MD182Y - Process for the production of dehydrated ethyl alcohol - Google Patents
Process for the production of dehydrated ethyl alcohol Download PDFInfo
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- MD182Y MD182Y MDS20090143A MDS20090143A MD182Y MD 182 Y MD182 Y MD 182Y MD S20090143 A MDS20090143 A MD S20090143A MD S20090143 A MDS20090143 A MD S20090143A MD 182 Y MD182 Y MD 182Y
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- ethyl alcohol
- vol
- production
- alcohol
- dehydrated
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- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 125000005909 ethyl alcohol group Chemical class 0.000 title 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 136
- 235000019441 ethanol Nutrition 0.000 claims abstract description 66
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000004821 distillation Methods 0.000 claims abstract description 11
- 235000014101 wine Nutrition 0.000 claims abstract description 6
- 235000013339 cereals Nutrition 0.000 claims description 4
- 241000219094 Vitaceae Species 0.000 claims description 3
- 235000021021 grapes Nutrition 0.000 claims description 3
- 235000013379 molasses Nutrition 0.000 claims description 3
- 235000009754 Vitis X bourquina Nutrition 0.000 abstract 1
- 235000012333 Vitis X labruscana Nutrition 0.000 abstract 1
- 240000006365 Vitis vinifera Species 0.000 abstract 1
- 235000014787 Vitis vinifera Nutrition 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 43
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 22
- 229960004063 propylene glycol Drugs 0.000 description 12
- 239000000203 mixture Substances 0.000 description 10
- 230000018044 dehydration Effects 0.000 description 7
- 238000006297 dehydration reaction Methods 0.000 description 7
- 239000002808 molecular sieve Substances 0.000 description 6
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 6
- 239000010457 zeolite Substances 0.000 description 6
- 229910021536 Zeolite Inorganic materials 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 5
- 230000001476 alcoholic effect Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000012024 dehydrating agents Substances 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- MGKBJNVLJBEDCF-UHFFFAOYSA-N benzene;ethanol;hydrate Chemical group O.CCO.C1=CC=CC=C1 MGKBJNVLJBEDCF-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
Abstract
Description
Invenţia se referă la industria alcoolului, şi anume la un procedeu de obţinere a alcoolului etilic deshidratat. The invention relates to the alcohol industry, namely to a process for obtaining dehydrated ethyl alcohol.
Alcoolul etilic deshidratat poate fi utilizat în industria de producere a carburanţilor lichizi, în special, la producerea bioetanolului, folosit ca adaos la benzină. Dehydrated ethyl alcohol can be used in the liquid fuel production industry, in particular, in the production of bioethanol, used as an additive to gasoline.
După cum se ştie, bioetanolul, folosit ca adaos la benzină, trebuie să aibă un conţinut de 98,7% (Carburanţi pentru automobile. Etanol ca component de amestec pentru benzină. Cerinţe şi metode de încercare. EN15376:2007 idt) sau 99,3% vol. (Высокооктанновая кислородсодержащая добавка к бензину. ТУ 30183376.001/2000) de alcool etilic, pe când în instalaţiile de rectificare a alcoolului etilic el se obţine cu un conţinut de cel mult 96% vol. alcool etilic (GOST 5962-67). As is known, bioethanol, used as an additive to gasoline, must have a content of 98.7% (Automotive fuels. Ethanol as a blending component for gasoline. Requirements and test methods. EN15376:2007 idt) or 99.3% vol. (High-octane oxygen-containing additive to gasoline. TU 30183376.001/2000) of ethyl alcohol, while in ethyl alcohol rectification plants it is obtained with a content of no more than 96% vol. ethyl alcohol (GOST 5962-67).
Se cunoaşte procedeul de deshidratare a alcoolului etilic, care se bazează pe absorbţia moleculelor de apă din alcool cu utilizarea sitelor moleculare din zeolit sintetic granulat de 3 Å [1]. The process of dehydration of ethyl alcohol is known, which is based on the absorption of water molecules from alcohol using molecular sieves made of 3 Å granulated synthetic zeolite [1].
