CN1380274A - Alcohol refining process for producing several products - Google Patents
Alcohol refining process for producing several products Download PDFInfo
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- CN1380274A CN1380274A CN 02117068 CN02117068A CN1380274A CN 1380274 A CN1380274 A CN 1380274A CN 02117068 CN02117068 CN 02117068 CN 02117068 A CN02117068 A CN 02117068A CN 1380274 A CN1380274 A CN 1380274A
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 195
- 238000000034 method Methods 0.000 title claims abstract description 49
- 230000008569 process Effects 0.000 title claims abstract description 39
- 238000007670 refining Methods 0.000 title claims abstract description 35
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 100
- 238000001179 sorption measurement Methods 0.000 claims abstract description 72
- 238000011084 recovery Methods 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 claims abstract description 20
- 230000018044 dehydration Effects 0.000 claims abstract description 13
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims description 66
- 241000282326 Felis catus Species 0.000 claims description 33
- 238000005516 engineering process Methods 0.000 claims description 32
- 238000003795 desorption Methods 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 19
- 235000002595 Solanum tuberosum Nutrition 0.000 claims description 16
- 244000061456 Solanum tuberosum Species 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 16
- 238000007600 charging Methods 0.000 claims description 15
- 238000009833 condensation Methods 0.000 claims description 13
- 230000005494 condensation Effects 0.000 claims description 13
- 239000001760 fusel oil Substances 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 12
- 239000002351 wastewater Substances 0.000 claims description 11
- 238000010521 absorption reaction Methods 0.000 claims description 10
- 230000000274 adsorptive effect Effects 0.000 claims description 9
- 239000002808 molecular sieve Substances 0.000 claims description 9
- 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 9
- 239000012071 phase Substances 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 7
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- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims description 4
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- 238000011069 regeneration method Methods 0.000 claims description 3
- 210000000689 upper leg Anatomy 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 10
- 229960004756 ethanol Drugs 0.000 description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 34
- 239000002594 sorbent Substances 0.000 description 13
- 239000000446 fuel Substances 0.000 description 10
- 239000012535 impurity Substances 0.000 description 8
- 238000000855 fermentation Methods 0.000 description 7
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 3
- 235000013361 beverage Nutrition 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- 229910002796 Si–Al Inorganic materials 0.000 description 2
- 238000010533 azeotropic distillation Methods 0.000 description 2
- 230000000035 biogenic effect Effects 0.000 description 2
- 235000011089 carbon dioxide Nutrition 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
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- 229960000935 dehydrated alcohol Drugs 0.000 description 2
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
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- 229910052680 mordenite Inorganic materials 0.000 description 2
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- UPLPHRJJTCUQAY-WIRWPRASSA-N 2,3-thioepoxy madol Chemical compound C([C@@H]1CC2)[C@@H]3S[C@@H]3C[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@](C)(O)[C@@]2(C)CC1 UPLPHRJJTCUQAY-WIRWPRASSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000010364 biochemical engineering Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
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Abstract
本发明是涉及一种多产品酒精精制工艺。是根据无水酒精与食用酒精精制脱水的相同与不同的生产工艺特点研究开发的。实现无水酒精与食用酒精同时生产装置,它采用的设备有精流塔、脱醛塔、精塔、脱甲醇塔、回收塔、吸附塔,在各塔之间设置有阀门和相应的管线,还设置有冷凝器、再沸器、预热器,利用酒度为5－30%的原料液,根据需要开启所需要的塔和通过控制阀门,生产出所需要的酒精。该工艺流程既可以单独生产各种规格的食用酒精,又可以单独生产各种规格的无水酒精,也可以同时生产各种规格的食用酒精和无水酒精。
The invention relates to a multi-product alcohol refining process. It is researched and developed according to the same and different production process characteristics of anhydrous alcohol and edible alcohol refining and dehydration. Realize the simultaneous production of anhydrous alcohol and edible alcohol. The equipment it adopts includes a fine flow tower, a dealdehyde tower, a fine tower, a methanol removal tower, a recovery tower, and an adsorption tower. There are valves and corresponding pipelines between the towers. A condenser, a reboiler and a preheater are also provided, and the required alcohol is produced by opening the required towers and controlling the valves as required by using the raw material liquid with an alcohol content of 5-30%. The technological process can not only produce edible alcohol of various specifications alone, but also can produce various specifications of anhydrous alcohol alone, and can also produce various specifications of edible alcohol and anhydrous alcohol at the same time.
