CN102070401A - Energy-saving process for preparing absolute ethanol from bioethanol aqueous solution - Google Patents
Energy-saving process for preparing absolute ethanol from bioethanol aqueous solution Download PDFInfo
- Publication number
- CN102070401A CN102070401A CN2011100295362A CN201110029536A CN102070401A CN 102070401 A CN102070401 A CN 102070401A CN 2011100295362 A CN2011100295362 A CN 2011100295362A CN 201110029536 A CN201110029536 A CN 201110029536A CN 102070401 A CN102070401 A CN 102070401A
- Authority
- CN
- China
- Prior art keywords
- tower
- rectifying tower
- rectifying
- ethanol
- dehydrated alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- 238000005057 refrigeration Methods 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 229960004756 ethanol Drugs 0.000 claims description 36
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 35
- 239000007788 liquid Substances 0.000 claims description 31
- 241000282326 Felis catus Species 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000005516 engineering process Methods 0.000 claims description 17
- 238000009833 condensation Methods 0.000 claims description 13
- 230000005494 condensation Effects 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000010992 reflux Methods 0.000 claims description 13
- 238000003860 storage Methods 0.000 claims description 13
- 238000007599 discharging Methods 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 7
- 239000007791 liquid phase Substances 0.000 claims description 7
- 239000003507 refrigerant Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 239000012267 brine Substances 0.000 claims description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000012071 phase Substances 0.000 claims description 2
- 239000012808 vapor phase Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 19
- 238000005265 energy consumption Methods 0.000 abstract description 10
- 238000000855 fermentation Methods 0.000 abstract description 6
- 230000004151 fermentation Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 239000002918 waste heat Substances 0.000 abstract 1
- 239000002808 molecular sieve Substances 0.000 description 8
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 8
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 230000001476 alcoholic effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 3
- 238000010533 azeotropic distillation Methods 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000012266 salt solution Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 235000012255 calcium oxide Nutrition 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000004508 fractional distillation Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000011017 operating method Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 235000011132 calcium sulphate Nutrition 0.000 description 1
- 239000001175 calcium sulphate Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000010850 salt effect Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a production method for preparing absolute ethanol from bioethanol aqueous solution. In the method, main equipment comprises vacuum rectifying tower, a return tank, a heat exchanger, an air source heat pump system, a refrigeration system, a vacuum system and the like; and the absolute ethanol with mass concentration of 99.5 to 99.9 percent is obtained after 15 to 25 percent ethanol-aqueous solution subjected to biological fermentation passes through three gradually pressure-reducing rectifying towers. In the process, a heat source is provided to the next level rectifying tower by utilizing heat of the materials in the preceding level rectifying tower; and the insufficient part is supplemented by the air source heat pump system. The ethanol aqueous solution raw material is preheated by utilizing the unused waste heat of the materials discharged from the rectifying towers to form a thermally coupled network, so that energy consumption in the process for producing unit mass of absolute ethanol is reduced by 30 to 48 percent compared with that in other process. The process has the prominent advantages of low energy consumption, high efficiency, small pollution and the like.
Description
Invention field
The present invention relates to produce the new energy-saving process of dehydrated alcohol by the bio-ethanol aqueous solution.
Background technology
Bio-ethanol is meant that fermentation by microorganism with the ethanol that various Wood Adhesives from Biomass get, is a kind of renewable resources; Dehydrated alcohol is meant that water content is not higher than the ethanol of 0.3-0.5%wt, and its relative density is 0.7893(20 ℃), fusing point is :-114.5 ℃, boiling point is 78.32 ℃, and specific refractory power is 1.3614,14 ℃ of flash-points.Dehydrated alcohol is widely used in chemical reagent, agricultural chemicals, medicine, in all conglomeraties such as biology, paint, pigment, makeup, spices, electronics, especially under current petroleum resources situation in short supply, dehydrated alcohol has been joined the fuel of making oil engine in the gasoline in a large number.Because ethanol burning only produces carbonic acid gas and water, can not produce other obnoxious flavour, therefore use ethanol petrol to help reducing pollution to environment.
The production of dehydrated alcohol initial twenties in last century, produce dehydrated alcohol with the excessive moisture that CaO adsorbs in the industrial alcohol (95%), utilize salt effect to produce afterwards again, be about to CaCl
2Add the vapor-liquid equilibrium that changes aqueous ethanolic solution in the industrial alcohol Deng salt.The method for preparing at present dehydrated alcohol mainly contains unslaked lime evaporation, extraction fractional distillation, rectification under vacuum method, ion exchange method, azeotropic distillation, the molten rectification method of salt, anhydrous calciumsulphate method, molecular sieve adsorption and membrane separation process etc.Wherein azeotropic distillation, extraction fractional distillation and molecular sieve adsorption are the main method of present industrial production dehydrated alcohol, and obtained application in practice as the novel molecular sieve adsorption of producing dehydrated alcohol and membrane separation process, have bright development prospect.
