CN113860994A - Device and method for preparing absolute ethyl alcohol by acid-base neutralization and membrane separation coupling method - Google Patents
Device and method for preparing absolute ethyl alcohol by acid-base neutralization and membrane separation coupling method Download PDFInfo
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- CN113860994A CN113860994A CN202111275823.1A CN202111275823A CN113860994A CN 113860994 A CN113860994 A CN 113860994A CN 202111275823 A CN202111275823 A CN 202111275823A CN 113860994 A CN113860994 A CN 113860994A
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 239000012528 membrane Substances 0.000 title claims abstract description 62
- 238000000926 separation method Methods 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000006386 neutralization reaction Methods 0.000 title claims abstract description 22
- 238000010168 coupling process Methods 0.000 title claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 45
- 235000019441 ethanol Nutrition 0.000 claims abstract description 34
- 230000003068 static effect Effects 0.000 claims abstract description 30
- 238000001514 detection method Methods 0.000 claims abstract description 23
- 239000002585 base Substances 0.000 claims abstract description 20
- 239000003513 alkali Substances 0.000 claims abstract description 17
- 230000000149 penetrating effect Effects 0.000 claims abstract description 17
- 239000000872 buffer Substances 0.000 claims abstract description 15
- 239000012530 fluid Substances 0.000 claims abstract description 15
- 239000011552 falling film Substances 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000002253 acid Substances 0.000 claims abstract description 8
- 230000002378 acidificating effect Effects 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims description 17
- 239000002808 molecular sieve Substances 0.000 claims description 12
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 7
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 6
- 239000012071 phase Substances 0.000 claims description 6
- 239000012510 hollow fiber Substances 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 239000003507 refrigerant Substances 0.000 claims description 2
- 229920006395 saturated elastomer Polymers 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims 1
- 239000002351 wastewater Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 7
- 150000003839 salts Chemical class 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 28
- 239000011259 mixed solution Substances 0.000 description 15
- 239000000243 solution Substances 0.000 description 11
- 230000008878 coupling Effects 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000895 extractive distillation Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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Classifications
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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
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
-
- 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
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a device and a process method for preparing absolute ethyl alcohol by an acid-base neutralization and membrane separation coupling method. The device comprises a raw material tank, a preheater, a falling film evaporator, a superheater, a vapor permeable membrane separation device, a product condenser, a penetrating fluid condenser, a vacuum buffer tank and a vacuum unit, and further comprises an alkali liquor tank, a metering pump, a pipeline static mixer, a detection tank and a delivery pump. The process method comprises the steps of conveying acid-containing raw materials and alkali liquor into a pipeline static mixer for acid-alkali neutralization, enabling a neutralization product to enter a detection tank, exchanging heat of neutral or alkalescent raw materials from the detection tank, then enabling the neutral or alkalescent raw materials to enter a falling film evaporator to remove alkaline substances and salts to obtain raw material steam, heating the raw material steam to 110-150 ℃, and then enabling the raw material steam to enter a steam permeable membrane separation device for separation to obtain a high-purity ethanol product and penetrating fluid. By adopting the device and the process for treating the aqueous acidic ethanol raw material liquid, the water content in the product ethanol can be reduced to be below 0.5 wt.%.
Description
Technical Field
The invention belongs to the field of ethanol production, and particularly relates to a device and a method for preparing absolute ethanol by acid-base neutralization and membrane separation coupling.
Background
The absolute ethyl alcohol is an ethyl alcohol product with the ethyl alcohol content of more than or equal to 99.5 percent, plays a role in playing a role in lifting weight in modern industry, can be widely applied to the industries of pharmaceutical chemicals, fine chemicals, energy, electronics, environmental protection, food and the like as an organic solvent, and can be used as an important basic chemical raw material for producing acetaldehyde, acetic acid, ethylamine, ethyl acetate and the like. The traditional organic solvent dehydration method mainly comprises azeotropic distillation, extractive distillation, adsorption and other methods. The membrane refining and dewatering separation process is one new type of membrane separation technology for dewatering organic solvent and is one separation process with inorganic membrane material to separate components in different selective permeability and diffusion speed under the push of vapor partial pressure difference of the components in liquid mixture. However, the inorganic membrane material cannot treat the acidic raw material liquid due to the material characteristics, and the service life of the membrane is greatly reduced, thereby limiting the application range of the membrane separation method.
