CN106674059A

CN106674059A - Synthesis method of carbohydrazide

Info

Publication number: CN106674059A
Application number: CN201710001081.0A
Authority: CN
Inventors: 李亚杉
Original assignee: Individual
Current assignee: Individual
Priority date: 2017-01-03
Filing date: 2017-01-03
Publication date: 2017-05-17

Abstract

The invention relates to a synthesis method of carbohydrazide. The synthesis method is characterized in that the carbohydrazide is synthesized by taking methyl ethyl ketazine and urea as raw materials and reacting under a certain temperature. According to the synthesis method disclosed by the invention, the reaction yield is high, by-products are less, the energy consumption is low, and ammonia and butanone which are generated during a reaction process can be used for synthesizing the methyl ethyl ketazine; in addition, after the carbohydrazide in a reaction solution is centrifugally separated, residual mother liquid can be continuously used for synthesizing the carbohydrazide, so that the comprehensive utilization rate of the raw materials is increased, the production cost is reduced, and the generation of three wastes and the pollution to the environment are reduced.

Description

A kind of synthetic method of carbohydrazide

Technical field

The invention belongs to chemosynthesis technical field, and in particular to a kind of synthetic method of carbohydrazide.

Background technology

Carbohydrazide is a kind of important organic synthesis intermediate, can be synthesized with it a series of with the miscellaneous of bioactivity Cycle compound.Carbohydrazide is also a kind of boiler feed water oxygen scavenger for being progressively widely recognized in recent years and applying, its deoxygenation machine Reason is similar with hydrazine, but its oxygen scavenging ability and hydrazine is all substantially better than to iron, copper metallic face passivation ability, and toxicity compares and joins Ammonia is small, is readily transported.Additionally, carbohydrazide also acts as the component of propellant, colour development etc., purposes is quite varied.

The synthetic method of carbohydrazide is more, and synthetic route main at present has carbonic ester hydrazinolysis method, distilling alcohols method, urea hydrazine Solution, cyanuric acid hydrazinolysis method, phosgene hydrazinolysis method and carbazic acid Hydrolyze method etc..Above-mentioned synthetic method is all with hydrazine hydrate as former Material, it is relative complex to there is production technology, high to equipment requirement, and material toxicity is big, and accessory substance is more, and yield is low, the problems such as high energy consumption.

The content of the invention

For the disadvantages mentioned above for overcoming prior art to exist, the invention provides a kind of process is simple, accessory substance be few, yield Height, low in raw material price, energy-conserving and environment-protective, the carbohydrazide new synthetic method of economic security.

The technical solution adopted by the present invention is, with butanone azine and urea as raw material, phosphinylidyne to be synthesized at a certain temperature Hydrazine, the ammonia and butanone generated in course of reaction can be back to synthesis butanone azine.The concrete technology step of the inventive method is：Will Butanone azine and urea liquid are put into reactor, and its mol ratio is butanone azine: urea=2-3: 1, the concentration of urea liquid It is 25%~40%, is heated to 80 DEG C~130 DEG C and is reacted, the gas that will be steamed carries out rectifying in being introduced into rectifying column, in backflow Than producing butanone in the case of R=0.5~20 and reclaiming ammonia, tower bottoms continues to react in flowing into reactor, and reaction 12~18 is small When after sampling analysis, be terminal when the content of urea in reaction solution drops to 2g/l, stop heating, question response liquid is cooled to normal temperature Afterwards, through centrifugation, washing, drying to obtain carbohydrazide.Its reaction equation is as follows：

The present invention synthesizes carbohydrazide using butanone azine with urea reaction, and reaction yield is high, accessory substance is few, energy consumption is low, raw material disappears Consumption is few, and the ammonia and butanone reclaimed in course of reaction can be back to synthesis butanone azine, in addition, the carbohydrazide in reaction solution is centrifuged Remaining mother liquor after separation（Main component is butanone azine and urea）Can continue to be back to synthesis carbohydrazide, improve raw material Comprehensive utilization ratio, reduces production cost, reduces the generation and the pollution to environment of the three wastes.

Specific embodiment

Embodiment 1

The urea liquid 150ml that butanone azine 486g, concentration are 35% is placed in stirring, thermometer and reflux condensate device In four-hole boiling flask, receiver top connects a conduit to absorb ammonia.80~130 are progressively warming up under agitating heating backflow DEG C, butanone is produced in the case of reflux ratio R=0.5~20 and ammonia is reclaimed, sampling analysis after reacting 12~18 hours works as reaction Stop heating when the content of urea drops to 2g/l in liquid and terminate reaction, after question response liquid is cooled to normal temperature, carbohydrazide is centrifuged and is filtered Go out, the carbohydrazide 82g that fusing point is 152-154 DEG C is obtained after scrubbed, drying.

Embodiment 2

The urea liquid 370ml that butanone azine 1150g, concentration are 30% is placed in stirring, thermometer and reflux condensate device In four-hole boiling flask, receiver top connects a conduit to absorb ammonia.80~125 are progressively warming up under agitating heating backflow DEG C, butanone is produced in the case of reflux ratio R=0.5~20 and ammonia is reclaimed, sampling analysis after reacting 12~18 hours works as reaction Stop heating when the content of urea drops to 2g/l in liquid and terminate reaction, after question response liquid is cooled to normal temperature, carbohydrazide is centrifuged and is filtered Go out, the carbohydrazide 167g that fusing point is 152-154 DEG C is obtained after scrubbed, drying.

Embodiment 3

The urea liquid 440ml that butanone azine 1365g, concentration are 25% is placed in stirring, thermometer and reflux condensate device In four-hole boiling flask, receiver top connects a conduit to absorb ammonia.80~120 DEG C are progressively warming up in the case where being stirred at reflux, Butanone is produced in the case of reflux ratio R=0.5~20 and ammonia is reclaimed, sampling analysis after reacting 12~18 hours, when in reaction solution The content of urea stops heating and terminates reaction when dropping to 2g/l, after question response liquid is cooled to normal temperature, carbohydrazide centrifugation is leached, and passes through The carbohydrazide 172g that fusing point is 152-154 DEG C is obtained after washing, drying.

Claims

1. a kind of synthetic method of carbohydrazide, it is characterized in that：Butanone azine and urea liquid are put into reactor, 80 are heated to DEG C~130 DEG C reacted, the gas that will be steamed carries out rectifying in being introduced into rectifying column, is adopted in the case of reflux ratio R=0.5~20 Go out butanone and reclaim ammonia, tower bottoms continues to react in flowing into reactor, and sampling analysis after reacting 12~18 hours works as reaction solution The content of middle urea is terminal when dropping to 2g/l, stops heating, after question response liquid is cooled to normal temperature, is through centrifugation, washing, drying Obtain carbohydrazide.

2. the synthetic method of a kind of carbohydrazide according to claim 1, it is characterised in that：Butanone azine and urea mole Than being butanone azine: urea=2-3: 1, the concentration of urea liquid is 25%~40%.