CN219579904U - Recovery device for ethanol as byproduct of coal glycol synthesis - Google Patents
Recovery device for ethanol as byproduct of coal glycol synthesis Download PDFInfo
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- CN219579904U CN219579904U CN202320597691.2U CN202320597691U CN219579904U CN 219579904 U CN219579904 U CN 219579904U CN 202320597691 U CN202320597691 U CN 202320597691U CN 219579904 U CN219579904 U CN 219579904U
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Abstract
The utility model discloses a recovery device for ethanol which is a byproduct of coal glycol synthesis, which comprises an ethanol recovery tower, wherein the coal glycol byproduct is fed from the middle part of the ethanol recovery tower, a gas phase outlet at the top of the ethanol recovery tower is connected to an ethanol reflux tank through a first condenser, the ethanol reflux tank is connected to a reflux inlet at the upper part of the ethanol recovery tower (1) through a pipeline and a pump, the other part of the ethanol reflux tank is connected to an ethanol extraction storage tank, the bottom of the ethanol recovery tower is also respectively connected with a reboiler and a liquid phase extraction pipe, and the gas phase outlet of the reboiler enters the tower from the lower end of the ethanol recovery tower. The device can separate 99.5% ethanol products meeting the first grade standard of GB/T6820-2016 industrial ethanol from the coal glycol byproducts through continuous vacuum rectification separation, and the impurity alcohol after ethanol recovery is extracted from the tower bottom and sent to the terminal sewage as a carbon source required by the activated sludge of a biochemical sewage tank; the economic benefit of the coal-to-glycol project is improved.
Description
Technical Field
The utility model relates to the technical field of coal-to-ethylene glycol production, in particular to recovery of ethanol which is a byproduct of coal-to-ethylene glycol.
Background
Dimethyl oxalate (DMO) is recycled to H in the synthesis process of coal-to-glycol 2 Gasifying and mixing, and then entering an Ethylene Glycol (EG) synthesis reactor, and carrying out two-step hydrogenation under the action of a catalyst Cu to generate EG. The first step is to produce intermediate products methyl glycolate MG and methanol ME, the second step is to produce EG and methanol ME through hydrogenation, and the second step is to produce ethanol EA through transitional hydrogenation: the reaction formula involved is:
CH 3 OCOCOOCH 3 +2H 2 =CH 2 OHCOOCH 3 +CH 3 OH (first step)
CH 2 OHCOOCH 3 +2H 2 =CH 2 OHCH 2 OH+CH 3 OH (second step)
CH 2 OHCH 2 OH+H 2 =CH 3 CH 2 OH+H 2 O (ethanol produced by excessive hydrogenation)
Breaking and hydrogenating-CO-O-bond in DMO molecule to generate ethanol:
CH 3 OCOCOOCH 3 +5H 2 =2CH 3 OH+CH 3 CH 2 OH+H 2 O
in addition, the alcohol substances have more active-OH groups, so that the alcohol substances are easy to dehydrate between molecules and in molecules to generate butyl other dihydric alcohol substances, and side reactions are particularly obvious at the end of the catalyst operation and when the reaction temperature is higher.
CH 2 OHCH 2 OH+CH 3 CH 2 OH=CH 2 OHCHOHCH 2 CH 3 +H 2 O
So the synthetic product of the coal glycol can produce a small amount of water, ethanol, propanol, butanol and the like by side reaction besides the main reaction to produce the glycol and the methanol.
The ethylene glycol rectification is to rectify and separate the main reaction products of ethylene glycol and methanol into a polyester grade ethylene glycol product meeting the standard of GB/T4649-2018 industrial ethylene glycol and a methanol product meeting the standard of GB/T338-2011 industrial methanol; the byproduct ethanol in the current coal-to-ethylene glycol production is also used as byproduct fusel, namely other monohydric alcohol, dihydric alcohol and the like, and the byproduct fusel contains about 30 percent of ethanol, and because the boiling points of the byproduct ethanol, propanol, butanol and the like are not greatly different, an azeotrope is easy to form if common rectification separation is adopted, and the scale of the coal-to-ethylene glycol production device which is used in China at present is not large, and the amount of the byproduct fusel produced by the coal-to-ethylene glycol is small, so the byproduct fusel is generally not deeply processed, but is directly sold to a third party for treatment at a lower price as the byproduct fusel, so that a large amount of ethanol in the byproducts is not recycled. The ethanol has very wide application, and has very wide application in chemical industry, medical and health, food industry, industry and agriculture production; and the production scale of the coal-to-ethylene glycol is larger and larger, taking a 60 ten thousand ton/year coal-to-ethylene glycol production device as an example, the yield of the by-product fusel is about 12000 tons per year, and the components are shown in the table 1, for example, if 30% of ethanol is separated out as an ethanol product, considerable economic benefits can be generated.
