CN205774212U - The device of removing impurities matter butylcyclohexyl ether in process of cyclohexanone production - Google Patents

The device of removing impurities matter butylcyclohexyl ether in process of cyclohexanone production Download PDF

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Publication number
CN205774212U
CN205774212U CN201620707871.1U CN201620707871U CN205774212U CN 205774212 U CN205774212 U CN 205774212U CN 201620707871 U CN201620707871 U CN 201620707871U CN 205774212 U CN205774212 U CN 205774212U
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debutylize
hexamethylene
ether tower
tower
hexamethylene ether
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王昌飞
虞新建
罗建国
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Hunan Baili Engineering Sci & Tech Co ltd
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Hunan Baili Engineering Sci & Tech Co ltd
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Abstract

The utility model discloses the device of removing impurities matter butylcyclohexyl ether in a kind of process of cyclohexanone production, be mainly made up of Hexalin vaporizer, gas-liquid separator, debutylize hexamethylene ether tower feed pump, debutylize hexamethylene ether tower, debutylize hexamethylene ether tower cooler device, debutylize hexamethylene ether tower return tank, debutylize hexamethylene ether tower reflux pump, debutylize hexamethylene ether tower reactor pump, debutylize hexamethylene ether tower reactor reboiler.This utility model uses the rectification mode of air-distillation or malleation to remove the butylcyclohexyl ether in Hexalin, prevent butylcyclohexyl ether in the accumulation of whole production system, it also avoid butylcyclohexyl ether circulating load in systems excessive simultaneously, increase system energy consumption problem, steam consumption 5% can be reduced, cooling-water consumption 5%, has significant economic benefit.