Description
Technical field
The present invention relates to the organic preparation method of alcohols, particularly a kind of alcohol refining process for producing several products.
Background technology
Fermentation alcohol is a kind of reproducible important foundation raw material and product.Different according to functions of use with purity requirement, be divided into edible ethanol and raw spirit product.Raw spirit is mainly as the solvent and the widespread use of Chemical Manufacture raw material of fuel (also claiming fuel alcohol), electronic component manufacturing, superior cosmetics.The edible ethanol product specification mainly is general level alcohol, top grade alcohol and special top grade alcohol, is mainly used to beverages wine.
Entering in 20th century with the epoch of oil as the raw material of main energy sources and petroleum chemicals.But two serious problems have also appearred thereupon: the one, and oil is non-renewable resource, because a large amount of exploitation, consumes too fastly, has faced exhaustion; The 2nd, act as a fuel and the chemical raw material has caused the havoc, particularly CO of environment with oil
2Greenhouse effect.Based on the reason of above two aspects, the clean fuel that people are making great efforts to develop the new reproducible energy and can not pollute environment.
With the raw spirit of fermentative Production, have the combustionproperty similar with mineral fuel, its raw materials for production are biogenic, are a kind of reproducible energy.In addition, carbon monoxide and sulfurous gas that the ethanol combustion processes is discharged all are lower than gasoline combustion, remain basically stable on the quantity of carbonic acid gas that is produced and the carbonic acid gas that growth is consumed as the biogenic of raw material, this is to reducing atmospheric pollution and to suppress Greenhouse effect significant.Therefore, fuel alcohol is also referred to as " clean fuel ".
The alcohol that is used for fuel requires the water of alcohol is removed to below the 8000ppm.Because there is minimum boiling point in the mixture of second alcohol and water, the sepn process of traditional distillation technology.The essential technology such as azeotropic distillation, extracting rectifying that adopt.Method at azeotropic distillation will be introduced entrainer, entrainer commonly used has benzene, hexanaphthene, pentane, ether etc., these traditional special extract rectification process energy consumptions are higher, and steam mono-consumption is up to 7000 ~ 8000KJ/l ethanol, and the production that this type of technology is used for fuel alcohol is uneconomic.
People (USP4,273,621) such as Fornoff Louis L. have proposed a kind of CO of utilization
2Be carrier gas, adopt the adsorption process that thickens of molecular sieve gas phase selective adsorption water.The defective of this method is CO
2Degree of depth cooling need extra equipment and power consumption, the normal temperature cooling can't reach the ideal drying effect, and then makes CO
2Regenerative power to sorbent material is limited.
Edible ethanol is used for beverages and has a long history, over nearly 20 years, development along with the biochemical engineering technology, traditional workshop-based edible ethanol production technique is substituted by large-scale continuous production technique day by day, production cost descends, quality product improves, and has satisfied people to the quality of life and the health requirements of drinking.Adopt the high grade edible spirit beverages to become the main flow trend of market comsupton.China units concerned are with reference to the present alcohol quality standard of developed country in the world, and the national standard of existing alcohol product quality is revised in decision.The state quality standard of new alcohol product will be publicized and implemented soon.The quality standard of revised national alcohol product, product indexs such as high grade edible spirit integrate with mutually with present international edible ethanol standard.
The stock liquid of raw spirit and edible ethanol product purification dehydration workshop section, be example with the fermentation liquid, ethanol content is at 5-30% (V), and all the other are water, and contain impurity such as organic acid, aldehyde, ester and methyl alcohol.Edible ethanol and raw spirit product requirement are not quite similar, and raw spirit is had relatively high expectations to water-content, and the water-content of the raw spirit that acts as a fuel is less than 8000ppm according to national standard (GB18350-2001).And the water-content general requirement near the azeotropic point of ethanol and water, but has strict requirement to impurity such as aldehyde, ester and methyl alcohol less than 5% (V) (GB10343-2000 suggestion original text) in the edible ethanol, and the methanol content of wherein special top grade alcohol is less than 2ppm.Therefore, have identical point that difference is also arranged on refining dewatering process: the difference raw spirit need adopt special separation means such as smart gold-plating of azeotropic extraction or absorption that azeotropic water is removed, edible ethanol need not deviate from azeotropic water, but need take the precise distillation technology to remove impurity such as aldehyde, potato spirit, ester and methyl alcohol; Both identical points all need remove impurity such as water and organic acid, ethanol are carried dense, adopt technology such as thermal coupling to reduce the consumption of steam etc. in refining dewatering process.In the biomass to alcohol conversion process flow process, the product purification dehydration has critical role, and it has not only determined the quality of final alcohol product, and is controlling product yield and general facilities consumption, can be rated as the gordian technique of Alcohol Production process.