TABLE 1
Sequence number | Material name | Mass percent before entering the system |
1 | Water H 2 O | 41.6% |
2 | Methanol ME | 287ppm |
3 | Ethanol ET | 30% |
4 | Methyl glycolate MG | 11.5% |
5 | Ethylene glycol monomethyl ether | 1.1% |
6 | N-butanol NBA | 6.9% |
7 | Sec-butanol SBA | 1.67% |
8 | N-propanol NPA | 1.1% |
9 | Butanediol (butanediol) | 2% |
10 | Other impurities | 4% |
Disclosure of Invention
The utility model provides a recovery device of ethanol which is a byproduct of coal glycol synthesis, and the recovery device can separate ethanol from the byproduct of the coal glycol synthesis process, and the ethanol can reach the standard of first grade products.
The technical scheme adopted by the utility model is that the recovery device of ethanol which is a byproduct of the synthesis of ethylene glycol from coal comprises an ethanol recovery tower, wherein the ethylene glycol from coal is fed from the middle part of the ethanol recovery tower, a gas phase outlet at the top of the ethanol recovery tower is connected to an ethanol reflux tank through a first condenser, the ethanol reflux tank is connected to a reflux inlet at the upper part of the ethanol recovery tower through a pipeline and a pump, the other part of the ethanol reflux tank is connected to an ethanol extraction storage tank, the bottom of the ethanol recovery tower is also respectively connected with a reboiler and a liquid phase extraction pipe, and the gas phase outlet of the reboiler enters the tower from the lower end of the ethanol recovery tower.
Further, the gas phase outlet of the ethanol reflux tank is connected to a second condenser, and the non-condensable gas outlet of the second condenser is connected to the tail gas treatment system through a vacuum pump and a pipeline.
Further, the liquid phase material outlet of the second condenser is connected to an ethanol reflux tank.
Further, a liquid phase extraction pipe at the bottom of the ethanol recovery tower is connected to a terminal sewage treatment device through a tower kettle pump of the ethanol recovery tower.
Further, the bottom of the ethanol recovery tower is connected to the tube side of the reboiler through a pipeline, the shell side of the reboiler is connected to a steam pipeline, and the shell side outlet of the reboiler is connected to a steam condensate tank.
Further, a gas phase outlet of the steam condensate tank is connected to a steam pipeline, and a liquid phase outlet is connected to a steam condensate pipe network through a steam condensate pump.
Further, the steam pipeline is from the steam outlet of the byproduct of the glycol rectification section.
Further, the ethanol recovery tower is a negative pressure packing tower, a plurality of packing layers are arranged in the packing tower, a liquid distributor is arranged above the packing layers, and a demister is arranged at the uppermost layer in the packing tower.
Further, liquid spray heads are arranged at the feed inlet and the reflux inlet in the packed tower.
Further, the ethanol reflux tank is connected to the reflux inlet of the ethanol recovery tower and the ethanol extraction storage tank respectively after passing through the pipeline and the reflux pump, a reflux flow regulating valve is arranged on the pipeline between the reflux pump and the ethanol recovery tower, and an ethanol extraction regulating valve is arranged on the pipeline between the reflux pump and the ethanol extraction storage tank.
