CN105688591B - Cyclohexanol production device hydrogen containing tail gas recycles technique - Google Patents
Cyclohexanol production device hydrogen containing tail gas recycles technique Download PDFInfo
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- CN105688591B CN105688591B CN201610049926.9A CN201610049926A CN105688591B CN 105688591 B CN105688591 B CN 105688591B CN 201610049926 A CN201610049926 A CN 201610049926A CN 105688591 B CN105688591 B CN 105688591B
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- cyclohexanol
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/506—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification at low temperatures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/508—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by selective and reversible uptake by an appropriate medium, i.e. the uptake being based on physical or chemical sorption phenomena or on reversible chemical reactions
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C35/00—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a ring other than a six-membered aromatic ring
- C07C35/02—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a ring other than a six-membered aromatic ring monocyclic
- C07C35/08—Compounds having at least one hydroxy or O-metal group bound to a carbon atom of a ring other than a six-membered aromatic ring monocyclic containing a six-membered rings
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Abstract
The invention belongs to a kind of cyclohexanol production device hydrogen containing tail gas to recycle technique, the following steps are included: the hydrogen containing tail gas that cyclohexanol production device is generated is sent into gas-liquid separator, the gas that gas-liquid separator separates are gone out is through compressor compresses 0.8MPa, it is cooled to 8-12 DEG C, it finally enters filter separator and obtains waste liquid and raw hydrogen, raw hydrogen is obtained into product hydrogen after adsorption tower adsorbs.Filter separator obtains waste collection into sump tank, after settle and separate goes out moisture, by organic phase after accurate filter filters, is warming up to 120-140 DEG C, is then fed into desulfurizing tower, carries out cooling being sent to cyclohexanol production device and using as raw material later.The moisture and impurity in the tail gas of cyclohexanol production device hydrogenation reaction system outlet can be efficiently separated, and has recycled the ingredients such as benzene, cyclohexene and hexamethylene in tail gas well, cyclohexanol production device dehydrating tower can be returned to after the present invention and is recycled.
Description
Technical field
The invention belongs to partial hydrogenation of benzene to produce cyclohexanol technical field, and in particular to a kind of cyclohexanol production device is hydrogeneous
Tail gas recycle utilizes technique.
Background technique
Currently, comparing preferably partial hydrogenation of benzene technique production cyclohexanol in cyclohexanol production, but using the ring of this method
Hexanol process units is larger to the consumption of hydrogen, and annual hydrogen usage reaches tens million of standard cubes, and directly buy
Hydrogen unit price is about 2 yuan/standard cube, nearly hundred million yuan of 1 year hydrogen consumption expense, and hydrogen gas production cost is high.And simultaneously
The tail gas of cyclohexanol production device hydrogenation reaction system outlet hydrogen containing 95vol% is immediately discharged to torch burning, causes greatly
Waste.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide one kind can be effectively to cyclohexanol production device outlet
The cyclohexanol production device hydrogen containing tail gas that hydrogen in hydrogen containing tail gas is recycled recycles technique.
To achieve the above object, the present invention is a kind of cyclohexanol production device hydrogen containing tail gas recycling benefit using technical solution
With technique, comprising the following steps: the hydrogen containing tail gas for generating (partial hydrogenation of benzene) cyclohexanol production device is sent into gas-liquid separator,
The gas that gas-liquid separator separates are gone out first is cooled to 40-45 through water recirculator through compressor compresses to 0.7-0.8MPa
DEG C, it is cooled to 8-12 DEG C using chilled brine cooler, filter separator is finally entered and obtains waste liquid and raw hydrogen, by thick hydrogen
Gas obtains product hydrogen after adsorption tower adsorbs.Filter separator obtains waste collection into sump tank, and settle and separate goes out moisture
Afterwards, by organic phase after accurate filter filters, it is warming up to 120-140 DEG C, is then fed into desulfurizing tower, cooling is carried out later and is sent to
Cyclohexanol production device is used as raw material.
