CN105688591A - Hydrogen-containing tail gas recycling process of cyclohexanol production device - Google Patents
Hydrogen-containing tail gas recycling process of cyclohexanol production device Download PDFInfo
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- CN105688591A CN105688591A CN201610049926.9A CN201610049926A CN105688591A CN 105688591 A CN105688591 A CN 105688591A CN 201610049926 A CN201610049926 A CN 201610049926A CN 105688591 A CN105688591 A CN 105688591A
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- cyclohexanol production
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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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to a hydrogen-containing tail gas recycling process of a cyclohexanol production device. The hydrogen-containing tail gas recycling process comprises the following steps: conveying hydrogen-containing tail gas generated by the cyclohexanol production device into a gas-liquid separator, and compressing the gas separated from the gas-liquid separator to be 0.8MPa by a compressor; then cooling the gas to 8 DEG C to 12 DEG C; finally, enabling the gas to enter a filtering separator to obtain waste liquid and crude hydrogen gas, and adsorbing the crude hydrogen gas by an adsorption tower to obtain product hydrogen gas; collecting waste liquid obtained by the filtering separator to a waste oil tank, and standing and separating out water; filtering an organic phase with a fine filter, and heating to 120 DEG C to 140 DEG C; then conveying the organic phase into a desulfurizing tower, and then cooling and conveying the organic phase to the cyclohexanol production device to be used as the raw material. With the adoption of the hydrogen-containing tail gas recycling process of the cyclohexanol production device, moisture and impurities in the tail gas exhausted by a hydrogenation reaction system of the cyclohexanol production device can be effectively separated, and components including benzene, cyclohexene, cyclohexane and the like in the tail gas are recycled very well; with the adoption of the process, the tail gas can be returned back to a dehydration tower of the cyclohexanol production device to be recycled.
Description
Technical field
The invention belongs to partial hydrogenation of benzene and produce Hexalin technical field, be specifically related to a kind of cyclohexanol production device hydrogen containing tail gas and recycle technique。
Background technology
At present, cyclohexanol production compares preferably partial hydrogenation of benzene explained hereafter Hexalin, but the cyclohexanol production device adopting this method is bigger to the consumption of hydrogen, annual hydrogen usage reaches tens million of standard cube, and the hydrogen unit price directly bought is about 2 yuan/standard cube, the hydrogen consumption expense of 1 year nearly hundred million yuan, hydrogen gas production cost remains high。And simultaneously arrange the tail gas containing 95vol% hydrogen outside cyclohexanol production device hydrogenation reaction system and be immediately discharged to torch burning, cause great waste。
Summary of the invention
It is an object of the invention to for the deficiencies in the prior art, it is provided that a kind of cyclohexanol production device hydrogen containing tail gas that can effectively the hydrogen in row's hydrogen containing tail gas outside cyclohexanol production device be recycled recycles technique。
For achieving the above object, the present invention adopts the technical scheme to be, a kind of cyclohexanol production device hydrogen containing tail gas recycles technique, comprise the following steps: the hydrogen containing tail gas produced by (partial hydrogenation of benzene) cyclohexanol production device sends into gas-liquid separator, gas gas-liquid separator separates gone out is compressed to 0.7-0.8MPa through compressor, first it is cooled to 40-45 DEG C through water recirculator, it is cooled to 8-12 DEG C then through chilled brine cooler, finally enter filter separator and obtain waste liquid and raw hydrogen, raw hydrogen is obtained product hydrogen after adsorption tower adsorbs。Filter separator obtains waste collection to sump tank, after standing separation goes out moisture, by organic facies after accurate filter filters, is warming up to 120-140 DEG C, is then fed into desulfurizing tower, carries out cooling afterwards and is sent to cyclohexanol production device as raw material use。
The beneficial effect comprise that: by adopting cryogenic separation and Adsorption Phase to combine, the moisture that can efficiently separate outside cyclohexanol production device hydrogenation reaction system in the tail gas of row and impurity, and well reclaimed the compositions such as the benzene in tail gas, cyclohexene and hexamethylene, cyclohexanol production device dehydrating tower can be returned to after the present invention and be circulated utilization。
Accompanying drawing explanation
Fig. 1 is the process chart of embodiment 1。
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, but protection scope of the present invention is not limited to this。
Embodiment 1
