CN112023624B - Treatment method of waste acid - Google Patents
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- CN112023624B CN112023624B CN201910476986.2A CN201910476986A CN112023624B CN 112023624 B CN112023624 B CN 112023624B CN 201910476986 A CN201910476986 A CN 201910476986A CN 112023624 B CN112023624 B CN 112023624B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1487—Removing organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/72—Organic compounds not provided for in groups B01D53/48 - B01D53/70, e.g. hydrocarbons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Hydrology & Water Resources (AREA)
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- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention provides a treatment method of waste acid, which is characterized by comprising the following steps: waste hydrochloric acid or waste sulfuric acid (COD is 50000 mg/L-200000 mg/L) for absorbing tail gas of an RT base production device and nitrochlorobenzene waste water (COD is 100 mg/L-400 mg/L) are mixed according to the proportion of 1: (400-2000), adjusting the pH value to 3, carrying out oxidation reaction on the wastewater by using an oxidant, adjusting the COD value of the oxidized wastewater to be less than 200mg/L, and carrying out biochemical further treatment on the mixed wastewater after adjusting the pH value to be 6-9.
Description
Technical Field
The invention belongs to the field of environmental protection, and particularly relates to a method for treating waste acid, in particular to a method for treating waste acid for tail gas absorption of an RT base production device.
Background
RT base is an important intermediate for producing rubber antioxidant, and is widely applied to industries such as dye, textile, printing, pharmacy, rubber auxiliary agent and the like. The RT base industrial production line comprises an aniline method, a diphenylamine method, a formanilide method, a nitrobenzene method and the like, wherein the nitrobenzene method for producing the RT base has mild conditions, few byproducts and advanced process, and is the method which is most adopted. At present, RT is produced by adopting a nitrobenzene method, waste gas is generated in the production, and the waste gas of each section enters a waste gas main pipe and then enters a tail gas treatment system.
At present, RT device tail gas of China petrochemical and southern chemical company respectively passes through acid absorption-water absorption-photolysis-evacuation, the effect of the system is better, the treated tail gas can reach the standard emission, but the chroma of the absorbed waste acid is high, the smell is heavy, the treatment is difficult, because the COD (biochemical oxygen demand) value is too high, the biochemical treatment can not be directly carried out, if the tail gas is used as biochemical complex acid, trimethylamine gas can be generated in the alkali neutralization process, the odor threshold of the trimethylamine is low, the smell is large, the influence on the quality of the ambient air is large, the RT device tail gas does not accord with the environmental protection policy, and how to treat the RT device tail gas is a key problem to be solved urgently at present. The COD value of the nitrochlorobenzene wastewater is not high, but the nitrochlorobenzene wastewater is difficult to carry out biochemical treatment, so that the nitrochlorobenzene wastewater needs to be subjected to oxidation reaction pretreatment.
Foreign p-aminodiphenylamine (RT base) waste gas and waste water are mainly treated by a wet oxidation and biochemical method, wet oxidation reaction is carried out under the conditions that high-pressure air is pressed in and the reaction temperature is 300 ℃, the application range is wide, the treatment efficiency is high, but an intermediate product is often an organic acid, so the requirement on equipment materials is high, high temperature and high pressure resistance is required, and the corrosion resistance is realized, so the equipment cost is high, and the one-time investment of a system is high. The biochemical method for treating chemical wastewater is to degrade organic matters by utilizing the metabolism of microorganisms, the use of the chemical wastewater in the biochemical technology is limited due to the characteristics of poor biodegradability, high toxicity and the like of the chemical wastewater, and the RT waste acid is too strong in acidity and cannot be treated by the biochemical method.
The invention provides a waste acid treatment method, which comprises the steps of mixing waste acid and nitrochlorobenzene waste water according to a certain proportion, adjusting the pH value, carrying out oxidation reaction on the waste acid and the nitrochlorobenzene waste water by using an oxidant, adjusting the pH value of the mixed waste water after oxidation, and carrying out biochemical treatment.
Disclosure of Invention
The invention aims to provide a method for treating waste acid, which comprises the following steps: mixing waste acid and nitrochlorobenzene waste water according to a certain proportion, regulating pH value, using oxidant to make oxidation reaction, making COD value of waste water after oxidation be less than 200mg/L, regulating pH value of mixed waste water and making biochemical further treatment.