In the production technique of the refining dehydration of Alcohol Production at present, device is set up in raw spirit and edible ethanol production usually separately, the refining dewatering unit of raw spirit can only be used for producing the raw spirit product, the refining dewatering unit of edible ethanol can only be used for producing the edible ethanol product, product of less types, the market adaptability is relatively poor.According to the identical and different production technology characteristic of raw spirit with the refining dehydration of edible ethanol, the research and development alcohol refining process for producing several products.Realize raw spirit and edible ethanol production equipment simultaneously, make device have stronger anti-market risk ability, the market requirement is widely arranged.
Summary of the invention
Alcohol refining process for producing several products of the present invention is to research and develop with the identical and different production technology characteristic of the refining dehydration of edible ethanol according to raw spirit.Realize raw spirit and edible ethanol production equipment simultaneously, technical problem to be solved by this invention just.
Technology of the present invention is achieved in that
A kind of alcohol refining process for producing several products, the equipment that it adopts has smart stream tower, dealdehyder tower, smart tower, eparating methanol tower, recovery tower, adsorption tower, between each tower, be provided with valve and corresponding pipeline, also be provided with condenser, reboiler, preheater, utilize the stock liquid of wine degree for 5-30%, open needed tower as required and, produce needed alcohol by by-pass valve control.
The invention provides a kind of stock liquid that utilizes the wine degree for 5-30%, adopt refining dehydration techniques such as thermal coupling rectifying and the absorption of alternating temperature transformation, realize alcohol refining process for producing several products.Promptly can produce edible ethanol, the raw spirit of all size separately, also can produce the edible ethanol and the raw spirit of all size simultaneously.
This production technique adopts the high-efficiency and precision distillation technology, the quantity of rectification cell reasonably is set, guaranteed effectively shifting out of various different impurities, improve separation efficiency and product yield to greatest extent, dexterously high efficient packed column technology and tray column technology are combined, the separating power of rectification cell, the accuracy of side line extraction setting and the reliability of equipment all are greatly improved, have reduced process cost.Adopt advanced reasonably thermal coupling distillation technology simultaneously, as much as possible utilize the potential heat energy of each stream thigh, thereby farthest reduced steam and the consumption of cooling-water in the rectifying.The employing of technology such as unique condensation pressure and temperature varying adsorption dewatering and the design of high-efficiency energy-storage adsorber has realized the high-level efficiency that azeotropic water removes.This technical process both can have been produced the edible ethanol of all size separately, can produce the raw spirit of all size again separately, also can produce the edible ethanol and the raw spirit of all size simultaneously.
Owing to adopt whole process process simulation and emulation technology, realize the optimized design of whole process and each unit equipment in addition,, can obtain the edible ethanol and the raw spirit product of a plurality of grades by this flow process of adjusting process parameter.This flow process makes device realize the variation of product, and the market competitiveness is stronger.
Description of drawings
Fig. 1: alcohol refining process for producing several products schematic flow sheet.
Device symbols is described as follows: 1,2,3,4,5,6,7,8,10,11,12,13,14,15,16,17,18,19,20,21,22,23, and the 24-valve; The 25-topping still, 26-dealdehyder tower, the smart tower of 27-, 28-eparating methanol tower, the 29-recovery tower, 30A/B-adsorption tower, the thick tower reboiler of 31-, 32-methanol column reboiler, 33-revivifier preheater, 34-etna, 36-resurgent gases condenser, 37-raw spirit product condenser.
Concrete true mode
Embodiment 1: the edible ethanol processing step:
As shown in Figure 1, the rectified purified operation of edible ethanol thermal coupling mainly is made up of unit equipments such as topping still, smart tower, dealdehyder tower, eparating methanol tower and recovery towers.
