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Synthetic method ofphenylhydrazine

A synthesis method and technology of phenylhydrazine, applied in the field of synthesis of aromatic hydrazine compounds, can solve the problems of personnel and environmental hazards, high chemical oxygen demand, large amount of salt wastewater, etc., and achieve low personnel and environmental hazards, biochemical treatment Simple, low COD effect

Pending Publication Date: 2020-03-27
XINHUA PHARM (SHOUGUANG) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, stannous chloride is mostly used in the reduction process, and the harm to personnel and the environment is inevitable; the waste liquid produced by acid analysis has high acidity and high chemical oxygen demand (COD); Difficulties increase the industrial production cost of phenylhydrazine and limit the market development of phenylhydrazine products

Method used

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  • Synthetic method ofphenylhydrazine

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Effect test

Embodiment 1

[0024] Embodiment 1: a kind of synthetic method of phenylhydrazine adopts aniline, hydrochloric acid, sodium nitrite, water, ammonium bisulfite solution, 98% sulfuric acid, liquid caustic soda, caustic soda to be main raw material, and concrete steps are as follows:

[0025] Step 1: Diazotization, turn on the switch of each metering pump, open the water inlet valve and outlet valve of the water flowmeter, flush away the dirt in the pipeline, and slowly open the inlet valve and The discharge valve passes through the tubular reactor at a speed of 2m / s to undergo a diazotization reaction, and the mass ratio of aniline: hydrochloric acid: sodium nitrite: water = 1: 2.5: 0.5: 3 When there is diazonium salt solution flowing out of the reaction pipeline , check the end point immediately and make adjustments to stabilize the rotor of the flowmeter as soon as possible, and the end point is normal. During the reaction process, the temperature of the diazotization reaction must be strictl...

Embodiment 2

[0034] Embodiment 2: a kind of synthetic method of phenylhydrazine, adopt aniline, hydrochloric acid, sodium nitrite, water, ammonium bisulfite solution, 98% sulfuric acid, liquid caustic soda, caustic soda is main raw material, and concrete steps are as follows:

[0035]Step 1: Diazotization, turn on the switch of each metering pump, open the water inlet valve and outlet valve of the water flowmeter, flush away the dirt in the pipeline, and slowly open the inlet valve and The discharge valve passes through the tubular reactor at a speed of 2m / s to undergo a diazotization reaction, and the mass ratio of aniline:hydrochloric acid:sodium nitrite:water=1:3.5:1.5:4 When the diazo salt solution flows out of the reaction pipeline , check the end point immediately, and make adjustments to stabilize the rotor of the flowmeter as soon as possible, and the end point is normal. During the reaction process, the temperature of the diazotization reaction must be strictly controlled at 65°C, ...

Embodiment 3

[0044] Embodiment 3: a kind of synthetic method of phenylhydrazine, adopt aniline, hydrochloric acid, sodium nitrite, water, ammonium bisulfite solution, 98% sulfuric acid, liquid caustic soda, caustic soda is main raw material, concrete steps are as follows:

[0045] Step 1: Diazotization, turn on the switch of each metering pump, open the water inlet valve and outlet valve of the water flowmeter, flush away the dirt in the pipeline, and slowly open the inlet valve and The discharge valve passes through the tubular reactor at a speed of 2m / s to undergo a diazotization reaction. The mass ratio of aniline:hydrochloric acid:sodium nitrite:water=1:4.5:2.5:5, when there is diazonium salt solution flowing out of the reaction pipeline When the end point is detected, the end point should be checked immediately and adjusted to stabilize the rotor of the flowmeter as soon as possible and the end point to be normal. During the reaction process, the temperature of the diazotization reacti...

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Abstract

The invention discloses a synthetic method of phenylhydrazine. Aniline, hydrochloric acid, sodium nitrite, water, an ammonium bisulfite solution, 98% sulfuric acid, caustic soda liquid and caustic soda flakes are adopted as main raw materials, aniline, hydrochloric acid, sodium nitrite and tap water are converged through a metering pump and a flowmeter respectively and then pass through a tubularreactor (a miller-grid tube reactor) at a high speed to be subjected to diazotization reaction and diazonium salt liquid is obtained. The diazonium salt solution subjected to the pipeline reaction flows into a reduction tank to be subjected to a cold reduction reaction with an ammonium bisulfite solution, and heating is performed to perform a thermal reduction reaction. Concentrated sulfuric acidis added into the reduction solution and heated for hydrolysis. The hydrolysate is cooled and then filter pressing operation is performed, solid crystals are obtained after filtering, caustic soda liquid is added for dissolving and then caustic soda flakes are added for neutralizing. Pressure filtration is performed to remove salt and the filtrate stands for layering to obtain an oil phase which is the phenylhydrazine finished product.

Description

technical field [0001] The invention relates to a method for synthesizing aromatic hydrazine compounds, in particular to a method for synthesizing phenylhydrazine. Background technique [0002] Phenylhydrazine, whose molecular formula is C 6 h 8 N 2 , its structural formula is as follows: . [0003] Phenylhydrazine is an important fine chemical intermediate, which is widely used in daily life. It is used in the production of pesticides to synthesize the intermediate of organophosphorus insecticide triazophos, 1-phenylsemicarbazide, and the intermediate of pyridazinphos 1-Phenyl-3,6-dihydroxypyridazine is also an intermediate of new fungicide species famoxadone and fenamidone. In addition, phenylhydrazine is also used as a raw material for organic synthesis. It is used as an intermediate in industries such as dyes and pharmaceuticals, and is also used as an analytical reagent. Therefore, the synthesis of phenylhydrazine plays an important role in industrial production. ...

Claims

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Application Information

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IPC IPC(8): C07C241/02C07C243/22
CPCC07C241/02C07C245/20
Inventor 王丽曼靳延辉马李伟李道先徐文辉
Owner XINHUA PHARM (SHOUGUANG) CO LTD
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