The traditional technology of being produced dehydrated alcohol by biological fermentation process is shown in accompanying drawing one, biomass are joined among the fermentation vat V-1 ferment, after fermentation is finished the material among the V-1 is carried out filter at low temperature and separate wherein fermentation residue, obtain containing under the normal temperature fermented liquid of ethanol 15-25%, fermented liquid is obtained 85-90 ℃ feed liquid after by transferpump P-1 and interchanger E-4 to be entered into rectifying tower T-1 by pipeline 3 and carries out initial gross separation, the pressure of rectifying tower T-1 is 1-1.2 normal atmosphere, the temperature of reboiler E-4 is 105-110 ℃, heating medium is a 2-5 kilogram low-pressure steam, cat head obtains containing the mixing solutions of ethanol 85-90%, be mainly water and high-boiling-point impurity at the bottom of the tower, obtain high temperature at the bottom of the tower and contain minute quantity alcoholic acid water, this part water is used for preheating material.The mixing solutions of cat head is entered rectifying tower T-2 by pipeline 7 make with extra care separation, the working pressure of rectifying tower T-2 is generally normal pressure, the temperature of reboiler E-5 is 100-105 ℃, heating medium is a 2-5 kilogram low-pressure steam, cat head obtains the azeotropic liquid of alcohol-water, and its ethanol quality percentage composition is 95.57%.The azeotropic liquid of the alcohol-water of T-2 cat head is entered adsorbing tower with molecular sieve T-3 through piping 11, remove moisture wherein.Obtain the dehydrated alcohol that ethanol content is 99.5%-99.7% after the absorption.Make regenerating molecular sieve with the warm air dehydration of doing afterwards.
The energy consumption that this traditional technology is produced dehydrated alcohol mainly comprises: low-pressure steam and the used hear rate of molecular sieve dehydration regenerated that the tower still reboiler of rectifying tower T-1, T-2 consumes.
Summary of the invention
The purpose of this invention is to provide and a kind ofly produce the more energy-conservation novel process and the device of dehydrated alcohol, shown in accompanying drawing two by the bio-ethanol aqueous solution.The present invention adopts three tower variable-pressure rectification technologies, and is equipped with air source heat pump system, utilizes at the bottom of the tower simultaneously and the used heat of cat head feed liquid and reboiler and feed preheater formation thermal coupling, thereby realizes energy-saving and cost-reducing by a relatively large margin purpose.
Purpose of the present invention can realize by following technical solution:
A kind ofly produce the technology of dehydrated alcohol by the bio-ethanol aqueous solution, it comprises the following steps:
Step 1. is transported to interchanger E-6 and E-8 heat exchange to 40-55 ℃ from will the ferment bio-ethanol feed liquid that contains the about 15-25% of ethanol that obtains of storage tank V-2 with pump P-2, heating medium be the first rectifying tower T-4 overhead vapours and heat the second rectifying tower T-5 tower bottom reboiler E-11 after the tower of the first rectifying tower T-4 at the bottom of the mixed liquor of discharging feed liquid at the bottom of discharging feed liquid and the second rectifying tower T-5 tower, then the bio-ethanol feed liquid being transported to the first rectifying tower T-4 by pipeline 15 separates, the operation absolute pressure of the first rectifying tower T-4 is a 0.3-0.35 normal atmosphere, tower top temperature is 50-55 ℃, the temperature of the first rectifying tower T-4 tower bottom reboiler E-10 is 65-72 ℃, and can provide the air source heat pump system E-13 of hot water more than 80 ℃ that the first rectifying tower T-4 tower bottom reboiler E-10 is heated by one;
After step 2. is distilled through the first rectifying tower T-4, ethanol content reaches 80-90% in the alcohol mixed solution of cat head, its part is refluxed by pipeline 18, part enters into the second rectifying tower T-5 by pipeline 19 and carries out rectifying, the operation absolute pressure of the second rectifying tower T-5 is a 0.15-0.25 normal atmosphere, reflux ratio is selected 0.8-1.2, tower top temperature is 40-45 ℃, the temperature of the second rectifying tower T-5 tower bottom reboiler E-11 is 50-55 ℃, the second rectifying tower T-5 tower bottom reboiler E-11(is provided with two of A/B in case of necessity) mainly heat by T-4 tower still discharging (for 65-72 ℃ the aqueous solution), the shortage of heat part is then by hot water more than air source heat pump system E-13(80 ℃) provide, can obtain purity from the second rectifying tower T-5 top and be the aqueous ethanolic solution more than 95%, it will be as the charging of the 3rd rectifying tower T-6;
The alcohol vapour that the step 3. second rectifying tower T-5 cat head is 40-45 ℃ heats the feed liquid among the E-12 as thermal source by the tower bottom reboiler E-12 that pipeline 20 enters the 3rd rectifying tower T-6, Partial Liquid Phase after the alcohol vapour condensation is delivered to the second rectifying tower T-5 cat head as backflow by reflux pump P-5 after metering, the rest part liquid phase then is admitted among the 3rd rectifying tower T-6 carries out high vacuum rectification, the operation absolute pressure of the 3rd rectifying tower T-6 is a 0.03-0.05 normal atmosphere, reflux ratio is decided (being generally between the 1-3) according to the product purity requirement, the cat head vapor phase temperature is 12-20 ℃, and liquidus temperature is 25-32 ℃ at the bottom of the tower.The 3rd rectifying tower T-6 tower bottom reboiler E-12(is provided with two of A/B in case of necessity) insufficient section of heat is then by hot water more than air source heat pump system E-13(80 ℃) provide, rectifying tower T-6 cat head can continuously extraction mass concentration be the dehydrated alcohol of 99.5-99.9%.
