CN110694425A - Chlorinated organic matter low-energy-consumption recovery improvement process for chlorinated organic matter-containing mixed gas - Google Patents
Chlorinated organic matter low-energy-consumption recovery improvement process for chlorinated organic matter-containing mixed gas Download PDFInfo
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- CN110694425A CN110694425A CN201910915814.0A CN201910915814A CN110694425A CN 110694425 A CN110694425 A CN 110694425A CN 201910915814 A CN201910915814 A CN 201910915814A CN 110694425 A CN110694425 A CN 110694425A
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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
- B01D53/02—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 adsorption, e.g. preparative gas chromatography
- B01D53/04—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 adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/0407—Constructional details of adsorbing systems
- B01D53/0423—Beds in columns
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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
- B01D53/002—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 condensation
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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
- B01D53/02—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 adsorption, e.g. preparative gas chromatography
- B01D53/04—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 adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/0407—Constructional details of adsorbing systems
- B01D53/0438—Cooling or heating systems
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/116—Molecular sieves other than zeolites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
- B01D2257/206—Organic halogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
- B01D2259/40088—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating
- B01D2259/40092—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating using hot liquid
Abstract
The invention discloses an improved low-energy-consumption recovery process for chlorinated organic compounds containing chlorinated organic compound mixed gas, which comprises the steps of cooling mixed gas containing 5 ~% of chlorinated organic compounds by water cooling and freezing to-20 ~ -35 ℃, recovering chlorinated organic compounds, carrying out heat exchange to-10 ~ ℃, sending saturated gas which is not liquefied by the chlorinated organic compounds into an adsorption tower, enabling the concentration of the chlorinated organic compounds in primary purified gas after adsorption and separation to be below 0.01 ~%, switching another adsorption tower to continuously separate organic chlorides after the adsorption of the chlorinated organic compounds reaches a certain time, enabling the adsorption tower which finishes adsorption to carry out pressure reduction and first-stage purified gas blowing and desorption, sending the desorbed gas back to raw gas to continuously separate the organic chlorides, sending the primary purified gas into the adsorption tower, enabling the concentration of the chlorinated organic compounds in secondary purified gas after adsorption and separation to reach below 0.0001.01%, switching another adsorption tower to continuously separate the organic chlorides after the adsorption of the chlorinated organic compounds reaches a certain time, enabling the adsorption tower which finishes pressure reduction to carry out desorption and second-stage purified gas to carry out pressure boosting, and sending back to the raw gas to realize full-cycle of the organic compounds recovery.
Description
Technical Field
The invention relates to the fields of chemical industry and environmental protection, and discloses a method for effectively reducing environmental pollution of chlorinated organic gases and reducing energy recovery of chlorinated organic compounds.
Background
As for the recovery method of the gas containing chlorinated organic compounds, the method which is used conventionally is to compress, freeze, liquefy and recover the chlorinated organic compounds, and the separation of the liquefied chlorinated organic compounds is realized under the saturated vapor pressure of the chlorinated organic compounds under high pressure, generally, in order to ensure that the concentration of the chlorinated organic compounds in the gas is less than 10ppb, the liquefaction temperature is required to be less than-160 ℃, the energy consumption is high, and the economic benefit is not good.
The temperature swing adsorption method is a common method for removing the moisture in the air, has low energy consumption, and is more effective in removing the moisture by low-pressure gas. Due to the high regeneration temperature, the adsorbent is easily regenerated. Typically, two or more adsorbent beds are used to alternately adsorb and regenerate. CN101596396A "a method for deeply drying gas" discloses a method for drying gas by using multi-layer segmented adsorbent, but since high concentration of unsaturated chlorinated organic gas is self-polymerized when the regeneration temperature is higher than 90 ℃, the invention can not be used for adsorption separation of unsaturated chlorinated organic gas.
The desorption of chlorinated organic compounds by using a vacuum system has two modes, one mode is a mechanical vacuum pump, and the pump cannot be used because the outlet temperature is higher than 90 ℃, and the chlorinated organic compounds are easy to cause self-polymerization reaction. The other is a water ring or oil ring vacuum pump, which operates at low temperature, but water or oil pollutes chlorinated organic matters and is not easy to separate.
