Sulfamic acid production process

A production process and sulfamic acid technology, which is applied in the directions of sulfamic acid, organic chemistry, nitrogen and non-metallic compounds, etc., can solve the problems of difficulty in transferring pastes, difficulty in filtering sulfamic acid materials, etc., and achieves low labor intensity for workers. , The effect of high product yield and easy operation

Active Publication Date: 2009-03-25
中国中化股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problems of material filtration difficulty and paste transfer difficulty in the prior art of sulfamic acid production process, the present invention proposes a more concise and rapid post-treatment process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0012] Add 1000 liters of 23% fuming sulfuric acid into a 5000 liter reactor, add 300 kg of urea in batches, and control the temperature not exceeding 45°C when feeding. After adding urea, slowly raise the temperature to 90° C. and keep it warm for 1 hour to complete the reaction. After the reaction was completed, the temperature was lowered to 40°C with stirring, and 300 liters of 20% sulfuric acid was added to adjust the concentration of sulfuric acid in the kettle to 70%. Stirring was stopped, and the material was allowed to stand for 1 hour, and the upper layer of sulfuric acid was vacuumed out. Add 4200 liters of 10% sulfuric acid in the still to adjust the concentration of sulfuric acid, be heated to 70°C, and the material is all dissolved. Then cool down to 20°C, filter, and dry to obtain 849 kg of sulfamic acid with a purity of 99.5% and a yield of 86%.

example 2

[0014] Add 1350 liters of 23% fuming sulfuric acid in 5000 liters of reactor, add 450 kilograms of urea in batches. Reaction condition is with example 1. After the reaction was finished, stir and cool down to 40°C, add 540 liters of filtrate obtained by filtering in Example 1, and adjust the concentration of sulfuric acid in the kettle to 67%. Stirring was stopped, and the material was allowed to stand for 2.5 hours, and the upper layer of sulfuric acid was vacuumed out. Add 4500 liters of 5% sulfuric acid in the still to adjust the concentration of sulfuric acid, be heated to 70°C, and the material is all dissolved. Cool down to 10-20°C, filter and dry to obtain 1255.8 kg of sulfamic acid with a purity of 99.5% and a yield of 85%.

example 3

[0016] Feeding and reaction conditions are with example 1. The post-processing operation is the same as Example 1. The only difference is that 10% sulfuric acid is used for the first acid adjustment, and 1800 kg of deionized water is used for the second acid adjustment. Dry to obtain 828.4 kg of sulfamic acid with a purity of 99.6% and a yield of 84%.

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PUM

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Abstract

The invention discloses a novel sulfamic acid after-treatment process, which comprises: carbamide is adopted to be sulfonated with oleum for preparing sulfamic acid; after the reaction the dilute sulphuric acid with the concentration of 5 to 30 percent is added to regulate the concentration of the sulphuric acid in an reaction kettle to be about 70 percent, and the sulphuric acid is isolated after holding; then the dilute sulphuric acid with the concentration of 1 to 10 percent or water is added into the reaction kettle for a second time acidity regulation to regulate the concentration of the sulphuric acid in the reaction kettle to be 5 to 20 percent; then the high pure product with the purity greater than 99.9 percent can be obtained after recrystallization, filtering and drying. The after-treatment process is easy for operation and the labor hardship is lower; and the purity of the product is high and the quality is better.

Description

technical field [0001] The invention belongs to the field of inorganic synthesis, and in particular relates to a production process of sulfamic acid. technical background [0002] Sulfamic acid is an important fine chemical, mainly used in the production of sodium cyclamate cyclamate in recent years, and also used in herbicides, fire retardants, metal and ceramic cleaners, softening of paper and textiles And bleach and other uses. At present, the main production process of sulfamic acid manufacturers at home and abroad is sulfonation of urea by oleum. Because this process has the advantages of large production capacity, good product quality, safety, and less waste, people have been constantly researching this process and striving for further improvement and perfection. For example, Russian patent RU 2240997C in 2004 improved the post-treatment method and proposed a new simplified post-treatment process: the sulfonate was directly filtered without dilution, and the obtained...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/096C07C307/02
Inventor 李付刚白雪松李文骁
Owner 中国中化股份有限公司
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