CN105801346A - Method for recovering tetrachloroethylene and hexachloroethane from waste liquid of heavy components produced by tetrachloroethylene apparatus - Google Patents
Method for recovering tetrachloroethylene and hexachloroethane from waste liquid of heavy components produced by tetrachloroethylene apparatus Download PDFInfo
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- CN105801346A CN105801346A CN201410842332.4A CN201410842332A CN105801346A CN 105801346 A CN105801346 A CN 105801346A CN 201410842332 A CN201410842332 A CN 201410842332A CN 105801346 A CN105801346 A CN 105801346A
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- tetrachloroethylene
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Abstract
The invention relates to a method for recovering tetrachloroethylene and hexachloroethane from the waste liquid of heavy components produced by a tetrachloroethylene apparatus. The method comprises the following steps: (1) delivering the waste liquid of heavy components produced by the tetrachloroethylene apparatus to a heavy component rectifying tower for rectification; (2) subjecting components obtained at the top of the heavy component rectifying tower to condensation, then sending a part of the condensed components back to the heavy component rectifying tower and delivering the rest condensed components to a refining unit of the tetrachloroethylene apparatus for refining so as to obtain a tetrachloroethylene product; (3) delivering components obtained at the bottom of the heavy component rectifying tower to a hexachloroethane rectifying tower for rectification; and (4) subjecting components obtained at the top of the hexachloroethane rectifying tower to condensation and crushing so as to obtain a hexachloroethane product. The method prevents the problem that pipelines and equipment are prone to obstruction in the process of recovery by accurately controlling tower-top and tower-bottom temperatures of the heavy component rectifying tower and the hexachloroethane rectifying tower, and effectively overcomes the technical problems that the waste liquid of heavy components produced by the tetrachloroethylene apparatus is difficult to treat, the smell of the discharged waste liquid is great and the like.
Description
Technical field
The present invention relates to the processing method of the heavy constituent waste liquid that a kind of tetrachloroethylene device produces, particularly relate to a kind of method reclaiming tetrachloroethylene and hexachlorethane from the heavy constituent waste liquid that tetrachloroethylene device produces, belong to chemical technology field.
Background technology
Domestic existing tetrachloroethylene device capbility is more than 300,000 tons/year, tetrachloroethylene device can generate the mixture waste liquid containing gas chromatographies such as carbon tetrachloride, tetrachloroethylene, hexachlorethane, hexachlorobutadiene, Perchlorobenzenes in process of production, and these Organic substances mostly are heavy constituent (below by said mixture waste liquid referred to as heavy constituent waste liquid).Heavy constituent discharging of waste liquid abnormal smells from the patient is big, complex treatment process and not environmentally, is worth significantly high tetrachloroethylene and hexachlorethane in heavy constituent waste liquid containing more application；At present, most domestic producer all without well reclaiming tetrachloroethylene and hexachlorethane in heavy constituent, mostly directly discharge or burning after simple process, not only to environmental concerns, and cause the waste of tetrachloroethylene and hexachlorethane, uneconomical.Accordingly, it is desirable to provide a kind of production technology recycling tetrachloroethylene heavy constituent.
Tetrachloroethylene and hexachlorethane, the domestic technique having complete process but without producer at present is reclaimed from heavy constituent waste liquid.In removal process, pipeline and equipment easily block, and technological parameter difficulty controls, and the continuous production run of device is difficult to ensure.
Summary of the invention
For the deficiencies in the prior art, solving the problem that in tetrachloroethylene production process, the heavy constituent liquid waste processing difficulty of generation is big, the present invention provides a kind of method reclaiming tetrachloroethylene and hexachlorethane from the heavy constituent waste liquid that tetrachloroethylene device produces.
Technical scheme is as follows:
A kind of method reclaiming tetrachloroethylene and hexachlorethane from the heavy constituent waste liquid that tetrachloroethylene device produces, comprises the following steps:
(1) the heavy constituent waste liquid that tetrachloroethylene device produces is sent into heavy constituent rectifying column and carry out rectification, control tower top temperature 122～130 DEG C, column bottom temperature 190～200 DEG C, tower reactor pressure 0.001～0.01MPa；
(2) the condensed rear portion of component that heavy constituent rectifying column tower top obtains sends back to heavy constituent rectifier column reflux, and reflux ratio is 0.4～0.6, and another part sends back to tetrachloroethylene device of refining unit and refines, and obtains tetrachloroethylene product；
(3) component obtained at the bottom of heavy constituent rectifying tower is sent into hexachlorethane rectifying column and is carried out rectification, controls tower top temperature 186 DEG C～190 DEG C, column bottom temperature 195 DEG C～205 DEG C, tower reactor pressure 0.05～0.1MPa；
(4) hexachlorethane rectifying column overhead components condensed, pulverize, obtain hexachlorethane product.
