CN105967977A - Technology for preparing fuel ethanol through adsorption method - Google Patents

Technology for preparing fuel ethanol through adsorption method Download PDF

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Publication number
CN105967977A
CN105967977A CN201610463499.9A CN201610463499A CN105967977A CN 105967977 A CN105967977 A CN 105967977A CN 201610463499 A CN201610463499 A CN 201610463499A CN 105967977 A CN105967977 A CN 105967977A
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China
Prior art keywords
adsorbent
adsorber
adsorbers
ethanol
water
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CN201610463499.9A
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Chinese (zh)
Inventor
马晓建
王根灿
杨旭
王娟
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HENAN TIANGUAN BIOFUEL ENGINEERING TECHNOLOGY Co Ltd
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HENAN TIANGUAN BIOFUEL ENGINEERING TECHNOLOGY Co Ltd
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Priority to CN201610463499.9A priority Critical patent/CN105967977A/en
Publication of CN105967977A publication Critical patent/CN105967977A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

The invention belongs to the technical field of fuel ethanol production and preparation, and discloses a technology for preparing fuel ethanol through an adsorption method. Technical process comprises a raw material superheater, a plurality of adsorbers, a fuel ethanol condenser-cooler, a weak liquor condenser-cooler, a vacuum system and an adsorbent heating device. Ethanol-water mixture enters the superheater and is heated into superheat state gas, and then enters the adsorbers at the adsorption state; an adsorbent adsorbs water in the gas; fuel ethanol with extremely low water content flows out from the adsorbers, and a liquid product is obtained after cooling. When water in the adsorbent reaches a certain degree, material charging to the adsorbers is stopped, the adsorbers are connected with the weak liquor condenser-cooler, water in the adsorbers is pumped out under the action of heating and vacuum, and the adsorbent is regenerated. States of absorption in the adsorbers and the regeneration of the adsorbent are carried out alternately. The technology has the advantages that when the adsorbent is regenerated, fuel ethanol vapor is not required to be adopted, the volume of produced weak liquor is small, and when the concentration of ethanol in raw materials is 95 percent (v/v), the volume of weak liquor is 5 to 15 percent of product volume. The energy saving effect is obvious.