The waste acid is waste hydrochloric acid or waste sulfuric acid for absorbing tail gas of an RT base production device, the COD (chemical oxygen demand) of the waste acid is 50000-200000 mg/L, the acid concentration of the waste acid is 20-30%, and organic substances contained in the waste acid are mainly methanol, aniline, trimethylamine and the like. The absorption saturation degree of the tail gas absorption waste acid is different according to different seasons and different absorption acids, so the COD value is different.
The nitrochlorobenzene waste water is waste water of a nitrochlorobenzene production device, and COD of the nitrochlorobenzene waste water is 100 mg/L-400 mg/L.
The mixing ratio of the waste acid to the nitrochlorobenzene wastewater is 1: (400-2000). The waste water and waste acid produced by the actual device of a company are regulated, and the waste water and waste acid produced can be ensured to be treated in time.
The oxidant is a mixture of one or two of ferrous sulfate and tourmaline and hydrogen peroxide, or ozone.
The temperature of the oxidation reaction is 25-80 ℃.
The oxidation reaction time is 0.5h-5 h.
And the pH value of the mixed wastewater is adjusted to 3.
The COD of the oxidized mixed wastewater is 50 mg/L-200 mg/L.
And adjusting the pH value of the oxidized wastewater to 6-9.
Trimethylamine is a colorless and liquefiable flammable gas at normal temperature, has offensive and unpleasant ammonia-like odor and fishy smell, is toxic, has a low odor threshold value and can be smelled when the concentration is very low, and the solubility in acid is higher than that in water. Therefore, trimethylamine can not be dissipated into the air in the waste acid treatment process, and the environmental protection is not qualified.
Compared with the prior art, the method of the invention has the advantages that:
1) the trimethylamine is not dissipated in the treatment process, and no adverse effect is caused on the environment;
2) the waste water after mixed oxidation can be directly subjected to biochemical treatment, so that the problem that waste acid cannot be treated is solved;
3) the nitrochlorobenzene waste water needs to be acidified by adding acid in the treatment process, and the nitrochlorobenzene waste water is mixed with waste acid, so that the aim of preparing waste by using waste can be fulfilled, and the acid consumption for acidifying the nitrochlorobenzene waste water can be reduced.
Detailed Description
The process of the present invention is described in detail below with reference to examples.
Example 1
Adding 800 mL of nitrochlorobenzene wastewater (the COD value is 300 mg/L) into 2mL of waste sulfuric acid (the COD value is 80000 mg/L), adding sulfuric acid to adjust the pH value to about 3, placing the waste sulfuric acid into a four-mouth bottle, heating the waste sulfuric acid to 75 ℃, adding 1.2g of 10% ferrous sulfate solution, dropwise adding 2mL of hydrogen peroxide, reacting for 0.5 hour, adding alkali to neutralize the waste sulfuric acid until the pH value is 8, filtering and removing sediment in water, sampling and analyzing the COD, wherein the COD value is 156mg/L, no trimethylamine taste is emitted in the experimental process, and the wastewater after the reaction can directly enter biochemical treatment.
Comparative example 1
200 mL of waste sulfuric acid (COD value is 80000 mg/L) is placed in a four-mouth bottle, after the waste sulfuric acid is heated to 75 ℃, 0.6g of 10% ferrous sulfate solution is added, 100mL of hydrogen peroxide is dropwise added, the reaction is carried out for 0.5 hour, after the neutralization by adding alkali, the waste sulfuric acid is filtered to remove water and precipitate, then sampling is carried out, and the COD value is 56300 mg/L, the trimethylamine taste is diffused in the experimental process, and the sulfuric acid can not directly enter biochemical treatment after the reaction.
Example 2
Adding 2000 mL of nitrochlorobenzene wastewater (the COD value is 100 mg/L) into 1 mL of waste sulfuric acid (the COD value is 50000 mg/L), adding sulfuric acid to adjust the pH value to about 3, placing the waste sulfuric acid into a four-mouth bottle, heating the waste sulfuric acid to 80 ℃, adding 3 g of 10% ferrous sulfate solution, dropwise adding 1 mL of hydrogen peroxide, reacting for 5 hours, adding alkali to neutralize, filtering to remove water and precipitate, sampling and analyzing the COD, wherein the COD value is 52mg/L, no trimethylamine taste is emitted in the experimental process, and the wastewater after the reaction can directly enter biochemical treatment.