Disclosure of Invention
The invention aims to provide a device and a process method for preparing absolute ethyl alcohol by acid-base neutralization and membrane separation coupling. The pH value of the raw material liquid entering the membrane separation unit is effectively ensured by coupling the acid-base neutralization process with the membrane separation. By adopting the process to treat the aqueous acidic ethanol raw material solution, the water content in the product ethanol can be reduced to be below 0.5 wt.%.
In order to achieve the purpose, the invention is realized by the following technical scheme.
The invention provides a device for preparing absolute ethyl alcohol by acid-base neutralization and membrane separation coupling method, which comprises: the method comprises the following steps: raw material tank, charge pump, pre-heater, falling film evaporator, over heater, vapor permeation membrane separator, product condenser, product jar, penetrant condenser, vacuum buffer tank, vacuum unit, wherein: the device also comprises an alkali liquor tank, a metering pump, a pipeline static mixer, a detection tank and a delivery pump; the raw material tank, the feeding pump and the pipeline static mixer are sequentially communicated through pipelines; the alkali liquor tank, the metering pump and the pipeline static mixer are communicated in sequence through pipelines; the outlet of the pipeline static mixer, the detection tank, the delivery pump, the preheater, the falling film evaporator, the superheater and the steam permeable membrane separation device are communicated in sequence through pipelines; the product side outlet, the preheater, the product condenser and the product tank of the vapor permeable membrane separation device are communicated in sequence through pipelines; the penetrating fluid outlet of the steam permeable membrane separation device, the penetrating fluid condenser, the vacuum buffer tank and the vacuum unit are communicated in sequence through pipelines.
Further, the vapor permeable membrane configuration of the vapor permeable membrane separation device includes a tubular type, a hollow fiber type.
Further, the vapor permeable membrane is an organic or inorganic membrane, and comprises a NaA molecular sieve membrane, a T-type molecular sieve membrane, a MOR molecular sieve membrane and a ZSM-5 molecular sieve membrane.
The invention also provides a process for preparing absolute ethyl alcohol by the acid-base neutralization-membrane separation coupling method, and a device for preparing absolute ethyl alcohol by the acid-base neutralization-membrane separation coupling method, wherein the process comprises the following steps:
conveying an acid-containing raw material to be treated from a raw material tank to a pipeline static mixer through a feeding pump, meanwhile, conveying alkali liquor with certain concentration from an alkali liquor tank to the pipeline static mixer through a metering pump, carrying out acid-alkali neutralization on the acid-containing raw material and the alkali liquor in the pipeline static mixer, feeding the neutralized raw material into a detection tank, and detecting the pH value in real time through an online remote pH meter; if the solvent in the detection tank is neutral or weakly alkaline, the solvent is qualified, and the qualified solvent is conveyed to the preheater through a pump; if the solvent in the detection tank is acidic, the solvent is unqualified, the unqualified solvent is pumped back to the pipeline mixer by a pump, and the unqualified acid solvent is further subjected to acid-base neutralization reaction in the pipeline static mixer until the pH value of the solvent is qualified; qualified neutral or weakly alkaline raw materials from the buffer tank are pressurized by a delivery pump, enter a raw material preheater, exchange heat with product steam, enter a falling film evaporator, are heated and vaporized by saturated steam, discharge concentrated solution from the bottom of the evaporator, and discharge alkaline substances and salts dissolved in the solution through the falling film evaporator concentrated acid discharge. Meanwhile, raw material steam is heated to 110-150 ℃ by a heater and then enters a membrane module for separation, the separated intercepted component enters a preheater for heat exchange with raw material liquid, and then enters a product condenser for further cooling and enters a product tank; the penetrating fluid enters a penetrating fluid condenser to exchange heat with a low-temperature refrigerant, the liquid phase enters a vacuum buffer tank, and the gas phase maintains the vacuum pressure of about 1KPaA through a vacuum pump unit.
Further, the acid-containing raw material to be treated is acidic ethanol with the concentration of 85-99% (V/V) and H+The concentration is less than or equal to 1000 ppm.
Further, the alkali liquor is 10-50% sodium hydroxide, calcium hydroxide, sodium bicarbonate, sodium carbonate, etc.
Further, the pH value of the qualified solvent in the detection tank is 7.0-8.0.
Further, the temperature of the preheated preheater is 65-85 ℃.
