CN111099779A - Method for efficiently removing aniline compounds in wastewater - Google Patents
Method for efficiently removing aniline compounds in wastewater Download PDFInfo
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- CN111099779A CN111099779A CN201911353873.XA CN201911353873A CN111099779A CN 111099779 A CN111099779 A CN 111099779A CN 201911353873 A CN201911353873 A CN 201911353873A CN 111099779 A CN111099779 A CN 111099779A
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- aniline
- wastewater
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- rectifying
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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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
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
A method for efficiently removing aniline compounds in wastewater comprises the following steps: the method comprises the following steps of (1) pretreating the wastewater containing the aniline to remove alcohols with low boiling points; adding the wastewater from which the low-boiling point alcohols are removed into a rectifying tower for rectification, controlling the temperature and reflux ratio of the rectifying tower to distill off water and aniline together, and rectifying until the fraction at the top of the tower is clear and transparent; collecting the distillate distilled from the tower top, cooling, and recovering aniline by layering; the rectified waste water is removed by an oxidation method: adding a mixed solution of hydrogen peroxide and absolute ethyl alcohol into the rectified wastewater, and introducing ozone into an oxidation system to degrade the residual aniline compounds in the wastewater. The invention adopts a rectification method to separate most of aniline in the wastewater and recycle the aniline, and the wastewater with the residual trace aniline content is removed by an oxidation method, so that the removal rate of the aniline in the wastewater reaches more than 99 percent.
Description
Technical Field
The invention relates to a method for efficiently removing aniline compounds in wastewater, belonging to the technical field of wastewater treatment.
Background
The aniline compound is an important organic chemical raw material and a fine chemical intermediate, and is also a harmful substance which seriously pollutes the environment and harms the human health. A large amount of aniline wastewater is generated in domestic various refineries, dye plants, pesticide plants and the like in the production process, and the mass concentration of the aniline wastewater can be up to thousands of mg/L sometimes. Aniline species have been listed on the "chinese environmental priority pollutants black list" due to their toxicity to ecological organisms, requiring strict control in industrial drainage. At present, the treatment of aniline wastewater at home and abroad mainly comprises biological, physical and chemical methods, but most of the methods have unsatisfactory treatment effect and generally have the problems of high cost, serious secondary pollution, substandard emission and the like.
Disclosure of Invention
The invention provides a method for efficiently removing aniline compounds in wastewater to overcome the defects of the prior art, a rectification method is adopted to separate most of aniline in the wastewater for recycling, the wastewater with the residual trace aniline content is removed by an oxidation method, and the removal rate of the aniline in the wastewater reaches more than 99%.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for efficiently removing aniline compounds in wastewater comprises the following steps:
a. carrying out rectification pretreatment on the wastewater containing the aniline to remove alcohols with low boiling points;
b. adding the wastewater from which the low-boiling point alcohols are removed into a rectifying tower for rectification, controlling the temperature and reflux ratio of the rectifying tower to distill off water and aniline together, and rectifying until the fraction at the top of the tower is clear and transparent;
c. collecting the distillate distilled from the tower top, cooling, and recovering aniline by layering;
d. the rectified waste water is removed by an oxidation method: adding hydrogen peroxide into the rectified wastewater, and introducing ozone into an oxidation system to degrade residual aniline compounds in the wastewater.
In the step b, the temperature of the bottom of the rectifying tower is controlled to be 105-107 ℃, and the temperature of the top of the rectifying tower is controlled to be 99-101 ℃.
In the step b, the reflux ratio is controlled to be 1.5-2. Ensuring the separation effect of the distillate fraction.
In the step c, the collected fraction is cooled to 5-10 ℃. At a lower temperature, the solubility of the aniline substances in water is extremely low, and at the moment, the water and the aniline substances can be layered, so that the layered aniline substances can be separated and recovered.