Capacitatea de adsorbţie a apei de către zeolit depinde de presiunea şi temperatura apei. Cu cât presiunea şi temperatura vaporilor alcoolului este mai mare, cu atât se măreşte saturaţia zeolitului cu apă. Moleculele de apă, având diametrul mai mic decât al alcoolului etilic, se adsorb în porii zeolitului. Când sita moleculară este saturată cu apă, ea este readusă în starea iniţială. Procesul de desorbţie a apei din sitele moleculare are loc în vid. Cu ajutorul sitelor moleculare pe bază de zeoliţi se poate obţine alcool etilic cu concentraţia de 99,0...99,8% vol. The water adsorption capacity of zeolite depends on the pressure and temperature of water. The higher the pressure and temperature of alcohol vapor, the higher the saturation of the zeolite with water. Water molecules, having a smaller diameter than ethyl alcohol, are adsorbed in the pores of the zeolite. When the molecular sieve is saturated with water, it is returned to its original state. The process of desorption of water from molecular sieves takes place in a vacuum. With the help of molecular sieves based on zeolites, ethyl alcohol with a concentration of 99.0...99.8% vol. can be obtained.
Dezavantajele acestui procedeu constau în următoarele: The disadvantages of this procedure are the following:
- sitele moleculare pe bază de zeoliţi au rezistenţă mecanică joasă, din care cauză repede se uzează şi necesită a fi înlocuite; - zeolite-based molecular sieves have low mechanical resistance, which is why they wear out quickly and need to be replaced;
- alcoolul etilic rectificat trebuie să fie de o puritate înaltă, deoarece sitele moleculare nu sunt regenerabile; - rectified ethyl alcohol must be of high purity, because molecular sieves are not renewable;
- este foarte greu de dirijat procesul de absolutizare, deoarece atât procesul de adsorbţie a apei, cât şi procesul de desorbţie sunt specifice şi nu pot fi automatizate. - it is very difficult to direct the absolutization process, because both the water adsorption process and the desorption process are specific and cannot be automated.
Soluţia cea mai apropiată este procedeul de obţinere a alcoolului etilic deshidratat cu utilizarea benzenului. Acest procedeu de deshidratare a alcoolului etilic prin utilizarea amestecurilor triple, constă în următoarele. La alcoolul etilic rectificat se adaugă benzen. Amestecul triplu etanol-apă-benzen formează un azeotrop, care constă din, % mas.: etanol 19,5, apă 7,4 şi benzen 74,1, care fierbe la temperatura de 64,85°C. Amestecul azeotrop la distilare se comportă ca un complex uşor volatil. La răcire el se separă uşor în două straturi: de sus - format preponderent din benzen, şi de jos - din etanol şi apă. La temperatura de 15°C în stratul de sus se conţine: benzen 85%, alcool etilic 13,3% şi apă 1,7%, în cel de jos alcool etilic 49,7%, apă 41,3% şi benzen 9% [2]. The closest solution is the process of obtaining dehydrated ethyl alcohol using benzene. This process of dehydration of ethyl alcohol using triple mixtures consists of the following. Benzene is added to rectified ethyl alcohol. The triple mixture ethanol-water-benzene forms an azeotrope, which consists of, wt.%: ethanol 19.5, water 7.4 and benzene 74.1, which boils at a temperature of 64.85°C. The azeotropic mixture during distillation behaves as a slightly volatile complex. Upon cooling, it easily separates into two layers: the upper one - consisting mainly of benzene, and the lower one - of ethanol and water. At a temperature of 15°C, the upper layer contains: 85% benzene, 13.3% ethyl alcohol and 1.7% water, the lower one contains 49.7% ethyl alcohol, 41.3% water and 9% benzene [2].
La distilarea amestecului de alcool etilic, apă şi benzen primul se distilează alcoolul etilic, iar în soluţie rămâne benzenul şi apa. Deoarece temperaturile de fierbere a benzenului este de 80,1°C, iar a alcoolului etilic de 78,37°C, alcoolul etilic distilat conţine urme de benzen. Cu ajutorul benzenului se poate obţine alcool etilic cu concentraţia de 99,0…99,5% vol. When distilling a mixture of ethyl alcohol, water and benzene, the ethyl alcohol is distilled first, and the benzene and water remain in solution. Since the boiling point of benzene is 80.1°C and that of ethyl alcohol is 78.37°C, the distilled ethyl alcohol contains traces of benzene. Using benzene, ethyl alcohol with a concentration of 99.0…99.5% vol. can be obtained.
