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Process for preparing 5,5-dimethyl-2,4-imidazolinedione by intermittent presurizing method

A technology of imidazolidinedione and dimethyl, which is applied in the field of pressurized batch method preparation 5, can solve the problems of complex reaction equipment, difficulty in industrialization, high toxicity of sodium cyanide, etc., and achieve simple preparation process and easy control of conditions Effect

Inactive Publication Date: 2002-07-03
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the reaction equipment is complex, the process is difficult, and the energy consumption is high
(4), acetone and sodium cyanide direct method: directly use acetone, sodium cyanide and ammonia water as raw materials, and the yield can reach 90%. Realize industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Example 1: Add 34 grams (36.48 mL) of acetone cyanohydrin, 40 milliliters of water, and 35 grams of ammonium bicarbonate in a 140 milliliter autoclave, heat to 65-75 ° C, and the pressure rises to 0.8-1.4 MPa. Insulate and react at 70° C. for 1.5 hours until the pressure drops by 0.26 MPa. Pressure relief, cooling, filtering and drying. Yield: 35 g, 70% yield.

Embodiment 2

[0009] Example 2: Add 34 grams (36.48 mL) of acetone cyanohydrin, 45 milliliters of reaction mother liquor, and 35 grams of ammonium bicarbonate into a 140 milliliter autoclave, heat to 65-75 ° C, and the pressure rises to 0.8-1.4 MPa. Insulate and react at 70°C for 1.5 hours until the pressure drops to 0.25MPa. Release the pressure, cool down to 20°C, filter and dry. Yield: 46.5 g, yield 92-94%.

Embodiment 3

[0010] Embodiment 3: add 340 kilograms (364.8L) acetone cyanohydrin in 1500 liters of autoclaves, 450 liters of mother liquors, 350 kilograms of ammonium bicarbonate, under stirring, pass steam in jacket and heat to 40 ℃, stop heating, naturally warming up to 70~ At 75°C, the pressure rises to 1.4-1.8MPa. Insulate and react at 70-75°C for 2 hours until the pressure drops below 0.3MPa. Cool down to 40°C with cooling water, release the pressure, continue cooling to 20°C, discharge, filter, and dry. Yield: 468 kg, yield 92-94%.

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PUM

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Abstract

A process for preapring 5,5-dimethyl-2,4-imidazolinedione by intermittent pressurizing method includes dissolving the acetone cyanohydrin and ammonium dicarbonate as raw material in water or mother liquid, heating, cyclizing reaction at 50-90 deg.C and 0.8-1.8 MPa for 0.5-20 hrs, cooling-crystallizing filtering and drying. Its advantages include simple process, easy control, and high purity and output rate of product.

Description

technical field [0001] The invention relates to a method for preparing 5,5-dimethyl-2,4-imidazolidinedione by a pressurized batch method. It belongs to the preparation technology of 5,5-dimethyl-2,4-imidazolidinedione. The structural formula of 5,5-dimethyl-2,4-imidazolidinedione is shown in the following formula: Background technique [0002] 5,5-Dimethyl-2,4-imidazolidinedione (dimethylhydantoin) is a highly effective disinfectant for the preparation of dichlorodimethylhydantoin, dibromodimethylhydantoin, and bromochlorodimethylhydantoin The main raw material of hydantoin; it is also the main raw material for the preparation of hydantoin resin. Especially bromochlorodimethylhydantoin, which has high activity (it can kill bacteria, algae, etc. in water very effectively at a concentration lower than 1ppm), broad-spectrum biocidal property, long-lasting effect, and wide application pH range , Insensitivity to nitrogenous compounds in wat...

Claims

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Application Information

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IPC IPC(8): C07D233/74
Inventor 张文勤赵温涛齐欣赵海涛
Owner TIANJIN UNIV
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