(1) be that the stock liquid of 5-30% enters topping still 25 with ethanol content, after vapour-liquid mass separated, waste liquid was discharged from the tower still, delivered to off-side and handled.Open valve 1, the thick wine of cat head extraction is delivered to dealdehyder tower 26.This tower decompression operation pressure is-0.02～-0.08Mpa, the heating medium of reboiler 31 is the overhead vapours of smart tower 27.The main task of topping still is to remove most of water, organic acid and the heavy component impurity etc. of coming with the fermentation liquid band.
(2) send into dealdehyder tower 26 from the light wine of topping still top extraction, reflux through eparating methanol tower reboiler 32 heat exchange condensation rear sections, recovery tower 29 is delivered in the extraction of part cat head.Open valve 3 is delivered to smart tower 27 chargings after the light wine preheating of tower still extraction.The overhead vapours of this tower is as the reboiler heating medium of eparating methanol tower, and this tower working pressure is 0.0～0.1Mpa.
(3) smart tower 27 composite structure that adopts high efficient packed column technologies and tray column to combine, smart tower is the wine degree that guarantees the finished product, the important separating device of control potato spirit and other foreign matter content.Light wine from full gear Tata still is sent into smart tower.The overhead vapours of smart tower is delivered to thick tower reboiler 31 as heating medium.Eparating methanol tower is further refining delivering near the alcohol in high concentration of the side line place extraction of cat head.Open valve 7,4 is delivered to the recovery tower charging with the rich fusel-oil fraction and the cat head extraction stream thigh of the side line extraction of tower middle and lower part.The processing wastewater of tower still extraction is discharged system. and this tower working pressure is 0.0～0.3Mpa.
(4) deliver to eparating methanol tower 28 from the alcohol in high concentration of smart tower side line extraction.Open valve 23, eparating methanol tower cat head extraction industrial spirit.Open valve 13, the edible ethanol product by all sizes such as adjusting process parameter top grades is from the extraction of tower still.This tower decompression operation pressure is-0.02～-0.08Mpa.
(5) deliver to recovery tower 29 from the potato spirit wine of smart tower side line extraction stream strand and dealdehyder tower cat head extraction stream strand etc., open valve 11, recovery tower cat head extraction industrial spirit, open valve 12, potato spirit wine is from the side line extraction of tower bottom, obtain fusel-oil fraction through the potato spirit tripping device, light wine returns recovery tower.Tower still waste water is discharged system, and this tower working pressure is a normal pressure.
By this embodiment, selecting raw material is the fermentation liquid that contains ethanol 12% (V), technical process according to above narration, by fecund product alcohol refining plant shown in Figure 1, can obtain the wine degree is 96.5% (V), methanol content≤2ppm, potato spirit content≤2ppm, the special high grade edible spirit product of oxidization time 〉=40min.Embodiment 2: the raw spirit processing step:
As shown in the figure 1, the refining dehydration procedure of raw spirit mainly is made up of operating units such as topping still, smart tower, adsorption towers.
(1) be that the stock liquid of 5-30% enters topping still with content, after vapour-liquid mass separated, waste liquid was discharged from the tower still, delivered to off-side and handled.Open valve 2, the thick wine of cat head extraction is delivered to smart tower.This tower decompression operation pressure is 0～-0.08Mpa, the heating medium of reboiler 31 is the overhead vapours of smart tower.The main task of topping still is to remove most of water of coming with the fermentation liquid band, organic acid impurity etc.
(2) smart tower adopts the composite structure that high efficient packed column technology and tray column combine, and it is the wine degree that further improves the raw material of adsorption dewatering operation that smart tower mainly acts on, and more forms more desirable near azeotropic.Send into smart tower charging from the thick wine of thick column overhead, open valve 6, the overhead vapours part of smart tower is as the heating medium of reboiler 31, and part is delivered to adsorption tower 30 and is removed azeotropic water.Open valve 8, the rich fusel-oil fraction of tower middle and lower part side line extraction obtains fusel-oil fraction through the potato spirit tripping device, and light wine returns smart tower.The processing wastewater of tower still extraction is discharged system.This tower working pressure is 0.0～0.5Mpa.
(3) from the alcohol vapor of smart column overhead after etna 34 heating, open valve 14,18 and carry out the adsorption dewatering operation by the adsorbing tower with molecular sieve 30A that is in adsorbed state from bottom to top.Alcohol steam after the dehydration enters raw spirit product condenser 37 and carries out condensation, and phlegma is sent into raw spirit finished product jar.The adsorptive pressure scope is 0.2 ~ 0.5Mpa.
