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Method for preparing energy-saving and environment-friendly triazole sodium

A triazole sodium, energy-saving and environmentally-friendly technology, applied in the direction of organic chemistry, can solve the problems of energy waste, environmental pollution, etc., and achieve the effects of improving purity, saving energy, and simple and effective production

Inactive Publication Date: 2012-09-12
CHANGSHA XINBEN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

During the reaction between formamide and hydrazine hydrate, water and ammonia gas will be released, which will be released as 6-8% ammonia water and ammonia gas after condensation. 6-8% ammonia water cannot be used for industrial use, and 20% ammonia water must be formed by evaporation and recovery. For industrial ammonia water, the energy consumption per ton of ammonia water reaches 1.2 to 1.5 tons of steam, and the remaining 1% ammonia water after evaporation is discharged through acid neutralization, which causes a waste of energy and pollutes the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Formamide and hydrazine hydrate were reacted at 150°C for 13 hours at a weight ratio of 2:1;

[0019] (2) After the reaction, cool down to 70°C, add a mixed solvent, the weight ratio of the mixed solvent to formamide is 1:2.5, then add dropwise 30% sodium hydroxide solution to adjust the pH to 10, and keep warm at 70°C for 3 hours; , the mixed solvent is prepared by butanediol and methanol in a weight ratio of 5:1;

[0020] (3) Cool to 20°C for crystallization, centrifuge at 850r / min for 10min, and recover the centrifuged mother liquor by distillation;

[0021] (4) Dry the crystals in vacuum to obtain the sodium triazole product.

[0022] The purity of the triazole sodium product produced is 99.5%.

[0023]

Embodiment 2

[0025] (1) Formamide and hydrazine hydrate were reacted at 160°C for 12 hours at a weight ratio of 1.8:1;

[0026] (2) After the reaction, cool down to 60°C, add a mixed solvent, the weight ratio of the mixed solvent to formamide is 1:2, then add dropwise 50% sodium hydroxide solution to adjust the pH to 11, and keep the temperature at 60°C for 4 hours; , the mixed solvent is prepared by butanediol and methanol in a weight ratio of 3:1;

[0027] (3) Cool to 25°C for crystallization, centrifuge at 900r / min for 15min, and recover the centrifuged mother liquor by distillation;

[0028] (4) Dry the crystals in vacuum to obtain the sodium triazole product.

[0029] The purity of the sodium triazole produced is 99.6%.

[0030]

Embodiment 3

[0032] (1) Formamide and hydrazine hydrate were reacted at 180°C for 15 hours at a weight ratio of 1.8:1;

[0033] (2) After the reaction, cool down to 80°C, add a mixed solvent, the weight ratio of the mixed solvent to formamide is 1:2, then add 60% sodium hydroxide solution dropwise to adjust the pH to 10, and keep the temperature at 80°C for 3 hours; , the mixed solvent is prepared by butanediol and methanol in a weight ratio of 3:1;

[0034] (3) Cool to 30°C for crystallization, centrifuge at 900r / min for 13min, and recover the centrifuged mother liquor by distillation;

[0035] (4) Dry the crystals in vacuum to obtain the sodium triazole product.

[0036] The purity of the triazole sodium product produced is 99.5%. .

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PUM

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Abstract

The invention discloses a method for preparing energy-saving and environment-friendly triazole sodium. The method comprises the followings steps of reacting formamide with hydrazine hydrate at the temperature of between 150 and 180 DEG C for 12 to 15 hours; after reaction, reducing the temperature to 60 to 80 DEG C, adding a mixed solvent prepared from butanediol and methanol, adding a 30 to 60 percent sodium hydroxide solution dropwise, and keeping the temperature of the mixture at 60 to 80 DEG C for 3 to 4 hours; and cooling and crystallizing, centrifuging and distilling, recycling centrifugal mother liquid, and drying crystals to obtain the triazole sodium product. The method has the advantages of eliminating a pilot process, separating by-products and intermediates by using the mixed solvent, realizing the production of triazole sodium in one step, shortening the process flow, lowering labor intensity, improving the purity of triazole sodium, recycling the intermediates, really saving energy and realizing environment-friendly and pollution-free production.

Description

technical field [0001] The invention relates to a preparation method of triazole sodium, in particular to an energy-saving and environment-friendly preparation method of triazole sodium. Background technique [0002] The currently used production process of triazole sodium is to react with triazole and sodium hydroxide to add solvent after complete reaction of formamide and hydrazine hydrate, after cooling, crystallization and separation, to obtain the product by azeotropic dehydration crystallization, cooling and centrifugation . During the reaction between formamide and hydrazine hydrate, water and ammonia gas will be released, which will be released as 6-8% ammonia water and ammonia gas after condensation. 6-8% ammonia water cannot be used for industrial use, and 20% ammonia water must be formed by evaporation and recovery. For industrial ammonia water, the energy consumption per ton of ammonia water reaches 1.2-1.5 tons of steam, and the remaining 1% ammonia water after...

Claims

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Application Information

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IPC IPC(8): C07D249/08
Inventor 刘建谭亲凯
Owner CHANGSHA XINBEN CHEM
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