Comparative example 2
100 mL of waste sulfuric acid (COD value is 50000 mg/L) is placed in a four-mouth bottle, after the waste sulfuric acid is heated to 80 ℃, 0.2g of 10% ferrous sulfate solution is added, 20mL of hydrogen peroxide is dropwise added, the mixture reacts for 5 hours, after the mixture is neutralized by adding alkali, the mixture is filtered and the water is removed, and after precipitation, sampling is carried out to analyze COD value which is 35400 mg/L, trimethylamine taste is scattered in the experimental process, and the sulfuric acid can not directly enter biochemical treatment after the reaction.
Example 3
Adding 2000 mL of nitrochlorobenzene wastewater (COD value is 100 mg/L) into 2 mL of waste sulfuric acid (COD value is 200000 mg/L), adding sulfuric acid to adjust the pH value to about 3, placing the mixture into a four-mouth bottle, heating the mixture to 50 ℃, adding 3 g of 10% ferrous sulfate solution, dropwise adding 2.5 mL of hydrogen peroxide, reacting for 3 hours, adding alkali to neutralize, filtering to remove water and precipitate, sampling and analyzing COD, wherein the COD value is 132 mg/L, no trimethylamine taste is emitted in the experimental process, and the wastewater after the reaction can directly enter biochemical treatment.
Example 4
Adding 1600 mL of nitrochlorobenzene wastewater (the COD value is 400 mg/L) into 3 mL of waste sulfuric acid (the COD value is 100000 mg/L), adding sulfuric acid to adjust the pH value to about 3, placing the waste sulfuric acid into a four-mouth bottle, heating the waste sulfuric acid to 30 ℃, adding 2.3 g of 10% ferrous sulfate solution, dropwise adding 3.75 mL of hydrogen peroxide, reacting for 3 hours, adding alkali to neutralize, filtering to remove water and precipitate, sampling and analyzing the COD, wherein the COD value is 185 mg/L, no trimethylamine taste is emitted in the experimental process, and the wastewater can directly enter biochemical treatment after reaction.
Example 5
Adding 1000 mL of nitrochlorobenzene wastewater (the COD value is 200 mg/L) into 1 mL of waste hydrochloric acid (the COD value is 80000 mg/L), adding sulfuric acid to adjust the pH value to about 3, placing the mixture into a four-mouth bottle, heating the mixture to 70 ℃, adding 10 g of tourmaline, dropwise adding 1.2 mL of hydrogen peroxide, reacting for 2 hours, adding alkali to neutralize the mixture until the pH value is 7, filtering to remove water and precipitate, sampling and analyzing the COD, wherein the COD value is 53 mg/L, no trimethylamine taste is emitted in the experimental process, and the wastewater after the reaction can directly enter biochemical treatment.
Example 6
Adding 2000 mL of nitrochlorobenzene wastewater (the COD value is 150 mg/L) into 2 mL of waste sulfuric acid (the COD value is 60000 mg/L), adding sulfuric acid to adjust the pH value to about 3, placing the mixture into a four-mouth bottle, heating the mixture to 75 ℃, adding 1.2g of 10% ferrous sulfate solution, dropwise adding 1.8 mL of hydrogen peroxide, reacting for 3.5 hours, adding alkali to neutralize the mixture until the pH value is 7, filtering the mixture to remove water, precipitating the precipitate, sampling and analyzing the COD, wherein the COD value is 92 mg/L, no trimethylamine taste is emitted in the experimental process, and the wastewater after the reaction can be directly subjected to biochemical treatment.
Example 7
Adding 2000 mL of nitrochlorobenzene wastewater (the COD value is 300 mg/L) into 3 mL of waste hydrochloric acid (the COD value is 70000 mg/L), adding sulfuric acid to adjust the pH value to about 3, placing the mixture into a four-mouth bottle, heating the mixture to 75 ℃, adding 12g of tourmaline, dropwise adding 3.3 mL of hydrogen peroxide, reacting for 2.5 hours, adding alkali to neutralize the mixture until the pH value is 7, filtering the mixture to remove water and precipitate, sampling and analyzing the COD, wherein the COD value is 121 mg/L, no trimethylamine taste is emitted in the experimental process, and the wastewater can directly enter biochemical treatment after reaction.
