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A kind of production method of high-purity thiourea

A production method, pure thiourea technology, applied in the field of preparation of high-purity thiourea, to achieve the effect of improving purity

Active Publication Date: 2020-10-02
XILONG SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The present invention mainly deals with residual organic impurities and metal ion impurities that affect product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] at 2m 3 Add 1000Kg of pure water into the reaction kettle and heat to 70°C, add 500Kg of industrial thiourea under stirring, and dissolve to obtain a thiourea solution. The measured specific gravity is 1.06g / ml. Stir and react at 70°C for 2 hours, raise the temperature to 90°C and keep stirring for 2 hours, cool down to 60°C, filter the feed liquid with a polypropylene material filter element with a pore size of 0.22 μm, dilute the filtrate with 720Kg of water, and the specific gravity is 1.025g / ml. to room temperature, pass through 732-type cation exchange resin and 717-type anion-exchange resin in turn at a flow rate of 2BV / h, the solution is filtered again, and the filtrate is put into a concentration kettle and concentrated in vacuum to 1 / 2 volume, stirred and cooled to crystallize, and after crystallization is completed, separate crystals and mother liquor, the resulting crystals are rinsed with pure water, centrifuged to dry, and dried at 80°C to obtain high-purit...

Embodiment 2

[0026] at 2m 3 Add 1000Kg of pure water to the reaction kettle and heat it to 60°C. Add 430Kg of industrial thiourea under stirring to obtain a thiourea solution. The measured specific gravity is 1.05 g / ml. Adjust the pH value of the solution to 9 with ammonia water. Activated carbon, stir and react at 70°C for 2 hours, heat up to 90°C and keep stirring for 2 hours, cool down to 60°C, filter the feed liquid with a polypropylene material filter element with a pore size of 0.22 μm, dilute the filtrate with 600Kg of water, and the specific gravity is 1.026g / ml, lowered to room temperature, passed through 732-type cation exchange resin and 717-type anion-exchange resin in turn at a flow rate of 3BV / h, the solution was filtered again, the filtrate was put into a concentration kettle and concentrated in vacuum to 1 / 2 volume, stirred and cooled to crystallize, and the crystallization was completed Afterwards, the crystals and the mother liquor are separated, and the obtained crystal...

Embodiment 3

[0028] at 2m 3 Add 1000Kg of pure water into the reaction kettle and heat it to 70°C. Add 450Kg of industrial thiourea under stirring to obtain a thiourea solution. The measured specific gravity is 1.05g / ml. Use ammonia water to adjust the pH of the solution to 8. Stir and react at 70°C for 2 hours, raise the temperature to 90°C and keep stirring for 2 hours, dilute the filtrate with 700Kg of water, the specific gravity is 1.025g / ml, cool down to room temperature, and pass through D101 macroporous adsorption resin and 732 cationic resin at a flow rate of 2BV / h Exchange resin and 717-type anion exchange resin, the solution is filtered through a polypropylene material filter element with a pore size of 0.22 μm, the filtrate is put into a concentration kettle and concentrated in vacuum to 1 / 2 volume, stirred and cooled to crystallize, after the crystallization is completed, separate the crystal and mother liquor, The resulting crystals were rinsed with pure water, centrifuged to ...

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Abstract

The invention discloses a method for preparation of high purity thiourea from industrial thiourea. The method includes: dissolving industrial thiourea in pure water, adjusting the pH value of the solution with ammonia water, adding a formaldehyde solution for reaction, and then conducting ion exchange. The method can effectively remove residual organic impurities and metal ion impurities, improvethe purity of thiourea, and meet the requirements of pharmacy, biological reagents, fine chemical industry, chemical reagents and other industries for high purity thiourea.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and relates to a method for preparing high-purity thiourea by utilizing industrial thiourea. [0002] technical background [0003] Thiourea, also known as thiourea, has the molecular formula (NH 2 ) 2 CS, the relative molecular mass is 76.12, white orthorhombic or needle-like bright crystals. Bitter, flammable, density 1.046, melting point 170-182°C, it will decompose when heated again. Sublimes under reduced pressure at 150-160°C. Soluble in cold water, ammonium thiocyanate solution and ethanol, almost insoluble in ether. [0004] At present, lime nitrogen and hydrogen sulfide gas are used in the industry, and the aminonitrile and calcium hydroxide generated by hydrolysis of lime nitrogen and hydrogen sulfide gas are used in the synthesis kettle to carry out absorption synthesis reaction to prepare a suspension containing thiourea. After the first filtration and purification, it is con...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C335/02
CPCC07C335/02
Inventor 王宇许振良李湛江马晓华宋振李燕平杨志锋
Owner XILONG SCI CO LTD
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