The above-mentioned technology of producing dehydrated alcohol, the negative pressure of the described first rectifying tower T-4, the second rectifying tower T-5 and the 3rd rectifying tower T-6 is to be provided by vacuum system VS-1, VS-2 and VS-3 respectively, before vacuum system, all need be equipped with vacuum buffer device, to keep the stable of pressure.
The above-mentioned technology of producing dehydrated alcohol, step 3, because the 3rd rectifying tower T-6 overhead product steam is 12-20 ℃, so 0-5 ℃ the chilled brine that provides by a refrigeration system R-1 as refrigerant with condensation cat head vapour phase, while is in the exit of three vacuum pump VS-1, VS-2 and VS-3, the cold-trap device that interchanger E-14 and cold-trap V-6 form is set, as the organism that will not be condensed as yet in the vacuum outlet gas once more deep cooling trap among the cold-trap V-6.So, the ethanol loss can be avoided on the one hand, the environmental pollution that causes thus can be prevented on the other hand.
The above-mentioned technology of producing dehydrated alcohol, the refrigerant of described deep cooling interchanger E-14 also are 0-5 ℃ the chilled brines that is provided by refrigeration system R-1.
The present invention optimizes the purifying production process of traditional bio-ethanol, the reboiler E-10 of rectifying tower T-4 is heated by an air source heat pump system E-13, feed liquid and T-5 overhead vapours that the tower bottom reboiler E-11 of rectifying tower T-5 and the tower bottom reboiler E-12 of rectifying tower T-6 then discharge by T-4 tower still respectively heat, insufficient heat part is then replenished by air source heat pump system E-13, makes the heat of whole flow process consumption reduce greatly.Compare with conventional art, it is low that the present invention has energy consumption, pollutes for a short time, and need not carry out the outstanding advantage that azeotropic distillation or extracting rectifying or molecular sieve adsorbing and dewatering can obtain the dehydrated alcohol product.
Technology of the present invention has the following advantages: used heat and reboiler and feed preheater formation thermal coupling at the bottom of cat head and the tower between the three-tower rectification system that (1) utilization is reduced pressure step by step, and energy utilization is more scientific and reasonable; (2) application of vacuum system reduces rectifying tower T-4, T-5, T-6 service temperature greatly, for the use of air source heat pump system provide may, thereby significantly saved the high-grade energy that must adopt in the traditional technology--give birth to steam; (3) rectifying utilizes the thermodynamics ultimate principle--and system pressure exerts an influence to the vapor-liquid equilibrium of system, thereby breaks the normal pressure azeotropic point of alcohol-water, and then can directly obtain dehydrated alcohol by the rectification under vacuum mode; Confirm through theoretical and experimental study that (4) the present invention produces the required total energy consumption of dehydrated alcohol per ton and reduces 33～48% than traditional technology, and relatively low to the grade requirement of the energy.The energy consumption that the present invention produces dehydrated alcohol mainly comprises: vacuum system energy consumption, air source heat pump system energy consumption and refrigeration system energy consumption, and the energy consumption of material-handling pump.
Description of drawings
Figure one is the conventional process flow synoptic diagram.Wherein:
V-1 is a raw material feed liquid storage tank, and T-1, T-2 are rectifying tower, and T-3 is the molecular sieve dehydration tower, E-1, E-2, E-3 are interchanger, and P-1, P-2 are the fluid transferpump, and E-4, E-5 are tower bottom reboiler, F1-1, F1-2 are valve, and 1,2,3,4,5,6,7,8,9,10,11,12 is pipeline.