Description

The device of removing impurities matter butylcyclohexyl ether in process of cyclohexanone production
Technical field
This utility model belongs to chemical technology field, relates to removing impurities matter butylcyclohexyl ether in a kind of process of cyclohexanone production Device.
Background technology
Ketohexamethylene is a kind of important Organic Chemicals.In China, the Ketohexamethylene of 65% is as producing the former of caprolactam Material, the Ketohexamethylene of 20% is as the raw material of production adipic acid, and remaining Ketohexamethylene is as relevant industrial chemicals.It addition, Ketohexamethylene is also It is excellent solvent, can be used as painting nitrocellulose, vinyl chloride-base polymer and the solvent of copolymer.Along with China's chemical fibre industry Developing rapidly, caprolactam, adipic acid yield increase year by year, and the demand of Ketohexamethylene the most all increases, and exploitation prospect is wide Wealthy.
At present, produce Ketohexamethylene technique and mainly have cyclohexane oxidation process and cyclohexene hydration method.Cyclohexane oxidation technique is Prevailing technology both at home and abroad, although cyclohexene hydration method Ketohexamethylene technique is risen now, but due to cyclohexene hydration method by-product hexamethylene Alkane, the producer having now cyclohexene hydration subtraction unit is considering that newly-built cyclohexane oxidation subtraction unit digestion cyclohexene hydration method is secondary The hexamethylene produced, the most beneficially comprehensive utilization of resources, make conventional industries shine new machine.
In process of cyclohexanone production, owing to cyclohexane oxidation generates cyclohexyl hydroperoxide, cyclohexyl hydroperoxide decomposes During produce by-product butylcyclohexyl ether, cannot remove during follow-up rectification always, butylcyclohexyl ether is with Hexalin Entering cyclohexanol dehydrogenation response system together, in cyclohexanol dehydrogenation is reacted, butylcyclohexyl ether is not involved in reaction, last and dehydrogenation Product returns to the most again alcohol ketone (alcohol ketone refers to Hexalin and Ketohexamethylene, lower same) refining system, such butylcyclohexyl ether Refine at alcohol ketone and circulate between cyclohexanol dehydrogenation response system always, cause butylcyclohexyl ether constantly to be accumulated in system, dense Spend more and more higher, finally affect cyclohexanol dehydrogenation reaction efficiency and alcohol ketone purification operations pressure stability, and increase public work Consume;When the mass concentration of alcohol column overhead cyclohexanone Yu butylcyclohexyl ether reaches 5%, will have a strong impact on dehydrogenation reaction with Alcohol ketone refining system, ultimately results in parking, and the mass concentration of alcohol column overhead ketone can be by controlling in ketone tower bottom extraction material The content of ketone, and butylcyclohexyl ether mass concentration cannot control in existing apparatus.
This utility model is the device of removing impurities matter butylcyclohexyl ether in a kind of process of cyclohexanone production, is processed by this device Butylcyclohexyl ether content in systems will be reduced, it is to avoid butylcyclohexyl ether accumulation in systems, reduce the public affairs of system Use engineering consumption, reduce the operating cost of device, and reduce stop frequency, extend the cycle of operation of device.From energy-conservation, economical Upper and stable operation runs certain meaning.
Summary of the invention
This utility model purpose is to provide the device of removing impurities matter butylcyclohexyl ether in a kind of process of cyclohexanone production, passes through This device processes and reduces butylcyclohexyl ether content in systems, it is to avoid butylcyclohexyl ether accumulation in systems, fall The low public work consumption of system, reduces the operating cost of device, and reduces stop frequency, extends the operation week of device Phase.From energy-conservation, economically and stable operation run have certain meaning.
The technical solution of the utility model is:
In a kind of process of cyclohexanone production, the device of removing impurities matter butylcyclohexyl ether, is mainly divided by Hexalin vaporizer, gas-liquid From tank, debutylize hexamethylene ether tower feed pump, debutylize hexamethylene ether tower, debutylize hexamethylene ether tower cooler device, debutylize hexamethylene ether tower Return tank, debutylize hexamethylene ether tower reflux pump, debutylize hexamethylene ether tower reactor pump, debutylize hexamethylene ether tower reactor reboiler form;Ring The outlet of hexanol tower reflux pump is connected with Hexalin evaporator, and Hexalin evaporator outlet connects with knockout drum, gas-liquid Knockout drum top gas phase outlet be connected with cyclohexanol dehydrogenation reactor, bottom liquid phases export respectively with Hexalin tower and debutylize ring Hexyl ether tower feed pump connects, and debutylize hexamethylene ether tower feed pump is connected in the middle part of debutylize hexamethylene ether tower, debutylize hexamethylene ether tower Top gas phase outlet is connected with debutylize hexamethylene ether tower condenser and cyclohexanol dehydrogenation reactor