Pentru producerea a 0,01 m3 de alcool etilic anhidru se consumă aproximativ 0,25 m3 apă şi 0,01 kg de benzen. Pierderile ultimului se compensează prin adaosul periodic al lui în coloana de deshidratare. Pierderile maximale admisibile la absolutizare constituie 1% de alcool etilic. For the production of 0.01 m3 of anhydrous ethyl alcohol, approximately 0.25 m3 of water and 0.01 kg of benzene are consumed. The losses of the latter are compensated by its periodic addition to the dehydration column. The maximum admissible losses during absolutization constitute 1% of ethyl alcohol.
Dezavantajele acestui procedeu constau în faptul că: The disadvantages of this process are that:
- la distilarea alcoolului etilic o parte din benzen rămâne în alcoolul deshidratat; - when distilling ethyl alcohol, part of the benzene remains in the dehydrated alcohol;
- benzenul şi produsele lui de ardere sunt toxice, din această cauză el a fost interzis pentru utilizare; - benzene and its combustion products are toxic, for this reason it has been banned for use;
- la producerea alcoolului etilic anhidru sunt mari cheltuielile de vapori de apă. - the production of anhydrous ethyl alcohol requires high water vapor costs.
Problema pe care o soluţionează invenţia dată constă în utilizarea unui agent de deshidratare care nu este toxic şi la distilare nu trece în alcoolul etilic deshidratat. The problem solved by this invention consists in using a dehydrating agent that is not toxic and does not pass into dehydrated ethyl alcohol upon distillation.
Esenţa procedeului de obţinere a alcoolului etilic deshidratat până la concentraţia de 98,9…99,5% vol, constă în distilarea alcoolului etilic cu concentraţia de 95,5…96,5% vol. în contracurent cu 1,2 propilenglicol în raport de 1:1, lichefierea vaporilor de alcool etilic şi colectarea alcoolului etilic deshidratat. The essence of the process for obtaining dehydrated ethyl alcohol up to a concentration of 98.9…99.5% vol. consists of distilling ethyl alcohol with a concentration of 95.5…96.5% vol. in countercurrent with 1,2 propylene glycol in a ratio of 1:1, liquefying ethyl alcohol vapors and collecting dehydrated ethyl alcohol.
La distilarea amestecului triplu din alcool etilic, apă şi 1,2 propilenglicol se obţine alcool etilic cu concentraţia de 99,0...99,5% vol. Produsul obţinut poate fi folosit ca solvent în industria chimică sau ca adaos la benzină. When distilling the triple mixture of ethyl alcohol, water and 1,2 propylene glycol, ethyl alcohol with a concentration of 99.0...99.5% vol is obtained. The product obtained can be used as a solvent in the chemical industry or as an additive to gasoline.
În calitate de alcool etilic se utilizează fracţiile de coadă de la producerea alcoolului etilic rectificat din cereale şi melasă, distilatului de vin şi alcoolului etilic rectificat de struguri, preventiv concentrat până la 95,5…96,5% vol. The tail fractions from the production of rectified ethyl alcohol from cereals and molasses, wine distillate and rectified ethyl alcohol from grapes, pre-concentrated to 95.5…96.5% vol., are used as ethyl alcohol.