Figure two is a schematic flow sheet of the present invention.Wherein:
P-2 is the fluid transferpump, V-2 is a raw material feed liquid storage tank, V-3, V-5 is a snubber assembly, V-4, V-6 is a cold-trap, T-4, T-5, T-6 is the rectification under vacuum tower, E-6, E-7, E-8, E-9, E-14, E-15 is an interchanger, E-10, E-11A, B, E-12A, B is a tower bottom reboiler, E-13 is an air source heat pump system, F2-1, F2-2, F2-3, F2-4, F2-5, F2-6, F2-7, F2-8, F2-9, F2-10, F2-11, F2-12, F2-13, F2-14, F2-15 is a valve, VS-1, VS-2, VS-3 is a vacuum system, and R-1 is a refrigeration system, 13,14,15,16,17,18,19,20,21,22,23,24,25,26,27,28,29,30,31,32 is fluid-transporting tubing, 33 is drain, 34,35,36,37,38,39,40,41 is the air source heat pump system pipeline, 42,43,44,45,46,47 is the refrigeration system pipeline, 48,49,50,51,52,53,54 is the vacuum system pipeline.
Embodiment
Further specify the present invention by the following examples.
Embodiment 1: the rectification under vacuum method is produced 10000 tons of/year dehydrated alcohols
The production method operation steps of dehydrated alcohol as shown in Figure 2.This system mainly is made up of equipment such as rectifying tower, return tank, interchanger, air source heat pump system, refrigeration system, vacuum systems.Be provided with metering and control instruments and pipeline at each equipment room.The bio-ethanol that will contain ethanol 22% enters rectifying tower T-4 after interchanger E-6 is preheated to 45 ℃, the theoretical plate number of rectifying tower T-4 tower is 35, tower diameter is 1.2 meters, adopt regular packing without wall flow in the tower, the operation absolute pressure is 0.32 normal atmosphere, it is 70.6 ℃ that reflux ratio is selected 1.0, the first rectifying tower T-4 bottom liquid temperature.Adopt a hot water temperature to provide thermal source for rectifying tower T-4 reboiler for 83 ℃ air source heat pump system E13.After the distillation, the alcohol mixture alcoholic acid content of the first rectifying tower T-4 cat head reaches 90.3%.The condensation rear section is as backflow, and part is sent to the second rectifying tower T-5 by pipeline 19 and carries out rectifying.
The second rectifying tower T-5 theoretical plate number is 40,1.3 meters of tower diameters, working pressure is 0.2 normal atmosphere, reflux ratio selects 1.2, the temperature of tower bottom reboiler E-11 is about 54.1 ℃, the heating medium of tower bottom reboiler E-11A is the discharging (aqueous solution, temperature are 70.6 ℃) of the first rectifying tower T-4 tower still, and the heating medium of tower bottom reboiler E-11B is the hot water that air source heat pump system E13 provides.The second rectifying tower T-5 top can obtain the alcohol vapour more than 95.5%, this steam is introduced in the 3rd rectifying tower T-6 tower bottom reboiler E-12A shell as the heating thermal source, condensed feed liquid enters storage tank V-4, the steam that is not condensed rises to the further condensation of interchanger E-15 by tower bottom reboiler E-12A upper pipe, 2 ℃ of icy salt solutions that the refrigerant of E-15 provides for refrigeration system R-1.Also drop to storage tank V-4 by the liquid phase that obtains after the E-15 condensation.Feed liquid among the storage tank V-4 (ethanol content is more than 95.5%) is then by transferpump P-3, after metering its part be sent to the second rectifying tower T-5 cat head as backflow, another part then is transported to the 3rd rectifying tower T-6 after metering as charging.The shortage of heat part of the 3rd rectifying tower T-6 is then passed through tower bottom reboiler E-12B by air source heat pump system E-13 heat make-up.
The 3rd rectifying tower T-6 theoretical plate number is 120, and 1.6 meters of tower diameters, working pressure are 0.06 normal atmosphere, and tower top temperature is 19.8 ℃, and the temperature of tower bottom reboiler E-12 is 33 ℃.But the 3rd rectifying tower T-6 cat head extraction 1251.0 kg/hr concentration are the dehydrated alcohol of 99.7%wt, and ethanol content is lower than 0.013%wt in the bottom product.