Further, the raw material steam is heated by a heater and then enters a membrane module for separation, the separated intercepted component membrane residual liquid obtains high-purity ethanol steam with the concentration of 99.5-99.9% (V/V), the dehydrated ethanol steam is condensed to obtain an ethanol product, and the ethanol content in the penetrating liquid at the penetrating side is 1-5% (V/V).
The device and the process method effectively ensure the pH value of the raw material liquid entering the membrane separation unit by coupling the acid-base neutralization process with the membrane separation. By adopting the process to treat the aqueous acidic ethanol raw material solution, the water content in the product ethanol can be reduced to be below 0.5 wt.%.
Drawings
FIG. 1 is a flow chart of a process for preparing absolute ethanol by acid-base neutralization-membrane separation coupling method according to an embodiment of the present invention.
Wherein: 1 is a raw material tank; 2 is a feed pump; 3 is an alkali liquor tank; 4 is a metering pump; 5 is a pipeline static mixer; 6 is a detection tank; 7 is a delivery pump; 8 is a preheater; 9 is a falling film evaporator; 10 is a superheater; 11 is a vapor permeable membrane separation device; 12 is a product condenser; 13 is a product tank; 14 is a permeate condenser; 15 is a vacuum buffer tank; 16 is a vacuum unit.
Detailed Description
To further illustrate the technical solution of the present invention, the following specific examples are given. It should be understood that the present invention has been shown and described only by way of illustration and description, and it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention or exceeding the scope of the claims.
The core of the specific embodiment of the invention is to provide a device for preparing absolute ethyl alcohol by acid-base neutralization and membrane separation coupling method (as shown in figure 1), which comprises a raw material tank 1, a feed pump 2, an alkali liquor tank 3, a metering pump 4, a pipeline static mixer 5, a detection tank 6, a delivery pump 7, a preheater 8, a falling film evaporator 9, a superheater 10, a vapor permeable membrane separation device 11, a product condenser 12, a product tank 13, a penetrating fluid condenser 14, a vacuum buffer tank 15 and a vacuum unit 16. The raw material tank 1, the feeding pump 2 and the pipeline static mixer 5 are communicated in sequence through pipelines; the lye tank 3, the metering pump 4 and the pipeline static mixer 5 are communicated in sequence through pipelines; an outlet of the pipeline static mixer 5, a detection tank 6, a delivery pump 7, a preheater 8, a falling film evaporator 9, a superheater 10 and a vapor permeable membrane separation device 11 are communicated in sequence through pipelines; a product side outlet of the vapor permeable membrane separation device 11, a preheater 8, a product condenser 12 and a product tank 13 are communicated in sequence through pipelines; the penetrating fluid outlet of the vapor permeable membrane separation device 11, the penetrating fluid condenser 14, the vacuum buffer tank 15 and the vacuum unit 16 are communicated in sequence through pipelines.
Example 1
Ethanol content of 85% (V/V), H+Conveying the mixed raw materials with the content of 1000ppm to a pipeline static mixer through a feeding pump, performing acid-base neutralization in the pipeline static mixer by using 50% sodium hydroxide solution through a metering pump to a detection tank to obtain an alkalescent mixed solution with the pH value of 8.0, delivering to a preheater through a delivery pump, preheating to 90 ℃, obtaining raw material steam and concentrated solution through a falling film evaporator, removing alkaline substances and inorganic salts in the mixed solution through the discharged concentrated solution, continuously heating the raw material steam to 150 ℃ through a heater, introducing the raw material steam into a tubular NaA molecular sieve membrane separation device, performing heat exchange between the ethanol gas at the product side and a preheater, cooling the ethanol gas at the product side through a condenser to obtain an ethanol product with the purity of 99.5% (V/V), condensing the mixed solution at the permeation side, the liquid phase is stored in a vacuum buffer tank, the ethanol content is 1% (V/V), and the gas phase is pumped away by a vacuum unit.
Example 2
Ethanol content of 90% (V/V), H+Conveying a mixed raw material with the content of 800ppm to a pipeline static mixer through a feeding pump, performing acid-base neutralization in the pipeline static mixer to a detection tank by using a 30% calcium hydroxide solution through a metering pump to obtain a weakly-alkaline mixed solution with the pH of 7.8, conveying the weakly-alkaline mixed solution to a preheater through a conveying pump, preheating to 80 ℃, removing alkaline substances and inorganic salts in the mixed solution through a film evaporator, continuously heating to 130 ℃ through a heater, entering a hollow fiber type T-shaped molecular sieve membrane separation device, performing heat exchange and temperature reduction on an ethanol gas at a product side and the preheater, further cooling through a condenser to obtain an ethanol product with the purity of 99.7% (V/V), condensing the mixed solution at a permeation side, storing a liquid phase in a vacuum buffer tank, wherein the ethanol content is 2% (V/V), and pumping a gas phase away through a vacuum unit.
