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Method for preparing high-purity chlorine dioxide by using agronomic crop stalk and method for preparing catalyst used therein

A technology of crop straw and chlorine dioxide, which is applied in the direction of chlorine oxidation, can solve the problems of difficult control of reaction conditions, slow reaction speed, and poor purity, and achieve the effects of extending the agricultural industry chain, mild reaction conditions, and reducing production costs

Inactive Publication Date: 2010-06-23
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, Li Ruizhen et al. reported (Journal of Qiongzhou University, 2003, 10 (2) 15-17) that sodium chlorate was dissolved in a certain concentration of sulfuric acid solution to prepare high-purity chlorine dioxide under the action of a catalyst. Metal oxides are dissolved in hydrochloric acid, n-butanol is added, and dried porcelain tubes are used for adsorption treatment, and then the porcelain tubes adsorbed with catalysts are added to the reaction solution at a certain temperature to prepare chlorine dioxide, and the purity of chlorine dioxide reaches 98.4-99.8%; And if do not adopt catalyzer in this reaction, sodium chlorate and sulfuric acid reaction are violently difficult to control, and the productive rate of chlorine dioxide is low, poor in purity; The absorption of %KI solution will increase the production cost. This method can only be used as a research method and has no practical value
In the existing method for preparing chlorine dioxide, either the reaction speed is slow, or the reaction is violent and dangerous, not only the reaction conditions are difficult to control, but also the operation is complicated. The key is that the chlorine dioxide yield is low, the purity is poor, and the production cost is high. also higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Take 20 mL of 500 g / L sodium chlorate solution and add it to a 250 mL three-necked flask equipped with electric stirring, then add 1.40 g of dry 120-mesh bagasse and 0.06 g of catalyst, and heat to 60°C in a water bath while stirring. Add 31.5mL of 1:1 sulfuric acid dropwise to the three-necked flask with a constant pressure separating funnel, and at the same time start the vacuum pump, draw out the newly generated chlorine dioxide with an air duct, and absorb it with five-grade ice water. When the 1:1 sulfuric acid is added (the concentration of sulfuric acid in the system is about 5.5mol / L), the temperature of the water bath is raised to 70°C to continue the reaction. After the yellow-green color of the reaction solution in the three-necked flask fades, it becomes a light blue transparent solution. To end the reaction, use about 70mL. After mixing the chlorine dioxide aqueous solution in the five absorption bottles evenly, take a sample and measure the chlorine dioxid...

Embodiment 2

[0014] Take 20 mL of 500 g / L sodium chlorate solution and add it to a 250 mL three-necked flask equipped with electric stirring, then add 1.50 g of dry 120-mesh bagasse and 0.06 g of catalyst, and heat to 60°C in a water bath while stirring. Add 25.0mL of 1:1 sulfuric acid dropwise to the three-necked flask with a constant-pressure separating funnel, and at the same time start the vacuum pump, draw out the newly generated chlorine dioxide with an air duct, and absorb it with five-grade ice water. When the 1:1 sulfuric acid is added (the concentration of sulfuric acid in the system is about 5.0mol / L), raise the temperature of the water bath to 65°C and continue the reaction. After the yellow-green color of the reaction solution in the three-necked flask fades, it becomes a light blue transparent solution. End the reaction, about 66mi.. After mixing the chlorine dioxide aqueous solution in the five absorption bottles evenly, take a sample and measure the chlorine dioxide content...

Embodiment 3

[0016] Take 20 mL of 500 g / L sodium chlorate solution and add it to a 250 mL three-necked flask equipped with electric stirring, then add 1.35 g of dry 120-mesh rice straw and 0.06 g of catalyst, heat to 70 ° C in a water bath while stirring, and use Add 31.5mL of 1:1 sulfuric acid dropwise into the three-necked flask through the constant-pressure separating funnel, and at the same time start the vacuum pump, draw out the newly generated chlorine dioxide with the air duct, and absorb it with five-grade ice water. When the 1:1 sulfuric acid is added (the concentration of sulfuric acid in the system is about 5.5mol / L), the temperature of the water bath is raised to 80°C to continue the reaction. After the yellow-green color of the reaction solution in the three-necked flask fades, it becomes a light blue transparent solution. End the reaction, about 50mi.. After mixing the chlorine dioxide aqueous solution in the five absorption bottles evenly, take a sample and measure the chlo...

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PUM

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Abstract

The invention discloses a method for adopting crop stalk to prepare high-pure chlorine dioxide. The crushed and dried crop stalks and catalyst are added into the sodium chlorate solution and the mass ratio between the sodium chlorate, crop stalk and catalyst is controlled to be 10:1.20 to 2.20:0.01 to 0.10; then the reaction system is heated to 60 to 70 DEG C in water, the sulfuric acid of 1 / 1 isslowly added into the mixture while stirring, the reaction temperature is controlled to be 50 to 90 DEG C, the concentration of the sulfuric acid in the system is 4.5 to 8.0mol / L, and then the chlorine dioxide is guided out under the negative pressure and is absorbed by iced water; and the catalyst is the complex-type ammonium citrate vanadyl. The reaction condition of the invention is gentle andthe reaction speed is quick; the reaction is stable and safe; the operation is convenient; the productivity of chlorine dioxide is high, the purity is high; and the manufacturing cost is low.

Description

technical field [0001] The invention relates to the technical field of preparation of disinfectant compounds, in particular to a method for preparing high-purity chlorine dioxide with crop stalks under the action of a catalyst and a preparation method of the catalyst used. Background technique [0002] Chlorine dioxide is a yellow-green or orange-yellow gas at normal temperature and pressure. Due to its special unsaturated electronic layer structure, it has strong oxidation ability in a wide range of pH values ​​(redox electrode potential is about 1.50V), and is Known as a high-efficiency, broad-spectrum sterilizing disinfectant, it is recommended by the World Health Organization (WHO) as an A1-level safe disinfectant. Chlorine dioxide is widely used in drinking water disinfection, pulp and fabric bleaching, food processing, vegetable and fruit preservation, industrial cooling water and wastewater treatment, water injection oil production and oil well deblocking, sanitation ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B11/02
Inventor 吴本来张鸿云牛云垠张铁财王凤珍徐金霞张超
Owner ZHENGZHOU UNIV