Embodiment 2: the rectification under vacuum method is produced 8000 tons of/year dehydrated alcohols
Operating method such as embodiment 1.The bio-ethanol that will contain ethanol 18% enters the first rectifying tower T-4 after interchanger E-6 is preheated to 43 ℃, the theoretical plate number of the first rectifying tower T-4 tower is 35, tower diameter is 1.2 meters, adopt regular packing without wall flow in the tower, working pressure is 0.31 normal atmosphere, it is 68.7 ℃ that reflux ratio is selected 1.1, the first rectifying tower T-4 bottom liquid temperature.Adopt a hot water temperature to provide thermal source for the first rectifying tower T-4 reboiler for 83 ℃ air source heat pump system E13.After the distillation, the alcohol mixture alcoholic acid content of the first rectifying tower T-4 cat head reaches 88.7%.The condensation rear section is as backflow, and part is sent to the second rectifying tower T-5 by pipeline 19 and carries out rectifying.
The second rectifying tower T-5 theoretical plate number is 40,1.3 meters of tower diameters, working pressure is 0.19 normal atmosphere, reflux ratio selects 1.1, the temperature of reboiler E-11 is about 54 ℃, the heating medium of tower bottom reboiler E-11A is the discharging (aqueous solution, temperature are 68.7 ℃) of the first rectifying tower T-4 tower still, and the heating medium of tower bottom reboiler E-11B is the hot water that air source heat pump system E13 provides.The second rectifying tower T-5 top can obtain the alcohol vapour more than 94.8%, this steam is introduced in the 3rd rectifying tower T-6 tower bottom reboiler E-12A shell as the heating thermal source, condensed feed liquid enters storage tank V-4, and the steam that is not condensed rises to the further condensation of interchanger E-15 by reboiler E-12A upper pipe.2 ℃ of icy salt solutions that the refrigerant of E-15 provides for refrigeration system R-1.Also drop to storage tank V-4 by the liquid phase that obtains after the E-15 condensation.Feed liquid among the storage tank V-4 (ethanol content is more than 94.8%) is then by transferpump P-3, after metering its part be sent to the second rectifying tower T-5 cat head as backflow, another part then is transported to the 3rd rectifying tower T-6 after metering as charging.The shortage of heat part of the 3rd rectifying tower T-6 is then passed through reboiler E-12B by air source heat pump system E-13 heat make-up.
The 3rd rectifying tower T-6 theoretical plate number is 120, and 1.6 meters of tower diameters, working pressure are 0.05 normal atmosphere, and tower top temperature is 19.6 ℃, and the temperature of tower bottom reboiler E-12 is 32.5 ℃.But the 3rd rectifying tower T-6 cat head extraction 1111.2 kg/hr concentration are the dehydrated alcohol of 99.8%wt, and ethanol content is lower than 0.011%wt in the bottom product.
Embodiment 3: the rectification under vacuum method is produced 12000 tons of/year dehydrated alcohols
Operating method such as embodiment 1.The bio-ethanol that will contain ethanol 25.2% enters the first rectifying tower T-4 after interchanger E-6 is preheated to 45 ℃, the theoretical plate number of the first rectifying tower T-4 tower is 35, tower diameter is 1.2 meters, adopt regular packing without wall flow in the tower, working pressure is 0.33 normal atmosphere, it is 70.1 ℃ that reflux ratio is selected 1.2, the first rectifying tower T-4 bottom liquid temperature.Adopt a hot water temperature to provide thermal source for the first rectifying tower T-4 tower bottom reboiler for 83 ℃ air source heat pump system E13.After the distillation, the alcohol mixture alcoholic acid content of the first rectifying tower T-4 cat head reaches 91.2%.The condensation rear section is as backflow, and part is sent to the second rectifying tower T-5 by pipeline 19 and carries out rectifying.
The second rectifying tower T-5 theoretical plate number is 40,1.3 meters of tower diameters, working pressure is 0.2 normal atmosphere, reflux ratio selects 1.05, the temperature of tower bottom reboiler E-11 is about 55 ℃, the heating medium of tower bottom reboiler E-11A is the discharging (aqueous solution, temperature are 70.1 ℃) of the first rectifying tower T-4 tower still, and the heating medium of tower bottom reboiler E-11B is the hot water that air source heat pump system E13 provides.The second rectifying tower T-5 top can obtain the alcohol vapour more than 95.3%, this steam is introduced in the 3rd rectifying tower T-6 tower bottom reboiler E-12A shell as the heating thermal source, condensed feed liquid enters storage tank V-4, and the steam that is not condensed rises to the further condensation of interchanger E-15 by tower bottom reboiler E-12A upper pipe.2 ℃ of icy salt solutions that the refrigerant of interchanger E-15 provides for refrigeration system R-1.Also drop to storage tank V-4 by the liquid phase that obtains after the interchanger E-15 condensation.Feed liquid among the storage tank V-4 (ethanol content is more than 95.3%) is then by transferpump P-3, after metering its part be sent to the second rectifying tower T-5 cat head as backflow, another part then is transported to the 3rd rectifying tower T-6 after metering as charging.The shortage of heat part of the 3rd rectifying tower T-6 is then passed through tower bottom reboiler E-12B by air source heat pump system E-13 heat make-up.
