CN109453615B - Treatment method of tail gas in production of methanesulfonyl chloride - Google Patents
Treatment method of tail gas in production of methanesulfonyl chloride Download PDFInfo
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- CN109453615B CN109453615B CN201811556679.7A CN201811556679A CN109453615B CN 109453615 B CN109453615 B CN 109453615B CN 201811556679 A CN201811556679 A CN 201811556679A CN 109453615 B CN109453615 B CN 109453615B
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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
- B01D53/1406—Multiple stage absorption
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- 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
- B01D53/1418—Recovery of products
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- 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
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- 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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- B01D2257/20—Halogens or halogen compounds
- B01D2257/202—Single element halogens
- B01D2257/2025—Chlorine
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D2257/20—Halogens or halogen compounds
- B01D2257/204—Inorganic halogen compounds
- B01D2257/2045—Hydrochloric acid
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Abstract
The invention discloses a method for treating tail gas in the production of methylsulfonyl chloride, which comprises the following steps: (1) absorbing chlorine in the tail gas from the production of the methanesulfonyl chloride by a first-stage absorption device filled with an absorbent, wherein the absorbent contains Fe2+The acid pickling waste liquid of (1); (2) introducing the gas from the first-stage absorption device into a second-stage absorption device containing water to absorb hydrogen chloride gas in the tail gas generated in the production of the methanesulfonyl chloride, so as to obtain a hydrochloric acid solution; (3) and (3) recycling the hydrochloric acid solution for steel pickling, taking the waste liquid after pickling as an absorbent in the step (1), and circulating the steps (1) to (3). The invention is provided by containing Fe2+Compared with the traditional method, the method can recycle the pickling waste liquid, treat the tail gas generated by the production of the methylsulfonyl chloride, change waste into valuable and greatly reduce the treatment cost.
Description
Technical Field
The invention relates to the technical field of chemical tail gas treatment, in particular to a treatment method of tail gas in methanesulfonyl chloride production.
Background
At present, the industrial preparation of the methanesulfonyl chloride mainly adopts a chlorine wet oxidation process, and the process mainly comprises the steps of continuously introducing chlorine into a dimethyl disulfide solution to generate a chlorine oxidation reaction to obtain the methanesulfonyl chloride and hydrogen chloride tail gas. However, in order to oxidize completely, the process generally needs to introduce excessive chlorine, and the excessive chlorine can overflow with the hydrogen chloride tail gas, so that the main components of the tail gas produced by the methanesulfonyl chloride are hydrogen chloride and excessive chlorine.
If chlorine in the tail gas is not removed, the chlorine is directly absorbed into hydrochloric acid by water, and the obtained hydrochloric acid inevitably contains a large amount of residual chlorine, so that the quality of the hydrochloric acid cannot meet the requirement, and a large amount of chlorine can overflow in the using process to pollute the environment. At present, sodium hypochlorite is obtained by mainly using caustic soda to neutralize excessive chlorine, but the reaction of the chlorine and the caustic soda is difficult to control, if the reaction process is not well controlled, the generated sodium hypochlorite and the chlorine continue to react to release a large amount of chlorine, so that the excessive chlorine cannot be effectively treated; and the excessive chlorine is neutralized by using the caustic soda, so that a large amount of caustic soda is consumed, the treatment cost is high, and the obtained sodium hypochlorite has low effective chlorine content and cannot be sold as a commodity.
The hydrochloric acid is commonly used by steel enterprises and steel product factories to carry out surface treatment on various metal products, so that a large amount of pickling waste liquid is generated, wherein the pickling waste liquid contains a large amount of ferrous ions and free acid, and the concentration of the pickling liquid is continuously reduced along with the increase of the pickling times in the pickling process, but the concentration of the metal ions in the pickling liquid is continuously increased, so that the pickling liquid can lose the pickling effect and generate a large amount of waste acid. At present, the pickling waste liquid is mainly treated by the following three methods: (1) concentrating the pickling waste liquor by a pre-concentrator, spraying the concentrated pickling waste liquor into a high-temperature roasting reaction furnace, decomposing the concentrated pickling waste liquor into hydrogen chloride and ferric oxide, performing cyclone dust removal on the hydrogen chloride gas, enabling the hydrogen chloride gas to enter an absorption tower by the pre-concentrator, absorbing the hydrogen chloride into 18-20% hydrochloric acid by using water, and recycling the hydrochloric acid for pickling the strip steel, wherein the ferric oxide is used as a byproduct for recycling; (2) evaporating hydrogen chloride and water in the pickling waste liquid by adopting an evaporation method, cooling and absorbing by using water to obtain dilute hydrochloric acid, and cooling and crystallizing the concentrated solution to obtain ferrous chloride crystals; (3) adjusting the content of iron and hydrochloric acid in the pickling waste liquid, oxidizing ferrous ions into ferric ions by using strong oxidants such as sodium chloride and the like, and then producing and preparing the polyferric chloride coagulant under certain conditions. Although the three methods can effectively treat the pickling waste liquid, the treatment process is complex, the treatment cost is high, and the method is not suitable for treating the pickling waste liquid in a large scale in an industrialized mode.