respectively, and debutylize hexamethylene ether tower is cold Condenser outlet is connected with debutylize hexamethylene ether tower return tank, and the outlet of debutylize hexamethylene ether tower return tank is returned with debutylize hexamethylene ether tower Stream pump inlet is connected, and the outlet of debutylize hexamethylene ether tower reflux pump is connected, at debutylize hexamethylene ether with debutylize hexamethylene ether tower top Tower reactor is connected with debutylize hexamethylene ether tower reactor reboiler, and debutylize hexamethylene ether tower reactor pump inlet is connected with debutylize hexamethylene ether tower reactor, Debutylize hexamethylene ether tower reactor pump inlet is connected with X oil tank, and the connection between described each equipment is that pipeline connects.
Using said apparatus debutylize hexamethylene ether method, the operation pressure of debutylize hexamethylene ether tower is that 100-180 KPa(is exhausted Pressure, lower same), tower reactor operation temperature is 160-200 DEG C, and tower reactor reboiler uses middle pressure steam or high steam as thermal source, ring Hexanol top of tower reflux pump discharge ring hexanol material is through Hexalin evaporator evaporation, liquid phase conduct after knockout drum separates The charging of debutylize hexamethylene ether tower, utilizes Hexalin and butylcyclohexyl ether relative volatility in 100-180 KPa pressure limit Difference, by rectification mode, butylcyclohexyl ether is separated from Hexalin, debutylize hexamethylene ether top gaseous phase material one Part is directly entered cyclohexanol dehydrogenation reactor, and another part refluxes after debutylize hexamethylene ether tower cooler device cools down;De-fourth Extraction material at the bottom of basic ring hexyl ether tower tower is the butylcyclohexyl ether containing finite concentration Hexalin, by debutylize hexamethylene ether tower tower reactor It is pumped to X oil tank sell as side-product.
In this utility model, it is also possible to without Hexalin vaporizer and knockout drum, directly return from Hexalin tower Stream pump draws a pipeline and is connected in the middle part of debutylize hexamethylene ether tower.Concrete technical scheme is: removing impurities in a kind of process of cyclohexanone production The device of matter butylcyclohexyl ether, mainly by debutylize hexamethylene ether tower 1, debutylize hexamethylene ether tower cooler device 2, debutylize hexamethylene ether tower Return tank 3, debutylize hexamethylene ether tower reflux pump 5, debutylize hexamethylene ether tower reactor pump 6, debutylize hexamethylene ether tower reactor reboiler 7 groups Become;The outlet of Hexalin tower reflux pump is connected in the middle part of debutylize hexamethylene ether tower 1, the outlet point of debutylize hexamethylene ether tower 1 top gas phase Not being connected with debutylize hexamethylene ether tower cooler device 2 and cyclohexanol dehydrogenation reactor, the outlet of debutylize hexamethylene ether tower cooler device 2 is with de- Butylcyclohexyl ether tower return tank 3 connects, the outlet of debutylize hexamethylene ether tower return tank 3 and debutylize hexamethylene ether tower reflux pump 5 import Being connected, debutylize hexamethylene ether tower reflux pump 5 exports and is connected with debutylize hexamethylene ether tower 1 top, in debutylize hexamethylene ether tower reactor even Debutylize hexamethylene ether tower reactor reboiler 7, debutylize hexamethylene ether tower reactor pump 6 import is had to be connected with debutylize hexamethylene ether tower reactor, de-fourth Basic ring hexyl ether tower reactor pump inlet is connected with X oil tank, and the connection between described each equipment is that pipeline connects.
Below the technique of removing impurities matter butylcyclohexyl ether in process of cyclohexanone production is further described:
Use debutylize hexamethylene ether Tower System technological process as it is shown in figure 1, its technical process is as follows:
Entering Hexalin evaporator evaporation from Hexalin tower reflux pump outlet material, vaporizer divides in gas-liquid separator Entering in the middle part of debutylize hexamethylene ether tower from, liquid phase material by flow-control, debutylize hexamethylene ether tower uses air-distillation or just Pressure distillation.Debutylize hexamethylene ether tower gas phase enters debutylize hexamethylene ether tower condenser and is condensed, and condensed fluid enters debutylize hexamethylene Ether tower return tank.The condensed fluid of return tank returns debutylize hexamethylene the most as reflux through debutylize hexamethylene ether tower reflux pump Ether tower.Debutylize hexamethylene ether tower bottoms is the Hexalin solution of butylcyclohexyl ether mass content 25-35%, through debutylize hexamethylene Ether tower reactor pump, delivers to X oil tank and sells as side-product.
Removing butylcyclohexyl ether operating process in this utility model is continuous operation process.
Removing butylcyclohexyl ether operating process in this utility model is batch process procedures.
Feeding butylcyclohexyl ether mass content in Hexalin in this utility model is 1.0%-10.0%.
The preferred 150KPa-170KPa of operation absolute pressure of debutylize hexamethylene ether tower in this utility model.
