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Oxidation treatment device and method for AK sugar crystallization waste liquid

A technology for oxidation treatment and waste liquid, applied in the direction of oxidized water/sewage treatment, chemical instruments and methods, feeding devices, etc., can solve the problems of low purity of potassium salt crude products, unresolved organic impurities, multiple secondary pollution, etc. , to achieve the effect of increasing yield, reducing production cost and reducing pollution

Inactive Publication Date: 2022-03-25
ANHUI JINGHE IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Generally, the primary crystallization mother liquor will be discharged as wastewater because of its darker color. For each ton of AK sugar produced, about 0.5 tons of wastewater will be generated. Direct discharge will cause environmental pollution and increase the cost of the product, because it contains 20~30% of potassium salt. , mainly potassium carbonate, a small amount of potassium sulfamate, potassium sulfate and potassium hydroxide, and 1~3% of AK sugar, and a small amount of organic polymers (mainly polymerized acetoacetylsulfonic acid compounds), these strong The direct discharge of alkaline crystallization mother liquor will cause environmental pollution and great economic loss
[0004] Patent No. Publication No. CN102336647B provides the use of AK sugar crystallization mother liquor and the method of using the crystallization mother liquor to prepare potassium salt. It directly mixes the crystallization mother liquor with organic acid or inorganic acid, cools, filters, and recrystallizes to obtain potassium salt product; Because this technical scheme does not consider the impact of components such as sulfamate and AK sugar by-products in the crystallization mother liquor, the purity of the potassium salt crude product obtained is not high and needs to be recrystallized to obtain a relatively pure potassium salt product, while the original crystallization mother liquor proposed The remaining waste liquid after potassium salt (containing sulfamate and AK sugar by-products and other components) needs to be treated, and the recrystallization of impure potassium salt also produces a secondary mother / waste liquid; therefore, this technology only uses the potassium resource in it. The problem of organic impurities is not solved, but more secondary pollution will be generated

Method used

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  • Oxidation treatment device and method for AK sugar crystallization waste liquid
  • Oxidation treatment device and method for AK sugar crystallization waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The primary crystallization waste liquid (potassium carbonate 10%, potassium sulfamate 2%, potassium sulfate 2.5%, potassium hydroxide 5%, acesulfame potassium 2.5%) 100mL and hydrogen peroxide (concentration of 50% %) 30mL were pumped into the fast mixer (40°C) for mixing (a lot of air bubbles and heat generated after mixing), and then entered the top of the tower reactor, as the reaction progressed, a lot of gas and heat generated, the tower The temperature in the reactor naturally rises to 90°C, and after 20 minutes of reaction, it drops to room temperature. The solution changes from dark brown before the reaction to a bright yellow transparent solution (potassium salt solution) 130mL (almost no organic components detected by gas chromatography), and enters the solution Storage tank spare.

[0030] Take 130mL of the bright yellow transparent solution obtained in Example 1, and add dropwise to 500mL of the dichloromethane solution after sulfonation and cyclization hyd...

Embodiment 2

[0032] The primary crystallization waste liquid (potassium carbonate 15%, potassium sulfamate 5%, potassium sulfate 3%, potassium hydroxide 8%, acesulfame potassium 1%) 500mL produced in the AK sugar production process was mixed with hydrogen peroxide (concentration is 50 %) 50mL were pumped into the fast mixer (80°C) for mixing (a lot of air bubbles and heat generated after mixing), and then entered the top of the tower reactor, as the reaction progressed, a lot of gas and heat generated, the tower The temperature in the reactor naturally rises to 100°C, reacts for 60 minutes and then drops to room temperature. The solution changes from dark brown before the reaction to a bright yellow transparent solution (potassium salt solution) 550mL (almost no organic components detected by gas chromatography), and enters the solution Storage tank spare.

Embodiment 3

[0034]The primary crystallization waste liquid (potassium carbonate 20%, potassium sulfamate 1%, potassium sulfate 1%, potassium hydroxide 2%, acesulfame potassium 5%) 1000mL produced in the AK sugar production process was mixed with hydrogen peroxide (concentration is 50 %) 200mL were pumped into the fast mixer (10°C) for mixing (a lot of air bubbles and heat generated after mixing), and then entered the top of the tower reactor, as the reaction progressed, a lot of gas and heat generated, the tower The temperature in the reactor naturally rises to 90°C, and after 20 minutes of reaction, it drops to room temperature. The solution changes from dark brown before the reaction to a bright yellow transparent solution (potassium salt solution) 1200mL (almost no organic components detected by gas chromatography), and enters the solution Storage tank spare.

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Abstract

The invention relates to an oxidation treatment device and method for AK sugar crystallization waste liquid, and is characterized in that a crystallization waste liquid storage tank and a hydrogen peroxide storage tank are respectively connected with a rapid mixer through pipelines, and the rapid mixer is sequentially connected with a tower reactor and a solution storage tank through pipelines; the primary crystallization waste liquid and hydrogen peroxide with the concentration of 10-55% are pumped into a rapid mixer to be mixed, the content of the hydrogen peroxide after adding is controlled to be 3-60% of the total volume concentration, then the liquid enters the top of a tower reactor, the temperature of the tower reactor is controlled to be 0-100 DEG C, the reaction time is 1-240 min, the liquid from the tower reactor enters a solution storage tank, and the liquid is discharged out of the tower reactor. The method can be applied to AK sugar production. The method has the advantages that harm caused by local overheating and overpressure due to generation of a large amount of gas and heat is avoided, and the process is efficient and safe; after hydrogen peroxide treatment, the organic high-molecular compound with deep chroma is oxidized into small molecules to be removed, a yellow clear solution is obtained and can be recycled, material consumption is reduced, and the quality of the recycled product is not affected.

Description

technical field [0001] The invention belongs to the technical field of acesulfame potassium production, and relates to an oxidation treatment device and method for AK sugar crystallization waste liquid. Background technique [0002] AK sugar, also known as acesulfame potassium, chemical name is acesulfame potassium, full name 6-methyl-2,2-dioxo-1,2,3-oxathiazepin-4-cyclohexenone potassium salt , the English name is Acesulfame Potassium (Acesulfame K), referred to as ASK. With diketene, sulfamic acid, triethylamine and sulfur trioxide as the main raw materials, it has the advantages of easy access to raw materials, mild reaction conditions, high yield, low cost, and good product quality. Now most of the AK sugar Manufacturers use this method. Its production process includes the following steps: (1) Preparation of acetoacetylsulfamate: suspending sulfamic acid and triethylamine in a solvent, and feeding diketene under temperature-controlled conditions to obtain a nearly colo...

Claims

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Application Information

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IPC IPC(8): C02F1/72B01J19/30B01J19/00B01J4/00B01J4/02C02F103/34C02F101/34
CPCC02F1/722B01J19/305B01J19/0013B01J4/008B01J4/02C02F2103/34C02F2101/34
Inventor 周睿肖世东陈永旭陈朝晖张正颂
Owner ANHUI JINGHE IND