In adsorber, the sorbent material that can carry out selective adsorption to ethanol, water is housed.This kind sorbent material can be a Si-Al molecular sieve, and selectable molecular sieve is A type, X type, mordenite type, ZSM type etc.In adsorption tower, water is adsorbed agent absorption, and ethanol is discharged outside the adsorption tower by bed, obtains the very low alcohol product of water-content through condensation.The pressure of this technology adsorption operations is gauge pressure 0 ~ 0.6Mpa.System pressure is provided when ethanol water mixture is vaporized by vaporizer, and the moving equipment that gas blower etc. is used for supercharging need be set.In this technology desorption manipulation, adopt the negative pressure desorb, this falls adsorbed water to the adsorption tower desorption is very favorable.Proceed to a certain degree at the negative pressure desorption manipulation, to introduce the adsorption tower that carries out desorption by very low ethanol from the water-content that adsorption tower obtains, water to the adsorption tower institute desorption that carries out desorption manipulation purges completely, further removes the adsorbed water of adsorption tower of desorption.Through desorption, purging, water adsorbed in the adsorption tower is thoroughly removed.Reenter adsorption operations.For whole technology is carried out continuously, 2 above adsorption towers are set, the adsorption-desorption operation hockets.
In finishing experiment of the present invention, find, the raising of adsorptive pressure is favourable to the absorption content of water and sorbent material to the adsorption selectivity of second alcohol and water to sorbent material, and the raising of adsorptive pressure can improve the pressure difference of adsorption operations and desorption manipulation, and this helps the desorption of the adsorbed water of sorbent material.For the selected adsorptive pressure of this this technology at 0 ~ 0.6MPa, the preferred pressure scope is 0.2 ~ 0.5Mpa.Sweeping gas temperature of the present invention is 120 ~ 220 ℃, and preferred service temperature is 150 ~ 200 ℃.
(4) after adsorption tower absorption 30A operation was finished, adsorption tower 30B entered adsorption operations, and shut-off valve 14,18, open valve 15 carry out transformation and alternating temperature desorb operation.Switch- valve 21,22,19,20 successively according to switch-valve 14,15, and 17,18 switching sequences are operated.Stripping gas is through 36 condensations of resurgent gases condenser, and open valve 5, phlegma are delivered to the smart tower charging of ethanol refinery workshop section.After pressure is reduced to certain value, open valve 16,17, adopt the raw spirit product steam after dewatering to wash through 33 heating of revivifier preheater.Shut-off valve 16,17,15, the adsorption tower of finishing desorption and regeneration reenters the adsorption operations situation.Desorption pressures is-0.05 ~ 0.5Mpa, and the service temperature of sweeping gas is that 150 ~ 200 light wine return smart tower, and the processing wastewater of tower still extraction is discharged system.
The main effect of adsorption tower is finally to obtain the raw spirit product by the remaining moisture content that sorbent material removes in alcohol and the water azeotropic mixture, and adsorption tower is common more than two, alternately finishes the adsorption-desorption operation successively, realizes charging extraction operate continuously.
By this embodiment, selecting raw material is the fermentation liquid that contains ethanol 12% (V), technical process according to above narration, by fecund product alcohol refining plant shown in Figure 1, can obtain water-content less than 4000ppm, acidity (with acetometer) is less than 56ppm (mg/L), the qualified dehydrated alcohol product of pH value 6.5～9.0.
Embodiment 3: edible ethanol and raw spirit be production craft step simultaneously:
As shown in Figure 1: mainly form by unit equipments such as topping still, smart tower, dealdehyder tower, eparating methanol tower, recovery tower and adsorption towers.
(1) be that the stock liquid of 5-30% enters topping still with ethanol content, after vapour-liquid mass separated, waste liquid was discharged from the tower still, delivered to off-side and handled.Shut-off valve 2, the thick wine of cat head extraction is delivered to dealdehyder tower.This tower decompression operation pressure is 0～-0.08Mpa, the heating medium of thick tower reboiler is the overhead vapours and the raw spirit product vapour of smart tower.The main task of topping still is to remove most of water, organic acid and the heavy component impurity etc. of coming with the fermentation liquid band.
(2) send into dealdehyder tower from the light wine of thick cat head extraction, the cat head extraction refluxes through eparating methanol tower reboiler heat exchange condensation rear section, and alcohol distillation column is delivered in the extraction of part cat head.Open valve 3 is delivered to smart tower charging after the light wine preheating of tower still extraction.The overhead vapours of this tower is as the reboiler heating medium of eparating methanol tower, and this tower working pressure is 0.0～0.1Mpa.
