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Method for simultaneously synthesizing chlorine dioxide and glyoxylic acid by catalyzing nitric compound

A chlorine dioxide, nitric acid technology, applied in chemical instruments and methods, chlorine oxide, preparation of organic compounds, etc., can solve the problems of slow chlorine dioxide production, incomplete conversion of glyoxal, and low equipment production capacity, etc. To achieve the effect of reducing energy consumption and production costs, improving equipment production capacity and saving resources

Inactive Publication Date: 2012-06-20
TIANJIN VOCATIONAL INST
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  • Summary
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  • Description
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AI Technical Summary

Problems solved by technology

[0014] The purpose of the present invention is to provide a kind of method stably and rapidly synthesizing chlorine dioxide and glyoxylic acid simultaneously under the presence of nitric acid compound catalyst, solves the slow production rate of chlorine dioxide under low acidity conditions in the prior art, low equipment production capacity and glyoxylic acid The problem of incomplete conversion of dialdehyde

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1 (comparative example)

[0030] In the 1000ml glass chlorine dioxide reactor, add dropwise 40% glyoxal solution 72.5g (0.5mol) with the speed of 18.1g / h, drop 50% sulfuric acid solution 300g (1.5mol) with the speed of 75.0g / h , drip 320g (1.0mol) of 50% sodium chlorate solution at the speed of 80.0g / h, heat the reactor to 45 ℃ with water bath simultaneously, blow into the air stirring solution in the reactor solution with the water jet vacuum pump, maintain the reactor pressure -0.07MPa. The water jet vacuum pump quickly separates the generated chlorine dioxide gas, and then it is completely absorbed by the sodium percarbonate solution in the absorber to obtain a stable chlorine dioxide aqueous solution. The concentration and volume of the absorption solution were regularly sampled and calculated. The average rate of chlorine dioxide generation was estimated to be 7.37g / h. After 8 hours, the conversion rate of sodium chlorate was 87.3%, the conversion rate ...

Embodiment 2

[0032]Add 10.0g of 50% nitric acid solution in the 1000ml glass chlorine dioxide reactor, add dropwise 72.5g (0.5mol) of 40% glyoxal solution with the speed of 18.1g / h, drop 50% with the speed of 75.0g / h Sulfuric acid solution 300g (1.5mol), add dropwise 50% sodium chlorate solution 320g (1.0mol) with the speed of 80.0g / h, heat the reactor to 45 ℃ with water bath simultaneously, blow air into the reactor solution with a water jet vacuum pump Stir the solution to maintain the pressure of the reactor at -0.07MPa. After about 3 minutes, the reaction starts and a large amount of chlorine dioxide gas is generated. The water jet vacuum pump quickly separates the generated chlorine dioxide gas, and the gas enters the washing column to wash and recover nitrogen oxides, and then is completely absorbed by the sodium percarbonate solution in the absorber to obtain a stable chlorine dioxide aqueous solution. Sampling is taken regularly to measure the concentration and volume of the absorb...

Embodiment 3

[0034] In embodiment 2 reactor, add 30% hydrochloric acid solution 5.0g and 50% nitric acid solution 5.0g, then react at 45 ℃, regularly take samples and measure absorption liquid concentration and volume, calculate that chlorine dioxide produces average speed and is 16.7g / h, after 4 hours, the conversion rate of sodium chlorate was 99.1%, and the conversion rate of glyoxal was 98.1%. After the completion of the reaction, measure the residual glyoxal concentration of 0.5% in the reaction solution, concentrate the reaction mother liquor in vacuo, cool, crystallize, and separate out the by-product oxalic acid crystals to obtain 70.5 g of 40.5% glyoxylic acid solution, and the glyoxylic acid yield is 77.2%.

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Abstract

The invention relates to a method for simultaneously synthesizing chlorine dioxide and glyoxylic acid by catalyzing a nitric compound, which is characterized in that: the nitric compound including nitrogen oxide, nitrogen dioxide, nitrites, nitrates or nitric acid and the like or mixture of the nitric compound and a chloride is used as a catalyst; the adding concentration of the nitric compound in a reaction solution is 0.01-0.2 mol / l; the adding concentration of a chloride catalyst is 0-0.2 mol / l; the adding mol ratio of the raw materials is that: sodium chlorate to glyoxal to sulfuric acid is equal to (0.5-1):1:(2-3); the reaction temperature is 40-60 DEG C and the concentration of the sulfuric acid is 1-3 mol / l. According to the invention, by utilizing the nitric compound catalyst, the method provided by the invention has the advantages of obviously accelerating generation speed of the chlorine dioxide, improving the production capability of equipment, improving the conversion rate of the raw material glyoxal, saving resources, and reducing the energy consumption and the production cost.

Description

technical field [0001] The invention relates to a method for synthesizing chlorine dioxide and glyoxylic acid simultaneously by reacting sodium chlorate and glyoxal in a dilute sulfuric acid medium, especially a method for synthesizing chlorine dioxide and glyoxylic acid stably and rapidly in the presence of a nitric acid compound catalyst , belonging to the field of fine chemicals. Background technique [0002] Chlorine dioxide is the 4th generation A1 safe disinfectant confirmed by the World Health Organization, and it is also an excellent bleaching agent, food preservation agent, deodorant, oxidizing agent and industrial water treatment agent. With the in-depth research on the production and application of chlorine dioxide, its new efficacy is constantly being discovered, and its application fields are also expanding. The main problems in the production of chlorine dioxide are that the production cost of chlorine dioxide is too high and the reaction waste liquid is diffi...

Claims

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Application Information

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IPC IPC(8): C01B11/02C07C59/147C07C51/275
Inventor 李建生刘炳光李霞王少杰齐国鹏吕英芳孙宝丰刘文斌唐文齐
Owner TIANJIN VOCATIONAL INST
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