According to the present invention, preferably, the key component of the heavy constituent waste liquid that the tetrachloroethylene device described in step (1) produces is as follows: carbon tetrachloride 0.58～1.86%, tetrachloroethylene 47.52～48.52%, Pentalin. 0.04～0.16%, hexachlorethane 18.84～20.62%, hexachlorobutadiene 28.58～34.1%.
According to the invention it is preferred to, the reflux ratio described in step (2) is 0.5, and the temperature of described condensation is 30～50 DEG C.
According to the invention it is preferred to, described in step (4), the temperature of condensation is 120～150 DEG C.
According to the invention it is preferred to, step (4) also includes component at the bottom of hexachlorethane rectifying tower is carried out burning disposal step.
According to the present invention, the component that heavy constituent rectifying column tower top obtains is mainly the light component such as carbon tetrachloride, tetrachloroethylene, component at the bottom of hexachlorethane rectifying tower is mainly the heavy constituent such as hexachlorobutadiene, Perchlorobenzene, hexachlorethane rectifying column overhead components is mainly hexachlorethane gas, and condensed, pulverizing obtains hexachlorethane product；Reclaiming the tetrachloroethylene purity obtained is more than 99.8%, and the response rate reaches more than 95%；Reclaiming the hexachlorethane purity obtained is more than 98%, and the response rate reaches more than 85%.
Tetrachloroethylene device of the present invention is tetrachloroethylene production process, technical process well known to those skilled in the art, wherein, in step (2), the condensed another part component obtained of heavy constituent rectifying column tower top sends back to the process that tetrachloroethylene device of refining unit carries out refining and can be undertaken by prior art.
Principles of the invention:
Principles of the invention is, by rectification, each component is easily separated recovery, the first step first passes through the method for rectification and reclaims tetrachloroethylene and carbon tetrachloride, this step is controlled mainly through controlling bottom temperature and reflux ratio, should be noted that the composition of tower reactor heavy constituent, ensure that the content of tower reactor hexachlorobutadiene is within proper range, if tower reactor hexachlorobutadiene content is too low, then can block tower reactor and follow-up process pipe；Then reclaiming hexachlorethane again through the method for rectification, this step major control tower reactor, tower top temperature, it is impossible to too high and too low, too high hexachlorethane purity is not high, too low, easily blocks.Therefore, the main technological operation point of the present invention is exactly tower reactor, tower top temperature, by accurate control, it is to avoid in removal process, and pipeline and the susceptible to plugging problem of equipment.
Device therefor of the present invention all available this area conventional equipment, on heavy constituent rectifying column and hexachlorethane rectifying column locus near as much as possible, the hexachlorethane condensation heat exchanger used that hexachlorethane rectifying column tower top obtains can use U-tube heat exchanger, can be fixed on hexachlorethane rectifying column tower top.
Beneficial effects of the present invention is as follows:
1, the heavy constituent waste liquid that tetrachloroethylene device is produced by the present invention method by rectification, reclaims tetrachloroethylene therein and hexachlorethane, is then processed by the heavy constituent castoff burning such as hexachlorobutadiene, Perchlorobenzene.Effectively solve and the heavy constituent waste liquid that tetrachloroethylene device produces is difficult to resolve certainly, the difficult problems such as discharge abnormal smells from the patient is big, and tetrachloroethylene and hexachlorethane are recycled more economical, save cost.
2, the present invention is by accurately controlling heavy constituent rectifying column and hexachlorethane rectifying tower top column bottom temperature, it is to avoid in removal process, pipeline and the susceptible to plugging problem of equipment.
Detailed description of the invention
Below by specific embodiment, the invention will be further described.
In embodiment, device therefor is this area conventional equipment, commercial products.
Embodiment 1
The mainly comprising of heavy constituent waste liquid that the present embodiment tetrachloroethylene device produces: carbon tetrachloride 1.86%, tetrachloroethylene 48%, Pentalin.: 0.16%, hexachlorethane 20.62%, hexachlorobutadiene 29.35%.
