Product Competitiveness of Solid Hydroxylamine Sulfate

Method used

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  • Preparation method of high-purity solid hydroxylamine sulphate

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Embodiment 1

[0039] Control the temperature of the first reactor to be 23.9°C, add a hydroxylamine sulfate aqueous solution with a mass percentage concentration of 15% to the first reactor 1, slowly add ammonia water with a mass percentage concentration of 18.8% therein, stir and mix, and the stirring speed is 110rpm, Adjust the pH value of the solution to 5.9 and set aside. The extraction agent dioctyl phosphate, the diluent sulfonated kerosene, and the stabilizer dimethyl phosphite are fully mixed according to the volume ratio of 1:3:0.001 to obtain the extraction mixture, which is set aside; the temperature of the second reactor is controlled at 24.8°C, and the Add the above-mentioned mixed extraction mixture into the second reactor 2, slowly add ammonia water with a mass percentage concentration of 18.8% to it, the stirring speed is 110rpm, adjust the pH value of the solution to 7.1, the first reactor 1, the second reactor 2 reaction products enter the first extraction tower 3 simultan...

Embodiment 2

[0041] Control the temperature of the first reactor to be 25.4°C, add a hydroxylamine sulfate aqueous solution with a mass percentage concentration of 13.9% to the first reactor 1, slowly add ammonia water with a mass percentage concentration of 19.4% therein, stir and mix, and the stirring speed is 110rpm, Adjust the pH value of the solution to 6.0 and set aside. The extraction agent dioctyl phosphate, the diluent sulfonated kerosene, and the stabilizer dimethyl phosphite are fully mixed according to the volume ratio of 1:3.1:0.001 to obtain the extraction mixture, which is set aside; the temperature of the second reactor is controlled at 25.2°C, and the Add the above-mentioned mixed extraction mixture into the second reactor 2, slowly add ammonia water with a mass percentage concentration of 18.8% to it, the stirring speed is 110rpm, adjust the pH value of the solution to 7.1, the first reactor 1, the second reactor 2 reaction products enter the first extraction tower 3 simu...

Embodiment 3

[0043] Control the temperature of the first reactor to be 26.2°C, add a hydroxylamine sulfate aqueous solution with a mass percentage concentration of 12.1% to the first reactor 1, slowly add ammonia water with a mass percentage concentration of 20.7% therein, stir and mix, and the stirring speed is 110rpm, Adjust the pH of the solution to 6.1. The extractant dioctyl phosphate, the diluent sulfonated kerosene, and the stabilizer dimethyl phosphite are fully mixed according to the volume ratio of 1:3.2:0.0015 to obtain the extraction mixture, which is set aside; the temperature of the second reactor is controlled at 25.6°C, and the second Add the above-mentioned mixed extraction mixture into the reactor 2, slowly add ammonia water with a mass percentage concentration of 18.4% to it, the stirring speed is 110rpm, adjust the pH value of the solution to 7.3, the first reactor 1, the second reactor 2 Reaction product enters the first extraction tower 3 simultaneously according to v...

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Abstract

The invention discloses a preparation method of high-purity solid hydroxylamine sulphate. The preparation method of the high-purity solid hydroxylamine sulphate comprises the following steps: adding a 5-15% hydroxylamine sulphate aqueous solution into a first reactor, mixing the hydroxylamine sulphate aqueous solution with 18-23% ammonia water, controlling the temperature of the first reactor to 20-30 DEG C, and regulating the pH value of the solution to 5.8-6.5, so that a first reaction product is obtained; fully mixing an extracting agent, a diluter and a stabilizer in a volume ratio of 1:(3-3.5):(0.001-0.002), putting the obtained mixture into a second reactor, regulating the pH value to 7.0-7.8 by adopting 18-23% ammonia water, and controlling the temperature of the second reactor to 20-30 DEG C, so that a second reaction product is obtained; carrying out extraction, concentration, cold crystallization, centrifugation and vacuum drying on the first reaction product and the second reaction product, so that the target product high-purity solid hydroxylamine sulphate is obtained. The preparation method of the high-purity solid hydroxylamine sulphate has the advantages of simple temperature, mild reaction conditions, high yield and low cost.

Description

technical field [0001] The invention relates to a preparation method of high-purity solid hydroxylamine sulfate, in particular to a method for obtaining high-purity solid hydroxylamine sulfate by using a hydroxylamine sulfate aqueous solution as a raw material through complex extraction and other processes. Background technique [0002] High-purity hydroxylamine sulfate can be used to synthesize pesticide raw materials, pharmaceutical raw materials, rubber additive raw materials, natural rubber stabilizers, and synthetic rubber non-polluting shortstops, metal treatment agents, fiber modifiers, developers, reducing agents, and It can be used in the refining of polymer synthesis raw materials and compounds, polymerization catalysts, etc. [0003] The domestic and foreign solid hydroxylammonium sulfate synthesis routes and techniques disclosed in the prior art mainly include nitromethane route, natural gas (methane) nitration route, acetone oxime route, disulfonate ammonium sal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/14
Inventor 郭志毅谷灿波屠仁华姜雨土孙江浩
Owner QUZHOU JUHUA POLYAMIDE FIBER
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