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A method utilizing ammonium thiocyanate to convert thiourea

A technology of ammonium thiocyanate and thiourea, applied in organic chemistry and other directions, can solve the problems of complex process, high cost and low operating cost, and achieve the effect of simple process, less impurities and high purity

Inactive Publication Date: 2018-12-07
泰安金塔化工机械有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The first object of the present invention is to provide a kind of method utilizing ammonium thiocyanate to convert thiourea, to solve the problems such as complex process, high cost, high energy consumption of the existing method for preparing thiourea, described conversion with ammonium thiocyanate The method of thiourea, using ammonium thiocyanate to convert thiourea, has the advantages of simple process, energy consumption, no secondary pollution and low operating cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Mix ammonium thiocyanate with a mass content >96% and ammonia water with a concentration of 20% according to a mass ratio of 3:1, and react in a closed reaction kettle, heat up to 65°C, and stir While heating, control the pressure in the kettle within the range of 0.1MPa, and react for 3 hours;

[0041] (2), when the transformation rate of ammonium thiocyanate is analyzed to 80%, the ammonia distillation operation is started, the ammonia gas is absorbed by the spray absorption tower, and the ammonia water obtained is returned to the step (1) for recycling, and the remaining solids are discharged through the kettle , the resulting product is crude product thiourea, the product purity is 83%, and the main component of impurities is unconverted ammonium thiocyanate;

[0042] (3), heat the thiourea obtained in step (2) to 150°C in the sublimator, keep the vacuum constant temperature state, make the thiourea sublime, and the sublimation gas enters the first-stage desubli...

Embodiment 2

[0046] (1) Mix ammonium thiocyanate with a mass content > 96% and ammonia water with a concentration of 30% according to a mass ratio of 4:1, and react in a closed reaction kettle, heat up to 90°C, and stir While heating, control the pressure in the kettle within the range of 1.0MPa, and react for 6 hours;

[0047] (2), when the conversion rate of ammonium thiocyanate is analyzed to 88%, the ammonia distillation operation is started, the ammonia gas is absorbed by the spray absorption tower, and the ammonia water obtained is returned to the step (1) for recycling, and the remaining solid is discharged through the kettle , the resulting product is crude product thiourea, the product purity is 80%, and the main component of impurities is unconverted ammonium thiocyanate;

[0048] (3), heat the thiourea obtained in step (2) to 160° C. in a sublimator, keep a vacuum constant temperature state, make the thiourea sublimate, and the sublimation gas enters a section of desublimator th...

Embodiment 3

[0052] (1) Mix ammonium thiocyanate with a mass content > 96% and ammonia water with a concentration of 25% according to a mass ratio of 5:1, and react in a closed reaction kettle, heat up to 75°C, and stir While heating, control the pressure in the kettle within the range of 0.6MPa, and react for 4 hours;

[0053] (2), when the conversion rate of ammonium thiocyanate is 88-95% according to the laboratory analysis, the ammonia distillation operation is started, the ammonia gas is absorbed by the spray absorption tower, and the obtained ammonia water is returned to the step (1) for recycling, and the remaining solid is passed through the kettle The product obtained is crude product thiourea, with a product purity of 95%, and the main component of impurities is unconverted ammonium thiocyanate;

[0054] (3), heat the thiourea obtained in step (2) to 155°C in the sublimator, keep the vacuum constant temperature state, make the thiourea sublime, the sublimation gas enters the firs...

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Abstract

The invention provides a thiourea conversion method using ammonium thiocyanate. Ammonium thiocyanate is used as a material and reacts with moderate ammonium hydroxide in a certain weight ratio, ammonia gas is removed when the conversion rate of the ammonium thiocyanate reaches 78-95%, the obtained solid is crude thiourea, and the purity of the crude thiourea is 80-95%. After that, the principle that thiourea and impurities have different desublimation temperatures is used, thiourea with high purity is obtained through sublimation and repeated desublimation, and the yield can reach 47.2%. The thiourea conversion method using ammonium thiocyanate has the advantages of being simple in process, low in energy consumption and running cost, having no secondary pollution and the like. By the adoption of the thiourea conversion method using ammonium thiocyanate, the ammonium thiocyanate can be prepared from products extracted from coking desulfurization waste solutions, an industry chain of extracting salt from desulfurization waste solutions is extended, and a new path is provided for secondary salt extraction of desulfurization waste solutions. The product purity of the thiourea prepared by the method is 99%.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for converting thiourea with ammonium thiocyanate. Background technique [0002] At present, the methods for industrial production of thiourea mainly include lime nitrogen-calcium hydrogen sulfide synthesis method and cyanamide-hydrogen sulfide synthesis method. The lime nitrogen-calcium hydrogen sulfide synthesis method is suitable for extensive production methods, but lime nitrogen is a product with high energy consumption and high pollution, so the production cost is high and the environmental cost is high. The cyanamide-hydrogen sulfide synthesis method is complex in process and high in cost. [0003] In view of this, the present invention is proposed. [0004] The conversion of ammonium thiocyanate into thiourea has the advantages of simple process, low energy consumption and low operation cost. Ammonium thiocyanate can be extracted from coking desulfurization w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C335/02
CPCC07C335/02
Inventor 焦广磊朱葛张京旭
Owner 泰安金塔化工机械有限公司
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