Example 3
Ethanol content of 95% (V/V), H+Conveying the mixed raw material with the content of 600ppm to a pipeline static mixer through a feed pump, performing acid-base neutralization in the pipeline static mixer by using a 20% sodium bicarbonate solution through a metering pump to a detection tank to obtain a weakly alkaline mixed solution with the pH of 7.6, conveying the weakly alkaline mixed solution to a preheater through a conveying pump, preheating the solution to 65 ℃, and performing evaporation by using a film evaporatorRemoving alkaline substances and inorganic salts in the mixed solution, continuously heating to 110 ℃ through a heater, entering a tubular MOR molecular sieve membrane separation device, carrying out heat exchange and temperature reduction on the ethanol gas at the product side and a preheater, further cooling through a condenser to obtain an ethanol product with the purity of 99.8% (V/V), condensing the mixed solution at the permeation side, storing a liquid phase in a vacuum buffer tank, wherein the ethanol content is 3% (V/V), and pumping a gas phase away through a vacuum unit.
Example 4
Ethanol content of 99% (V/V), H+Conveying the mixed raw material with the content of 200ppm to a pipeline static mixer through a feeding pump, performing acid-base neutralization in the pipeline static mixer by using a 10% sodium bicarbonate solution through a metering pump to a detection tank to obtain a weakly-alkaline mixed solution with the pH of 7.2, conveying the weakly-alkaline mixed solution to a preheater through a conveying pump, preheating to 70 ℃, removing alkaline substances and inorganic salts in the mixed solution through a film evaporator, continuously heating to 120 ℃ through a heater, entering a hollow fiber type ZSM-5 molecular sieve membrane separation device, performing heat exchange and temperature reduction on ethanol gas at a product side and the preheater, further cooling through a condenser to obtain an ethanol product with the purity of 99.9% (V/V), condensing the mixed solution at a permeation side, storing the liquid phase in a vacuum buffer tank, wherein the ethanol content is 5% (V/V), and pumping a gas phase away through a vacuum unit.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
The invention is not the best known technology.
Claims (9)
1. The device for preparing the absolute ethyl alcohol by the acid-base neutralization and membrane separation coupling method comprises a raw material tank, a preheater, a falling film evaporator, a superheater, a steam permeable membrane separation device, a product condenser, a penetrating fluid condenser, a vacuum buffer tank and a vacuum unit, and is characterized in that: the device comprises a raw material tank, a metering pump, a pipeline static mixer, a detection tank and a delivery pump, wherein the raw material tank, the feeding pump and the pipeline static mixer are sequentially communicated through pipelines; the alkali liquor tank, the metering pump and the pipeline static mixer are communicated in sequence through pipelines; the outlet of the pipeline static mixer, the detection tank, the delivery pump, the preheater, the falling film evaporator, the superheater and the steam permeable membrane separation device are communicated in sequence through pipelines; the product side outlet, the preheater, the product condenser and the product tank of the vapor permeable membrane separation device are communicated in sequence through pipelines; the penetrating fluid outlet of the steam permeable membrane separation device, the penetrating fluid condenser, the vacuum buffer tank and the vacuum unit are communicated in sequence through pipelines.
2. The device for preparing the absolute ethyl alcohol by the acid-base neutralization and membrane separation coupling method according to claim 1, which is characterized in that: the steam permeable membrane of the steam permeable membrane separation device is in a tubular or hollow fiber type.
3. The device for preparing the absolute ethyl alcohol by the acid-base neutralization and membrane separation coupling method according to claim 1, which is characterized in that: the vapor permeable membrane is an organic or inorganic membrane and comprises a NaA molecular sieve membrane, a T-shaped molecular sieve membrane, an MOR molecular sieve membrane and a ZSM-5 molecular sieve membrane.