Rezultatul tehnic al invenţiei constă în aceea că: The technical result of the invention consists in that:
- se obţine alcool etilic de 98,9...99,5% vol.; - ethyl alcohol of 98.9...99.5% vol. is obtained;
- alcoolul etilic deshidratat poate fi folosit ca adaos la benzină; - dehydrated ethyl alcohol can be used as an additive to gasoline;
- 1,2 propilenglicolul utilizat poate fi deshidratat la încălzirea lui până la temperatura de fierbere, care este de 187°C la presiune normală sau în vid la temperaturi mai joase; - the 1,2 propylene glycol used can be dehydrated by heating it to its boiling point, which is 187°C at normal pressure or in vacuum at lower temperatures;
- 1,2 propilenglicolul este stabil, nu se modifică în procesul de deshidratare a alcoolului sau la regenerarea lui; - 1,2 propylene glycol is stable, it does not change during the alcohol dehydration process or its regeneration;
- folosind 1,2 propilenglicolul se pot utiliza fracţiile de coadă de la producerea alcoolului etilic rectificat din cereale şi melasă, distilatului de vin şi alcoolului etilic rectificat de struguri, preventiv concentrat până la 95,5…96,5% vol. - using 1,2 propylene glycol, the tail fractions from the production of rectified ethyl alcohol from cereals and molasses, wine distillate and rectified ethyl alcohol from grapes, preventively concentrated to 95.5…96.5% vol. can be used.
Rezultatul tehnic al invenţiei se datorează faptului că: The technical result of the invention is due to the fact that:
- se utilizează 1,2 propilenglicolul ca agent de deshidratare, care nu este toxic; - 1,2 propylene glycol is used as a dehydrating agent, which is non-toxic;
- 1,2 propilenglicolul formează cu apa hidraţi mai stabili, asigurând un grad mai ridicat de concentrare a alcoolului etilic. - 1,2 propylene glycol forms more stable hydrates with water, ensuring a higher degree of ethyl alcohol concentration.
Exemplul 1 Example 1
Pentru deshidratare se utilizează 2000 cm3 de alcool etilic rectificat conform (GOST 5962-67) cu concentraţia alcoolului etilic de 96% vol., care se introduce în alambicul coloanei de distilare, unde se încălzesc. Vaporii de alcool şi apă se ridică în coloana de distilare, iar prin partea de sus se debitează 1,2 propilenglicolul în raport de 1:1 faţă de alcoolul utilizat. 1,2 propilenglicolul leagă apa din vapori şi coboară în jos prin coloană nimerind în alambic. Vaporii de alcool fără apă ieşind din coloana de distilare sunt răciţi şi lichidul format este colectat. Concentraţia alcoolului etilic în produsul final este de 99,5% vol. For dehydration, 2000 cm3 of rectified ethyl alcohol according to (GOST 5962-67) with an ethyl alcohol concentration of 96% vol. is used, which is introduced into the distillation column still, where it is heated. The alcohol and water vapors rise into the distillation column, and 1,2 propylene glycol is discharged from the top in a ratio of 1:1 to the alcohol used. 1,2 propylene glycol binds the water in the vapors and descends down the column into the still. The anhydrous alcohol vapors leaving the distillation column are cooled and the liquid formed is collected. The ethyl alcohol concentration in the final product is 99.5% vol.
Exemplul 2 Example 2
Pentru deshidratare s-a utilizat: fracţia de la producerea alcoolului etilic rectificat de origine vinicolă cu concentraţia alcoolică de 96% vol. în cantitate de 30%, alcool etilic rectificat din cereale cu concentraţia alcoolului etilic de 96,4% vol. în cantitate de 60% şi fracţia de coadă de la producerea distilatului de vin cu concentraţia alcoolului etilic de 40% vol. în cantitate de 10%. Concentraţia alcoolică medie a amestecului constituie 91% vol. Acest amestec este concentrat într-o instalaţie de distilare până la concentraţia alcoolului etilic de 95,5...96,6% vol., apoi este încălzit în alambicul coloanei de distilare şi vaporii formaţi se ridică în sus în coloana de distilare. În partea de sus a coloanei se debitează 1,2 propilenglicol în raport de 1:1 faţă de amestecul concentrat, care venind în contact cu vaporii leagă apa şi se acumulează în alambicul coloanei. Vaporii de alcool, precum şi ai componentelor fracţiilor de coadă fără apă din coloana de distilare nimeresc în sistemul de răcire unde sunt lichefiaţi, iar alcoolul etilic deshidratat este colectat. For dehydration, the following were used: the fraction from the production of rectified ethyl alcohol of wine origin with an alcoholic strength of 96% vol. in an amount of 30%, rectified ethyl alcohol from cereals with an ethyl alcohol strength of 96.4% vol. in an amount of 60% and the tail fraction from the production of wine distillate with an ethyl alcohol strength of 40% vol. in an amount of 10%. The average alcoholic strength of the mixture is 91% vol. This mixture is concentrated in a distillation plant to an ethyl alcohol strength of 95.5...96.6% vol., then it is heated in the distillation column still and the vapors formed rise up in the distillation column. At the top of the column, 1.2 propylene glycol is discharged in a ratio of 1:1 to the concentrated mixture, which, coming into contact with the vapors, binds water and accumulates in the column still. The alcohol vapors, as well as the components of the anhydrous tail fractions from the distillation column, enter the cooling system where they are liquefied, and the dehydrated ethyl alcohol is collected.