A kind of cyclohexanol production device hydrogen containing tail gas recycles technique, comprise the following steps: the hydrogen containing tail gas (0.40MPa that cyclohexanol production device is produced, ≤ 40 DEG C) send into gas-liquid separator, separate machinery drop therein, gas gas-liquid separator separates gone out compresses 0.8MPa through compressor, it is cooled to 40 DEG C through water recirculator, it is cooled to 8 DEG C then through chilled brine cooler (to be separated by filtration device at this temperature and may separate out a large amount of cyclohexene, the impurity such as hexamethylene and benzene), finally enter filter separator to obtain waste liquid and raw hydrogen and (now in raw hydrogen, also have the cyclohexene of trace, hexamethylene, the impurity compositions such as benzene), raw hydrogen is removed through adsorption tower the cyclohexene of trace, hexamethylene, the impurity such as benzene, obtain product hydrogen。Filter separator obtains waste liquid (mainly containing benzene, cyclohexene and hexamethylene) and collects to sump tank, after standing separation goes out moisture, by organic facies after accurate filter filters, it is warming up to 120 DEG C through middle pressure steam preheater, it is then fed into desulfurizing tower (filling activated alumina ball and palladium catalyst) carry out desulfurization and remove rust and dust, cool down through water recirculator after discharging from desulfurizing tower, liquid is returned to cyclohexanol production device dehydrating tower and is circulated utilization。
Adsorption tower and desulfurizing tower in the present embodiment are two, and wherein one is in adsorbed state, and another is in reproduced state。
The filler in adsorption tower in the present embodiment is upper and lower two-layer, and upper strata is activated carbon+synthetic fibers, is used for removing the impurity such as hexamethylene, cyclohexene and benzene；Lower floor is activated alumina, and specification is Φ 3-5, is used for removing free water。
Embodiment 2
Embodiment 2 and embodiment 1 are different in that, the gas that gas-liquid separator separates goes out compresses 0.7MPa through compressor, is cooled to 45 DEG C through water recirculator, is cooled to 12 DEG C then through chilled brine heat exchanger；Organic facies, after accurate filter filters, is warming up to 140 DEG C through middle pressure steam preheater。
Embodiment 3
Embodiment 3 and embodiment 1 are different in that, the gas that gas-liquid separator separates goes out compresses 0.7MPa through compressor, is cooled to 42 DEG C through water recirculator, is cooled to 10 DEG C then through chilled brine heat exchanger；Organic facies, after accurate filter filters, is warming up to 130 DEG C through middle pressure steam preheater。
Claims (3)
1. a cyclohexanol production device hydrogen containing tail gas recycles technique, it is characterized in that, comprise the following steps: the hydrogen containing tail gas produced by cyclohexanol production device sends into gas-liquid separator, gas gas-liquid separator separates gone out is compressed to 0.7-0.8MPa through compressor, it is cooled to 8-12 DEG C, finally enter filter separator and obtain waste liquid and raw hydrogen, raw hydrogen is obtained product hydrogen after adsorption tower adsorbs。
2. cyclohexanol production device hydrogen containing tail gas as claimed in claim 1 recycles technique, it is characterized in that, filter separator obtains waste collection to sump tank, after standing separation goes out moisture, by organic facies after accurate filter filters, it is warming up to 120-140 DEG C, is then fed into desulfurizing tower, carry out cooling afterwards and be sent to cyclohexanol production device as raw material use。
3. cyclohexanol production device hydrogen containing tail gas as claimed in claim 1 recycles technique, it is characterized in that, gas compression is as follows to the 0.7-0.8MPa step being cooled to 8-12 DEG C: is first cooled to 40-45 DEG C through water recirculator, is cooled to 8-12 DEG C then through 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 |
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| 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 true CN105688591A (en) | 2016-06-22 |
| CN105688591B CN105688591B (en) | 2019-03-15 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109908700A (en) * | 2017-12-12 | 2019-06-21 | 万华化学集团股份有限公司 | A kind of exhaust gas recovery system and method for neopentyl glycol process units |
| CN110013758A (en) * | 2018-01-09 | 2019-07-16 | 中国石油化工股份有限公司 | Hydrogenated tail gas safe reuse and processing method in hydrogenation apparatus |
| CN110013735A (en) * | 2018-01-09 | 2019-07-16 | 中国石油化工股份有限公司 | The safe absorbing treatment device and method of hydrogeneous periodic off-gases |
| CN110013733A (en) * | 2018-01-09 | 2019-07-16 | 中国石油化工股份有限公司 | Aromatic hydrogenation system periodic off-gases VOC absorption and tail hydrogen secure processing device and method |
| CN111439725A (en) * | 2020-03-21 | 2020-07-24 | 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 |
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| 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 |
-
2016
- 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 |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109908700A (en) * | 2017-12-12 | 2019-06-21 | 万华化学集团股份有限公司 | A kind of exhaust gas recovery system and method for neopentyl glycol process units |
| 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 |
| CN110013758A (en) * | 2018-01-09 | 2019-07-16 | 中国石油化工股份有限公司 | Hydrogenated tail gas safe reuse and processing method in hydrogenation apparatus |
| CN110013735A (en) * | 2018-01-09 | 2019-07-16 | 中国石油化工股份有限公司 | The safe absorbing treatment device and method of hydrogeneous periodic off-gases |
| CN110013733A (en) * | 2018-01-09 | 2019-07-16 | 中国石油化工股份有限公司 | Aromatic hydrogenation system periodic off-gases VOC absorption and tail hydrogen secure processing device and method |
| 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 |
| 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 |
| 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 |
| 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 |
| CN111439725A (en) * | 2020-03-21 | 2020-07-24 | 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 |
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| CN105688591B (en) | 2019-03-15 |
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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. |