Method for bipolar membrane electrodialysis treatment of 3-aminopyrazole-4-carboxamide hemisulfate production wastewater and recycling of sulfuric acid

A bipolar membrane electrodialysis and aminopyrazole technology, which is applied to membrane separation technology in the field of wastewater recycling, can solve the problems of low purity of sodium sulfate, environmental pollution, and high requirements for anticorrosion of distillation towers, so as to reduce resource consumption and improve environmental pollution. , the effect of significant economic and social benefits

Inactive Publication Date: 2014-07-23
ZHEJIANG CIRCLE TECH MEMBRANE TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current treatment method is to add alkali to neutralize sulfuric acid to free the morpholine, and then recover the morpholine by evaporation. This treatment method not only needs to consume a large amount of alkali, but also has a high concentration of sodium sulfate in the mother liquor and is highly corrosive. High anti-corrosion requirements, large investment and high maintenance costs
At the same time, the by-product sodium sulfate has low purity and low value
If the residual reaction liquid is discharged directly without treatment, it will not only cause environmental pollution, but also waste a lot of precious recyclable resources

Method used

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  • Method for bipolar membrane electrodialysis treatment of 3-aminopyrazole-4-carboxamide hemisulfate production wastewater and recycling of sulfuric acid
  • Method for bipolar membrane electrodialysis treatment of 3-aminopyrazole-4-carboxamide hemisulfate production wastewater and recycling of sulfuric acid
  • Method for bipolar membrane electrodialysis treatment of 3-aminopyrazole-4-carboxamide hemisulfate production wastewater and recycling of sulfuric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 5L of 3-aminopyrazole-4-carboxamide hemisulfate production wastewater is filtered through a cartridge filter with a filtration accuracy of 0.45 microns to remove particulate impurities and suspended solids present therein. The conductivity of the filtered wastewater is 48.9ms / cm, and the pH value is 2.32. 10 sets of 20cm*40cm bipolar membrane-cathode membrane 1-cathode membrane 2 three-compartment membrane stack are used. Both the cathode and the anode use titanium-coated ruthenium electrodes. clapboard. The filtered wastewater is pumped into the salt chamber / alkali chamber of the bipolar membrane. The compartment between the negative membrane 1 and the negative membrane 2 is called the intermediate chamber. The mass fraction of the pump is 0.1% dilute sulfuric acid, and the acid chamber of the membrane stack is the same Pump in 0.1% dilute sulfuric acid, the polar solution is 3% sodium sulfate solution, connect the cathode and anode of the device to the negative and p...

Embodiment 2

[0020] 1L of 3-aminopyrazole-4-carboxamide hemisulfate production wastewater is filtered through a cartridge filter with a filtration accuracy of 0.45 microns to remove particulate impurities and suspended solids present therein. The conductivity of the filtered wastewater is 48.9ms / cm, and the pH value is 2.32. 10 groups of 11cm*27cm bipolar membrane-cathode membrane two-compartment membrane stack are used. Both the cathode and the anode use titanium-coated ruthenium electrodes. Pump the pretreated wastewater into the salt chamber / alkali chamber of the bipolar membrane, pump 0.1% dilute sulfuric acid into the acid chamber, and 3% sodium sulfate solution as the polar liquid, and control the current density of its DC electric field to 30mA / cm 2 , the temperature is 25°C, and the bipolar membrane electrodialysis equipment is started, and the sulfuric acid with a concentration of 4.3% is recovered through the bipolar membrane electrodialysis treatment, and the deacidified wastewa...

Embodiment 3

[0022] Five groups of 11cm*27cm bipolar membrane-cathode membrane-positive membrane-bipolar membrane three-compartment membrane stack are used. Both the cathode and the anode use titanium-coated ruthenium electrodes, and the separator adopts 3 layers of anti-leakage and Elastic partition that leaks inside and outside. Pump 500ml of pretreated wastewater into the salt chamber of the bipolar membrane stack, pump 0.1% dilute sulfuric acid into the acid chamber of the membrane stack, and pump purified water or 0.1% morpholine aqueous solution into the alkali chamber of the membrane stack, The polar liquid is 1% sulfuric acid solution, and the current density of its DC electric field is controlled to be 25mA / cm 2 , the temperature is 25°C, start the bipolar membrane electrodialysis equipment, and recover the sulfuric acid with a concentration of 4% after the bipolar membrane electrodialysis treatment, and obtain morpholine by distillation and separation from the deacidified wastewa...

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Abstract

The invention discloses a method which does not pollute the environment and is used for bipolar membrane electrodialysis treatment of 3-aminopyrazole-4-carboxamide hemisulfate production wastewater and recycling of sulfuric acid. The method comprises the following steps: the 3-aminopyrazole-4-carboxamide hemisulfate production wastewater is filtered by a microporous filter with the accuracy of 0.1-0.45; the filtered wastewater is pumped into one of a salt chamber or a salt / alkali chamber or a salt / acid chamber of a bipolar membrane electrodialysis device, and an electrolyte solution with a certain concentration is injected into other compartments; a cathode and an anode of the bipolar membrane electrodialysis device are respectively connected with a negative electrode and a positive electrode of a direct-current power source, the current density of a direct-current electric field is controlled to be 10-500 mA / cm<2>, the temperature is controlled at 5-40 DEG C, the bipolar membrane electrodialysis device is started, sulfuric acid in the wastewater is removed and recycled, the sulfuric acid removal rate is above 90%, and the concentration of the recycled sulfuric acid reaches more than 4%; and the wastewater after deacidification is subjected to morpholine recycling by a distillation method.

Description

technical field [0001] The invention belongs to the application of membrane separation technology in the field of waste water recycling, and in particular relates to a method for treating 3-aminopyrazole-4-carboxamide hemisulfate waste water and recovering sulfuric acid in waste water. Background technique [0002] 3-aminopyrazole-4-carboxamide hemisulfate is an important pharmaceutical intermediate, which can be used to synthesize the anti-gout drug allopurinol, which is mainly used for gout caused by the increase of uric acid after eating high protein, It is an effective drug for treating gout, and it has a good auxiliary therapeutic effect on leukemia and hepatitis B. In industrial production, cyanoacetamide, morpholine and triethyl orthoformate are mostly used as starting materials, and the compounds are obtained through condensation, replacement, salt formation, and cyclization reactions. Due to the need to add concentrated sulfuric acid during the reaction process, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C01B17/90C07D295/023C07D295/027C02F1/469C02F103/36
Inventor 沈江南黄杰叶云飞王利祥刘晓瑞陈珏洁
Owner ZHEJIANG CIRCLE TECH MEMBRANE TECH
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