Rezultatele obţinute sunt prezentate în tabel. The results obtained are presented in the table.
Tabel Table
Amestecul alcoolic Alimentarea cu 1,2 propilenglicol, m3/h Durata ex-perimentului, h Cantitatea de produs obţinut, cm3 Concentraţia alcoolică, % vol. Viteza selectării etanolului, cm3/h Volumul, cm3 Concentraţia alcoolică, % vol. 2000 95,5 500 2 1250 98,9 450 2000 96,1 500 2 1250 98,9 450 2000 96,6 500 2 1250 99,15 450Alcoholic mixture 1.2 propylene glycol feed, m3/h Experiment duration, h Amount of product obtained, cm3 Alcohol concentration, % vol. Ethanol selection rate, cm3/h Volume, cm3 Alcohol concentration, % vol. 2000 95.5 500 2 1250 98.9 450 2000 96.1 500 2 1250 98.9 450 2000 96.6 500 2 1250 99.15 450
După finalizarea procesului de deshidratare amestecul de 1,2 propilenglicol şi apă, acumulat în cazan şi 10% de alcool restant se dirijează spre regenerare. Regenerarea 1,2 propilenglicolului se efectuează în evaporator deschis prin încălzire la presiune normală până la temperatura de 287°C sau într-un sistem închis în vacuum de 750...800 Pa până la temperatura de 132°C, care corespunde temperaturii de fierbere a 1,2 polietilenglicolului. After the dehydration process is completed, the mixture of 1,2 propylene glycol and water accumulated in the boiler and 10% of the remaining alcohol is sent for regeneration. The regeneration of 1,2 propylene glycol is carried out in an open evaporator by heating at normal pressure to a temperature of 287°C or in a closed system in a vacuum of 750...800 Pa to a temperature of 132°C, which corresponds to the boiling point of 1,2 polyethylene glycol.
1,2 polietilenglicolul regenerat se răceşte până la t = 80°C şi poate fi utilizat din nou pentru deshidratarea altei porţii de alcool. The regenerated 1,2 polyethylene glycol is cooled to t = 80°C and can be used again to dehydrate another portion of alcohol.
1. Технические условия. Цеолиты синтетические. Ярославль, 2007. с.7. 1. Technical conditions. Synthetic zeolites. Yaroslavl, 2007. p.7.
2. Яровенко В.Л. Технология спирта. Москва, Колос, 2002, с. 372-374 2. Яровенко В.Л. Spirit technology. Moscow, Kolos, 2002, p. 372-374
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| MDS20090143A MD182Z (en) | 2009-07-30 | 2009-07-30 | Process for the production of dehydrated ethyl alcohol |
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| MDS20090143A MD182Z (en) | 2009-07-30 | 2009-07-30 | Process for the production of dehydrated ethyl alcohol |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104585811A (en) * | 2014-12-11 | 2015-05-06 | 惠州学院 | Litchi and amino acid complex drink |
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| RU2265473C1 (en) * | 2004-07-09 | 2005-12-10 | Закрытое акционерное общество Научно-производственное объединение "Химсинтез" | Method of production of a dehydrated ethyl alcohol |
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| CN104585811A (en) * | 2014-12-11 | 2015-05-06 | 惠州学院 | Litchi and amino acid complex drink |
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