Improved K acid synthesis technology

A synthesis process, acid analysis technology, applied in the field of improved K-acid synthesis process, to achieve the effects of mild reaction conditions, easy industrialization, and less land occupation

Inactive Publication Date: 2016-02-24
ZHEJIANG QICAI ECO TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The invention discloses an improved K-acid synthesis process. The K-acid wastewater is treated by pretreatment, electrodialysis and bipolar membrane...

Method used

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  • Improved K acid synthesis technology

Examples

Experimental program
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Effect test

Embodiment 1

[0060] K acid wastewater, black, COD 25000-26000mg / L, pH 2.

[0061] (1) Pretreatment: wet oxidation

[0062] Take K-acid wastewater, adjust the pH of the wastewater to about 7 with potassium hydroxide solution, place it in a wet oxidation reaction kettle, and perform a wet oxidation reaction at a pressure of 3 MPa and a temperature of 220°C for 120 minutes, then filter to obtain the filtrate, and its COD is measured to be 1724 mg / L.

[0063] (2) Concentration by electrodialysis: the filtrate obtained in the above steps is treated by an ordinary electrodialysis device, and the concentrated water obtained is the concentrated salt solution, and the obtained fresh water is mixed with the pretreated filtrate and concentrated by electrodialysis. Reaction conditions of electrodialysis: 2% sodium sulfate solution is used as the polar liquid, and the current density is 200A / m 2 , and the reaction temperature was 30°C.

[0064] (3) Bipolar membrane desalination: The concentrated wa...

Embodiment 2

[0067] K acid wastewater, black, COD 25000-26000mg / L, pH 2.

[0068] (1) Pretreatment: catalytic wet oxidation

[0069] Take the K-acid wastewater, adjust the pH to about 7 with potassium hydroxide solution, and add 0.5% copper sulfate (based on the quality of the K-acid wastewater), put it in a wet oxidation reactor, at a pressure of 3MPa, at a temperature of 220°C, wet oxidation After oxidizing for 90 minutes, filter to obtain the filtrate, whose COD was determined to be 1467 mg / L.

[0070] (2) Concentration by electrodialysis: The filtrate is treated by ordinary electrodialysis equipment, and the obtained concentrated water is the concentrated salt solution, and the obtained fresh water is then mixed with the pretreated filtrate and concentrated by electrodialysis. Reaction conditions of electrodialysis: 2% sodium sulfate solution is used as the polar liquid, and the current density is 200A / m 2 , and the reaction temperature was 30°C.

[0071] (3) Bipolar membrane desali...

Embodiment 3

[0074] K acid wastewater, black, COD 25000-26000mg / L, pH 2.

[0075] (1) Pretreatment: diazotization-micro-electrolysis-flocculation-adsorption

[0076] Diazotization: Take K acid wastewater and place it in an ice bath at 0-10°C, then add dropwise a 30% sodium nitrite aqueous solution until the starch potassium iodide test paper turns blue, use sulfuric acid to keep the pH of the system constant, and stir for 1 hour. After the reaction was completed, stand still for 1 h, and filter to obtain the filtrate.

[0077] Micro-electrolysis: Add 0.3% activated carbon and 0.2% iron powder (based on the quality of K-acid wastewater) to the above-mentioned filtrate after diazotization reaction, stir for 4 hours, and always maintain the system pH=3, filter and separate to obtain the filtrate .

[0078] Flocculation: Use potassium hydroxide solution to adjust the pH of the above filtrate to 8-9, stir quickly at 300-500rpm for 5-10min, stir slowly at 1-200rpm for 10-20min, add 0.1% activa...

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Abstract

The invention discloses an improved K acid synthesis technology. Through primary sulfonation, salting-out, ammonification, acidification and secondary sulfonation, a K acid product and K acid waste water are prepared from 2-naphthol. The K acid waste water treatment process comprises 1, pre-treatment: pre-treating K acid waste water to remove organic impurities of the waste water and to obtain a filtrate, 2, electroosmosis concentration: carrying out common electroosmosis concentration on the pretreated filtrate to obtain concentrated water and fresh water, 3, bipolar membrane desalination: carrying out bipolar membrane electroosmosis on the concentrated water obtained by the step 2 to obtain a sulfuric acid solution, a potassium hydroxide solution and dilute brine, recycling the sulfuric acid solution and the potassium hydroxide solution in the K acid synthesis process and/or the step 1, returning the dilute brine into an electroosmosis device and carrying out re-condensation. The improved K acid synthesis technology realizes standard discharge of waste water produced by the K acid synthesis technology, utilizes an effective resource in waste water by the bipolar membrane electroosmosis technology, realizes use in the technology and reduces a K acid synthesis cost.

Description

technical field [0001] The invention relates to the technical field of dye intermediate synthesis process improvement and wastewater treatment thereof, in particular to an improved K acid synthesis process. Background technique [0002] K acid, scientific name is 2-naphthylamine-3,6,8-trisulfonic acid naphthalene, colorless or light brown powder, slightly soluble in hot water, soluble in soda ash or caustic soda solution, yellow-green when reacted with ferric oxide . K acid is an important intermediate of azo dyes, reactive dyes and organic pigments, used in the production of cationic dyes, reactive brilliant red K-2G, 2R acid, etc. [0003] At present, the domestic traditional K acid production process is that 2-naphthol is sulfonated with concentrated sulfuric acid and oleum to obtain 2-naphthol-6,8 disulfonic acid, and then salted out with KCl / NaCl to obtain G salt, and G salt is further K acid can be obtained after ammoniation, acid analysis and secondary sulfonation. ...

Claims

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Application Information

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IPC IPC(8): C02F9/06C02F103/36
CPCC02F9/00C02F1/00C02F1/28C02F1/461C02F1/4693C02F1/52C02F1/66C02F1/72C02F2103/36C02F2201/46115C02F2305/026
Inventor 张云保梁伟陈丽娜施孟华
Owner ZHEJIANG QICAI ECO TECH CO LTD
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