The beneficial effects of the utility model are as follows:
the utility model aims to solve the problem that ethanol which is a byproduct of the synthesis of the coal-to-ethylene glycol is not recycled; the recovery device for the ethanol which is a byproduct of the synthesis of the coal glycol is provided, and the recovery device adopts reduced pressure continuous rectification, has simple process flow and less equipment, adopts reduced pressure rectification and less heat, and can rectify and separate a first-grade ethanol product with 95.5 percent of standard purity which meets GB/T6820-2016 ethanol for industry. The economic benefit of the coal-to-glycol project is improved. Taking 60 ten thousand tons/year of coal glycol as an example, about 3600 tons of 99.5 percent ethanol product can be recovered each year
Because the boiling point of the liquid changes along with the pressure of the system, the boiling point of the liquid increases along with the pressure rise, the utility model can reduce the boiling point of the fusel in the tower by adopting the reduced pressure rectification, and prevent the high-temperature fusel from generating polymerization and coke collection reaction in the tower; according to the different volatility properties of each component in the fusel, evaporating and condensing for multiple times in a tower, transferring heavy components (high boiling point) into a tower kettle liquid phase, extracting from the tower kettle as a fusel byproduct, transferring fusel (low boiling point) ethanol into a gas phase, and rectifying and separating from the tower top as an ethanol product; the packing tower is a gas-liquid mass transfer device with wide application, and has the advantages of simple structure, low operating pressure, uniform distribution of liquid and gas on the packing during working, and increased gas-liquid contact area.
The utility model perfects the whole process of the coal glycol distillation, fully utilizes the 0.1MPa low-grade steam as a byproduct of the glycol distillation, and plays a role in comprehensive utilization of heat energy. In addition, the mixed alcohol extracted from the ethanol recovery tower kettle contains a large amount of water and a small amount of organic matters, can be used as a carbon source required by activated sludge in a sewage treatment biochemical sewage tank, and reduces the supplementing frequency of the carbon source in the biochemical sewage tank.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model.
In the figure, an ethanol recovery tower 1, a reboiler 2, an ethanol recovery tower kettle pump 3, a vacuum pump 4, a first condenser 5, a second condenser 6, an ethanol reflux tank 7, a reflux pump 8, a steam condensate tank 9, a steam condensate pump 10, a demister 11, a liquid spray head 12, a liquid distributor 13, a filler 14, a tail gas treatment device 15, an ethanol storage tank 16, a terminal sewage treatment device 17, a steam condensate pipe network 18, a reflux flow rate regulating valve 19, an ethanol extraction regulating valve 20 and a fusel extraction regulating valve 21.
Detailed Description
The utility model will be further elucidated with reference to the examples and the accompanying drawings.
As shown in figure 1, the recovery device for ethanol which is a byproduct of coal glycol synthesis comprises an ethanol recovery tower 1, wherein the coal glycol byproduct is fed from the middle part of the ethanol recovery tower, a gas phase outlet at the top of the ethanol recovery tower is connected to an ethanol reflux tank 7 through a first condenser 5, the ethanol reflux tank 7 is connected to a reflux inlet at the upper part of the ethanol recovery tower 1 through a pipeline and a pump, the other part of the ethanol reflux tank is connected to an ethanol extraction storage tank, a reboiler 2 and a liquid phase extraction pipe are respectively connected to the bottom of the ethanol recovery tower 1, and a gas phase outlet of the reboiler enters the tower from the lower end of the ethanol recovery tower.
In a preferred embodiment, the gas phase outlet of the ethanol reflux drum 7 is connected to a second condenser 6, the non-condensable gas outlet of which is connected to the tail gas treatment system 15 via a vacuum pump 4 and a pipe. Noncondensable gas containing trace organic matter ethanol, which is not condensed in the shell pass of the second condenser, is sent to a tail gas treatment device for further treatment, so that the tail gas emission is ensured to reach the environmental protection requirement. The gas phase material at the top of the ethanol recovery tower is cooled to 40 ℃ by indirect heat exchange between the first condenser and circulating water, and then cooled to 0 ℃ by the second condenser and circulating refrigerating fluid, so that the ethanol in the noncondensable gas at the top of the ethanol recovery tower can be better condensed and the temperature at the top of the ethanol recovery tower can be controlled.
More preferably, the liquid phase material outlet of the second condenser 6 is connected to an ethanol reflux drum 7.
In the preferred scheme, a liquid phase extraction pipe at the bottom of the ethanol recovery tower 1 is connected to a terminal sewage treatment device 17 through an ethanol recovery tower kettle pump 3. A mixed alcohol extraction regulating valve 21 is arranged between the tower kettle pump 3 and the terminal sewage treatment device 17, and mixed alcohol after ethanol recovery is extracted from the tower kettle is used as a carbon source required by activated sludge in a terminal sewage treatment biochemical sewage tank.