The invention has the beneficial effects that: the invention utilizes a rectification method to separate more than 92 percent of aniline in wastewater from the wastewater, controls the temperature of the bottom and the top of a rectification tower to lead aniline substances to be entrained in water and carry out rectification at a lower boiling point, and leads the aniline compounds to be separated from the water and recycled after the mixture of the rectified water and the aniline compounds is cooled, so that the recovery rate of the aniline reaches 92.4 percent, the invention is more energy-saving, and the problems of high ammonia nitrogen concentration in the water and difficult processing caused by the traditional fenton or biochemical treatment method are avoided. And (3) the rectified wastewater contains a trace amount of aniline compounds, the wastewater is oxidized by hydrogen peroxide, and ozone is introduced into an oxidation system, so that the removal rate of the residual aniline compounds in the wastewater is up to more than 99%.
Detailed Description
The technical solution of the present invention is further explained with reference to specific examples below.
Example 1
Carrying out rectification pretreatment on the wastewater containing the aniline to remove alcohols with low boiling points; adding the wastewater without the low-boiling point alcohols into a rectifying tower for rectification, controlling the tower bottom temperature of the rectifying tower to be 105 ℃, the tower top temperature to be 99 ℃, controlling the reflux ratio to be 1.5, distilling off the water and the aniline together, and rectifying until the fraction at the tower top is clear and transparent; collecting the distillate distilled from the top of the tower, cooling to 5 ℃, so that aniline substances are layered in water, and recovering aniline; the aniline recovery rate was 89.6%.
And (3) removing trace aniline substances in the rectified wastewater by an oxidation method: adding hydrogen peroxide into the rectified wastewater, and introducing ozone into an oxidation system to degrade residual aniline compounds in the wastewater.
Example 2
The method comprises the following steps of (1) pretreating the wastewater containing the aniline to remove alcohols with low boiling points; adding the wastewater without the low-boiling point alcohols into a rectifying tower for rectification, controlling the tower bottom temperature of the rectifying tower to be 106 ℃, the tower top temperature to be 100 ℃, controlling the reflux ratio to be 1.8, distilling off the water and the aniline together, and rectifying until the fraction at the tower top is clear and transparent; collecting the distillate distilled from the top of the tower, cooling to 8 ℃, so that aniline substances are layered in water, and recovering aniline; the aniline recovery was 91.3%.
And (3) removing trace aniline substances in the rectified wastewater by an oxidation method: adding hydrogen peroxide into the rectified wastewater, and introducing ozone into an oxidation system to degrade residual aniline compounds in the wastewater.
Example 3
The method comprises the following steps of (1) pretreating the wastewater containing the aniline to remove alcohols with low boiling points; adding the wastewater without the low-boiling point alcohols into a rectifying tower for rectification, controlling the bottom temperature of the rectifying tower to be 107 ℃, the top temperature of the rectifying tower to be 101 ℃, controlling the reflux ratio to be 2, distilling off the water and the aniline together, and rectifying until the fraction at the top of the rectifying tower is clear and transparent; collecting the distillate distilled from the top of the tower, cooling to 10 ℃, so that aniline substances are layered in water, and recovering aniline; the aniline recovery was 92.2%.
And (3) removing trace aniline substances in the rectified wastewater by an oxidation method: adding hydrogen peroxide into the rectified wastewater, and introducing ozone into an oxidation system to degrade residual aniline compounds in the wastewater.
Example 4
The method comprises the following steps of (1) pretreating the wastewater containing the aniline to remove alcohols with low boiling points; adding the wastewater without the low-boiling point alcohols into a rectifying tower for rectification, controlling the bottom temperature of the rectifying tower to be 107 ℃, the top temperature of the rectifying tower to be 99 ℃, controlling the reflux ratio to be 2, distilling off the water and the aniline together, and rectifying until the fraction at the top of the rectifying tower is clear and transparent; collecting the distillate distilled from the top of the tower, cooling to 5 ℃, so that aniline substances are layered in water, and recovering aniline, wherein the recovery rate of aniline is 92.4%;
and (3) removing trace aniline substances in the rectified wastewater by an oxidation method: adding hydrogen peroxide into the rectified wastewater, and introducing ozone into an oxidation system to degrade residual aniline compounds in the wastewater.