The 3rd rectifying tower T-6 theoretical plate number is 120, and 1.6 meters of tower diameters, working pressure are 0.053 normal atmosphere, and tower top temperature is 20.5 ℃, and the temperature of tower bottom reboiler E-12 is 33.1 ℃.But T-6 cat head extraction 1501.7 kg/hr concentration are the dehydrated alcohol of 99.6%wt, and ethanol content is lower than 0.009%wt in the bottom product.
Claims (7)
1. produce the technology of dehydrated alcohol by the bio-ethanol aqueous solution for one kind, it is characterized in that it comprises the following steps:
Step 1. is transported to interchanger (E-6 and E-8) heat exchange to 40-55 ℃ from raw material feed liquid storage tank (V-2) the bio-ethanol feed liquid that contains the about 15-25% of ethanol that obtains of will fermenting with pump (P-2), heating medium be first rectifying tower (T-4) overhead vapours and heat second rectifying tower (T-5) tower bottom reboiler (E-11) after the tower of first rectifying tower (T-4) at the bottom of the mixed liquor of discharging feed liquid at the bottom of discharging feed liquid and second rectifying tower (T-5) tower, then the bio-ethanol feed liquid being transported to first rectifying tower (T-4) by pipeline (15) separates, the operation absolute pressure of first rectifying tower (T-4) is a 0.3-0.35 normal atmosphere, tower top temperature is 50-55 ℃, the temperature of first rectifying tower (T-4) tower bottom reboiler (E-10) is 65-72 ℃, and can provide the air source heat pump system (E-13) of hot water more than 80 ℃ that first rectifying tower (T-4) tower bottom reboiler (E-10) is heated by one;
After step 2. is distilled through first rectifying tower (T-4), ethanol content reaches 80-90% in the alcohol mixed solution of cat head, its part is refluxed by pipeline (18), part enters into second rectifying tower (T-5) by pipeline (19) and carries out rectifying, the operation absolute pressure of the second rectifying tower T-5 is a 0.15-0.25 normal atmosphere, reflux ratio is selected 0.8-1.2, tower top temperature is 40-45 ℃, the temperature of second rectifying tower (T-5) tower bottom reboiler (E-11) is 50-55 ℃, second rectifying tower (T-5) tower bottom reboiler (E-11) mainly heats by the discharging of (T-4) tower still, the shortage of heat part is then provided by air source heat pump system (E-13), can obtain purity from second rectifying tower (T-5) top and be the aqueous ethanolic solution more than 95%, it will be as the charging of the 3rd rectifying tower (T-6);
The alcohol vapour that step 3. second rectifying tower (T-5) cat head is 40-45 ℃ heats the feed liquid in the tower bottom reboiler (E-12) as thermal source by the tower bottom reboiler (E-12) that pipeline (20) enters the 3rd rectifying tower (T-6), Partial Liquid Phase after the alcohol vapour condensation is delivered to second rectifying tower (T-5) cat head as backflow by reflux pump (P-5) after metering, the rest part liquid phase then is admitted in the 3rd rectifying tower (T-6) carries out high vacuum rectification, the operation absolute pressure of the 3rd rectifying tower (T-6) is a 0.03-0.05 normal atmosphere, reflux ratio requires according to product purity and decides, the cat head vapor phase temperature is 12-20 ℃, and liquidus temperature is 25-32 ℃ at the bottom of the tower; The insufficient section of the 3rd rectifying tower (T-6) tower bottom reboiler (E-12) heat is then provided by air source heat pump system (E-13), and rectifying tower (T-6) cat head can continuously extraction mass concentration be the dehydrated alcohol of 99.5-99.9%.
2. the technology of producing dehydrated alcohol according to claim 1 is characterized in that: described second rectifying tower of step 2 (T-5) is provided with two tower bottom reboilers of A/B (E-11) in case of necessity.
3. the technology of producing dehydrated alcohol according to claim 1 is characterized in that: described the 3rd rectifying tower of step 3 (T-6) is provided with two tower bottom reboilers of A/B (E-12) in case of necessity.
4. the technology of producing dehydrated alcohol according to claim 1 is characterized in that: the reflux ratio of described the 3rd rectifying tower of step 3 (T-6) is 1-3.