The beneficial effect comprise that: it is combined by using cryogenic separation and absorption, hexamethylene can be efficiently separated
Moisture and impurity in the tail gas of alcohol production device hydrogenation reaction system outlet, and benzene, hexamethylene in tail gas have been recycled well
The ingredients such as alkene and hexamethylene can return to cyclohexanol production device dehydrating tower after the present invention and recycle.
Detailed description of the invention
Fig. 1 is the process flow chart of embodiment 1.
Specific embodiment
The present invention is further explained in the light of specific embodiments, and but the scope of the present invention is not limited thereto.
Embodiment 1
A kind of cyclohexanol production device hydrogen containing tail gas recycling technique, comprising the following steps: by cyclohexanol production device
The hydrogen containing tail gas (0.40MPa ,≤40 DEG C) of generation is sent into gas-liquid separator, mechanical drop therein is separated, by gas-liquid separation
The gas that device is isolated is cooled to 40 DEG C through compressor compresses 0.8MPa, through water recirculator, cooling using chilled brine
Device is cooled to 8 DEG C (being separated by filtration device at this temperature may separate out the impurity such as a large amount of cyclohexene, hexamethylene and benzene), most laggard
Enter filter separator to obtain waste liquid and raw hydrogen (there are also the impurity groups such as micro cyclohexene, hexamethylene, benzene in raw hydrogen at this time
Point), raw hydrogen is removed into the impurity such as micro cyclohexene, hexamethylene, benzene through adsorption tower, obtains product hydrogen.Filter separator
It obtains waste liquid (mainly containing benzene, cyclohexene and hexamethylene) to collect into sump tank, after settle and separate goes out moisture, by organic phase through essence
After the filtering of close filter, be warming up to 120 DEG C through middle pressure steam preheater, be then fed into desulfurizing tower (filling activated alumina ball and
Palladium catalyst) it carries out desulfurization and removes iron rust and dust, it is cooling through water recirculator after desulfurizing tower discharge, liquid is returned to
Cyclohexanol production device dehydrating tower is recycled.
Adsorption tower and desulfurizing tower in the present embodiment are two, wherein one is in adsorbed state, and another is in
Reproduced state.
The filler in adsorption tower in the present embodiment is upper layer and lower layer, and upper layer is activated carbon+synthetic fibers, for removing
The impurity such as hexamethylene, cyclohexene and benzene；Lower layer is activated alumina, and specification is Φ 3-5, for removing free water.
Embodiment 2
Embodiment 2 difference from example 1 is that, gas-liquid separator separates go out gas through compressor compresses
0.7MPa, is cooled to 45 DEG C through water recirculator, is cooled to 12 DEG C using chilled brine heat exchanger；Organic phase is through accurate mistake
After filter filtering, 140 DEG C are warming up to through middle pressure steam preheater.
Embodiment 3
Embodiment 3 difference from example 1 is that, gas-liquid separator separates go out gas through compressor compresses
0.7MPa, is cooled to 42 DEG C through water recirculator, is cooled to 10 DEG C using chilled brine heat exchanger；Organic phase is through accurate mistake
After filter filtering, 130 DEG C are warming up to through middle pressure steam preheater.
