CN116789525A - Purification method of coal-to-ethylene glycol byproduct ethanol based on membrane separation method - Google Patents
Purification method of coal-to-ethylene glycol byproduct ethanol based on membrane separation method Download PDFInfo
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- CN116789525A CN116789525A CN202310513568.2A CN202310513568A CN116789525A CN 116789525 A CN116789525 A CN 116789525A CN 202310513568 A CN202310513568 A CN 202310513568A CN 116789525 A CN116789525 A CN 116789525A
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- ethanol
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- byproduct
- ethylene glycol
- membrane separation
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 284
- 239000012528 membrane Substances 0.000 title claims abstract description 71
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Substances OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000000926 separation method Methods 0.000 title claims abstract description 53
- 239000006227 byproduct Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000000746 purification Methods 0.000 title claims abstract description 19
- 239000000047 product Substances 0.000 claims abstract description 37
- 238000007670 refining Methods 0.000 claims abstract description 32
- 239000012510 hollow fiber Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000012466 permeate Substances 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000003245 coal Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000010992 reflux Methods 0.000 claims description 9
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 235000019441 ethanol Nutrition 0.000 description 75
- 238000005516 engineering process Methods 0.000 description 13
- 238000003786 synthesis reaction Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010170 biological method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 238000000895 extractive distillation Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
-
- 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
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a purification method of byproduct ethanol of coal-to-ethylene glycol based on a membrane separation method, which comprises the steps of firstly, feeding byproduct ethanol materials from a main device for preparing ethylene glycol from coal into a raw material buffer tank; then taking a byproduct ethanol material in a raw material buffer tank as a feed, sending the feed into a hollow fiber membrane separation unit for separation to obtain an ethanol membrane finished product, and allowing water and a small amount of ethanol in a feed liquid side solution to permeate through the hollow fiber membrane in a steam form to obtain a permeate; and finally, sending the ethanol film finished product obtained in the steps into a refining tower for refining to finally obtain the finished product ethanol. The invention has the advantages of realizing the purification and separation of the byproduct ethanol, removing the light component and the heavy component impurities while rectifying in one step, improving the energy utilization rate in the system, and reducing the operation energy consumption and the heating load of the refining tower.
Description
Technical Field
The invention relates to the technical field of hollow fiber membrane separation application, in particular to a purification method of ethanol as a byproduct in the preparation of ethylene glycol from coal based on a membrane separation method.
Background
At present, the ethanol production method mainly comprises a biological fermentation method and a chemical synthesis method. The production technology for preparing ethanol from the synthesis gas in the chemical synthesis method is mature, the production cost is obviously lower than that of a grain route, and the method has stronger competitiveness and wide development prospect. Three types of ethanol are produced by the synthesis gas, namely, the ethanol is directly produced by the synthesis gas; secondly, preparing ethanol by a synthesis gas biological method; thirdly, the synthesis gas is hydrogenated by acetic acid to prepare ethanol. In addition, there is another ethanol production technology, which is the purification and utilization of ethanol which is a byproduct of chemical industry, and the ethanol has the remarkable advantage of low cost as a byproduct of chemical products, but because of the characteristics of the byproduct, the ethanol contains more kinds of organic impurities and water, and if the ethanol is required to obtain a qualified ethanol finished product, the ethanol is required to be separated and purified.
Because of the azeotropic point of ethanol and water, the traditional method cannot directly obtain absolute ethanol, and the existence of water can also influence the separation of ethanol from other organic impurities in byproduct ethanol, such as methanol, dimethyl carbonate and the like. The industrial absolute ethanol is mainly produced by adopting methods such as extractive distillation, adsorption separation and the like, and the traditional ethanol dehydration modes have the problems of complex process, high energy consumption, serious pollution and the like. The membrane dehydration technology is a novel separation technology, and has the outstanding advantages that the separation process is not limited by the gas-liquid balance of components, and the separation of the azeotropic mixture of ethanol and water is realized with low energy consumption. At present, a technology for separating and purifying ethanol by adopting a rectification and separation membrane technology is adopted, such as an environment-friendly and energy-saving production process method of ultra-dry absolute ethyl alcohol disclosed in China patent CN115340442A, which describes that the technology adopts the separation membrane technology and a molecular sieve adsorption device as core technologies, and a rectification device is matched for recycling process wastewater; chinese patent CN108083979A discloses a method and a device for producing ethanol, which describe a dehydration process for preparing ethanol by adopting synthesis gas by adopting a rectification and separation membrane technology as a process.
