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Method for preparing cyanuric acid by using ionic liquid

A technology of ionic liquid and cyanuric acid, applied in organic chemistry, bulk chemical production, etc., can solve the problems of not conforming to the concept of green chemistry, complex recycling process, expensive solvent, etc., to solve the problem of solvent evaporation and high heat transfer efficiency , the effect of reducing energy consumption

Active Publication Date: 2021-06-04
山东大明消毒科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing research, there are still many problems in the solvent method. For example, the solvent is expensive, the recycling process is complicated, and it is difficult to industrialize; there is still the problem of solvent volatilization in actual operation, which does not conform to the concept of green chemistry, etc.

Method used

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  • Method for preparing cyanuric acid by using ionic liquid
  • Method for preparing cyanuric acid by using ionic liquid
  • Method for preparing cyanuric acid by using ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Take an appropriate amount of 1-ethyl-3-methylimidazolium tetrafluoroborate ionic liquid, add it into the reaction kettle, start the stirring device, and start the vacuum circulation pump. When heating to 150°C, feed at a rate of 20Kg / min, and feed urea according to the ratio of solvent volume (mL) to urea mass (g) at 2:1. Rapidly heat to 210°C for condensation reaction. After reacting for 3 hours, the obtained slurry is cooled to room temperature and then centrifuged for 3 hours at a speed of 500 r / min. The centrifuged product is washed with distilled water and is crude cyanuric acid. Compared with the traditional direct pyrolysis method, the energy consumption is saved by 16%, the reaction yield is 89.4%, the purity of cyanuric acid is 90.7%, and the urea conversion rate is 81.1%.

Embodiment 2

[0028] Take an appropriate amount of 1-butyl-3-methylimidazolium tetrafluoroborate ionic liquid, add it into the reaction kettle, start the stirring device, and start the vacuum circulation pump. When heating to 140°C, feed at a rate of 30Kg / min, and the ratio of solvent volume (mL) to urea mass (g) is 2.5:1. Rapidly heat to 200°C for condensation reaction. After 4 hours of reaction, cool the resulting slurry to room temperature and centrifuge for 2.5 hours at a speed of 700r / min. The centrifuged product is washed with pure water, and the centrifuged product is crude cyanuric acid. Compared with the traditional direct pyrolysis method, the energy consumption is saved by 20%, the reaction yield is 87.3%, the purity of cyanuric acid is 93.5%, and the urea conversion rate is 81.6%.

Embodiment 3

[0030] Take an appropriate amount of 1-butyl-3-methylimidazolium dicyandiamide salt ionic liquid, add it to the reaction kettle, turn on the stirring device, turn on the vacuum circulation pump, and when heated to 145°C, feed at a constant speed of 20Kg / min. The ratio of solvent volume (mL) to urea mass (g) is 4:1. Rapidly heat to 190°C for condensation reaction. After reacting for 5 hours, the resulting slurry is cooled to room temperature and then centrifuged for 2 hours at a speed of 1000r / min. The centrifuged product is washed with distilled water, and the centrifuged product is crude cyanuric acid. Compared with the traditional direct pyrolysis method, energy consumption is saved by 24%, the reaction yield is 90.7%, the purity of cyanuric acid is 96.4%, and the conversion rate of urea is 87.4%.

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Abstract

The invention discloses a method for preparing cyanuric acid by using ionic liquid, and the method comprises the following steps: carrying out condensation reaction on the ionic liquid serving as a solvent and urea in vacuum, stirring and heating states, centrifuging the reaction product, and washing the obtained solid product with water to obtain crude cyanuric acid. The ionic liquid serves as a novel solvent for preparing cyanuric acid through a solvent method, urea is effectively dissolved, heat transfer efficiency is high, energy consumption is reduced, the condensation temperature is reduced to 190-210 DEG C from 220-280 DEG C of a traditional direct pyrolysis method, energy consumption is saved by 16%-24%, the yield of the prepared crude cyanuric acid is 86.6%-90.7%, the purity is 90.7%-96.4%, and the urea conversion rate is 80% or above. The operation process is reduced, the generation of wastes and the use of sulfuric acid in the subsequent refining process are reduced, the problem of solvent volatilization is solved, and the method is simple in recovery and environment-friendly.

Description

technical field [0001] The invention relates to a production method for preparing cyanuric acid, in particular to a production method for preparing cyanuric acid by using an ionic liquid method, and belongs to the field of fine chemicals. Background technique [0002] Cyanuric acid, also known as cyanuric acid, can be used directly as a stabilizer for swimming pool chlorine treatment agents, as a flame retardant for nylon and polyester, and as an important intermediate product for a series of fine chemical products, involving pharmaceuticals, pesticides, Fuel paint, light industry and other fields. Its chlorinated derivative, chloroisocyanuric acid, is an excellent water treatment agent and fungicide, and has played an important role in sterilization and disinfection during the prevention and control of the "new crown pneumonia epidemic". [0003] Theoretically, there are five routes for synthesizing cyanuric acid: phosgene method, cyanuric acid trimerization, hydrocyanic a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/32
CPCC07D251/32Y02P20/54
Inventor 门吉帅邵腾邵长银李成顺李刚翟浩志
Owner 山东大明消毒科技有限公司
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