CN110813064A - Method for comprehensively treating chlorine-containing tail gas in production of titanium tetrachloride through boiling chlorination - Google Patents
Method for comprehensively treating chlorine-containing tail gas in production of titanium tetrachloride through boiling chlorination Download PDFInfo
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- CN110813064A CN110813064A CN201911255900.XA CN201911255900A CN110813064A CN 110813064 A CN110813064 A CN 110813064A CN 201911255900 A CN201911255900 A CN 201911255900A CN 110813064 A CN110813064 A CN 110813064A
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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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- 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
- B01D53/1456—Removing acid components
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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
- B01D53/1493—Selection of liquid materials for use as absorbents
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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
- B01D53/68—Halogens or halogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/50—Inorganic acids
- B01D2251/502—Hydrochloric acid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/10—Inorganic absorbents
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Abstract
A method for comprehensively treating chlorine-containing tail gas in the production of titanium tetrachloride through boiling chlorination comprises the steps of carrying out seven-stage leaching on the chlorinated tail gas, carrying out first-stage dilute hydrochloric acid leaching, controlling the acid concentration to be more than or equal to 30%, carrying out second-stage dilute hydrochloric acid leaching, controlling the acid concentration to be less than or equal to 15%, carrying out third-stage dilute hydrochloric acid leaching, controlling the acid concentration to be less than or equal to 5%, carrying out first-stage ferrous chloride leaching, wherein the ferrous chloride solution concentration is 40-50 g/L, carrying out second-stage ferrous chloride leaching, the ferrous chloride solution concentration is 40-50 g/L, carrying out first-stage clear water. The invention breaks the industrial bottleneck that chlorinated tail gas is treated without alkali liquor, and effectively avoids the problems of secondary pollution caused by using strong alkali and pipeline blockage caused by using lime water. The on-line acidity monitoring of the three-stage diluted hydrochloric acid leaching is realized, and the concentration of the recovered hydrochloric acid can be ensured to be more than 30%; because the ferrous chloride is produced by adopting a self-preparation mode, the treatment cost of the tail gas is obviously reduced. The chlorinated tail gas is stably discharged up to the standard, and the production cost is low.
Description
Technical Field
The invention belongs to the technical field of titanium tetrachloride production, and particularly relates to a method for comprehensively treating chlorine-containing tail gas in the production of titanium tetrachloride by boiling chlorination.
Background
At present, the production method of titanium tetrachloride is mainly a boiling chlorination method, i.e. after a titanium-rich material and petroleum coke are mixed according to a certain proportion, chlorine gas is added into a chlorination furnace to carry out closed chemical reaction, so as to obtain titanium tetrachloride, the process is called boiling chlorination, in the actual production, chlorinated tail gas contains a large amount of harmful gases such as hypochlorite, dilute hydrochloric acid and other chlorides, so that the tail gas must be absorbed and treated and then discharged after reaching the standard, and the existing chlorinated tail gas absorption method generally adopts water leaching, then NaOH or NaoCOl neutralization, and finally adopts lime milk to absorb and discharge. Because the boiling chlorination reaction process is dynamic, the fluctuation of the chlorine content and the components is large, the content of chlorine-containing gases such as hydrogen chloride in the chlorination tail gas is easy to exceed the standard by adopting the existing method, the environment is influenced, and an ideal effect is difficult to achieve.
Disclosure of Invention
The invention aims to solve the technical problems that the content of chlorine-containing gases such as hydrogen chloride in chlorination tail gas exceeds the standard in the existing boiling chlorination method, and when strong base NaOH is adopted to absorb ClO, the generated NaCIO is easily decomposed into ClO for the second time, which causes adverse effects on the environment, and the cost of another treatment method is higher.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for comprehensively treating chlorine-containing tail gas in the production of titanium tetrachloride by boiling chlorination,
the method is characterized in that: the method comprises the steps of leaching chlorination tail gas by seven levels;
(1) the first stage dilute hydrochloric acid leaching is carried out, the acid concentration is controlled to be more than or equal to 30 percent,
(2) the second stage dilute hydrochloric acid leaching, the acid concentration is controlled to be less than or equal to 15 percent,
(3) the third stage of dilute hydrochloric acid leaching, the acid concentration is controlled to be less than or equal to 5 percent,
(4) leaching the first-stage ferrous chloride, wherein the concentration of a ferrous chloride solution is 40-50 g/L,
(5) leaching the second-stage ferrous chloride, wherein the concentration of a ferrous chloride solution is 40-50 g/L,
(6) the first-stage clear water is used for leaching,
(7) and (5) leaching and absorbing by first-stage lime water.