However, the process route of the scheme is mainly focused on solving the problem of separation of ethanol and water, and separation and purification of ethanol cannot be realized under the working condition that the byproduct ethanol material contains light and heavy organic components, water and other impurities; in addition, the rectifying tower is arranged in front of the separation membrane device, and positive pressure operation is needed by the rectifying tower so as to provide positive driving force for the separation membrane, but positive pressure can influence the rectifying separation efficiency, and meanwhile, the steam grade requirement is improved.
Disclosure of Invention
The invention aims to solve the problems that the existing byproduct ethanol cannot be separated and purified, the rectification separation efficiency is low and the requirement is high, and provides a purification method for preparing glycol byproduct ethanol by using coal based on a membrane separation method, which realizes the purification and separation of the byproduct ethanol, removes light component and heavy component impurities while rectifying in one step, improves the energy utilization rate of a system, and reduces the operation energy consumption and the heating load of a refining tower.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a purification method of ethanol as a byproduct of coal-to-ethylene glycol based on a membrane separation method comprises the following specific steps:
(1) Feeding the byproduct ethanol material from a main device for preparing ethylene glycol from coal into a raw material buffer tank;
(2) Then taking a byproduct ethanol material in a raw material buffer tank as a feed, sending the feed into a hollow fiber membrane separation unit for separation to obtain an ethanol membrane finished product, and allowing water and a small amount of ethanol in a feed liquid side solution to permeate through the hollow fiber membrane in a steam form to obtain a permeate;
(3) And (3) sending the ethanol film finished product obtained in the step (2) into a refining tower for refining, and finally obtaining the finished product ethanol.
Further, in the step (2), the operation pressure of the feed liquid side of the hollow fiber separation membrane is 100-400 kpa, and the operation temperature is a temperature corresponding to the saturation vapor pressure of the feed material, and is overheated by 10-30 ℃.
Further, in the step (2), the water content of the ethanol film finished product is controlled to be 0.05-0.5 wt%.
Further, in the step (2), the obtained ethanol film finished product vapor is not condensed, and is sent into the refining tower in the step (3) in a saturated gas phase form, and the temperature of the ethanol film finished product is 90-120 ℃.
Further, in the step (3), the reflux ratio of the refining tower is controlled to be 0.1-10, the volume ratio of the flow extracted from the side line to the reflux amount of the tower top is controlled to be 1:2-1:5, and the operating pressure of the refining tower is controlled to be-0.05-0.1 MPa (G).
Further, in the step (3), heat exchange is performed between the ethanol finished product steam extracted from the side line of the refining tower and the byproduct ethanol material fed by the hollow fiber membrane separation device, so as to further reduce the operation energy consumption.
Further, in the step (2), the membrane adopted by the hollow fiber membrane separation unit is a preferential water permeable membrane, which may be an organic membrane, an inorganic membrane or an inorganic-organic composite membrane.
In the step (2), the hollow fiber membrane separation units are connected in series, parallel or series-parallel by 1-100 hollow fiber membrane separators so as to achieve different treatment requirements and production capacities.
Compared with the prior art, the invention has the following advantages:
(1) The invention adopts the hollow fiber membrane separation technology to break the ethanol-water azeotropic composition to finish ethanol dehydration, and has simple technical process, high safety coefficient and simple operation;
(2) The invention firstly adopts a membrane separation technology to break the ethanol-water azeotropy, and then adopts a rectification technology to remove light and heavy component organic impurities in the ethanol, thereby completing the dehydration, separation and purification of the ethanol in one step;
(3) According to the invention, the membrane separation product is not condensed and enters the refining tower in a vapor form, so that the energy utilization rate in the system is improved, and the heating load of the refining tower is further reduced;
(4) The method adopts a mode of extracting the finished product steam from the side line of the refining tower to collect the ethanol finished product, so that light component and heavy component impurities can be removed simultaneously in the one-step rectification process;
(5) According to the invention, the heat exchange is carried out on the finished product steam extracted from the side line of the refining tower and the ethanol feed, so that the energy utilization rate in the system is improved, and the operation energy consumption of the whole system is reduced.
