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Preparation of granular 1,2,4-triazole sodium salt

A technology of triazole sodium salt and triazole sodium, which is applied in the field 1, can solve the problems of harsh operating environment, unfavorable process, and inaccurate measurement of workers, and achieves easy feeding and storage, good fluidity, and uniform particle size Effect

Active Publication Date: 2011-10-12
SINOMAX SOLUTIONS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, all domestic manufacturers produce powdery triazole sodium salt, but there are many defects in powdery triazole sodium salt: on the one hand, powdery triazole sodium salt is inconvenient in transportation and transmission as a raw material; On the one hand, during use, especially when feeding downstream, the dust is too large, resulting in a poor operating environment for the staff; in addition, for the pipeline transmission feeding method, the powdered triazole sodium salt is likely to cause inaccurate metering, not Conducive to accurate quantitative control of the process
[0005] Up to now, there are no literatures at home and abroad to report the preparation method of granular 1,2,4-triazole sodium salt

Method used

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  • Preparation of granular 1,2,4-triazole sodium salt
  • Preparation of granular 1,2,4-triazole sodium salt
  • Preparation of granular 1,2,4-triazole sodium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 164g of formic acid in a 500mL three-necked flask, add 350mL 25% ammonia water dropwise at 20-30℃, stir for 30min, heat up to 165-170℃, slowly add 80g hydrazine hydrate dropwise, while steaming ammonia water, keep warm Hours, cooling to obtain triazole. Add 45% NaOH solution dropwise to the triazole system. The temperature is at 30-40°C and the pH is 10-11. Stop the dropwise addition. Stir for 2-3 hours to precipitate crystals to obtain 1,2,4-triazole The crude sodium azole product is in powder form, and the particle size of more than 80% by weight of the powder is less than 60 microns.

[0040] Add 250g of pure water to the obtained crude sodium triazole, stir, heat to clear, reflux for 30 minutes, adjust the stirring speed to 20-30 revolutions / min, and slowly reduce to 8-10 at a speed of 2-3°C / min ℃, filter. First, in a vacuum state at 50-60℃, after drying off most of the surface water, slowly heat up to 105℃, continue to bake until the moisture content is less tha...

Embodiment 2

[0046] Add 180g of formic acid to a 500mL three-necked flask, add 400mL of 25% ammonia water dropwise at 25-35°C, stir for 50min, heat to 160-165°C, slowly add 90g hydrazine hydrate dropwise, while steaming ammonia water, keep warm for about 3.5 hours , Cool to obtain triazole. Add 48% NaOH solution dropwise to the triazole system. The temperature is at 35-45°C and the pH is 11-12. Stop the dropwise addition. Stir for 3-4 hours to precipitate crystals to obtain 1,2,4-triazole The crude sodium azole product is in powder form, and the particle size of more than 70% by weight of the powder is less than 55 microns.

[0047] Add 250g of methanol to the obtained crude sodium triazole, stir, heat to clear, reflux for 60min, adjust the stirring speed to 20-30 rpm, and slowly reduce to 8-10 ℃ at a speed of 5-8 ℃ / min ,filter. First, in a vacuum at 30-40℃, after drying off most of the surface methanol, slowly increase the temperature to 70℃ for 2 hours, and finally rise to 110℃, and conti...

Embodiment 3

[0051] Add 150g of formic acid to a 500mL three-necked flask, add 320mL of 25% ammonia water dropwise at 30-35°C, stir for 50min, heat to 150-160°C, slowly add 75g hydrazine hydrate dropwise, while steaming ammonia water, keep warm for about two hours , Cool to obtain triazole. Add 40% NaOH solution dropwise to the triazole system. The temperature is at 20-30°C and the pH is 10.5-11.5. Stop the dropwise addition. Stir for 3-4 hours to precipitate crystals to obtain 1,2,4-triazole The crude sodium azole product is in powder form, and the particle size of more than 85% by weight of the powder is less than 70 microns.

[0052] Add 300 g of ethanol to the crude sodium triazole product, stir, heat to clear, reflux for 90 min, adjust the stirring speed to 40-50 revolutions / min, and slowly reduce to 0-5°C at a rate of 10-15°C / min ,filter. First, in a vacuum state of 30-40℃, after drying off most of the surface ethanol, slowly increase the temperature to 80℃ for 2 hours, and finally ri...

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Abstract

The invention relates to a method for preparing granular 1,2,4-triazole sodium salt. The method comprises the following steps of: 1, preparing 1,2,4-triazole sodium salt by using formic acid, liquid ammonia and hydrazine hydrates as raw materials; and 2, obtaining the granular 1,2,4-triazole sodium salt by controlling the crystallization process, wherein in the step 2, the crystallization refluxing solvent is one of water, alcohol-type solvents, tetrahydrofuran and dioxane or the mixture of the solvents, the refluxing time is controlled to between 20 and 120 minutes, the rotary speed of the crystallization refluxing is controlled to between 10 and 60 revolutions per minute, the de-temperature rate of the crystallization refluxing is controlled to between 0 and 30 Celsius degrees per minute, the crystallization refluxing temperature finally drops to between 0 and 35 Celsius degrees, the initial drying temperature is controlled to between 30 and 60 Celsius degrees, and the final drying temperature is controlled to between 80 and 120 Celsius degrees. In the method, the granular 1,2,4-triazole sodium salt is obtained by controlling the processes of crystallization, refluxing, drying and the like of the 1,2,4-triazole sodium salt, which brings a lot of convenience and benefit to transportation and production, particularly the charging process.

Description

Technical field [0001] The present invention relates to a preparation method of 1,2,4-triazole sodium salt. More specifically, the present invention relates to a synthetic crystallization method of granular 1,2,4-triazole sodium salt. Background technique [0002] 1,2,4-Triazole sodium salt is a very versatile organic chemical intermediate. Due to the rapid development of triazole agricultural chemicals, especially triazole fungicides, it is 1,2,4-triazole The sodium salt of azole has opened up new application areas. 1,2,4-Triazole (ST) is an important intermediate for the synthesis of pesticide fungicides, plant growth regulators, paclobutrazol, diniconazole, triadimefon, fenpropion, etc. It can also be used as a variety of pesticides, medicines, and dyes. The demand for intermediates is increasing with the expansion of the scope of application. [0003] In recent years, there have been continuous reports in the literature on the production method of 1,2,4-triazole sodium salt. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D249/08
Inventor 高建勋周东王碧波董洪荣
Owner SINOMAX SOLUTIONS CO LTD
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