Adopt above-mentioned technical scheme's beneficial effect:
1. the invention breaks the industrial bottleneck that chlorinated tail gas is treated without alkali liquor, and effectively avoids the problems of secondary pollution caused by using strong alkali and pipeline blockage caused by using lime water.
2. The invention realizes on-line acidity monitoring for three-stage diluted hydrochloric acid leaching and can ensure that the concentration of the recovered hydrochloric acid reaches more than 30 percent.
3. The invention adopts a self-preparation mode to produce the ferrous chloride, thereby obviously reducing the treatment cost of the tail gas.
4. The invention has the advantages of stable standard emission of the chlorination tail gas and low production cost.
Detailed Description
The present invention will be described in further detail below.
A method for comprehensively treating chlorine-containing tail gas in the production of titanium tetrachloride by boiling chlorination adopts seven-level leaching as follows:
(1) the first stage dilute hydrochloric acid leaching is carried out, the acid concentration is controlled to be more than or equal to 30 percent,
(2) the second stage dilute hydrochloric acid leaching, the acid concentration is controlled to be less than or equal to 15 percent,
(3) the third stage of dilute hydrochloric acid leaching, the acid concentration is controlled to be less than or equal to 5 percent,
(4) leaching the first-stage ferrous chloride, wherein the concentration of a ferrous chloride solution is 40-50 g/L,
(5) leaching the second-stage ferrous chloride, wherein the concentration of a ferrous chloride solution is 40-50 g/L,
(6) the first-stage clear water is used for leaching,
(7) and (5) leaching and absorbing by first-stage lime water.
And automatically discharging the acid generated in the third-stage diluted hydrochloric acid leaching when the concentration of the acid reaches 5%, and adding new water, wherein if the concentration of the acid does not reach 5%, the diluted hydrochloric acid is sent to the second-stage diluted hydrochloric acid leaching for use.
And after the concentration of acid generated in the second-stage diluted hydrochloric acid leaching process reaches 15%, sending the diluted hydrochloric acid to a third-stage diluted hydrochloric acid leaching process for use, and if the concentration of acid generated in the second-stage diluted hydrochloric acid leaching process does not reach 15%, sending the diluted hydrochloric acid to the first-stage diluted hydrochloric acid leaching process for use.
And when the concentration of acid generated in the first-stage diluted hydrochloric acid leaching reaches more than 30%, pumping the hydrochloric acid into a hydrochloric acid storage tank to serve as a product for sale.
And respectively installing a drip catcher at the second-stage diluted hydrochloric acid leaching outlet and the third-stage diluted hydrochloric acid leaching outlet to prevent acid water liquid drips after the second-stage diluted hydrochloric acid leaching outlet and the third-stage diluted hydrochloric acid leaching outlet from entering a subsequent system.
The first and second stages of ferrous chloride leaching are closed cycle.
And (3) leaching and recovering hydrochloric acid with a concentration value of 30% by using the three-stage diluted hydrochloric acid, reacting with scrap iron to generate ferrous chloride, and performing a ferrous chloride leaching procedure again.
Claims (7)
1. A method for comprehensively treating chlorine-containing tail gas in the production of titanium tetrachloride by boiling chlorination is characterized by comprising the following steps: the method comprises the steps of leaching chlorination tail gas by seven levels;
(1) the first stage dilute hydrochloric acid leaching is carried out, the acid concentration is controlled to be more than or equal to 30 percent,
(2) the second stage dilute hydrochloric acid leaching, the acid concentration is controlled to be less than or equal to 15 percent,
(3) the third stage of dilute hydrochloric acid leaching, the acid concentration is controlled to be less than or equal to 5 percent,
(4) leaching the first-stage ferrous chloride, wherein the concentration of a ferrous chloride solution is 40-50 g/L,
(5) leaching the second-stage ferrous chloride, wherein the concentration of a ferrous chloride solution is 40-50 g/L,
(6) the first-stage clear water is used for leaching,
(7) and (5) leaching and absorbing by first-stage lime water.