Description of the embodiments
Examples
In order that the invention may be more clearly understood, a method for purifying ethanol, a byproduct of ethylene glycol from coal by membrane separation, according to the present invention will be further described, and the specific examples described herein are provided for illustration only and are not intended to limit the invention.
A method for purifying ethanol from a coal-to-ethylene glycol byproduct ethanol material comprises the following steps of:
(1) Feeding the byproduct ethanol material into a raw material buffer tank from a main device for preparing ethylene glycol from coal;
(2) The byproduct ethanol material in the raw material buffer tank is taken as feed, preheated by a preheater, enters an evaporator, is overheated in the superheater to 15 ℃, and enters a hollow fiber membrane separation unit formed by connecting a plurality of hollow fiber membranes in series, wherein the area of each stage of membrane component is 8m 2 Separating to obtain ethanol film products with water content of 0.5, 0.2 and 0.1. 0.1 wt respectively;
(3) Water and a small amount of ethanol in the solution at the feed liquid side permeate through the hollow fiber membrane in the form of steam to obtain permeate, wherein the feed liquid side pressure is 0.25 MPa, which is the gauge pressure, the permeate side pressure is respectively controlled at 2000, 1000 and 700 and Pa, and the permeate obtained at the permeate side is condensed by a permeate condenser under the suction of a vacuum pump;
(4) The ethanol film finished product steam enters a refining tower for refining, the operating pressure of the refining tower is 0.05 MPa, the operating pressure is also gauge pressure, the operating reflux ratio is 5, and the ethanol finished product with the purity of more than or equal to 99.5wt.% is obtained and condensed in a side line condenser after heat exchange with the raw material.
In this example, when ethanol membrane products with different water contents are used as the feed materials for the refining tower, the required number of membrane modules, the water content of the permeate, the flux, the running cost and other data are shown in the following table 1.
As can be seen from the table, the optimization of the purity of the ethanol finished product and the required membrane area of the whole equipment can be effectively obtained by controlling the water content of the finished product of the membrane separation unit in a proper range.
Examples
A method for purifying ethanol from a coal-to-ethylene glycol byproduct ethanol material comprises the following steps of:
(1) Feeding the byproduct ethanol material from a main device for preparing ethylene glycol from coal into a raw material buffer tank;
(2) The byproduct ethanol material in the raw material buffer tank is taken as feed, preheated by a preheater and enters an evaporator, after being overheated in the superheater to 10 ℃, the feed enters a hollow fiber membrane separation unit formed by connecting six hollow fiber membranes in series, and the area of each stage of membrane component is 8m 2 Separating to obtain ethanol film product with water content of 0.3 wt%;
(3) Water and a small amount of ethanol in the feed liquid side solution permeate through the hollow fiber membrane in a steam form to obtain permeate. The side pressure of the feed liquid is 0.20 MPa, the side pressure of the permeation is controlled at 1500Pa, the permeation side is sucked by a vacuum pump, and the obtained permeation liquid is condensed by a permeation liquid condenser;
(4) And (3) refining the ethanol film finished product steam in a refining tower, wherein the operating pressure of the refining tower is 0.05 MPa, the operating reflux ratio is respectively controlled to be 3, 5 and 10, and the ethanol finished product with the purity of more than or equal to 99.5wt.% is obtained and condensed in a side line condenser after heat exchange with the raw material.
In this example, when the refining columns were operated at different reflux ratios, the required operating costs, purity of the ethanol product, etc. were as shown in Table 2 below.
As can be seen from the table, the optimization of the purity of the ethanol finished product and the running cost of the whole equipment can be effectively obtained by controlling the operation reflux ratio of the refining tower in a proper range.
Examples
A method for purifying ethanol from a coal-to-ethylene glycol byproduct ethanol material comprises the following steps of:
(1) Feeding the byproduct ethanol material from a main device for preparing ethylene glycol from coal into a raw material buffer tank;
(2) The byproduct ethanol material in the raw material buffer tank is taken as the feed, preheated by a preheater and enters an evaporator, and after being respectively overheated at 0, 10, 20 and 30 ℃ in the superheater, the feed enters a hollow fiber membrane section formed by connecting five hollow fiber membranes in seriesSeparating unit, wherein the area of each stage of membrane component is 8m 2 Separating to obtain ethanol film product with water content of 0.5. 0.5 wt%;
(3) Water and a small amount of ethanol in the solution at the feed liquid side permeate through the hollow fiber membrane in the form of steam to obtain permeate, wherein the side pressure of the feed liquid is 0.25MP, the side pressure of the permeate is controlled at 2000Pa, and the permeate obtained at the permeate side is condensed by a permeate condenser under the suction of a vacuum pump;
(4) The ethanol film finished product steam enters a refining tower for refining, the operating pressure of the refining tower is 0.03 MPa, the operating reflux ratio is respectively controlled to be 5, and the ethanol finished product with the purity of more than or equal to 99.5wt.% is obtained and condensed in a side line condenser after heat exchange with the raw materials.
