Synthesis method and application of dimercaptothiadiazole sodium salt

A technology of sodium dimercaptothiadiazole, synthesis method, applied in chemical instruments and methods, water/sludge/sewage treatment, organic chemistry, etc., can solve the problem of multiple wastes and pollutants, excessive carbon disulfide, and long reaction time and other problems, to achieve the effect of simple reaction operation, reduced production amount, and strong catalytic reaction ability.

Inactive Publication Date: 2020-09-08
青岛中科荣达新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The target product of the existing DMTD preparation method is DMTD instead of DMTD sodium salt, and the process has the disadvantages of long reaction time, large energy consumption, complicated operation, large excess carbon disulfide, and easy to generate more waste and pollutants. place

Method used

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  • Synthesis method and application of dimercaptothiadiazole sodium salt
  • Synthesis method and application of dimercaptothiadiazole sodium salt
  • Synthesis method and application of dimercaptothiadiazole sodium salt

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Effect test

Embodiment 1

[0042] Embodiment 1: the synthesis of dimercaptothiadiazole sodium salt

[0043] 1. Prepare raw materials. After measuring 65Kg of raw material 80% hydrazine hydrate, vacuum inhale the low-temperature reactor and start stirring; Guanidine 195g and triisopropylamine 796g are measured respectively and added to the low-temperature reactor; carbon disulfide is pressed into the carbon disulfide metering tank from the storage tank with compressed air (it must be ensured that the height of the liquid seal water in the metering tank is not less than 15mm), and the amount of carbon disulfide is 159.5 mm. Kg;

[0044] 2. Dropping reaction Feed freezing liquid into the jacket of the low-temperature reaction kettle, wait until the temperature in the kettle drops to 10°C, start adding carbon disulfide dropwise, control the dropping speed, and maintain the reaction temperature at 22°C. Carbon disulfide was added dropwise within 52 minutes;

[0045] 3. Insulation reaction After the additio...

Embodiment 2

[0047] Embodiment 2: the synthesis of dimercaptothiadiazole sodium salt

[0048] 1. Prepare raw materials. After measuring 65Kg of raw material 80% hydrazine hydrate, vacuum inhale the low-temperature reactor and start stirring; 325g of guanidine and 1170g of triisopropylamine are measured respectively and added to the low-temperature reaction kettle; carbon disulfide is pressed from the storage tank into the carbon disulfide metering tank with compressed air (it must be ensured that the height of the liquid seal water in the metering tank is not less than 15mm), and the amount of carbon disulfide is 160Kg ;

[0049] 2. Dropping reaction Feed freezing liquid into the jacket of the low-temperature reaction kettle, wait until the temperature in the kettle drops to 12°C, start adding carbon disulfide dropwise, control the dropping speed, and maintain the reaction temperature at 32°C. Carbon disulfide was added dropwise within 72 minutes;

[0050] 3. Insulation reaction After th...

Embodiment 3

[0052] Embodiment 3: the synthesis of dimercaptothiadiazole sodium salt

[0053] 1. Prepare raw materials. After measuring 65Kg of raw material 80% hydrazine hydrate, vacuum inhale the low-temperature reactor, and start stirring; Measure 450g of guanidine and 650g of triisopropylamine respectively and add them to the low-temperature reaction kettle; use compressed air to press carbon disulfide from the storage tank into the carbon disulfide metering tank (it must be ensured that the height of the liquid seal water in the metering tank is not less than 15mm), and the amount of carbon disulfide is 160Kg ;

[0054] 2. Dropping reaction Feed freezing liquid into the jacket of the low-temperature reaction kettle, wait until the temperature in the kettle drops to 15°C, start adding carbon disulfide dropwise, control the dropping speed, and keep the reaction temperature at 28°C. Carbon disulfide was added dropwise within 60 minutes;

[0055]3. Insulation reaction After the addition...

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Abstract

The invention discloses a synthesis method of a dimercaptothiadiazole sodium salt and an application of the dimercaptothiadiazole sodium salt as a heavy metal trapping agent. The synthesis method comprises the following steps: respectively metering raw materials including hydrazine hydrate, a sodium hydroxide solution, a catalyst tetramethyl-2-tert-butyl guanidine and triisopropylamine, adding theraw materials into a low-temperature reaction kettle, pressing carbon disulfide into a carbon disulfide metering tank from a storage tank by using compressed air, cooling the interior of the low-temperature reaction kettle to 10-15 DEG C, starting to dropwise add carbon disulfide, controlling the reaction temperature to be 20-32 DEG C, pressing the materials from the low-temperature reaction kettle to a heat preservation reaction kettle by using compressed air, introducing nitrogen into the kettle, keeping the pressure in the kettle at 0.05-0.15 MPa, introducing steam into a jacket of the heat preservation reaction kettle, and carrying out heat preservation reaction for 40-60 minutes at 45-60 DEG C. According to the synthesis method provided by the invention, the generation amount of byproducts is reduced, the yield of the DMTD sodium salt is increased, the quality of a final product is improved, and the loss of carbon disulfide is reduced.

Description

technical field [0001] The invention belongs to the technical field of new chemical materials and applications, and in particular relates to a synthesis method of dimercaptothiadiazole sodium salt and its application in the treatment of waste water containing heavy metal ions and the removal of heavy metals in waste incineration fly ash. Background technique [0002] In recent years, with the rapid development of modern industries such as electronics, electroplating, mining, smelting, leather, and chemical industry, the problem of heavy metal pollution has become increasingly serious. There are more and more, which makes the treatment of heavy metal wastewater more difficult; the emergence of heavy metal collectors can overcome the shortcomings and deficiencies of traditional chemical precipitation methods, and meet the increasingly stringent requirements for heavy metal discharge, especially in the field of heavy metal wastewater treatment. The role in the field of treatmen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D285/125A62D3/33C02F1/62C02F1/64A62D101/08A62D101/43
CPCA62D3/33A62D2101/08A62D2101/43C02F1/62C02F1/64C07D285/125
Inventor 郭祥荣刘东华杨荣华王璀张燕青郭彦恺
Owner 青岛中科荣达新材料有限公司
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