(3) smart tower adopts the composite structure that high efficient packed column technology and tray column combine, and smart tower is the wine degree that guarantees the edible ethanol product, improves raw spirit adsorption dewatering raw wine degree.Light wine from full gear Tata still is sent into smart tower.Open valve 6, the overhead vapours of the smart tower of part is delivered to thick tower reboiler as heating medium, and part cat head extraction vapour phase or liquid phase are delivered to the adsorption tower etna, remove azeotropic water, produce raw spirit.Eparating methanol tower is further refining delivering near the alcohol in high concentration of the side line place extraction of cat head, according to edible ethanol and raw spirit turnout, adjusts cat head vapour phase produced quantity and alcohol in high concentration and delivers to the eparating methanol tower amount.Open valve 7 is delivered to the recovery tower charging with the rich fusel-oil fraction of tower middle and lower part side line extraction.The processing wastewater of tower still extraction is discharged system.This tower working pressure is 0.0～0.5Mpa.
(5) deliver to eparating methanol tower from the alcohol in high concentration of smart tower side line extraction, open valve 24, eparating methanol tower cat head extraction methyl alcohol alcohol, and deliver to recovery tower.Open valve 13, the edible ethanol product of all sizes such as top grade is from the extraction of tower still.This tower decompression operation pressure is-0.08～0Mpa.
Deliver to recovery tower from the potato spirit wine of smart tower side line extraction stream strand and dealdehyder tower cat head extraction stream strand etc., open valve 10, recovery tower cat head extraction vapour phase or liquid phase industrial spirit are delivered to the alcohol preheater.Open valve 12, potato spirit wine obtain fusel-oil fraction from the side line extraction of tower bottom through the potato spirit tripping device, and light wine returns recovery tower.Tower still waste water is discharged system, and this tower working pressure is 0～0.5Mpa.
(6) from the alcohol vapor of smart column overhead and recovery tower cat head after the etna heating, open valve 14,17 and carry out the adsorption dewatering operation by the adsorbing tower with molecular sieve 30 that is in adsorbed state from bottom to top.Alcohol steam after the dehydration enters raw spirit product condenser 37 and carries out condensation, and phlegma is sent into raw spirit finished product jar.
In adsorber, the sorbent material that can carry out selective adsorption to ethanol, water is housed.This kind sorbent material can be a Si-Al molecular sieve, and selectable molecular sieve is A type, X type, mordenite type, ZSM type etc.In adsorption tower, water is adsorbed agent absorption, and ethanol is discharged outside the adsorption tower by bed, obtains the very low alcohol product of water-content through condensation.The pressure of this technology adsorption operations is gauge pressure 0 ~ 0.6Mpa.System pressure is provided when ethanol water mixture is vaporized by vaporizer, and the moving equipment that gas blower etc. is used for supercharging need be set.In this technology desorption manipulation, adopt the negative pressure desorb, this falls adsorbed water to the adsorption tower desorption is very favorable.Proceed to a certain degree at the negative pressure desorption manipulation, to introduce the adsorption tower that carries out desorption by very low ethanol from the water-content that adsorption tower obtains, water to the adsorption tower institute desorption that carries out desorption manipulation purges completely, further removes the adsorbed water of adsorption tower of desorption.Through desorption, purging, water adsorbed in the adsorption tower is thoroughly removed.Reenter adsorption operations.For whole technology is carried out continuously, 2 above adsorption towers are set, the adsorption-desorption operation hockets.
In finishing experiment of the present invention, find, the raising of adsorptive pressure is favourable to the absorption content of water and sorbent material to the adsorption selectivity of second alcohol and water to sorbent material, and the raising of adsorptive pressure can improve the pressure difference of adsorption operations and desorption manipulation, and this helps the desorption of the adsorbed water of sorbent material.For the selected adsorptive pressure of this this technology at 0 ~ 0.6MPa, the preferred pressure scope is 0.2 ~ 0.5Mpa.Sweeping gas temperature of the present invention is 120 ~ 220 ℃, and preferred service temperature is 150 ~ 200 ℃.