Disclosure of Invention
The invention aims to overcome the technical defects and provides a method for treating tail gas in the production of methylsulfonyl chloride by using pickling waste liquid.
In order to achieve the technical purpose, the technical scheme of the invention provides a method for treating tail gas in the production of methanesulfonyl chloride, which comprises the following steps:
s1, enabling the tail gas generated in the production of the methanesulfonyl chloride to pass through a first-stage absorption device filled with an absorbent to absorb chlorine in the tail gas generated in the production of the methanesulfonyl chloride, wherein the absorbent contains Fe2+The acid pickling waste liquid of (1);
s2, introducing the gas from the first-stage absorption device into a second-stage absorption device containing water to absorb hydrogen chloride gas in the tail gas generated in the production of the methanesulfonyl chloride to obtain a hydrochloric acid solution;
and S3, reusing the hydrochloric acid solution for steel pickling, taking the waste liquid after pickling as an absorbent in the step S1, and circulating the steps S1 to S3.
Compared with the prior art, the invention has the beneficial effects that:
1、the invention firstly contains Fe2+The waste pickle liquor absorbs chlorine in the tail gas of the production of the methylsulfonyl chloride, and Fe is converted by the chlorine2+Is oxidized into Fe3+The chlorine in the tail gas generated in the production of the methanesulfonyl chloride is removed, hydrogen chloride in the tail gas generated in the production of the methanesulfonyl chloride is absorbed by water, the obtained hydrochloric acid has high quality and can be reused for steel pickling, the waste liquid after pickling can be used as pickling waste liquid for recycling, the chlorine in the tail gas generated in the production of the methanesulfonyl chloride is absorbed, and the pickling waste liquid after the chlorine is absorbed can be recycled by simply processing the waste liquid3+Compared with the traditional treatment method, the method can recycle the pickling waste liquid, can effectively treat the tail gas in the production of the methylsulfonyl chloride, changes waste into valuable, and greatly reduces the treatment cost;
2. according to the treatment method, the tail gas generated in the production of the methylsulfonyl chloride is fully utilized and cannot be discharged into the atmosphere, so that the environmental pollution is effectively reduced;
3. the treatment method provided by the invention has the advantages that the whole treatment process is easy to control, the operation is simple, and the method is suitable for industrial large-scale treatment.
Drawings
FIG. 1 is a process flow diagram of the method for treating tail gas from the production of methanesulfonyl chloride according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a method for treating tail gas in the production of methylsulfonyl chloride, which comprises the following steps:
(1) absorbing chlorine in the tail gas from the production of the methanesulfonyl chloride by passing the tail gas from the production of the methanesulfonyl chloride through a first-stage absorption device filled with an absorbent, wherein the absorbent contains Fe2+The acid pickling waste liquid of (1);
(2) introducing the gas from the first-stage absorption device into a second-stage absorption device containing water to absorb hydrogen chloride gas in the tail gas generated in the production of the methanesulfonyl chloride, so as to obtain a hydrochloric acid solution;
(3) and (3) reusing the hydrochloric acid solution in the step (2) for steel pickling, and recycling the waste liquid after pickling as the absorbent in the step (1) in the steps (1) to (3).
In some preferred embodiments of the invention, the absorbent is FeCl-containing2The acid pickling waste liquid of (1); the anion in the pickling waste liquid is Cl-So as to inhibit the dissolution of the hydrogen chloride in the first-stage absorption device and simultaneously facilitate the cyclic utilization of the hydrochloric acid pickling waste liquid.
In the present invention, Fe is contained2+The waste pickle liquor is further filtered and diluted to remove insoluble impurities in the waste pickle liquor and prevent Fe2+The impurities are wrapped by the crystallization and the Fe is reduced2+The effect of chlorine absorption.