A kind of method reclaiming tetrachloroethylene and hexachlorethane from the heavy constituent waste liquid that tetrachloroethylene device produces, comprises the following steps:
(1) the heavy constituent waste liquid that tetrachloroethylene device produces is entered heavy constituent rectifying column, control heavy constituent rectifying column column bottom temperature 192.6 DEG C, tower bottom pressure 0.003MPa, tower top temperature 123.8 DEG C；
(2) component that heavy constituent rectifying column tower top obtains sends back to heavy constituent rectifier column reflux, capacity of returns 0.5m through 42 DEG C of condensation rear portions3/ h, reflux ratio 0.5, another part sends back to tetrachloroethylene device of refining unit and refines, and obtains tetrachloroethylene product；
(3) component obtained at the bottom of heavy constituent rectifying tower is sent into hexachlorethane rectifying column and is carried out rectification, controls hexachlorethane rectifying column column bottom temperature 198.8 DEG C, tower bottom pressure 0.06MPa, tower top temperature 188.1 DEG C；
(4) hexachlorethane rectifying column overhead components is through 143 DEG C of condensations, pulverizing, obtains hexachlorethane product；Component at the bottom of hexachlorethane rectifying tower is sent into incinerator and is carried out burning disposal.
The tetrachloroethylene purity that the present embodiment obtains is 99.9%, and the response rate reaches 96%, and hexachlorethane purity is 98.5%, the response rate 87%.
Embodiment 2
Mainly comprising of the heavy constituent waste liquid that the present embodiment tetrachloroethylene device produces: carbon tetrachloride 0.58%, tetrachloroethylene 47.52%, Pentalin. 0.04%, hexachlorethane 18.84%, hexachlorobutadiene 33.01%.
A kind of method reclaiming tetrachloroethylene and hexachlorethane from the heavy constituent waste liquid that tetrachloroethylene device produces, comprises the following steps:
(1) the heavy constituent waste liquid that tetrachloroethylene device produces is entered heavy constituent rectifying column, control heavy constituent rectifying column column bottom temperature 195.2 DEG C, tower bottom pressure 0.005MPa, tower top temperature 124.9 DEG C；
(2) component that heavy constituent rectifying column tower top obtains sends back to heavy constituent rectifier column reflux, capacity of returns 0.49m through 45.8 DEG C of condensation rear portions3/ h, reflux ratio 0.48, another part sends back to tetrachloroethylene device of refining unit and refines, and obtains tetrachloroethylene product；
(3) component obtained at the bottom of heavy constituent rectifying tower is sent into hexachlorethane rectifying column and is carried out rectification, controls hexachlorethane rectifying column column bottom temperature 196.5 DEG C, tower bottom pressure 0.05MPa, tower top temperature 187.0 DEG C；
(4) hexachlorethane rectifying column overhead components is through 138 DEG C of condensations, pulverizing, obtains hexachlorethane product；Component at the bottom of hexachlorethane rectifying tower is sent into incinerator and is carried out burning disposal.
The tetrachloroethylene purity that the present embodiment obtains is 99.89%, and the response rate reaches 96.8%, and hexachlorethane purity is 98.1%, the response rate 86.7%.
Embodiment 3
Mainly comprising of the heavy constituent waste liquid that the present embodiment tetrachloroethylene device produces: carbon tetrachloride 1.75%, tetrachloroethylene 48.52%, Pentalin. 0.12%, hexachlorethane 19.58%, hexachlorobutadiene 30.02%.
A kind of method reclaiming tetrachloroethylene and hexachlorethane from the heavy constituent waste liquid that tetrachloroethylene device produces, comprises the following steps:
(1) the heavy constituent waste liquid that tetrachloroethylene device produces is entered heavy constituent rectifying column, control heavy constituent rectifying column column bottom temperature 197.3 DEG C, tower bottom pressure 0.007MPa, tower top temperature 127.1 DEG C；
(2) component that heavy constituent rectifying column tower top obtains sends back to heavy constituent rectifier column reflux, capacity of returns 0.52m through 36.9 DEG C of condensation rear portions3/ h, reflux ratio 0.52, another part sends back to former tetrachloroethylene device of refining unit and refines, and obtains tetrachloroethylene product；
(3) component obtained at the bottom of heavy constituent rectifying tower is sent into hexachlorethane rectifying column and is carried out rectification, controls hexachlorethane rectifying column column bottom temperature 202.9 DEG C, tower bottom pressure 0.068MPa, tower top temperature 189.2 DEG C；
(4) hexachlorethane rectifying column overhead components is through 147 DEG C of condensations, pulverizing, obtains hexachlorethane product；Component at the bottom of hexachlorethane rectifying tower is sent into incinerator and is carried out burning disposal.
The tetrachloroethylene purity that the present embodiment obtains is 99.93%, and the response rate reaches 95.8%, and hexachlorethane purity is 98.2%, the response rate 86.4%.
What finally illustrate is, above example is only in order to illustrate technical scheme and unrestricted, although the present invention being described in detail with reference to preferred embodiment, it will be understood by those within the art that, technical scheme can be modified or equivalent replacement, without deviating from objective and the scope of technical solution of the present invention, it all should be contained in the middle of scope of the presently claimed invention.