Claims (4)
1. A method for efficiently removing aniline compounds in wastewater is characterized by comprising the following steps: the processing method comprises the following steps:
a. carrying out rectification pretreatment on the wastewater containing the aniline to remove alcohols with low boiling points;
b. rectifying the wastewater from which the low-boiling point alcohols are removed in a rectifying tower, controlling the temperature and reflux ratio of the rectifying tower to distill off water and aniline together, and rectifying until the fraction at the top of the tower is clear and transparent;
c. collecting the distillate distilled from the tower top, cooling, and recovering aniline by layering;
d. the rectified waste water is removed by an oxidation method: adding hydrogen peroxide into the rectified wastewater, and introducing ozone into an oxidation system to degrade residual aniline compounds in the wastewater.
2. The method for efficiently removing the aniline compounds in the wastewater according to claim 1, wherein the method comprises the following steps: in the step b, the temperature of the bottom of the rectifying tower is controlled to be 105-107 ℃, and the temperature of the top of the rectifying tower is controlled to be 99-101 ℃.
3. The method for efficiently removing the aniline compounds in the wastewater according to claim 2, wherein the method comprises the following steps: in the step b, the reflux ratio is controlled to be 1.5-2.
4. The method for efficiently removing the aniline compounds in the wastewater according to claim 3, wherein the method comprises the following steps: in the step c, the collected fraction is cooled to 5-10 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201911353873.XA CN111099779A (en) | 2019-12-25 | 2019-12-25 | Method for efficiently removing aniline compounds in wastewater |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911353873.XA CN111099779A (en) | 2019-12-25 | 2019-12-25 | Method for efficiently removing aniline compounds in wastewater |
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| CN111099779A true CN111099779A (en) | 2020-05-05 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070203364A1 (en) * | 2006-02-18 | 2007-08-30 | Markus Dugal | Process for preparing aniline |
| CN102304017A (en) * | 2011-07-20 | 2012-01-04 | 济南圣泉集团股份有限公司 | Method for recycling aniline and methanol from mixed waste water of aniline and methanol |
| CN104609491A (en) * | 2015-01-13 | 2015-05-13 | 青岛双桃精细化工（集团）有限公司 | Recycling device for nigrosine production wastewater |
| CN109607895A (en) * | 2018-11-30 | 2019-04-12 | 河北彩客化学股份有限公司 | A kind of processing method of the wastewater from chemical industry containing phenyl amines |
-
2019
- 2019-12-25 CN CN201911353873.XA patent/CN111099779A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070203364A1 (en) * | 2006-02-18 | 2007-08-30 | Markus Dugal | Process for preparing aniline |
| CN102304017A (en) * | 2011-07-20 | 2012-01-04 | 济南圣泉集团股份有限公司 | Method for recycling aniline and methanol from mixed waste water of aniline and methanol |
| CN104609491A (en) * | 2015-01-13 | 2015-05-13 | 青岛双桃精细化工（集团）有限公司 | Recycling device for nigrosine production wastewater |
| CN109607895A (en) * | 2018-11-30 | 2019-04-12 | 河北彩客化学股份有限公司 | A kind of processing method of the wastewater from chemical industry containing phenyl amines |
Non-Patent Citations (2)
| Title |
|---|
| 祁鲁梁，李永存: "《水处理工艺与运行管理实用手册》", 31 May 2002, 中国石化出版社 * |
| 陈淑鑫等: "苯胺废水回收精馏装置控制设计优化", 《化工自动化及仪表》 * |
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Address after: 061600 DAZHANGZHUANG, Dongguang County, Cangzhou City, Hebei Province Applicant after: Hebei caike New Material Technology Co.,Ltd. Address before: 061600 Chengnan Da Zhang Zhuang, Dongguang County, Cangzhou City, Hebei Province Applicant before: TSAKER CHEMICAL (ZHANGZHOU) CO.,LTD. |
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Application publication date: 20200505 |