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The purification method of thiourea and thiourea

A purification method and technology of thiourea, applied in the direction of organic chemistry, etc., can solve the problem that thiourea is difficult to meet the requirements of use, and achieve the effects of improving various indicators, simple operation steps and simple equipment

Active Publication Date: 2020-11-24
GUIZHOU REDSTAR DEVING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above application fields, especially the pharmaceutical field, have high requirements on the purity of thiourea, and it is difficult for general industrial thiourea to meet the use requirements.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042]Add 3000L deionized water to the 5000L reactor, heat up with steam, and start adding 1000KG of industrial thiourea with a main content of 98.00% when the temperature of the deionized water in the reactor reaches 40°C, stir until the thiourea is completely dissolved, Add 1KG of industrial sodium carbonate with a total alkali content ≥ 98.8%, and add 1KG of activated carbon. When the temperature of the material in the reaction kettle reaches 75°C, control the amount of steam, keep the material in the kettle at 75°C for 1 hour, and then use a centrifugal pump to pump the material in the kettle into the filter for primary and secondary filtration Finally, the filtrate was transferred to a crystallization tank, cooled to crystallize, centrifugally filtered at 10°C, washed, and dried to obtain 746KG product with a yield of 75.7%.

Embodiment 2

[0044] Add 3000L of deionized water to the 5000L reactor, heat up with steam, when the temperature of the deionized water in the reactor reaches 95°C, start to add 1000KG of industrial thiourea with a main content of 98.20%, stir until the thiourea is completely dissolved, Add 1KG of industrial sodium carbonate with a total alkali content ≥ 98.8%, and add 1KG of activated carbon. Control the amount of steam, keep the material in the kettle at 95°C for 1 hour, then pump the material in the kettle into the filter with a centrifugal pump, transfer the filtrate to the crystallization tank after primary filtration and secondary filtration, and cool down for crystallization , centrifuged at 10°C, washed and dried to obtain 738KG product with a yield of 74.8%.

Embodiment 3

[0046] Add 3000L of deionized water to the 5000L reactor, heat up with steam, when the temperature of the deionized water in the reactor reaches 65°C, add 1000KG of industrial thiourea with a main content of 98.50%, stir until the thiourea is completely dissolved, Add 833g of industrial sodium carbonate with a total alkali content ≥ 98.8%, and add 833g of gac. When the temperature of the material in the reaction kettle reaches 75°C, control the amount of steam, keep the material in the kettle at 75°C for 1 hour, and then use a centrifugal pump to pump the material in the kettle into the filter for primary and secondary filtration Finally, the filtrate was transferred to a crystallization tank, cooled to crystallize, centrifugally filtered at 10°C, washed, and dried to obtain 733KG product with a yield of 73.9%.

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Abstract

The invention provides a thiourea purification method. The thiourea purification method comprises the following steps: dissolving industrial thiourea into a solvent to obtain a thiourea solution; adding a precipitating agent into the thiourea solution to perform reaction to generate precipitates, then filtering the precipitates, and collecting filtrate; and cooling, crystallizing and centrifugallyseparating the filtrate to obtain a solid, and then, drying the solid to obtain a thiourea product. The invention also provides the thiourea obtained by adopting the purification method, and the purity of the thiourea is greater than or equal to 99.3%. The purification method provided by the invention has the advantages that the operation steps are simple, the reaction period is short, the energyconsumption is low, the required equipment is simple, and the added materials are cheap and easy to obtain. The purification method provided by the invention is suitable for preparing high-purity thiourea from industrial thiourea, has a good purification effect, obviously improves all indexes and can meet the technical requirements of the market on high-purity thiourea.

Description

technical field [0001] The invention belongs to the field of chemical industry. Specifically, the invention relates to a method for purifying thiourea and the thiourea purified by the method. Background technique [0002] Thiourea is a compound formed after the oxygen in urea is replaced by sulfur, which belongs to thioamide (RC(S)NR 2 , R is a hydrocarbon group). Thiourea is a colorless to pale yellow orthorhombic crystal or needle-shaped shiny crystal, with a bitter taste and an ammoniacal odor. Thiourea is slightly soluble in cold water but easily soluble in hot water, soluble in ethanol when heated and precipitated from ethanol when cooled, almost insoluble in ether, flammable, relative density 1405kg / m 3 , melting point 170 ° C ~ 173 ° C. Thiourea can form stable compounds with metals. Adding a small amount of thiourea to the acid solution during metal cleaning can inhibit the corrosion of the metal by the acid solution; thiourea can also be used as a catalyst for th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C335/02
CPCC07C335/02
Inventor 郭汉光梁启波杨德林罗帅威丁志文曾开文
Owner GUIZHOU REDSTAR DEVING