In this example, the data for the change in average water flux, the average water content of permeate, etc. when the superheater was operated at different superheating temperatures are shown in table 3 below.
As can be seen from the table, the superheating temperature of the superheater is controlled in a proper range, so that the service life of the membrane can be effectively prolonged, and a better average water quantity of the permeate can be obtained
In addition to the embodiments described above, other embodiments of the invention are possible. All technical schemes formed by equivalent substitution or equivalent transformation fall within the protection scope of the invention.
Claims (8)
1. The purification method of the byproduct ethanol of the ethylene glycol prepared from coal based on the membrane separation method comprises the following specific steps of:
(1) Feeding the byproduct ethanol material from a main device for preparing ethylene glycol from coal into a raw material buffer tank;
(2) Then taking a byproduct ethanol material in a raw material buffer tank as a feed, sending the feed into a hollow fiber membrane separation unit for separation to obtain an ethanol membrane finished product, and allowing water and a small amount of ethanol in a feed liquid side solution to permeate through the hollow fiber membrane in a steam form to obtain a permeate;
(3) And (3) sending the ethanol film finished product obtained in the step (2) into a refining tower for refining, and finally obtaining the finished product ethanol.
2. The purification method of the byproduct ethanol of the coal-to-ethylene glycol based on the membrane separation method according to claim 1, which is characterized by comprising the following steps:
in the step (2), the operation pressure of the feed liquid side of the hollow fiber separation membrane is 100-400 kPa, and the operation temperature is the temperature corresponding to the saturated vapor pressure of the feed and is overheated by 10-30 ℃.
3. The purification method of the byproduct ethanol of the ethylene glycol prepared by the coal based on the membrane separation method according to claim 1 or 2, which is characterized by comprising the following steps:
in the step (2), the water content of the ethanol film finished product is controlled to be 0.05-0.5 wt%.
4. The purification method of the byproduct ethanol of the ethylene glycol prepared by the coal based on the membrane separation method according to claim 1 or 2, which is characterized by comprising the following steps:
in the step (2), the obtained ethanol film finished product steam is not condensed, and is sent into the refining tower in the step (3) in a saturated gas phase form, and the temperature of the ethanol film finished product is 90-120 ℃.
5. The purification method of the byproduct ethanol of the ethylene glycol prepared by the coal based on the membrane separation method according to claim 1 or 2, which is characterized by comprising the following steps:
in the step (3), the reflux ratio of the refining tower is controlled to be 0.1-10, the volume ratio of the flow extracted from the side line to the reflux amount of the tower top is controlled to be 1:2-1:5, and the operating pressure of the refining tower is controlled to be-0.05-0.1 MPa (G).
6. The purification method of the byproduct ethanol of the ethylene glycol prepared by the coal based on the membrane separation method according to claim 1 or 2, which is characterized by comprising the following steps:
in the step (3), heat exchange is carried out between the ethanol finished product steam extracted from the side line of the refining tower and the byproduct ethanol material fed by the hollow fiber membrane separation device.
7. The purification method of the byproduct ethanol of the ethylene glycol prepared by the coal based on the membrane separation method according to claim 1 or 2, which is characterized by comprising the following steps:
in the step (2), the membrane adopted by the hollow fiber membrane separation unit is a preferential water permeable membrane, and is an organic membrane, an inorganic membrane or an inorganic-organic composite membrane.
8. The purification method of the byproduct ethanol of the ethylene glycol prepared by the coal based on the membrane separation method according to claim 1 or 2, which is characterized by comprising the following steps:
in the step (2), the hollow fiber membrane separation units are connected in series, parallel or series-parallel by 1-100 hollow fiber membrane separators.
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