5. the technology of producing dehydrated alcohol according to claim 1, it is characterized in that: the negative pressure of described first rectifying tower (T-4), second rectifying tower (T-5) and the 3rd rectifying tower (T-6) is to be provided by three vacuum systems (VS-1, VS-2 and VS-3) respectively, before vacuum system, all need be equipped with vacuum buffer device, to keep the stable of pressure.
6. the described technology of producing dehydrated alcohol arbitrary according to claim 1 to 5, it is characterized in that: in step 3, because the 3rd rectifying tower (T-6) overhead product steam is 12-20 ℃, so 0-5 ℃ the chilled brine that provides by refrigeration system (R-1) as refrigerant with condensation cat head vapour phase, while is in the exit of three vacuum pumps (VS-1, VS-2 and VS-3), the cold-trap device that interchanger (E-14) and cold-trap (V-6) are formed is set, as the organism that will not be condensed as yet in the vacuum outlet gas once more deep cooling trap among the cold-trap (V-6).
7. the technology of producing dehydrated alcohol according to claim 5 is characterized in that: the refrigerant of described deep cooling interchanger (E-14) is 0-5 ℃ the chilled brine that is provided by refrigeration system (R-1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100295362A CN102070401B (en) | 2011-01-27 | 2011-01-27 | Energy-saving process for preparing absolute ethanol from bioethanol aqueous solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100295362A CN102070401B (en) | 2011-01-27 | 2011-01-27 | Energy-saving process for preparing absolute ethanol from bioethanol aqueous solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102070401A true CN102070401A (en) | 2011-05-25 |
| CN102070401B CN102070401B (en) | 2013-12-04 |
Family
ID=44029183
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100295362A Expired - Fee Related CN102070401B (en) | 2011-01-27 | 2011-01-27 | Energy-saving process for preparing absolute ethanol from bioethanol aqueous solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102070401B (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102294204A (en) * | 2011-07-07 | 2011-12-28 | 南京大学 | Integrated system technology of fixed bed and injection floating bed coupled with separating unit |
| CN102380217A (en) * | 2011-11-24 | 2012-03-21 | 中国船舶重工集团公司第七�三研究所 | Automatic alcohol recycling system |
| 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 |
| CN104610019A (en) * | 2015-02-05 | 2015-05-13 | 中石化上海工程有限公司 | Method for producing absolute ethyl alcohol |
| CN105566065A (en) * | 2015-12-31 | 2016-05-11 | 济南开发区星火科学技术研究院 | Extraction apparatus for preparing mixed alcohol through fermenting cellulose, and method thereof |
| CN106349935A (en) * | 2016-08-23 | 2017-01-25 | 广西兴业县新贵松脂厂 | Efficient energy-saving processing method of rosin |
| CN106349944A (en) * | 2016-08-23 | 2017-01-25 | 广西兴业县新贵松脂厂 | Energy-saving rosin processing method |
| CN106397471A (en) * | 2016-08-16 | 2017-02-15 | 湖北兴发化工集团股份有限公司 | Vaporization energy saving equipment for silicone monomer raw material methyl chloride and process thereof |
| CN116531788A (en) * | 2023-06-20 | 2023-08-04 | 泰兴市凌飞化学科技有限公司 | Nonylphenol polyoxyethylene ether rectification system and rectification method |
| CN118161872A (en) * | 2024-05-13 | 2024-06-11 | 北京理工大学 | Ethanol refining device and method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1186450C (en) * | 2003-05-13 | 2005-01-26 | 南京工业大学 | Method for preparing absolute ethyl alcohol by biomass fermentation and membrane pervaporation |
| CN101225017A (en) * | 2008-01-24 | 2008-07-23 | 复旦大学 | Method and device for producing fuel alcohol by fermentation liquor distillation-free whole molecular sieve adsorptive separation |
| CN101891590A (en) * | 2010-08-05 | 2010-11-24 | 湖南农业大学 | Method for producing anhydrous ethanol from fermentation liquid by gas adsorption |
-
2011
- 2011-01-27 CN CN2011100295362A patent/CN102070401B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1186450C (en) * | 2003-05-13 | 2005-01-26 | 南京工业大学 | Method for preparing absolute ethyl alcohol by biomass fermentation and membrane pervaporation |
| CN101225017A (en) * | 2008-01-24 | 2008-07-23 | 复旦大学 | Method and device for producing fuel alcohol by fermentation liquor distillation-free whole molecular sieve adsorptive separation |
| CN101891590A (en) * | 2010-08-05 | 2010-11-24 | 湖南农业大学 | Method for producing anhydrous ethanol from fermentation liquid by gas adsorption |
Non-Patent Citations (1)
| Title |
|---|