Claims (6)
1. the method reclaiming tetrachloroethylene and hexachlorethane from the heavy constituent waste liquid that tetrachloroethylene device produces, comprises the following steps:
(1) the heavy constituent waste liquid that tetrachloroethylene device produces is sent into heavy constituent rectifying column and carry out rectification, control tower top temperature 122～130 DEG C, column bottom temperature 190～200 DEG C, tower reactor pressure 0.001～0.01MPa；
(2) the condensed rear portion of component that heavy constituent rectifying column tower top obtains sends back to heavy constituent rectifier column reflux, and reflux ratio is 0.4～0.6, and another part sends back to tetrachloroethylene device of refining unit and refines, and obtains tetrachloroethylene product；
(3) component obtained at the bottom of heavy constituent rectifying tower is sent into hexachlorethane rectifying column and is carried out rectification, controls tower top temperature 186 DEG C～190 DEG C, column bottom temperature 195 DEG C～205 DEG C, tower reactor pressure 0.05～0.1MPa；
(4) hexachlorethane rectifying column overhead components condensed, pulverize, obtain hexachlorethane product.
2. the method reclaiming tetrachloroethylene and hexachlorethane from the heavy constituent waste liquid that tetrachloroethylene device produces according to claim 1, it is characterized in that, the key component of the heavy constituent waste liquid that the tetrachloroethylene device described in step (1) produces is as follows: carbon tetrachloride 0.58～1.86%, tetrachloroethylene 47.52～48.52%, Pentalin. 0.04～0.16%, hexachlorethane 18.84～20.62%, hexachlorobutadiene 28.58～34.1%.
3. the method reclaiming tetrachloroethylene and hexachlorethane from the heavy constituent waste liquid that tetrachloroethylene device produces according to claim 1, it is characterised in that the reflux ratio described in step (2) is 0.5.
4. the method reclaiming tetrachloroethylene and hexachlorethane from the heavy constituent waste liquid that tetrachloroethylene device produces according to claim 1, it is characterised in that described in step (2), the temperature of condensation is 30～50 DEG C.
5. the method reclaiming tetrachloroethylene and hexachlorethane from the heavy constituent waste liquid that tetrachloroethylene device produces according to claim 1, it is characterised in that described in step (4), the temperature of condensation is 120～150 DEG C.
6. the method reclaiming tetrachloroethylene and hexachlorethane from the heavy constituent waste liquid that tetrachloroethylene device produces according to claim 1, it is characterised in that also include in step (4) component at the bottom of hexachlorethane rectifying tower is carried out burning disposal step.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410842332.4A CN105801346B (en) | 2014-12-30 | 2014-12-30 | A kind of method that tetrachloro-ethylene and carbon trichloride are recycled in the heavy constituent waste liquid produced from tetrachloro-ethylene device |
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| CN201410842332.4A CN105801346B (en) | 2014-12-30 | 2014-12-30 | A kind of method that tetrachloro-ethylene and carbon trichloride are recycled in the heavy constituent waste liquid produced from tetrachloro-ethylene device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106187676A (en) * | 2016-08-19 | 2016-12-07 | 泸州鑫福化工有限公司 | The recovery method of distillation residual liquid in the production of a kind of tetrachloroethylene |
| CN107056580A (en) * | 2017-05-05 | 2017-08-18 | 乐山师范学院 | A kind of method that ionization prepares perchloroethane and perchloro- butane |
| CN110540486A (en) * | 2018-05-29 | 2019-12-06 | 乳源东阳光氟有限公司 | system and method for separating byproduct high-boiling residues in tetrachloroethylene production |
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| CN103086839A (en) * | 2012-12-20 | 2013-05-08 | 山东东岳氟硅材料有限公司 | Production process for production of tetrachloroethylene and coproduction of hexachloroethane by using methane chloride residual liquid |
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| CN103787823A (en) * | 2014-02-28 | 2014-05-14 | 重庆海洲化学品有限公司 | Method for recovering organic chloride from rectification residues of methane chloride or/and tetrachloroethylene |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106187676A (en) * | 2016-08-19 | 2016-12-07 | 泸州鑫福化工有限公司 | The recovery method of distillation residual liquid in the production of a kind of tetrachloroethylene |
| CN107056580A (en) * | 2017-05-05 | 2017-08-18 | 乐山师范学院 | A kind of method that ionization prepares perchloroethane and perchloro- butane |
| CN110540486A (en) * | 2018-05-29 | 2019-12-06 | 乳源东阳光氟有限公司 | system and method for separating byproduct high-boiling residues in tetrachloroethylene production |
| CN110540486B (en) * | 2018-05-29 | 2023-06-09 | 乳源东阳光氟有限公司 | Separation system and separation method for byproduct high-boiling-point substances in tetrachloroethylene production |
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