Claims (1)
1. a kind of cyclohexanol production device hydrogen containing tail gas recycles technique, which comprises the following steps: by cyclohexanol
The hydrogen containing tail gas that process units generates is sent into gas-liquid separator, separates mechanical drop therein, gas-liquid separator separates are gone out
Gas through compressor compresses to 0.7-0.8MPa, be cooled to 8-12 DEG C, finally enter filter separator and obtain waste liquid and thick
Raw hydrogen is removed the micro impurity based on cyclohexene, hexamethylene, benzene after adsorption tower adsorbs, obtains product hydrogen by hydrogen
Gas；The waste liquid that filter separator obtains mainly contains benzene, cyclohexene and hexamethylene, by waste collection into sump tank, settle and separate
Out after moisture, by organic phase after accurate filter filters, be warming up to 120-140 DEG C, be then fed into desulfurizing tower, carry out desulfurization and
Iron rust and dust are removed, carries out cooling being sent to cyclohexanol production device and using as raw material later；
Wherein, the step of gas is cooled to 8-12 DEG C through compressor compresses to 0.7-0.8MPa is as follows: first through circulating water
Device is cooled to 40-45 DEG C, is cooled to 8-12 DEG C using chilled brine cooler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610049926.9A CN105688591B (en) | 2016-01-26 | 2016-01-26 | Cyclohexanol production device hydrogen containing tail gas recycles technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610049926.9A CN105688591B (en) | 2016-01-26 | 2016-01-26 | Cyclohexanol production device hydrogen containing tail gas recycles technique |
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| CN105688591A CN105688591A (en) | 2016-06-22 |
| CN105688591B true CN105688591B (en) | 2019-03-15 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109908700B (en) * | 2017-12-12 | 2021-09-07 | 万华化学集团股份有限公司 | Tail gas recovery system and method for neopentyl glycol production device |
| CN110013735B (en) * | 2018-01-09 | 2022-07-05 | 中国石油化工股份有限公司 | Safe adsorption treatment device and method for hydrogen-containing purge gas |
| CN110013758B (en) * | 2018-01-09 | 2022-05-03 | 中国石油化工股份有限公司 | Safe recycling and treating method for hydrogenation tail gas in hydrogenation reaction device |
| CN110013733B (en) * | 2018-01-09 | 2022-05-03 | 中国石油化工股份有限公司 | Device and method for VOC adsorption and tail hydrogen safety treatment of purge gas of aromatic hydrogenation system |
| CN108147939A (en) * | 2018-01-25 | 2018-06-12 | 重庆华峰化工有限公司 | A kind of recovery method of cyclohexene hydrating process and its hydrogen containing tail gas |
| CN111439725B (en) * | 2020-03-21 | 2021-02-19 | 河南神马尼龙化工有限责任公司 | Hydrogen desulfurization system for device for producing cyclohexanol by partial hydrogenation of benzene and desulfurization method thereof |
| CN111548244A (en) * | 2020-05-11 | 2020-08-18 | 江苏中能化学科技股份有限公司 | Method for recovering benzene and high-purity hydrogen in high yield from tail gas of biphenyl preparation process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104677053A (en) * | 2015-01-30 | 2015-06-03 | 北方华锦化学工业集团有限公司 | Method for recycling hydrogen in ethylbenzene dehydrogenation waste gas |
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- 2016-01-26 CN CN201610049926.9A patent/CN105688591B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104677053A (en) * | 2015-01-30 | 2015-06-03 | 北方华锦化学工业集团有限公司 | Method for recycling hydrogen in ethylbenzene dehydrogenation waste gas |
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Inventor after: Wang Liushuan Inventor after: Li Yingchun Inventor after: Hu Xiaojing Inventor after: Yu Changjiang Inventor after: Liu Yanchao Inventor after: Jia Yaping Inventor after: Lv Yang Inventor after: Lin Jingyan Inventor after: Wang Maijian Inventor after: Ning Yongliang Inventor after: Li Jinyou Inventor after: Liu Guoliang Inventor after: E Zhi Inventor after: Ma Xiping Inventor after: Wu Xianghong Inventor after: Li Shen Inventor after: Yao Yong Inventor after: Wei Xinjun Inventor after: Pan Aijun Inventor after: Zhou Xusheng Inventor after: Li Zhongqiang Inventor after: Cheng Yuanming Inventor after: Ning Hongjun Inventor before: Wang Liushuan Inventor before: Li Yingchun Inventor before: Hu Xiaojing Inventor before: Yu Changjiang Inventor before: Liu Yanchao Inventor before: Jia Yaping Inventor before: Liu Guoliang Inventor before: Yao Yong Inventor before: Wei Xinjun Inventor before: Pan Aijun Inventor before: Zhou Xusheng Inventor before: Li Zhongqiang Inventor before: Cheng Yuanming Inventor before: Ning Hongjun |
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Effective date of registration: 20230625 Address after: 467000 the development zone of the east section of Jianshe Road, Pingdingshan, Henan. Patentee after: HENAN SHENMA NYLON CHEMICAL Co.,Ltd. Address before: 467000 high tech Development Zone, east section of Jianshe Road, Pingdingshan City, Henan Province Patentee before: PINGDINGSHAN SHENMA WANLI CHEMICAL Co.,Ltd. |