4. A process for the preparation of ethanol in waste water by means of a device according to any one of claims 1 to 3, comprising the following steps:
acid-containing raw materials and alkali liquor are respectively conveyed into a pipeline static mixer through a feeding pump and a metering pump, the acid-containing raw materials and the alkali liquor are subjected to acid-alkali neutralization in the pipeline static mixer, a neutralized product enters a detection tank, and the pH value is detected in real time through an online remote pH meter; if the solvent in the detection tank is neutral or weakly alkaline, the solvent is qualified, and the qualified solvent is conveyed to the preheater through a pump; if the solvent in the detection tank is acidic, the solvent is unqualified, the unqualified solvent is pumped back into the pipeline static mixer through a pump, and acid-base neutralization reaction is further carried out until the pH value of the solvent is qualified; the neutral or alkalescent raw material from the detection tank is pressurized by a delivery pump, enters a preheater, exchanges heat with product steam, enters a falling-film evaporator, is heated and vaporized by saturated steam to obtain raw material steam, and concentrated solution is discharged from the bottom of the falling-film evaporator; meanwhile, raw material steam is heated to 110-150 ℃ by a heater and then enters a steam permeable membrane separation device for separation, and the separated trapped component enters a preheater for heat exchange with raw material liquid and then enters a product condenser for further cooling and enters a product tank; the penetrating fluid obtained by separation enters a penetrating fluid condenser to exchange heat with a low-temperature refrigerant, the liquid phase enters a vacuum buffer tank, and the gas phase maintains the vacuum pressure of 1KPaA through a vacuum pump unit.
5. The process for preparing absolute ethanol according to claim 4, characterized in that: the raw materials to be treated are acidic ethanol with the volume concentration of 85-99%, and H+The concentration is less than or equal to 1000 ppm.
6. The process for preparing absolute ethanol according to claim 4, characterized in that: the alkali liquor is a solution of sodium hydroxide, calcium hydroxide, sodium bicarbonate and sodium carbonate with the mass concentration of 10-50%.
7. The process for preparing absolute ethanol according to claim 4, characterized in that: the pH value of the neutral or weakly alkaline qualified solvent in the detection tank is 7.0-8.0.
8. The process for preparing absolute ethanol according to claim 4, characterized in that: the temperature of the preheated preheater is 65-85 ℃.
9. The process for producing anhydrous ethanol according to claim 4, characterized in that: the volume content of ethanol in the penetrating fluid is 1-5%.
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| US20080207959A1 (en) * | 2007-02-28 | 2008-08-28 | Vaperma Inc. | Ethanol processing with vapour separation membranes |
| CN104262090A (en) * | 2014-09-22 | 2015-01-07 | 江苏九天高科技股份有限公司 | Method and device for producing biomass absolute ethyl alcohol |
| CN105218316A (en) * | 2014-11-28 | 2016-01-06 | 杭州奇纯膜技术有限公司 | A kind of hollow fiber pervaporation membrane prepares the device and method of dehydrated alcohol |
| CN206980472U (en) * | 2017-06-21 | 2018-02-09 | 武汉智宏思博化工科技有限公司 | A kind of industrial equipment of Pervaporation membrane and the tower-coupled production absolute ethyl alcohol of rectifying |
| CN110294665A (en) * | 2019-07-09 | 2019-10-01 | 常州制药厂有限公司 | The recyclable device and recovery method of ethyl alcohol in Doxycycline Hyclate refinement mother liquor |
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- 2021-10-29 CN CN202111275823.1A patent/CN113860994B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080207959A1 (en) * | 2007-02-28 | 2008-08-28 | Vaperma Inc. | Ethanol processing with vapour separation membranes |
| CN104262090A (en) * | 2014-09-22 | 2015-01-07 | 江苏九天高科技股份有限公司 | Method and device for producing biomass absolute ethyl alcohol |
| CN105218316A (en) * | 2014-11-28 | 2016-01-06 | 杭州奇纯膜技术有限公司 | A kind of hollow fiber pervaporation membrane prepares the device and method of dehydrated alcohol |
| CN206980472U (en) * | 2017-06-21 | 2018-02-09 | 武汉智宏思博化工科技有限公司 | A kind of industrial equipment of Pervaporation membrane and the tower-coupled production absolute ethyl alcohol of rectifying |
| CN110294665A (en) * | 2019-07-09 | 2019-10-01 | 常州制药厂有限公司 | The recyclable device and recovery method of ethyl alcohol in Doxycycline Hyclate refinement mother liquor |
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