Method for preparing urea peroxide

A technology of urea peroxide and hydrogen peroxide, applied in the preparation of organic compounds, chemical instruments and methods, preparation of urea derivatives, etc., can solve the problems of low production efficiency, high operation requirements, complex production process, etc., and achieve stable production. High efficiency, overcoming the effect of complex process and low equipment requirements

Inactive Publication Date: 2008-08-06
LIER CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires a very cumbersome treatment operation for the stabilizer, which is generally carried out at a relatively low temperature. The operation is very demanding, the composition is complex, and the operation process produces a lot of waste water. The drying process in the preparation process is completed in an oven. , and takes 45 to 105 minutes
Therefore, its method is only suitable for preparation in the laboratory, and is difficult to be suitable for industrial scale production
Although this method can overcome the disadvantages of complex process, high requirements on reaction conditions, low yield and poor product stability of the previous method using low-concentration hydrogen peroxide as a raw material, it still has the above-mentioned production process caused by the above-mentioned problems. Complex, long process, low yield, and the increase of production volume will inevitably lead to the extension of evaporation time, so the production efficiency is low, oven baking requires a large specific surface area, and requires a large space and area of ​​equipment, and occupies Insufficient such as large land area is not conducive to large-scale industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 5400g of 27.5% hydrogen peroxide and add it to a 10L three-necked bottle, add 2015g urea crystals, 0.5g disodium EDTA, 0.5g citric acid, 2g polyethylene glycol film-forming agent (280g / mol), heat in a water bath at 45°C, and stir mechanically Under the vacuum of -0.092Mpa, after 120min, after 3500g of water evaporated, the mixed solution was poured into a 5L beaker, crystallized rapidly in an ice-water bath at 15°C, centrifuged in a centrifuge, dried in an oven, and the filtrate was reduced again Evaporate under pressure, crystallize, dry, and combine the obtained crystals to obtain 3154 g of white flaky crystal product urea peroxide with a yield of 99.92%. The content of active oxygen in titration analysis is 16.97%.

Embodiment 2

[0019] Take 5400g of 27.5% hydrogen peroxide and add it to a 10L three-necked bottle, add 1782g of urea crystals, 0.5g of disodium EDTA, 1g of citric acid, and 1.5g of film-forming agent (367g / mol), heat in a water bath at 50°C, and under mechanical stirring, vacuum -0.090Mpa, after 100min, after 3520g of water evaporated, pour the mixed solution into a 5L beaker, crystallize rapidly in an ice-water bath at 10°C, centrifuge for centrifugation, put it in an oven for drying, and the filtrate is evaporated again under reduced pressure. Crystallize, dry, and combine the obtained crystals to obtain 2787.9 g of white flaky crystal product urea peroxide, with a yield of 99.86%, and the titration analysis shows that the active oxygen content is 17.00%.

Embodiment 3

[0021] Take 5400g of 27.5% hydrogen peroxide and put it into a 10L three-necked bottle, add 1635g of urea crystals, 1g of disodium EDTA, 3g of citric acid, 2g of film-forming agent (454g / mol), heat in a water bath at 60°C, and under mechanical stirring, the vacuum temperature is -0.087 Mpa, after 95 minutes, after 3496g of water evaporated, pour the mixed solution into a 10L beaker, crystallize rapidly in an ice-water bath at 20°C, centrifuge for centrifugation, put it in an oven for drying, and the filtrate is evaporated again under reduced pressure, crystallized, and dried Dry, combine gained crystal, obtain white flaky crystal product urea peroxide 2555g, yield 99.75%, titration analysis active oxygen content is 16.98%.

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Abstract

A preparation method of urea peroxide comprises uniformly mixing urea solution, 25-50% hydrogen dioxide solution, stabilizer and carbowax filming agent, to be dewatered, cooled and crystallized in vacuum of -0.085 to -0.095MPa at a temperature of 40 to 63 DEG C, wherein the weight ratio of hydrogen dioxide in urea and hydrogen dioxide is 1:(1.0-1.4), the stabilizer is a mixture of endrate disodium (EDTA sodium) and citrate at a weight ratio of 1:(1-3), the stabilizer is 0.001-0.5% of urea by weight, and the filming agent is 0.05-0.2% of the urea by weight. The preparation method of urea peroxide can obtain high-stability urea peroxide crystal of high yield, with better crystal form, high stability, simple production process, small volume, no generation of three wastes and application in industrial batch production, while the stabilizer and filming agent have single component to avoid complex treatment.

Description

technical field [0001] The invention relates to an improved preparation method of urea peroxide, in particular to an industrialized production method capable of realizing high stability and high yield of urea peroxide. Background technique [0002] Urea peroxide is also known as carbamide peroxide, carbamide peroxide, urea hydrogen peroxide, etc. It is a white flaky crystal or powdery solid, non-toxic and tasteless, and its molecular formula is CO(NH 2 ) 2 ·H 2 o 2 , its theoretical content of active oxygen is 17.02%. [0003] Urea peroxide is a new type of fine chemical, which effectively solves the problem of storage and transportation of high-concentration hydrogen peroxide, and can be widely used in many fields such as agriculture, medicine, textile, daily chemical industry, food, breeding, feed, metallurgy, construction, etc. . For example, it can be used as a highly efficient, safe, and easy-to-operate solid disinfectant, oxygen supply and bleaching agent; it can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C409/40C07C273/02
Inventor 周波范谦张杰胡玉容
Owner LIER CHEM CO LTD
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