| 韩秀丽等: "生物质吸附法制取无水乙醇的研究进展", 《酿酒科技》 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102294204A (en) * | 2011-07-07 | 2011-12-28 | 南京大学 | Integrated system technology of fixed bed and injection floating bed coupled with separating unit |
| CN102294204B (en) * | 2011-07-07 | 2013-07-10 | 南京大学 | Integrated system technology of fixed bed and injection floating bed coupled with separating unit |
| CN102380217A (en) * | 2011-11-24 | 2012-03-21 | 中国船舶重工集团公司第七�三研究所 | Automatic alcohol recycling system |
| 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 |
| CN104610019B (en) * | 2015-02-05 | 2017-01-04 | 中石化上海工程有限公司 | The method producing dehydrated alcohol |
| CN104610019A (en) * | 2015-02-05 | 2015-05-13 | 中石化上海工程有限公司 | Method for producing absolute ethyl alcohol |
| CN105566065A (en) * | 2015-12-31 | 2016-05-11 | 济南开发区星火科学技术研究院 | Extraction apparatus for preparing mixed alcohol through fermenting cellulose, and method thereof |
| CN106397471A (en) * | 2016-08-16 | 2017-02-15 | 湖北兴发化工集团股份有限公司 | Vaporization energy saving equipment for silicone monomer raw material methyl chloride and process thereof |
| CN106397471B (en) * | 2016-08-16 | 2018-09-28 | 湖北兴发化工集团股份有限公司 | A kind of the vaporizing energy-saving device and technique of organic silicon monomer raw material chloromethanes |
| CN106349935A (en) * | 2016-08-23 | 2017-01-25 | 广西兴业县新贵松脂厂 | Efficient energy-saving processing method of rosin |
| CN106349944A (en) * | 2016-08-23 | 2017-01-25 | 广西兴业县新贵松脂厂 | Energy-saving rosin processing method |
| CN116531788A (en) * | 2023-06-20 | 2023-08-04 | 泰兴市凌飞化学科技有限公司 | Nonylphenol polyoxyethylene ether rectification system and rectification method |
| CN118161872A (en) * | 2024-05-13 | 2024-06-11 | 北京理工大学 | Ethanol refining device and method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102070401B (en) | 2013-12-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102070401B (en) | Energy-saving process for preparing absolute ethanol from bioethanol aqueous solution | |
| CN100526274C (en) | Method for rectifying ethanol by three-tower heat integration device | |
| CN109908616B (en) | Energy-saving distillation system for preparing ethanol from carbon monoxide and distillation method thereof | |
| CN102343162A (en) | Energy-saving evaporating process and equipment for L-phenylalanine brine solution | |
| CN104262089B (en) | Method and device for dehydrating and refining biofuel | |
| CN1861553A (en) | Rectifying tech. and equipment of high purity methanol | |
| CN110256202B (en) | Four-tower four-effect crude methanol refining process method | |
| CN110143850A (en) | The not energy-saving methanol multi-effect distillation method of the single column steam drive of by-product fusel oil | |
| CN105344124A (en) | Double-rectifying-tower four-effect superior alcohol distillation method and device for preparing alcohol | |
| CN109704920B (en) | Energy-saving process and device for producing fuel ethanol from low-concentration fermentation liquor | |
| CN109438196B (en) | Method for preparing 2, 2-dimethoxypropane | |
| CN101357879B (en) | Methanol three-tower rectification system and technique | |
| CN103060480A (en) | Plate-type evaporator and application thereof to evaporation system in refined sugar factory | |
| CN204058301U (en) | A kind of production equipment of biomass dehydrated alcohol | |
| CN110483249A (en) | A kind of six tower quadruple effect rectificating method of single column steam drive type methanol of not by-product fusel oil | |
| CN101712592B (en) | Process for producing absolute ethanol through low-grade heat source | |
| CN201668968U (en) | Energy-saving system for five-tower three-stage differential-pressure distilling production of edible alcohol | |
| CN209721997U (en) | From the energy saving technique device of low concentration fermentation liquid production alcohol fuel | |
| CN210096970U (en) | Furfural multiple-effect reaction rectifying device | |
| CN208292896U (en) | The methanol recovery device of methyl tertiary butyl ether(MTBE) production | |
| CN210021208U (en) | Distillation energy-saving system for preparing ethanol from carbon monoxide | |
| CN203474692U (en) | Efficient and energy-saving preparation device of acetyl acetone | |
| CN203196360U (en) | Manufacturing device of acraldehyde | |
| CN101851152A (en) | Method for preparing dimethyl ether by methyl alcohol gaseous phase dehydration | |
| CN106316793A (en) | Alcohol preparing device and method based on the double rectification column and six-column and four-effect distillation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20131204 Termination date: 20210127 |