Claims (9)
1. A treatment method of waste acid is characterized in that: mixing waste acid and nitrochlorobenzene waste water in proportion, adjusting the pH value, carrying out oxidation reaction on the waste acid and the nitrochlorobenzene waste water by using an oxidant, adjusting the pH value of the mixed waste water after oxidation, and carrying out biochemical treatment; the waste acid is waste hydrochloric acid or waste sulfuric acid for absorbing tail gas of an RT base production device, the COD (chemical oxygen demand) of the waste acid is 50000 mg/L-200000 mg/L, the acid concentration of the waste acid is 20% -30%, and the waste acid contains organic matters of methanol, aniline and trimethylamine.
2. The method according to claim 1, wherein the wastewater from nitrochlorobenzene production facilities contains COD of 100 mg/L to 400 mg/L.
3. The method according to claim 1, wherein the mixing ratio of the waste acid to the nitrochlorobenzene waste water is 1 (400-2000).
4. The method of claim 1, wherein the oxidizing agent is a mixture of one or both of ferrous sulfate and tourmaline with hydrogen peroxide, or ozone.
5. The method of claim 1, wherein the oxidation reaction temperature is from 25 ℃ to 80 ℃.
6. The method of claim 1, wherein the oxidation reaction time is from 0.5 h to 5 h.
7. The method of claim 1, wherein the mixed wastewater is adjusted to a pH of 3.
8. The method according to claim 1, wherein the COD of the oxidized mixed wastewater is 50 mg/L to 200 mg/L.
9. The method of claim 1, wherein the pH of the oxidized wastewater is adjusted to 6 to 9.
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| CN102040302A (en) * | 2009-10-21 | 2011-05-04 | 中国石油化工股份有限公司 | Treatment method of nitrochlorobenzene production wastewater |
| CN103951101A (en) * | 2014-04-10 | 2014-07-30 | 洛阳理工学院 | Treatment method and treatment system for nitrochlorobenzene production waste water |
| CN104250053A (en) * | 2013-06-27 | 2014-12-31 | 中国石油化工股份有限公司 | Method for treating ammonia-nitrogen containing p-aminodiphenyl amine production wastewater |
| CN106186519A (en) * | 2016-07-22 | 2016-12-07 | 浙江嘉成化工有限公司 | A kind of processing method of sodium hydrosulfite wastewater |
| CN106830581A (en) * | 2017-04-20 | 2017-06-13 | 郑州大学 | Sodium hydrosulfite wastewater processing method |
| CN109455838A (en) * | 2018-10-26 | 2019-03-12 | 南京中工智泓环保产业发展有限公司 | A method of nigrosine is produced using aniline waste water and Waste Sulfuric Acid |
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- 2019-06-03 CN CN201910476986.2A patent/CN112023624B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005000875A (en) * | 2003-06-13 | 2005-01-06 | Kanazawa Univ Tlo Inc | Method for recycling acidic waste water component and acidic waste water treatment system |
| CN102040302A (en) * | 2009-10-21 | 2011-05-04 | 中国石油化工股份有限公司 | Treatment method of nitrochlorobenzene production wastewater |
| CN104250053A (en) * | 2013-06-27 | 2014-12-31 | 中国石油化工股份有限公司 | Method for treating ammonia-nitrogen containing p-aminodiphenyl amine production wastewater |
| CN103951101A (en) * | 2014-04-10 | 2014-07-30 | 洛阳理工学院 | Treatment method and treatment system for nitrochlorobenzene production waste water |
| CN106186519A (en) * | 2016-07-22 | 2016-12-07 | 浙江嘉成化工有限公司 | A kind of processing method of sodium hydrosulfite wastewater |
| CN106830581A (en) * | 2017-04-20 | 2017-06-13 | 郑州大学 | Sodium hydrosulfite wastewater processing method |
| CN109455838A (en) * | 2018-10-26 | 2019-03-12 | 南京中工智泓环保产业发展有限公司 | A method of nigrosine is produced using aniline waste water and Waste Sulfuric Acid |
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Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: SINOPEC NANJING CHEMICAL RESEARCH INSTITUTE Co.,Ltd. Address before: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee before: SINOPEC NANJING CHEMICAL RESEARCH INSTITUTE Co.,Ltd. Patentee before: CHINA PETROLEUM & CHEMICAL Corp. |