This utility model uses the rectification mode of air-distillation or malleation to remove the butylcyclohexyl ether in Hexalin, solves Can not realize, in high vacuum distillation process, the difficult problem that butylcyclohexyl ether separates with Hexalin, prevent butylcyclohexyl ether in whole production The accumulation of system, it also avoid butylcyclohexyl ether circulating load in systems excessive simultaneously, increases system energy consumption problem, it is possible to reduce System steam consumption 5%, cooling-water consumption 5%, there is significant economic benefit.Also solve whole production system due to fourth simultaneously The accumulation of basic ring hexyl ether causes the difficult problem that parking processes.
Accompanying drawing explanation
Removing impurities matter butylcyclohexyl ether process chart in Fig. 1, a kind of process of cyclohexanone production;
In figure: 1-debutylize hexamethylene ether tower, 2-debutylize hexamethylene ether tower cooler device, 3-debutylize hexamethylene ether tower return tank, 4-debutylize hexamethylene ether tower feed pump, 5-debutylize hexamethylene ether tower reflux pump, 6-debutylize hexamethylene ether tower reactor pump, 7-debutylize ring Hexyl ether tower reactor reboiler, 8-knockout drum, 9-Hexalin vaporizer
WC-cools down water SH-steam SHC-steam condensate (SC).
Detailed description of the invention
Embodiment 1:
Produce 100000 tons of pimelinketone devices per year, use technological process as shown in Figure 1 to carry out removing butylcyclohexyl ether, debutylize Hexamethylene ether tower operation pressure is 150-170KPa, and tower reactor operation temperature is 180-200 DEG C.
From Hexalin tower reflux pump outlet material, through Hexalin evaporator evaporation, liquid phase after knockout drum separates As the charging of debutylize hexamethylene ether tower, being entered in the middle part of debutylize hexamethylene ether tower by flow-control, debutylize hexamethylene ether tower is adopted With air-distillation or malleation rectification.A debutylize hexamethylene ether tower gas phase part is directly entered dehydrogenation reactor, and another part enters Debutylize hexamethylene ether tower condenser is condensed, and condensed fluid enters debutylize hexamethylene ether tower return tank.The condensed fluid of return tank passes through Debutylize hexamethylene ether tower reflux pump returns debutylize hexamethylene ether tower as reflux, and remainder is sent to Hexalin carburator.De- Butylcyclohexyl ether tower bottoms is the Hexalin solution of butylcyclohexyl ether mass content 25-35%, through debutylize hexamethylene ether tower reactor Pump, delivers to X oil tank and sells as side-product.
In charging, butylcyclohexyl ether mass content is 4% Hexalin, through distillation process, is sent to cyclohexanol dehydrogenation reactor Hexalin in butylcyclohexyl ether content can't check.
In this process of cyclohexanone production, removing impurities matter butylcyclohexyl ether technique institute's heat dissipation source energy reduces by 5% left side than original technique The right side, the original technique of low-temperature receiver observable index reduces about 5%.
Embodiment 2:
Produce the cyclohexane oxidation process preparing cyclohexanone technique of 100,000 tons of pimelinketone devices per year, use technique stream as shown in Figure 1 Cheng Jinhang removes butylcyclohexyl ether, and debutylize hexamethylene ether tower operation pressure is 100-120KPa, and tower reactor operation temperature is 165-175 ℃。
Divide one material pipeline after Hexalin tower reflux pump, enter debutylize hexamethylene ether tower by flow-control Middle part, debutylize hexamethylene ether tower uses air-distillation.Debutylize hexamethylene ether tower gas phase is partly into dehydrogenation reactor, another portion Dividing entrance debutylize hexamethylene ether tower condenser to be condensed, condensed fluid enters debutylize hexamethylene ether tower return tank.The condensation of return tank Liquid returns debutylize hexamethylene ether tower as reflux through debutylize hexamethylene ether tower reflux pump.Debutylize hexamethylene ether tower bottoms is fourth The Hexalin solution of basic ring hexyl ether mass content 25-35%, through debutylize hexamethylene ether tower reactor pump, delivers to X oil tank as side-product Sell.
In charging, butylcyclohexyl ether mass content is 4% Hexalin, through distillation process, is sent to cyclohexanol dehydrogenation reactor Hexalin in butylcyclohexyl ether content 0.5%.
In this process of cyclohexanone production, removing impurities matter butylcyclohexyl ether technique institute's heat dissipation source energy reduces by 4% left side than original technique The right side, the original technique of low-temperature receiver observable index reduces about 4%.
Comparative example 1:
Produce 100000 tons of pimelinketone devices per year, do not remove the distillation system of butylcyclohexyl ether, steam hexamethylene from Hexalin tower Alcohol, at the bottom of tower, extraction X oil, owing to Hexalin tower rectification needs rectification under a high vacuum, can't check butylcyclohexyl ether in X oil at the bottom of tower, Butylcyclohexyl ether enters Hexalin carburator together with Hexalin and goes dehydrogenation reactor system, butylcyclohexyl ether to return to the most again essence Evaporate system, circulate the most in systems, constantly accumulate.