2. The method for comprehensively treating chlorine-containing tail gas in the production of titanium tetrachloride through boiling chlorination as claimed in claim 1, characterized in that: and automatically discharging the acid generated in the third-stage diluted hydrochloric acid leaching when the concentration of the acid reaches 5%, and adding new water, wherein if the concentration of the acid does not reach 5%, the diluted hydrochloric acid is sent to the second-stage diluted hydrochloric acid leaching for use.
3. The method for comprehensively treating chlorine-containing tail gas in the production of titanium tetrachloride through boiling chlorination as claimed in claim 1, characterized in that: and after the concentration of acid generated in the second-stage diluted hydrochloric acid leaching process reaches 15%, sending the diluted hydrochloric acid to a third-stage diluted hydrochloric acid leaching process for use, and if the concentration of acid generated in the second-stage diluted hydrochloric acid leaching process does not reach 15%, sending the diluted hydrochloric acid to the first-stage diluted hydrochloric acid leaching process for use.
4. The method for comprehensively treating chlorine-containing tail gas in the production of titanium tetrachloride through boiling chlorination as claimed in claim 1, characterized in that: and when the concentration of acid generated in the first-stage diluted hydrochloric acid leaching reaches more than 30%, pumping the hydrochloric acid into a hydrochloric acid storage tank to serve as a product for sale.
5. The method for comprehensively treating chlorine-containing tail gas in the production of titanium tetrachloride through boiling chlorination as claimed in claim 1, characterized in that: and respectively installing a drip catcher at the second-stage diluted hydrochloric acid leaching outlet and the third-stage diluted hydrochloric acid leaching outlet to prevent acid water liquid drips after the second-stage diluted hydrochloric acid leaching outlet and the third-stage diluted hydrochloric acid leaching outlet from entering a subsequent system.
6. The method for comprehensively treating chlorine-containing tail gas in the production of titanium tetrachloride through boiling chlorination as claimed in claim 1, characterized in that: the first and second stages of ferrous chloride leaching are closed cycle.
7. The method for comprehensively treating chlorine-containing tail gas in the production of titanium tetrachloride through boiling chlorination as claimed in claim 1, characterized in that: and (3) leaching and recovering hydrochloric acid with a concentration value of 30% by using the three-stage diluted hydrochloric acid, reacting with scrap iron to generate ferrous chloride, and performing a ferrous chloride leaching procedure again.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911255900.XA CN110813064A (en) | 2019-12-10 | 2019-12-10 | Method for comprehensively treating chlorine-containing tail gas in production of titanium tetrachloride through boiling chlorination |
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| CN201911255900.XA CN110813064A (en) | 2019-12-10 | 2019-12-10 | Method for comprehensively treating chlorine-containing tail gas in production of titanium tetrachloride through boiling chlorination |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113184900A (en) * | 2021-05-12 | 2021-07-30 | 攀钢集团钒钛资源股份有限公司 | Titanium tetrachloride production method and system and raw material ratio adjusting method |
| CN114797415A (en) * | 2022-05-20 | 2022-07-29 | 攀钢集团钒钛资源股份有限公司 | Method for treating residual chlorine in chlorination tail gas |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028309A (en) * | 2012-12-26 | 2013-04-10 | 遵宝钛业有限公司 | Absorption method of chlorinated tail gas |
| CN104707464A (en) * | 2015-03-16 | 2015-06-17 | 富彤化学有限公司 | HCl gas recovery method under high vacuum condition |
| CN108434941A (en) * | 2018-05-17 | 2018-08-24 | 盐城工学院 | A kind of hydrogen chloride tail gas absorption strength detection method and automatic cycle absorption plant |
-
2019
- 2019-12-10 CN CN201911255900.XA patent/CN110813064A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103028309A (en) * | 2012-12-26 | 2013-04-10 | 遵宝钛业有限公司 | Absorption method of chlorinated tail gas |
| CN104707464A (en) * | 2015-03-16 | 2015-06-17 | 富彤化学有限公司 | HCl gas recovery method under high vacuum condition |
| CN108434941A (en) * | 2018-05-17 | 2018-08-24 | 盐城工学院 | A kind of hydrogen chloride tail gas absorption strength detection method and automatic cycle absorption plant |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113184900A (en) * | 2021-05-12 | 2021-07-30 | 攀钢集团钒钛资源股份有限公司 | Titanium tetrachloride production method and system and raw material ratio adjusting method |
| CN114797415A (en) * | 2022-05-20 | 2022-07-29 | 攀钢集团钒钛资源股份有限公司 | Method for treating residual chlorine in chlorination tail gas |
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