Yanhao discloses (201810774611. X) an improved low-energy-consumption chlorinated organic matter recovery process for a chlorinated organic matter-containing mixed gas, which comprises the steps of freezing a raw material gas to a state that 90% or less of chlorinated organic matters can be separated through liquefaction, separating and recovering supersaturated chlorinated organic matters in the gas through liquefaction, sending saturated gas in which the chlorinated organic matters are not liquefied into at least one of three established adsorption tower groups, and completely adsorbing and separating the chlorinated organic matters from the gas to enable the concentration of the chlorinated organic matters in the discharged gas to be below 10 ppb; the method comprises the steps of switching another adsorption tower to continuously separate organic chloride after the adsorption tower which adsorbs chlorinated organic matters reaches a certain time, reducing pressure, vacuumizing and heating the adsorption tower which finishes adsorption, sending desorption gas back to raw material gas after the desorption gas is boosted, and continuously separating organic chloride, so that low-energy-consumption total recovery of the chlorinated organic matters is realized, wherein a low-temperature chlorinated organic matter liquid ring vacuum pump is adopted as a vacuum pump type, a mechanical isolation cavity sealing mode is adopted for sealing the pump, inert gas is filled in a sealing cavity, and the pressure of the sealing gas is higher than 0.1MPa (shown).
Because the pressure swing adsorption device has the existence of evacuation process in the operation process, it may cause the program control valve piston rod to have certain abrasion, the leakage of chlorine-containing gas may cause the potential safety hazard, and the increase of desorption temperature may cause the polymerization of chloride, and the control difficulty of desorption temperature is higher, the invention is as follows.
Disclosure of Invention
A process for recovering chlorinated organic compounds from the gas mixture containing chlorinated organic compounds (5 ~%) includes such steps as cooling the gas mixture containing chlorinated organic compounds by water cooling and freezing to-20 ~ -35 deg.C, recovering chlorinated organic compounds, heat exchanging to-10 ~ deg.C, introducing the saturated gas containing non-liquefied chlorinated organic compounds to at least one of three adsorption towers, adsorbing and separating chlorinated organic compounds from gas to obtain chlorinated organic compounds with concentration of 0.01 ~%, purging by one of three adsorption towers, introducing the gas mixture to one of three adsorption towers, adsorbing and separating chlorinated organic compounds, introducing the gas mixture to another adsorption tower, purging by another adsorption tower, introducing the gas mixture to another adsorption tower, recovering chlorinated organic compounds, introducing the gas mixture to another adsorption tower, recovering organic compounds, and recovering chlorinated organic compounds.
Detailed Description
Example 1: the composition of a vinyl chloride gas mixture is as follows.
1. The raw material gas composition is as follows:
| composition (I) | Nitrogen gas | Vinyl chloride | Argon gas | Acetylene |
| V/V | 0.1166 | 0.7064 | 0.077 | 0.1 |
2. The gas amount of the raw materials is as follows: 700Nm3/H；
3. ~ 0.4MPa (gauge pressure);
4. the temperature is ~ 40 ℃;
under the working conditions, the temperature of the chloroethylene mixed gas is firstly reduced to-30 ℃, the chloroethylene is liquefied and separated, then the mixed gas with the chloroethylene separated is directly sent into one of three adsorption towers of 3 cubes, and at the outlet of the adsorption tower, a primary purified gas with the chloroethylene content of 1% is obtained and is directly sent into a secondary purification tower. Switching another adsorption tower to continuously separate the chloroethylene after the adsorption tower adsorbing the chloroethylene reaches a certain time, and sending the desorption gas back to the raw material gas after the desorption gas is boosted by reducing the pressure and using first-stage purified gas to purge and desorb the chloroethylene in the adsorption tower which finishes adsorption so as to continuously separate the organic chloride; feeding the primary purified gas into one of three adsorption towers to adsorb and separate chloroethylene from the gas, so that the concentration of chloroethylene in the fed gas reaches 0.01%, and hereinafter referred to as secondary purified gas; switching another adsorption tower to continuously separate chloroethylene after the adsorption tower adsorbing chloroethylene reaches a certain time, and sending the desorbed gas back to the raw material gas after the desorbed gas is pressurized by depressurizing the adsorption tower which finishes adsorption and using secondary purified gas to purge and desorb, and continuously separating chloroethylene; feeding the secondary purified gas into one of three adsorption towers to adsorb and separate chloroethylene from the gas, so that the concentration of chloroethylene in the delivered gas reaches 10ppb, hereinafter referred to as a third-level purified gas; switching another adsorption tower to continuously separate the organic chloride after the adsorption tower adsorbing the chloroethylene reaches a certain time, reducing the pressure of the adsorption tower which finishes adsorption, blowing and desorbing by using secondary purified gas, raising the pressure of the desorbed gas, sending the desorbed gas back to the raw material gas, and continuously separating the organic chloride; thereby realizing low-energy-consumption total recovery of the vinyl chloride.