In the preferred scheme, the bottom of the ethanol recovery tower 1 is connected to the tube side of a reboiler through a pipeline, the shell side of the reboiler is connected with a steam pipeline, and the shell side outlet of the reboiler is connected to a steam condensate tank.
More preferably, the vapor phase outlet of the vapor condensate tank is connected to a vapor pipe, and the liquid phase outlet is connected to the vapor condensate pipe network 18 through a vapor condensate pump. The steam condensate is pumped up by a condensate pump and then is sent to a steam condensate pipe network for recovery.
More preferably, the steam pipeline is from a steam outlet of a byproduct in the glycol rectification section. The steam pressure is 0.1MPa, and the comprehensive utilization of the low-grade steam of the byproduct of the glycol distillation is realized by controlling the temperature of the tower kettle to 90 ℃ through the steam, so that the glycol distillation energy consumption is reduced; the byproduct steam with the pressure of 0.1MPa is used as a heat source of the ethanol recovery tower, so that the polymerization and coke collection reaction of tower kettle materials due to overtemperature can be effectively prevented.
In the preferred scheme, the ethanol recovery tower 1 is a negative pressure packing tower, a plurality of packing layers 14 are arranged in the packing tower, specifically, plate ripple structured packing is adopted as packing, and 4 layers of packing are arranged in total; the liquid distributor 13 is arranged above the packing layer, so that liquid can be uniformly distributed on the packing, and the demister 11 is arranged at the uppermost layer in the packing tower to intercept liquid entrained in the ascending gas phase.
More preferably, the liquid spray heads 12 are arranged at the feed inlet and the reflux inlet in the packed tower, so that the liquid can be uniformly sprayed on the liquid distributor.
In another preferred scheme, the ethanol reflux tank 7 is connected to a reflux inlet of the ethanol recovery tower 1 and the ethanol extraction storage tank 16 respectively after passing through a pipeline and the reflux pump 8, a reflux flow regulating valve 19 is arranged on a pipeline between the reflux pump and the ethanol recovery tower 1, and an ethanol extraction regulating valve 20 is arranged on a pipeline between the reflux pump and the ethanol extraction storage tank 16. After the ethanol in the reflux tank is boosted by a reflux pump, a part of the ethanol is refluxed to the tower top to control the temperature of the tower top to be 64 ℃, and the other part of the ethanol is taken as an ethanol product to be extracted to an ethanol storage tank, and is arranged through a reflux flow regulating valve 19 and an ethanol extraction regulating valve 20 to control the reflux ratio of the tower top to be 5:1.
In the glycol rectification section, the mixed alcohol extracted from the tower kettle of the methanol recovery tower is continuously sent to the middle part of the ethanol recovery tower through a pump and a pipeline, the vacuum pump of the ethanol recovery tower controls the pressure of the top of the ethanol recovery tower to be-0.04 MPa, the temperature of the top of the tower to be 64 ℃, and the temperature of the tower kettle to be 90 ℃; the heat source of the reboiler of the ethanol recovery tower adopts 0.1MPa steam which is a byproduct in the glycol rectification section, the mixed alcohol is indirectly heated by the steam in the reboiler, and light components such as ethanol and the like are vaporized and continuously ascend along a tray and carry out mass and heat transfer on the reflux liquid from top to bottom on the tray; the gaseous phase ethanol light component rising from the top of the ethanol recovery tower is indirectly cooled to 40 ℃ in a first condenser through circulating water, then flows into a reflux tank automatically, gas-liquid separation is further carried out in the reflux tank, the separated gaseous phase material is indirectly cooled to 0 ℃ in a second condenser through glycol refrigerating fluid, the liquid phase material after deep cooling flows into the reflux tank automatically, and the non-condensable gas (mainly nitrogen and air leaking into a system, containing a small amount of methanol, ethanol, water and the like) at the top of the tower is further treated by a vacuum pump and a pipeline to be sent to a tail gas treatment device. After the pressure of 99.5% ethanol in the reflux tank of the ethanol recovery tower is increased by a reflux pump of the ethanol recovery tower, a part of the ethanol returns to the upper part of the ethanol recovery tower to be used as reflux to control the temperature of the top of the tower, and a part of the ethanol returns to the ethanol product tank to be used as 99.5% ethanol product. The materials at the tower bottom of the ethanol recovery tower are mixed alcohol heavy components for separating out ethanol, contain more water, and are sent to a terminal sewage treatment device after being boosted by a pump at the tower bottom of the ethanol recovery tower. The 0.1MPa steam in the reboiler shell side of the ethanol recovery tower exchanges heat with the mixed alcohol in the pipe layer indirectly, and the steam condensate is collected by a steam condensate tank and is sent to a steam condensate pipe network after being boosted by a steam condensate pump.