In some preferred embodiments of the invention, step (1) further comprises adding FeCl to the solution2Diluting the waste pickle liquor to FeCl2The mass content is 5-10%; by further optimizing FeCl in the waste pickle liquor2To achieve a better chlorine uptake effect.
In the present invention, to ensure Fe in the pickling waste liquid2+Is completely oxidized into Fe by chlorine3+Intermittently removing the absorbent from the first stage of the absorption unit and replenishing with fresh Fe2+The pickling waste liquid is prepared by the following steps: in the process of absorbing chlorine in the tail gas generated in the production of the methanesulfonyl chloride by the first-stage absorption device, the absorbent is sampled and detected, and when FeCl in the absorbent is absorbed2Is less than 0.5 percent, the absorbent in the first stage absorption device is removed, and fresh Fe-containing is supplemented into the first stage absorption device2+The method is repeated, the absorbent in the first-stage absorption device is intermittently removed, and fresh Fe-containing waste liquid is replenished2+Wherein fresh Fe is contained in the pickling waste liquid of (1)2+The waste pickle liquor refers to FeCl25-10% of pickling waste liquor by mass; so as to ensure that chlorine gas in the tail gas in the production of the methylsulfonyl chloride is fully absorbed and ferrous ions are completely oxidized.
In some of the present inventionIn a preferred embodiment, FeCl in the absorbent removed in the first stage of absorption means is2Is less than 0.5% and greater than or equal to 0.2%, and the method further comprises adding an oxidizing agent to the absorbent removed from the first stage absorption unit to oxidize Fe2+Oxidizing to a mass content of less than 0.2%, wherein the oxidant can be any one of colorless oxidants such as ozone, hydrogen peroxide, chlorate and the like, and the addition amount of the oxidant is according to Fe2+Determining the content of (A); adding proper amount of oxidant to react Fe2+Complete oxidation to Fe3+The ferric salt solution after oxidation can be prepared into ferric salt by conventional methods such as concentration and evaporation, and the ferric salt solution can also be prepared into polymeric ferric chloride, polymeric aluminum ferric chloride and other high molecular flocculants.
In some preferred embodiments of the present invention, the present invention adopts a multistage series absorption mode, specifically: the absorbent in the first stage of absorption device is FeCl2The mass content of the pickling waste liquid is 5-10%, and the absorbents in the second-stage absorption device and the third-stage absorption device … …, namely the Nth-stage absorption device (N is more than or equal to 3), are pure water, so that the hydrogen chloride in the tail gas generated in the production of the methylsulfonyl chloride is completely absorbed. Generally, N is 3 or 4, but a plurality of stages of absorption devices in series are specifically adopted to absorb hydrogen chloride in the tail gas generated in the production of the methanesulfonyl chloride, and the content of the hydrogen chloride in the tail gas can be determined by a person skilled in the art.
In the invention, the temperature in each absorption device is lower than 50 ℃, and the pressure is low negative pressure of 0-100 mm water column, so as to promote the absorption of chlorine and hydrogen chloride in the tail gas generated in the production of the methanesulfonyl chloride by the absorbent.
In the invention, each absorption device adopts a circulating absorption mode to absorb chlorine or hydrogen chloride in the tail gas, and the first-stage absorption device, the second-stage absorption device, the third-stage absorption device … … or the Nth-stage absorption device can adopt a graphite tube array absorber or a graphite round block hole type absorber.
In order to further illustrate the present invention, the following examples are given to further illustrate the present invention. The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified; the materials, reagents and the like used in the examples of the present invention are commercially available unless otherwise specified.
Example 1:
(1) will contain Fe2+、Cl-Filtering the waste pickle liquor to remove insoluble impurities, and diluting the waste pickle liquor to FeCl2The mass content is 6.5%; taking 5 tons of diluted acid washing waste liquid as an absorbent, adding the acid washing waste liquid into a primary polypropylene absorption tank, taking a graphite tube array absorber as a primary absorption device, enabling the tail gas generated in the production of the methanesulfonyl chloride to pass through the primary absorption device, controlling the temperature in the primary absorption device to be 45 ℃ and the pressure to be low negative pressure of 50mm water column, and circularly absorbing chlorine in the tail gas generated in the production of the methanesulfonyl chloride;
(2) gas from the first-stage absorption device sequentially passes through a second-stage absorption device, a third-stage absorption device and a fourth-stage absorption device which all adopt a graphite round block hole type absorber as an absorption device, pure water is used as an absorbent, the temperature in the three absorption devices is controlled to be 40 ℃, the pressure is controlled to be low negative pressure of 80mm water column, hydrogen chloride gas in the tail gas generated in the production of the methylsulfonyl chloride is circularly absorbed, and hydrochloric acid solution is obtained;
(3) and (3) transferring the hydrochloric acid solution in the second-stage absorption device, the third-stage absorption device and the fourth-stage absorption device, reusing the hydrochloric acid solution for steel pickling, diluting the waste liquid after pickling to be used as an absorbent in the step (1), and circulating the steps (1) - (3).