Example 2: the composition of a mixture gas of methyl chloride was as follows.
1. The raw material gas composition is as follows:
| composition (I) | Nitrogen gas | 1-4 Chloromethane | Hydrogen gas | Methane |
| V/V | 0.01 | 0.28 | 0. 54 | 0.17 |
2. The gas amount of the raw materials is as follows: 700Nm3/H；
3. ~ 0.4MPa (gauge pressure);
4. the temperature is ~ 40 ℃;
under the working conditions, the mixed gas of methyl chloride is cooled to-25 ℃, the methyl chloride is liquefied and separated, then the mixed gas with the methyl chloride separated is directly sent to one of three adsorption towers with 2.5 cubic volumes, a primary purified gas with the methyl chloride content of ~ 0.08.08% is obtained at the outlet of the adsorption tower, the mixed gas is directly sent to a secondary purification tower, after the adsorption tower absorbing the methyl chloride reaches a certain time, the other adsorption tower is switched to continue to separate the methyl chloride, the adsorption tower absorbing the methyl chloride is depressurized and purged and desorbed by using the primary purified gas, the desorbed gas is sent back to the raw gas after being pressurized, the organic chloride is continuously separated, the primary purified gas is sent to one of the three adsorption towers, the methyl chloride is absorbed and separated from the gas, the concentration of the methyl chloride in the outsourced gas reaches ~ 0.001.001% of the secondary purified gas, the adsorption tower absorbing the methyl chloride reaches a certain time, the other adsorption tower is switched to continue to separate the methyl chloride, the adsorbed and desorbed gas is sent back to the primary purified gas after being depressurized and purged by using the secondary purified gas, the low-energy-ppb, the adsorption tower is sent back to the absorption tower to continue to separate the methyl chloride, the absorbed and desorbed organic chloride, the methyl chloride, the absorbed and desorbed gas is sent to the three absorption towers, the absorption tower, and desorbed gas, the three absorption tower, and desorbed gas is sent to the absorption tower, and desorbed gas is sent to the three absorption tower, and desorbed gas, the three absorption.
Example 3: the composition of a certain chloroethane gas mixture is as follows.
1. The raw material gas composition is as follows:
| composition (I) | Nitrogen gas | 1-4 Chloroethane | Ethane (III) | Methane |
| V/V | 0.01 | 0.05 | 0. 77 | 0.17 |
2. The gas amount of the raw materials is as follows: 700Nm3/H；
3. ~ 0.4MPa (gauge pressure);
4. the temperature is ~ 40 ℃;
under the above working condition, the mixed gas of chloroethane is firstly cooled to-25 deg.C, liquefied and separated, then the mixed gas with chloroethane separated is directly fed into one of three adsorption towers with 2 cubic volumes, at the outlet of adsorption tower we can obtain first-stage purified gas with chloroethane content of 1%, and directly fed into second-stage purification tower, after the adsorption tower with chloroethane adsorbed is reached to a certain time, another adsorption tower is switched to continuously separate chloroethane, the adsorption tower with adsorbed chloroethane is passed through depressurization and purging desorption by using first-stage purified gas, after the desorbed gas is raised in pressure, the first-stage purified gas is fed back to raw material gas, and continuously separate organic chloride, the first-stage purified gas is fed into one of three adsorption towers, and chloroethane is adsorbed and separated from gas, so that the concentration of chloroethane in the gas can be up to 0.0001 ~ 0.01.01% of second-stage gas, after the adsorption tower with chloroethane adsorbed is reached to a certain time, another adsorption tower is switched to continuously separate chloroethane, after the adsorbed and desorbed gas is returned to raw material gas, after the desorbed gas is passed through depressurization and the second-stage purge purification tower, the low-stage chlorine-absorbed and the purified gas is fed back to the adsorption tower, and the three-stage chlorine-absorbed and the absorption towers are switched to the absorption tower, and the low-absorbed and the three-stage chlorine-absorbed and the three-absorbed and the purified gas is returned to the absorption tower, and the low-absorbed and the three-absorbed chloroethane-absorbed and the.