(7) after adsorption tower absorption 30A operation was finished, adsorption tower 30B entered adsorption operations, and shut-off valve 14,17, open valve 15 carry out transformation and alternating temperature desorb operation.Switch- valve 21,22,19,20 successively according to switch-valve 14,15, and 17,18 switching sequences are operated.Stripping gas is through 36 condensations of resurgent gases condenser, and open valve 5,17, phlegma are delivered to the smart tower charging of ethanol refinery workshop section.After pressure is reduced to certain value, open valve 16, adopt the raw spirit product steam after dewatering to wash through 33 heating of revivifier preheater.Shut-off valve 16,17,15, the adsorption tower of finishing desorption and regeneration reenters the adsorption operations situation.The adsorptive pressure scope is 0.2 ~ 0.5Mpa.The service temperature of sweeping gas is 150 ~ 200 ℃.Desorption pressures is-0.05 ~ 0.5Mpa.
The main effect of adsorption tower is finally to obtain the raw spirit product by the remaining moisture content that sorbent material removes in alcohol and the water azeotropic mixture, and adsorption tower is common more than two, alternately finishes the adsorption-desorption operation successively, realizes charging extraction operate continuously.
By this embodiment, selecting raw material is the fermentation liquid that contains ethanol 12% (V), technical process according to above narration, by fecund product alcohol refining plant shown in Figure 1, can obtain the wine degree simultaneously is 96.5% (V), methanol content≤2ppm, potato spirit content≤2ppm, the special high grade edible spirit product of oxidization time 〉=40min; And water-content≤4000ppm, acidity (with acetometer)≤56ppm (mg/L), the dehydrated alcohol product of pH value 6.5～9.0.
Claims (8)
1. alcohol refining process for producing several products, it is characterized by: the major equipment of employing has smart stream tower, dealdehyder tower, smart tower, eparating methanol tower, recovery tower, adsorption tower, between each tower, be provided with valve and corresponding pipeline, also be provided with condenser, reboiler, preheater, utilize the stock liquid of wine degree, adopt following any one processing step: 1.1. edible ethanol processing step for 5-30%:
The rectified purified operation of edible ethanol thermal coupling mainly is made up of topping still, smart tower, dealdehyder tower, eparating methanol tower and recovery tower operating unit:
(1) be that the stock liquid of 5-30% enters topping still with ethanol content, waste liquid is discharged from the tower still, and the thick wine of cat head extraction is delivered to dealdehyder tower, and the heating medium of topping still reboiler is the overhead vapours of smart tower;
(2) cat head vapour is as eparating methanol tower reboiler heating medium, and alcohol distillation column is delivered in the cat head extraction, and the light wine of tower still extraction is delivered to smart tower charging;
(3) smart tower adopts the composite structure that high efficient packed column technology and tray column combine, it is further refining to deliver to eparating methanol tower at the alcohol in high concentration of the side line place extraction on tower top, the rich fusel-oil fraction of tower middle and lower part side line extraction and cat head extraction stream thigh are delivered to the recovery tower charging, and the processing wastewater of tower still extraction is discharged system;
(4) eparating methanol tower cat head extraction industrial spirit, the edible ethanol product of all size, by the adjusting process parameter from the extraction of tower still;
(5) recovery tower cat head extraction industrial spirit, potato spirit wine obtain fusel-oil fraction from the side line extraction of tower bottom through the potato spirit tripping device, and light wine returns recovery tower, and tower still waste water is discharged system; 1.2. raw spirit processing step:
The refining dehydration procedure of raw spirit mainly is made up of topping still, smart tower, adsorption tower operating unit:
(1) ethanol content is that the stock liquid of 5-30% enters topping still, and waste liquid is discharged from the tower still, delivers to off-side and handles, and the thick wine of cat head extraction is delivered to smart tower, and the heating medium of topping still reboiler is the overhead vapours of smart tower;
(2) smart tower adopts the composite structure that high efficient packed column technology and tray column combine, smart column overhead vapour phase part is as the heating medium of reboiler, cat head extraction vapour phase or liquid phase part are delivered to the adsorption tower etna, the rich fusel-oil fraction of tower middle and lower part side line extraction, obtain fusel-oil fraction through the potato spirit tripping device, light wine returns smart tower, and the processing wastewater of tower still extraction is discharged system;
(3) after the stream stock-traders' know-how etna heating from smart column overhead extraction, carry out the adsorption dewatering operation by the adsorbing tower with molecular sieve A that is in adsorbed state from bottom to top, alcohol steam after the dehydration enters raw spirit product condenser (topping still reboiler) and carries out condensation, phlegma is sent into raw spirit finished product jar