Claims (2)

1. the device of removing impurities matter butylcyclohexyl ether in a process of cyclohexanone production, it is characterised in that: mainly evaporated by Hexalin Device (9), knockout drum (8), debutylize hexamethylene ether tower feed pump (4), debutylize hexamethylene ether tower (1), debutylize hexamethylene ether tower Cooler (2), debutylize hexamethylene ether tower return tank (3), debutylize hexamethylene ether tower reflux pump (5), debutylize hexamethylene ether tower reactor pump (6), debutylize hexamethylene ether tower reactor reboiler (7) composition;The outlet of Hexalin tower reflux pump is with Hexalin vaporizer (9) import even Connecing, Hexalin vaporizer (9) outlet connects with knockout drum (8), and the outlet of knockout drum (8) top gas phase takes off with Hexalin Hydrogen reactor connects, and bottom liquid phases outlet is connected with Hexalin tower and debutylize hexamethylene ether tower feed pump (4) respectively, debutylize ring Hexyl ether tower feed pump (4) is connected with debutylize hexamethylene ether tower (1) middle part, and the outlet of debutylize hexamethylene ether tower (1) top gas phase is respectively Be connected with debutylize hexamethylene ether tower cooler device (2) and cyclohexanol dehydrogenation reactor, debutylize hexamethylene ether tower cooler device (2) outlet with Debutylize hexamethylene ether tower return tank (3) connects, debutylize hexamethylene ether tower return tank (3) outlet and debutylize hexamethylene ether tower reflux pump (5) import is connected, and debutylize hexamethylene ether tower reflux pump (5) outlet is connected, at debutylize ring with debutylize hexamethylene ether tower (1) top Hexyl ether tower reactor is connected with debutylize hexamethylene ether tower reactor reboiler (7), debutylize hexamethylene ether tower reactor pump (6) import and debutylize hexamethylene ether Tower reactor connects, and debutylize hexamethylene ether tower reactor pump inlet is connected with X oil tank, and the connection between described each equipment is that pipeline connects.
The device of removing impurities matter butylcyclohexyl ether in process of cyclohexanone production the most according to claim 1, it is characterised in that: main Will be by debutylize hexamethylene ether tower (1), debutylize hexamethylene ether tower cooler device (2), debutylize hexamethylene ether tower return tank (3), debutylize Hexamethylene ether tower reflux pump (5), debutylize hexamethylene ether tower reactor pump (6), debutylize hexamethylene ether tower reactor reboiler (7) form;Hexalin The outlet of tower reflux pump is connected with debutylize hexamethylene ether tower (1) middle part, and the outlet of debutylize hexamethylene ether tower (1) top gas phase is respectively with de- Butylcyclohexyl ether tower cooler device (2) is connected with cyclohexanol dehydrogenation reactor, and debutylize hexamethylene ether tower cooler device (2) exports and takes off fourth Basic ring hexyl ether tower return tank (3) connects, debutylize hexamethylene ether tower return tank (3) outlet and debutylize hexamethylene ether tower reflux pump (5) Import is connected, and debutylize hexamethylene ether tower reflux pump (5) outlet is connected, at debutylize hexamethylene with debutylize hexamethylene ether tower (1) top Ether tower reactor is connected with debutylize hexamethylene ether tower reactor reboiler (7), debutylize hexamethylene ether tower reactor pump (6) import and debutylize hexamethylene ether tower Still connects, and debutylize hexamethylene ether tower reactor pump inlet is connected with X oil tank, and the connection between described each equipment is that pipeline connects.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108707065A (en) * 2018-08-10 2018-10-26 平顶山市神马万里化工股份有限公司 The method and its device of dicyclohexyl ether are extracted from cyclohexanol distillation residual liquid
CN111662160A (en) * 2019-03-06 2020-09-15 中国石油化工股份有限公司 Method for improving productivity of cyclohexanol dehydrogenation device
CN112521256A (en) * 2019-09-18 2021-03-19 中国石油化工股份有限公司 Method for efficiently separating cyclohexanone and removing impurities in cyclohexanol
CN114315522A (en) * 2021-12-31 2022-04-12 昌德新材科技股份有限公司 Method for purifying cyclohexanol and method for producing cyclohexanone
CN114920624A (en) * 2022-05-27 2022-08-19 辽宁石油化工大学 Separation and purification method and system for cyclohexanol and butyl cyclohexyl ether

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108707065A (en) * 2018-08-10 2018-10-26 平顶山市神马万里化工股份有限公司 The method and its device of dicyclohexyl ether are extracted from cyclohexanol distillation residual liquid
CN108707065B (en) * 2018-08-10 2021-10-08 平顶山市神马万里化工股份有限公司 Method and device for extracting dicyclohexyl ether from cyclohexanol rectification residual liquid
CN111662160A (en) * 2019-03-06 2020-09-15 中国石油化工股份有限公司 Method for improving productivity of cyclohexanol dehydrogenation device
CN111662160B (en) * 2019-03-06 2024-04-12 中国石油化工股份有限公司 Method for improving productivity of cyclohexanol dehydrogenation device
CN112521256A (en) * 2019-09-18 2021-03-19 中国石油化工股份有限公司 Method for efficiently separating cyclohexanone and removing impurities in cyclohexanol
CN112521256B (en) * 2019-09-18 2024-03-12 中国石油化工股份有限公司 Method for efficiently separating cyclohexanone and removing impurities in cyclohexanol
CN114315522A (en) * 2021-12-31 2022-04-12 昌德新材科技股份有限公司 Method for purifying cyclohexanol and method for producing cyclohexanone
CN114315522B (en) * 2021-12-31 2024-02-13 昌德新材科技股份有限公司 Purification method of cyclohexanol and preparation method of cyclohexanone
CN114920624A (en) * 2022-05-27 2022-08-19 辽宁石油化工大学 Separation and purification method and system for cyclohexanol and butyl cyclohexyl ether

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