Claims (1)
1. An improved process for recovering chlorinated organic compounds from the gas mixture containing chlorinated organic compounds features that the gas mixture containing 5 ~ 80% of chlorinated organic compounds is cooled by water and freezing to-20 ~ -35 deg.C for recovering chlorinated organic compounds, which is called raw gas, and then heat exchanged to-10 ~ 40 deg.C, the saturated gas without liquefied chlorinated organic compounds is fed to at least one of three adsorption towers, the chlorinated organic compounds are adsorbed and separated from the gas, the concentration of chlorinated organic compounds in the gas mixture is 0.01 ~ 1% and then to the first-stage purifying gas, the adsorption tower adsorbing chlorinated organic compounds is switched to another adsorption tower for separating organic chlorides, the adsorbed organic compounds are desorbed by the first-stage purifying gas, the desorbed gas is fed back to raw gas for separating organic chlorides, the first-stage purifying gas is fed to at least one of three adsorption towers for adsorbing and separating chlorinated organic compounds, the concentration of chlorinated organic compounds in the gas reaches 0. 0.0001 ~ 0.01.01% and the adsorbed organic compounds is desorbed by the second-stage purifying tower, the adsorbed and the desorbed gas is fed back to the third-stage purifying tower for recovering organic compounds, the adsorbed and desorbed gas is fed back to the second-stage purifying tower for separating organic compounds, and the adsorbed organic compounds.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006130216A (en) * | 2004-11-09 | 2006-05-25 | Canon Inc | Method and apparatus for decomposing organic chlorine compound |
| CN1850751A (en) * | 2005-11-28 | 2006-10-25 | 四川开元科技有限责任公司 | Pressure-variation adsorption separation recovering method for mixd gas containing chloroethylene and acetylene |
| CN101249370A (en) * | 2008-04-03 | 2008-08-27 | 上海穗杉实业有限公司 | Voltage transformation adsorption method for circulation valuable gas |
| CN103357242A (en) * | 2013-07-03 | 2013-10-23 | 中国海洋石油总公司 | Method for purifying and removing chlorides contained in chlorine-containing industrial mixed gas and recovering light hydrocarbon |
| CN105935537A (en) * | 2016-04-19 | 2016-09-14 | 杨皓 | Process for purifying chlorosilane and hydrogen chloride with hydrogen mixed gas |
| CN109012015A (en) * | 2018-07-09 | 2018-12-18 | 天吉人吉环保节能（苏州）有限公司 | A kind of chlorinated organics low energy consumption recovery process of chloride containing organic matter gaseous mixture |
-
2019
- 2019-09-26 CN CN201910915814.0A patent/CN110694425B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006130216A (en) * | 2004-11-09 | 2006-05-25 | Canon Inc | Method and apparatus for decomposing organic chlorine compound |
| CN1850751A (en) * | 2005-11-28 | 2006-10-25 | 四川开元科技有限责任公司 | Pressure-variation adsorption separation recovering method for mixd gas containing chloroethylene and acetylene |
| CN101249370A (en) * | 2008-04-03 | 2008-08-27 | 上海穗杉实业有限公司 | Voltage transformation adsorption method for circulation valuable gas |
| CN103357242A (en) * | 2013-07-03 | 2013-10-23 | 中国海洋石油总公司 | Method for purifying and removing chlorides contained in chlorine-containing industrial mixed gas and recovering light hydrocarbon |
| CN105935537A (en) * | 2016-04-19 | 2016-09-14 | 杨皓 | Process for purifying chlorosilane and hydrogen chloride with hydrogen mixed gas |
| CN109012015A (en) * | 2018-07-09 | 2018-12-18 | 天吉人吉环保节能（苏州）有限公司 | A kind of chlorinated organics low energy consumption recovery process of chloride containing organic matter gaseous mixture |
Non-Patent Citations (1)
| Title |
|---|
| 张顺泽等: "《分离工程》", 31 October 2011, 中国矿业大学出版社 * |
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