Treatment method of high-concentration high-salinity wastewater in nitrochlorobenzene meta-position oil separation

A nitrochlorobenzene meta-oil, high-concentration technology, applied in the direction of neutralization water/sewage treatment, water/sewage treatment, water treatment parameter control, etc. The three wastes of the chlorobenzene-meta-position oil separation technology have achieved the effect of saving processing time and low cost

Active Publication Date: 2021-12-03
SINOPEC NANJING RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN104557557A, CN101935281A, CN106496039A, and CN106883129A are all processes for separating nitrochlorobenzene meta-oil by etherification, but they do not describe and decompose the wastewater generated by the etherification process itself, nor provide corresponding methods
[0008]The above patents have not fundamentally solved the three wastes in the separation technology of nitrochlorobenzene meta-oil

Method used

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  • Treatment method of high-concentration high-salinity wastewater in nitrochlorobenzene meta-position oil separation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] ①Acidification process: Collect 1000mL of etherified wastewater with a COD of 75000 mg / L and a chroma of 4100, add 20% sulfuric acid dropwise for acidification, adjust the pH to 3~4, the color of the solution turns from brownish red to khaki yellow, and precipitates Yellow crystal, with vacuum filtration, the filtrate was taken for analysis, the COD was reduced to 45000 mg / L, and the filter residue was mainly o-nitrophenol (93.03%) and a small amount of nitroanisole (5.52%).

[0023] ② Oxidation process: take 30ml of acidified water sample and dilute it 10 times, then add it to a 500ml four-necked flask, raise the temperature to 80-90°C while stirring, maintain the temperature, and drop the measured 10 % ferrous sulfate solution and 25% hydrogen peroxide. After the addition, the reaction was cooled for 30 minutes. When it reached 50°C, start adding alkali to adjust the pH to 7~8. There was precipitation in the bottle. It is iron salt, the COD of the oxidized effluent i...

Embodiment 2

[0026] ① Acidification process: Collect 1000mL of etherification wastewater with a COD of 76000 mg / L and a chroma of 4200, add 20% phosphoric acid dropwise for acidification, adjust the pH to 3~4, the color of the solution turns from brownish red to earthy yellow, and precipitates Yellow crystal, with vacuum filtration, the filtrate was taken for analysis, the COD was reduced to 40000 mg / L, and the filter residue was mainly o-nitrophenol (94.25%) and a small amount of nitroanisole (3.89%).

[0027] ②Oxidation process: take 30ml of acidified water sample and dilute it 10 times, then add it to a 500ml four-necked flask, raise the temperature to 80-90°C while stirring, maintain the temperature, and drop the measured 12 % ferrous sulfate solution and 29% hydrogen peroxide. After adding, react for 20 minutes to cool down. When it reaches 50°C, start adding alkali to adjust the pH to 7~8. There is precipitation in the bottle. It is iron salt, the COD of the oxidized water is 630 mg...

Embodiment 3

[0030] ① Acidification process: Collect 1000mL of etherified wastewater with a COD of 59000 mg / L and a chroma of 3000, add 25% sulfuric acid dropwise for acidification, adjust the pH to 3~4, the color of the solution turns from brownish red to khaki yellow, and precipitates Yellow crystal, with vacuum filtration, the filtrate was taken for analysis, the COD was reduced to 20000 mg / L, and the filter residue was mainly o-nitrophenol (93.25%) and a small amount of nitroanisole (6.19%).

[0031] ② Oxidation process: Take 30ml of acidified water sample and dilute it 15 times, then add it into a 500ml four-necked flask, heat up to 80-90°C while stirring, and keep the temperature, dropwise add the measured 12 % ferrous sulfate solution and 20% hydrogen peroxide. After adding, react for 20 minutes to cool down. When it reaches 50°C, start adding alkali to adjust the pH to 7~8. There is precipitation in the bottle. It is an iron salt, the COD of the oxidized water is 350 mg / L, the chr...

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Abstract

The invention relates to a treatment process of high-concentration high-salinity wastewater in a nitrochlorobenzene meta-position oil separation process. The method comprises two links of acidification pretreatment and catalytic oxidation: collecting high-salt and high-concentration washing water which is difficult to biochemically degrade in a nitrochlorobenzene meta-position oil etherification process, firstly dropwise adding sulfuric acid for acidification, adjusting the pH value to 2-5, and filtering after the color of the solution is converted from brownish red to earthy yellow and earthy yellow crystals are separated out, and diluting the filtered water, adding hydrogen peroxide and ferrous sulfate to carry out catalytic oxidation treatment, adding alkali to adjust the pH value to be neutral, filtering again, carrying out biochemical treatment on the filtered water, directly discharging the filtered water, and mixing the filter residue and the filter residue in the acidification process to be incinerated. The method is low in cost and suitable for industrial production, and is a green and environment-friendly process route.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and relates to a treatment method for high-concentration and high-salinity wastewater in a nitrochlorobenzene meta-oil separation process. Background technique [0002] At present, China, the world's largest producer of nitrochlorobenzene, has an annual production capacity of 800,000 tons, and will produce more than 13,000 tons of meta-oil per year. The reuse of meta-oil due to nitrochlorobenzene has good economic and social benefits. The recycling process of nitrochlorobenzene meta-oil includes etherification method, ammonification method and chlorination method. [0003] The meta-oil etherification process is one of the meta-oil separation technologies. This method is to etherify the meta-oil of nitrochlorobenzene in the presence of a phase transfer catalyst - methoxylation, using meta-nitrochlorobenzene Difficult to etherification properties Separation of m-nitrochlorobenzene, o-nitroan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/04C02F101/12C02F101/30C02F101/34C02F101/36
CPCC02F9/00C02F2101/36C02F2101/34C02F2101/30C02F2209/08C02F2209/06C02F1/66C02F1/001C02F1/725C02F2101/12C02F1/722
Inventor 高留冕郁铭付春
Owner SINOPEC NANJING RES INST OF CHEM IND CO LTD
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