Taking 60 ten thousand tons/year of coal-made glycol as an example, about 3600 tons of 99.5% ethanol product can be recovered each year, and the components of ethanol and fusel are shown in Table 2:
TABLE 2
The ethanol recovered by the device can meet the first-grade standard of GB/T6820-2016 industrial ethanol, and the economic benefit of the coal-to-ethylene glycol project can be remarkably improved.
Claims (10)
1. A recovery device of ethanol which is a byproduct of coal glycol synthesis is characterized in that: the coal-made glycol byproduct recycling device comprises an ethanol recycling tower (1), wherein coal-made glycol byproducts are fed from the middle of the ethanol recycling tower, a gas phase outlet at the top of the ethanol recycling tower is connected to an ethanol reflux tank (7) through a first condenser (5), the ethanol reflux tank (7) is partially connected to a reflux inlet at the upper part of the ethanol recycling tower (1) through a pipeline and a pump, the other part of the ethanol reflux tank is connected to an ethanol extraction storage tank, a reboiler (2) and a liquid phase extraction pipe are respectively connected to the bottom of the ethanol recycling tower (1), and a gas phase outlet of the reboiler enters the tower from the lower end of the ethanol recycling tower.
2. The apparatus according to claim 1, wherein: the gas phase outlet of the ethanol reflux tank (7) is connected to a second condenser (6), and the non-condensable gas outlet of the second condenser is connected to a tail gas treatment system (15) through a vacuum pump (4) and a pipeline.
3. The apparatus according to claim 2, wherein: the liquid phase material outlet of the second condenser (6) is connected to an ethanol reflux tank (7).
4. The apparatus according to claim 1, wherein: the liquid phase extraction pipe at the bottom of the ethanol recovery tower (1) is connected to a terminal sewage treatment device (17) through an ethanol recovery tower kettle pump (3).
5. The apparatus according to claim 1, wherein: the bottom of the ethanol recovery tower (1) is connected to the tube side of the reboiler through a pipeline, the shell side of the reboiler is connected with a steam pipeline, and the shell side outlet of the reboiler is connected to the steam condensate tank.
6. The apparatus according to claim 5, wherein: the gas phase outlet of the steam condensate tank is connected to a steam pipeline, and the liquid phase outlet is connected to a steam condensate pipe network (18) through a steam condensate pump.
7. The apparatus according to claim 5, wherein: the steam pipeline is from the steam outlet of the byproduct in the glycol rectification section.
8. The apparatus according to any one of claims 1 to 7, wherein: the ethanol recovery tower (1) is a negative pressure packing tower, a plurality of packing layers (14) are arranged in the packing tower, a liquid distributor (13) is arranged above the packing layers, and a demister (11) is arranged at the uppermost layer in the packing tower.
9. The apparatus according to claim 8, wherein: and liquid spray heads (12) are arranged at the feed inlet and the reflux inlet in the packed tower.
10. The apparatus according to claim 8, wherein: the ethanol reflux tank (7) is connected to a reflux inlet of the ethanol recovery tower (1) and the ethanol extraction storage tank (16) respectively after passing through a pipeline and a reflux pump (8), a reflux flow regulating valve (19) is arranged on a pipeline between the reflux pump and the ethanol recovery tower (1), and an ethanol extraction regulating valve (20) is arranged on a pipeline between the reflux pump and the ethanol extraction storage tank (16).
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CN116966621A (en) * | 2023-09-12 | 2023-10-31 | 山西振钢生物科技股份有限公司 | Continuous rectifying device of sebacic acid |
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CN116966621A (en) * | 2023-09-12 | 2023-10-31 | 山西振钢生物科技股份有限公司 | Continuous rectifying device of sebacic acid |
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