Gradually changing the absorbent in the first-stage absorption device from green to yellow in the step (1), detecting the absorbent in the first-stage absorption device after 3 hours, and detecting FeCl in the pickling waste liquid2Is 0.43%, the absorbent in the first stage absorption unit is removed and 5 tons of fresh FeCl with a mass content of 6.5% are fed into the first stage absorption unit2The acid pickling waste liquid, the absorbent removed from the first-stage absorption device is 4.8 tons, FeCl2Is 0.43 percent, continuously introducing ozone into the transferred absorbent until FeCl is achieved2Less than 0.2% by mass of Fe2+Fully oxidized and can be used for polyaluminium ferric chlorideAnd (4) production.
The hydrochloric acid solution with the mass concentration of 31.5% is obtained in the second-stage absorption device, the quality of the hydrochloric acid solution meets the quality standard of industrial synthetic hydrochloric acid, and the hydrochloric acid solution can be used for steel pickling.
Example 2:
(1) will contain Fe2+、Cl-Filtering the waste pickle liquor to remove insoluble impurities, and diluting the waste pickle liquor to FeCl2The mass content is 8.1%; taking 5 tons of diluted acid washing waste liquid as an absorbent, adding the acid washing waste liquid into a primary polypropylene absorption tank, taking a graphite tube array absorber as a primary absorption device, enabling the tail gas generated in the production of the methanesulfonyl chloride to pass through the primary absorption device, controlling the temperature in the primary absorption device to be 40 ℃ and the pressure to be low negative pressure of 100mm water column, and circularly absorbing chlorine in the tail gas generated in the production of the methanesulfonyl chloride;
(2) gas from the first-stage absorption device sequentially passes through a second-stage absorption device, a third-stage absorption device and a fourth-stage absorption device which all adopt a graphite round block hole type absorber as an absorption device, pure water is used as an absorbent, the temperature in the three absorption devices is controlled to be 40 ℃, the pressure is controlled to be low negative pressure of 100mm water column, hydrogen chloride gas in the tail gas generated in the production of the methylsulfonyl chloride is circularly absorbed, and hydrochloric acid solution is obtained;
(3) and (3) transferring the hydrochloric acid solution in the second-stage absorption device, the third-stage absorption device and the fourth-stage absorption device, reusing the hydrochloric acid solution for steel pickling, diluting the waste liquid after pickling to be used as an absorbent in the step (1), and circulating the steps (1) - (3).
Gradually changing the absorbent in the first-stage absorption device from green to yellow in the step (1), detecting the absorbent in the first-stage absorption device after 4.5 hours, and detecting FeCl in the pickling waste liquid2Is 0.19%, the absorbent in the first stage absorption unit is removed and 5 tons of fresh FeCl with a mass content of 8.1% are fed into the first stage absorption unit2The acid pickling waste liquid, the absorbent removed from the first-stage absorption device is 4.65 tons, and FeCl is added2The mass content of the poly (aluminum ferric chloride) is 0.19 percent, and the poly (aluminum ferric chloride) can be directly used for producing poly (aluminum ferric chloride).
The hydrochloric acid solution with the mass concentration of 33.1% is obtained in the second-stage absorption device, the quality of the hydrochloric acid solution meets the quality standard of industrial synthetic hydrochloric acid, and the hydrochloric acid solution can be used for steel pickling.
