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Industrialized production method of 3,4-dimethylpyrazole and phosphate thereof

A technology of dimethylpyrazole and phosphoric acid, which is applied in the direction of organic chemistry, can solve the problems of expensive raw materials and harsh production process requirements, and achieve the effects of simple solvent recovery process, reduced operation difficulty and cost saving

Active Publication Date: 2013-05-22
林文斌
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It mainly solves the problems existing in the existing synthetic methods, such as harsh production process requirements and expensive raw materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] The production process in the No. 1 reactor:

[0014] Add 360 Kg of 2-butanone, 30 Kg of solid formaldehyde, and 90 Kg of water into Reactor No. 1, stir and cool to 0~10°C, stirring at a speed of 20 rpm, and dropwise add 90 Kg of 1 mol / L sodium hydroxide solution , control the rate of addition to keep the temperature of the reaction system at 5-12°C. After the dropwise addition, the reaction system was kept at normal pressure at 8~12°C for 1 hour, and then at 3~6°C for 18 hours, and 1 mol / L sulfuric acid aqueous solution was added to adjust the pH=6.5~7. Atmospheric distillation to collect unreacted excess 2-butanone (90°C / 750 mmHg). The residue was distilled under reduced pressure to collect 96 Kg of 3-hydroxymethyl-butanone (90~95°C / 10 mmHg). The gas phase detection purity was 96%, and the yield was 90%.

[0015] The production process in the No. 2 reactor:

[0016] Under normal pressure, add 130Kg of hydrazine sulfate and 180Kg of water to the No. 2 reaction kettl...

Embodiment 2

[0022] The production process in the No. 1 reactor:

[0023] Add 216 Kg of 2-butanone, 30 Kg of solid formaldehyde, and 90 Kg of water into the No. 1 reactor, stir and cool to 0~10°C, stirring at a speed of 30 rpm, and dropwise add 80 Kg of 1 mol / L sodium hydroxide solution , control the rate of addition to keep the temperature of the reaction system at 5-12°C. After the dropwise addition, the reaction system was kept at 8-12°C under normal pressure for 1 hour, then kept at 3-6°C for 18 hours, and 1 mol / L hydrochloric acid aqueous solution was added to adjust the pH to 6.5-7. Atmospheric distillation to collect unreacted excess 2-butanone (90°C / 750 mmHg). The residue was distilled under reduced pressure to collect 94 Kg of 3-hydroxymethyl-butanone (90~95°C / 10 mmHg). The gas phase detection purity was 96%, and the yield was 88%.

[0024] The production process in the No. 2 reactor:

[0025]Under normal pressure, add 68.5Kg of hydrazine hydrochloride and 400 Kg of concentrate...

Embodiment 3

[0031] The production process in the No. 1 reactor:

[0032] Add 108 Kg of 2-butanone, 30 Kg of solid formaldehyde, and 90 Kg of water into Reactor No. 1, stir and cool to 0~10°C, stirring at a speed of 30 rpm, and dropwise add 90 Kg of 1 mol / L sodium hydroxide solution , control the rate of addition to keep the temperature of the reaction system at 5-12°C. After the dropwise addition, the reaction system was kept at 8-12°C under normal pressure for 1 hour, then kept at 3-6°C for 18 hours, and 1 mol / L hydrochloric acid aqueous solution was added to adjust the pH to 6.5-7. Atmospheric distillation to collect unreacted excess 2-butanone (90°C / 750 mmHg). The residue was distilled under reduced pressure to collect 89 Kg of 3-hydroxymethyl-butanone (90~95°C / 10 mmHg). The gas phase detection purity was 95%, and the yield was 83%.

[0033] The production process in the No. 2 reactor:

[0034] Under normal pressure, add 110Kg of hydrazine sulfate and 100Kg of water to the No. 2 rea...

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PUM

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Abstract

The invention relates to an industrialized production method of 3,4-dimethylpyrazole and a phosphate thereof, and mainly solves problems of rigor production technology and expensive raw materials of a prior synthetic method. The technology of the invention is easily operated, at low costs and with high yield; reaction conditions are apt to realization of large-scale industrialized production. A technical scheme of the invention is as below: the industrialized production method of 3,4-dimethylpyrazole and the phosphate thereof comprises the steps that 2-butanone reacts with solid formaldehyde in an alkaline solution, and 3-hydroxymethyl-butanone is obtained after distillation and separation; the 3-hydroxymethyl-butanone reacts with hydrazonium salt under an acid condition to obtain 3,4-dimethylpyrazole, which reacts with phosphoric acid to form a salt of 3,4-dimethylpyrazole phosphate. The 3,4-dimethylpyrazole phosphate obtained by the invention is an efficient nitrifying ferment inhibitor.

Description

technical field [0001] The invention relates to a preparation method of 3,4-dimethylpyrazole and its phosphate, in particular to a method for industrial production of 3,4-dimethylpyrazole and its phosphate. Background technique [0002] 3,4-Dimethylpyrazole phosphate is a highly effective nitrase inhibitor. At present, urea, which is the most widely used in the world, must be converted into ammonium carbamate through the enzymatic hydrolysis of urokinase in the soil, and absorbed by plants in the form of ammonium nitrogen. Due to the high activity of urokinase in the soil, the conversion of urea to release ammonium nitrogen is very fast, and the crops have no time to absorb it, and part of the ammonium nitrogen that has not been absorbed by the crops is converted into nitrate nitrogen by nitrifying bacteria (enzymes) in the soil , causing deterioration of the atmosphere and soil environment through leaching and volatilization. 3,4-Dimethylpyrazole phosphate can be mixed wi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D231/12
Inventor 林文斌高晓伟黄国强
Owner 林文斌