(4) after adsorption tower absorption A operation is finished, carry out transformation and alternating temperature desorb operation, adsorption tower B enters adsorption operations, and the desorb phlegma is delivered to the smart tower charging of ethanol refinery workshop section, and the adsorption tower of finishing desorption and regeneration reenters the adsorption operations situation; 1.3. edible ethanol and raw spirit be production craft step simultaneously:
Edible ethanol and the raw spirit technological process of production simultaneously mainly are made up of topping still, smart tower, dealdehyder tower, eparating methanol tower, recovery tower and adsorption tower unit equipment;
(1) be that the stock liquid of 5-30% enters topping still with ethanol content, useless mash is discharged from the tower still, delivers to off-side and handles, and the thick wine of cat head extraction is delivered to dealdehyder tower, and the heating medium of thick tower reboiler is the overhead vapours and the raw spirit product vapour of smart tower;
(2) dealdehyder tower cat head vapour refluxes through eparating methanol tower reboiler heat exchange condensation rear section, and alcohol distillation column is delivered in the part extraction, and the light wine of tower still extraction is delivered to smart tower charging;
(3) smart tower adopts the composite structure that high efficient packed column technology and tray column combine, the overhead vapours of the smart tower of part is delivered to thick tower reboiler as heating medium, cat head extraction vapour phase or liquid phase are delivered to the adsorption tower etna, it is further refining that the alcohol in high concentration of the side line place extraction on tower top is delivered to eparating methanol tower, according to edible ethanol and raw spirit turnout ratio, adjust cat head produced quantity and alcohol in high concentration and deliver to the eparating methanol tower amount, the rich fusel-oil fraction of tower middle and lower part side line extraction is delivered to the recovery tower charging, and the processing wastewater of tower still extraction is discharged system;
(4) eparating methanol tower cat head extraction and deliver to recovery tower, all size edible ethanol products such as top grade are from the extraction of tower still;
(5) the alcohol preheater is delivered in recovery tower cat head vapour phase or liquid phase extraction, and potato spirit wine obtains fusel-oil fraction from the side line extraction of tower bottom through the potato spirit tripping device, and light wine returns recovery tower, and tower still waste water is discharged system;
(6) alcohol vapor after the preheating is carried out the adsorption dewatering operation by the adsorbing tower with molecular sieve A that is in adsorbed state from bottom to top, alcohol steam after the dehydration enters raw spirit product condenser (topping still reboiler) and carries out condensation, and phlegma is sent into raw spirit finished product jar;
(7) after adsorption tower absorption A operation is finished, carry out transformation and alternating temperature desorb operation, adsorption tower B enters adsorption operations, and stripping gas is through the resurgent gases condenser condenses, adopt the raw spirit product steam after dewatering to wash, condensation light wine is delivered to the smart tower charging of ethanol refinery workshop section.
2. according to the described a kind of alcohol refining process for producing several products of claim 1, it is characterized by the composite structure that smart tower adopts high efficient packed column technology and tray column technology to combine.
3. according to the described a kind of alcohol refining process for producing several products of claim 1, it is characterized by thick tower decompression operation pressure and be-0.02～-0.08Mpa.
4. according to the described a kind of alcohol refining process for producing several products of claim 1, it is characterized by the dealdehyder tower working pressure is 0.0～0.1Mpa.
5. according to the described a kind of alcohol refining process for producing several products of claim 1, it is characterized by smart tower working pressure is 0.0～0.3Mpa.
6. according to the described a kind of alcohol refining process for producing several products of claim 1, it is characterized by piptonychia aldehyde tower decompression operation pressure and be-0.02～-0.08Mpa.
7. according to the described a kind of alcohol refining process for producing several products of claim 1, it is characterized by the recovery tower working pressure is 0.0～0.5Mpa.
8. according to the described a kind of alcohol refining process for producing several products of claim 1, it is characterized by adsorption tower and be set to more than two, alternately finish the adsorption-desorption operation successively, adsorptive pressure is at 0 ~ 0.6MPa, and the preferred pressure scope is 0.2 ~ 0.5Mpa; Desorption pressures-0.05 ~ 0.5Mpa, sweeping gas temperature are 120 ~ 220 ℃, and preferred service temperature is 150 ~ 200 ℃.
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