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Energy-saving and environment-friendly synthesis technology for 1,2,4-1H triazole

An energy-saving, environmental-friendly, synthetic process technology, applied in the direction of organic chemistry, can solve the problems of high by-product treatment costs, high equipment maintenance costs, complex production processes, etc., achieve low production costs, solve corrosion problems, and simple production processes Effect

Active Publication Date: 2018-03-23
新泰市日进化工科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] This method has the advantages of low raw material price, easy availability, easy decomposition of impurity ammonium formate, high yield (85-90%), and low raw material cost. High, and the formic acid has great corrosion on the equipment, resulting in high equipment maintenance costs. At the same time, this method also has problems with the use of ammonia gas and emission absorption. The cost of by-product treatment is high, and ammonia is not recycled. It is also a waste of resources

Method used

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  • Energy-saving and environment-friendly synthesis technology for 1,2,4-1H triazole
  • Energy-saving and environment-friendly synthesis technology for 1,2,4-1H triazole
  • Energy-saving and environment-friendly synthesis technology for 1,2,4-1H triazole

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Experimental program
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Embodiment 1

[0040] Step S1, put all the formamide raw materials into the reaction kettle in advance, slowly add hydrazine hydrate into the formamide from the elevated tank, and react to form the main product 1,2,4-1H triazole;

[0041] The ammonia produced in step S2 and step S1 enters the acid shower device through the gas phase inlet, and the formic acid enters the acid shower device through the acid input port, and the cooled ammonia reacts with the formic acid sprayed to generate ammonium formate;

[0042] The ammonium formate generated in step S3 and step S2 is cooled and refluxed into the reactor in the leaching device, and reacts with hydrazine hydrate to generate the main product 1,2,4-1H triazole.

[0043] In steps S1 and S2, the reaction temperature is controlled at 150-160°C.

[0044] In order to make the reactants fully react and discharge waste gas as little as possible, preferably, the mass ratio of formamide, hydrazine hydrate, and formic acid is (1.3-1.7):(0.7-1.1):(0.1-0....

Embodiment 2

[0053] On the basis of Embodiment 1, the applicant has also made the following design, see figure 1 , in order to be able to monitor the temperature in the acid shower in real time, the top of the container body 1 is provided with a temperature sensor 11, and the temperature sensor 11 is inserted into the container body 1.

Embodiment 3

[0055] On the basis of Embodiment 1, the applicant has also made the following design, see figure 1 , in order to be able to monitor the pH value at the outlet of the gas phase in real time, an ammonia content detector 12 is provided at the outlet of the gas phase at 3 places, and a condenser 16 is set at the outlet of the gas phase at the same time. Exhaust gas absorption device 17.

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Abstract

The invention provides an energy-saving and environment-friendly synthesis technology for 1,2,4-1H triazole. The technology comprises following steps: S1, a formamide raw material is totally put in areaction kettle in advance, hydrazine hydrate is slowly added to formamide from an elevated tank, and a main product 1,2,4-1H triazole is produced through reaction; S2, ammonia produced in S1 enters an acid spraying device through a gas phase inlet, formic acid enters the acid spraying device through an acid inlet, and cooled ammonia and sprayed formic acid react to produce ammonium formate; S3, ammonium formate produced in S2 is cooled in the acid spraying device, flows back to the reaction kettle and reacts with hydrazine hydrate, and the main product 1,2,4-1H triazole is produced. Accordingto the energy-saving and environment-friendly synthesis technology for 1,2,4-1H triazole, formic acid is added to the acid spraying device, so that firstly, production of ammonia as a byproduct is reduced, secondly, the byproduct ammonia is used sufficiently, consumption of formamide is reduced, the use is convenient, and the raw materials are saved.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to an energy-saving and environment-friendly synthesis process of 1,2,4-1H triazole. Background technique [0002] 1,2,4-1H triazole, also known as 1,2,4-triazole, is a colorless needle-like crystal with a melting point of 120°C and a boiling point of 260°C, soluble in water and ethanol, and usually reacted by formamide and hydrazine It is mainly used in the production of pesticides, medicines (fluconazole), dyes, and rubber additives, and is also used in the photoconductor of the replication system. It is an important organic chemical intermediate, and its demand is increasing year by year with the market. . [0003] At present, there are two main methods for synthesizing 1,2,4-1H triazole: one is the reaction of formamide and hydrazine hydrate to generate 1,2,4-1H triazole, [0004] [0005] The method is by formamide and hydrazine hydrate as raw material, and produc...

Claims

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Application Information

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IPC IPC(8): C07D249/08
Inventor 张纪平张书青
Owner 新泰市日进化工科技有限公司
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