Example 3:
(1) will contain Fe2+、Cl-Filtering the waste pickle liquor to remove insoluble impurities, and diluting the waste pickle liquor to FeCl2The mass content is 9.7%; taking 5 tons of diluted acid washing waste liquid as an absorbent, adding the acid washing waste liquid into a primary polypropylene absorption tank, taking a graphite tube array absorber as a primary absorption device, enabling the tail gas generated in the production of the methanesulfonyl chloride to pass through the primary absorption device, controlling the temperature in the primary absorption device to be 45 ℃ and the pressure to be low negative pressure of 100mm water column, and circularly absorbing chlorine in the tail gas generated in the production of the methanesulfonyl chloride;
(2) gas from the first-stage absorption device sequentially passes through a second-stage absorption device, a third-stage absorption device and a fourth-stage absorption device which all adopt a graphite round block hole type absorber as an absorption device, pure water is used as an absorbent, the temperature in the three absorption devices is controlled to be 35 ℃, the pressure is controlled to be low negative pressure of 50mm water column, hydrogen chloride gas in the tail gas generated in the production of the methylsulfonyl chloride is circularly absorbed, and hydrochloric acid solution is obtained;
(3) and (3) transferring the hydrochloric acid solution in the second-stage absorption device, the third-stage absorption device and the fourth-stage absorption device, reusing the hydrochloric acid solution for steel pickling, diluting the waste liquid after pickling to be used as an absorbent in the step (1), and circulating the steps (1) - (3).
Gradually changing the absorbent in the first-stage absorption device from green to yellow in the step (1), detecting the absorbent in the first-stage absorption device after 5 hours, and detecting FeCl in the acid pickling waste liquid2Is 0.23%, the absorbent in the first stage absorption unit is removed and 5 tons of fresh FeCl with a mass content of 9.7% are fed into the first stage absorption unit2The acid pickling waste liquid, the absorbent removed from the first-stage absorption device is 4.74 tons, FeCl2The mass content of the organic acid is 0.23 percent, hydrogen peroxide is dripped into the transferred absorbent until FeCl2Less than 0.2% by mass of Fe2+Is completely oxidized, canFor the production of polyaluminum ferric chloride.
The hydrochloric acid solution with the mass concentration of 32.7% is obtained in the second-stage absorption device, the quality of the hydrochloric acid solution meets the quality standard of industrial synthetic hydrochloric acid, and the hydrochloric acid solution can be used for steel pickling.
The above-described embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
Claims (4)
1. A treatment method of tail gas in the production of methylsulfonyl chloride is characterized by comprising the following steps:
s1, enabling the tail gas generated in the production of the methanesulfonyl chloride to pass through a first-stage absorption device filled with an absorbent to absorb chlorine in the tail gas generated in the production of the methanesulfonyl chloride, wherein the absorbent contains Fe2+The acid pickling waste liquid of (1);
s2, introducing the gas from the first-stage absorption device into a second-stage absorption device containing water to absorb hydrogen chloride gas in the tail gas generated in the production of the methanesulfonyl chloride to obtain a hydrochloric acid solution;
s3, reusing the hydrochloric acid solution for steel pickling, taking the waste liquid after pickling as an absorbent in the step S1, and circulating the steps S1 to S3; the absorbent in step S1 contains FeCl2The step S1 further includes diluting the waste pickling solution to FeCl2The mass content is 5-10%, if FeCl is contained in the pickling waste liquid in the step S12Is less than 0.5 percent, removing the absorbent in the first stage absorption device, and supplementing fresh Fe-containing into the first stage absorption device2+The method is repeated, the absorbent in the first-stage absorption device is intermittently removed, and fresh Fe-containing waste liquid is replenished2+If FeCl in the absorbent removed from the first-stage absorption device2Is less than 0.5% and is not less than 0.2%, then adding an oxidizing agent to the absorbent to convert the Fe2+Oxidizing to a mass content of less than 0.2%, wherein the oxidant is ozone,Hydrogen peroxide and chlorate.
2. The method for treating the tail gas generated in the production of methanesulfonyl chloride as claimed in claim 1, wherein the method for treating the tail gas generated in the production of methanesulfonyl chloride employs a multistage series absorption mode, specifically comprising: the absorbent in the first stage of absorption device is FeCl2The mass content of the pickling waste liquid is 5-10%, the absorbents in the second-stage absorption device and the third-stage absorption device … …, namely the Nth-stage absorption device, are all water, and N is more than or equal to 3.
3. The method for treating the tail gas generated in the production of methanesulfonyl chloride as claimed in any one of claims 1 to 2, wherein the temperature in each absorber is lower than 50 ℃ and the pressure is low negative pressure of 0 to 100mm water.
4. The method for treating the tail gas generated in the production of methanesulfonyl chloride as claimed in any one of claims 1 to 2, wherein each absorption device is used for absorbing chlorine or hydrogen chloride in the tail gas generated in the production of methanesulfonyl chloride in a circulating absorption manner, and each absorption device can be a graphite tube-in-tube absorber or a graphite round block-hole absorber.
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