Description

A kind of absorption method prepares alcohol fuel technique
Technical field
The invention belongs to fuel ethanol production preparing technical field, particularly relate to one and prepare alcohol fuel generation technique with molecular sieve dehydration.
Background technology
Along with energy crisis and oil day are becoming tight in the world, petroleum fuel is replaced to be a kind of method solving energy problem with alcohol fuel.
Fermentation method is the main production process of ethanol, by the separation of ethanol in fermentation liquid out, is realized by distillation technique.Under normal circumstances, the system boiling temperature of alcohol-water composition is gradually reduced along with the rising of concentration of alcohol.At ambient pressure, ethanol-water solution reaches 95.57% at ethanol mass fraction, and when namely volume fraction reaches 97.2%, boiling point is 78.15 DEG C, and the ethanol-water solution boiling point under this CONCENTRATION STATE is minimum.This explanation is at ambient pressure, when wine ethanol-water mixture concentration reaches 97.2%(volume fraction) time, concentration of alcohol in gas phase and liquid phase is all 97.2%(volume fraction), under this concentration alcohol-water formed azeotropic mixture, use common rectificating method can not obtain concentration more than 97.2%(volume fraction) ethanol.In order to improve concentration of alcohol, it is necessary to take special method to realize.
Produce anhydrous alcohol many employings ternary azeotropic way of distillation, i.e. add the third material when distillation, such as benzene, cyclohexane or other solvents, make mixture produce azeotropic.The product so obtained can contain a small amount of residual solvent, affects product quality, and adds the consumption of solvent and the energy.Large-scale fuel ethanol production factory many employings molecular sieve adsorption produces alcohol fuel.
The superiority of molecular sieve adsorbing and dewatering: separation efficiency is high, and product water content is low;Simple to operation, labor intensity is low, it is simple to automatically control;Investment cost is low, and it is simple, convenient to install;Operating cost is low, and energy-saving effect is notable, Alcohol Production low cost;Molecular sieve technique eliminates process and the pollution problem of entrainer in ethanol-water azeotropic distillation;Product is without carrying other solvents secretly, and quality is good.
Molecular sieve is stronger to the absorbability of the gas phase hydrone under the condition of high temperature, aquiferous ethanol steam is superheated to uniform temperature and enters adsorbing tower with molecular sieve, stream of water molecule in gas is during molecular sieve filling layer, because the micropore of molecular sieve has the strongest affinity to hydrone, just by Water Molecular Adsorption in micropore, the water overwhelming majority in gas is adsorbed to be removed, realize fume dehydration, the fume discharged from dehydration device carries out condensing again, cool down after obtain the alcohol fuel that concentration is (99.5 ~ 99.9) %.
After molecular sieve uses certain time, the ability of adsorption moisture declines, and now it to be reversely dehydrated, and removes the moisture in molecular sieve, reaches the requirement of regeneration.
Patent CN1328987, CN1733666, CN101088975, CN102040471 disclose the method producing alcohol fuel with molecular sieve dehydration.In these methods, all use alcohol fuel purging adsorbent bed, in water transport therein to alcohol gas during regenerating molecular sieve, become aquiferous ethanol (light wine), which adds light wine amount, these light wine return again to Distallation systm re-distillation, increase energy expenditure.
Summary of the invention
It is an object of the invention to provide a kind of energy-conservation gas phase selective absorption from aquiferous ethanol, separate the technique of water outlet, use several adsorbers, adsorbent pressure swing regeneration.
For achieving the above object, the present invention is by the following technical solutions:
The ethanol-water mixture produced in still-process is heated into overheated gas in the superheater, and temperature is 80 ~ 160 DEG C.Overheated gas successively replaces from the multiple stage adsorber one end entrance equipped with adsorbent being in adsorbed state, and the water in gas is adsorbed by adsorbent, adsorptive pressure 0 ~ 1MPa(table), adsorption time 5 ~ 30 minutes;The gas that moisture is adsorbed flows out from the other end of adsorber, enters condensate cooler, and the liquid obtained is the alcohol fuel that ethanol content is 99.5 ~ 99.99%.
When in adsorber work certain time, adsorbent, moisture is higher, stop this adsorber feed;Adsorber is connected with the light wine condensate cooler with vacuum system simultaneously, lowered the temperature by condensation and the common effect of vacuum, moisture in adsorbent and the alcohol fuel remained in adsorber space and pipeline are drawn out of adsorber, adsorbent is regenerated, the gas condensation extracted out becomes light wine, returns distillation process;The pressure of adsorbent reactivation is-0.099 ~ 0MPa(table), the recovery time is 5 ~ 30 minutes.
Adsorber arranges heater, utilizes additional heat to heat adsorbent, makes the temperature of adsorbent maintain 101 ~ 150 DEG C.
Compared with prior art, the invention have the advantage that when adsorbent reactivation, being not required to utilize alcohol fuel steam, the light wine amount of generation is less;The heat that regenerative process needs relies on heater to provide.When in raw material, concentration of alcohol is 95% (v/v), light wine amount accounts for the 5 ~ 15% of product volume.Energy-saving effect is obvious.
Accompanying drawing explanation
Fig. 1 is two adsorber steam thermal regeneration operational flowcharts.
Fig. 2 is two adsorber alcohol fuel thermal regeneration operational flowcharts.
In figure: 1 superheater;2 light wine condensate coolers;3 alcohol fuel condensate coolers;4 vacuum pumps;5 heaters.
Detailed description of the invention
Embodiment 1:
Two adsorber steam thermal regeneration operating process as shown in Figure 1.The ethanol-water mixture produced in still-process is heated into overheated gas in the superheater, overheated gas enters adsorbent bed from the upper end of adsorber I, water in gas is adsorbed by adsorbent, from the effluent air of lower end, moisture is few, enter condensate cooler, be exactly process of alcohol products after cooling.When adsorbent can not adsorption moisture again time, close adsorber I top air inlet valve and bottom and give vent to anger valve, complete primary sorption operation.Then, opening the valve connected with vacuum system, adsorber I starts adsorbent reactivation operation.Open heater admission valve, the heat required for supply regeneration simultaneously.After in adsorbent, moisture is drawn out of, steam off valve and adsorber I evacuating valve, complete adsorbent reactivation operation.While adsorber I regenerates, adsorber II starts adsorption operations.Two adsorbers alternately adsorb and regenerate.
Embodiment 2:
Two adsorber alcohol fuel thermal regeneration operating process as shown in Figure 2.The ethanol-water mixture produced in still-process is heated into overheated gas in the superheater, overheated gas enters adsorbent bed from the upper end of adsorber I, water in gas is adsorbed by adsorbent, from the effluent air of lower end, moisture is few, enter the heater of adsorber II, regenerate thermal source as it.From heater effluent air, enter back into condensate cooler, obtain process of alcohol products after cooling.When adsorbent can not adsorption moisture again time, close adsorber I top air inlet valve and bottom and give vent to anger valve, complete primary sorption operation.Then, opening the valve connected with vacuum system, adsorber I starts adsorbent reactivation operation.Now adsorber II starts adsorption operations, and the alcohol fuel gas of production regenerates thermal source as it.After in adsorbent, moisture is drawn out of, steam off valve and adsorber I evacuating valve, complete adsorbent reactivation operation.Two adsorbers alternately adsorb and regenerate.

Claims (4)

1. absorption method prepares an alcohol fuel technique, comprises the following steps:
1) ethanol-water mixture produced in still-process being heated into overheated gas in the superheater, enter from the adsorber one end equipped with adsorbent being in adsorbed state, the water in gas is adsorbed by adsorbent;The gas that moisture is adsorbed flows out from the other end of adsorber, enters condensate cooler, and the liquid obtained is the alcohol fuel that ethanol content is 99.5 ~ 99.99%;
2) when in adsorber work certain time, adsorbent, moisture is higher, stop this adsorber feed;Adsorber is connected with the light wine condensate cooler with vacuum system simultaneously, lowered the temperature by condensation and the common effect of vacuum, moisture in adsorbent and the alcohol fuel remained in adsorber space and pipeline are drawn out of adsorber, adsorbent is regenerated, the gas condensation extracted out becomes light wine, returns distillation process;
3) adsorber arranges heater, utilizes additional heat to heat adsorbent;
4) every adsorber the most alternately adsorbs and regenerative operation, and the duty incorrect order of multiple stage adsorber arranges.
2. absorption method as claimed in claim 1 prepares alcohol fuel technique, it is characterised in that: process process equipment includes adsorber, superheater, alcohol fuel condensate cooler, light wine condensate cooler, vacuum system and adsorbent heater;Adsorber at least 2, at most can be 8;Adsorbent heater is indirectly heating, and available absorption wall is as heat-transfer area, it is possible to be arranged on adsorbent bed in.
3. the absorption method as described in claim 1 and 2 prepares alcohol fuel technique, it is characterised in that: the gas temperature entering adsorber is 80 ~ 160 DEG C;Adsorptive pressure is 0 ~ 1MPa(table), adsorption time 5 ~ 30 minutes;Adsorbent reactivation pressure is-0.099 ~ 0MPa(table), the recovery time is 5 ~ 30 minutes;The temperature of adsorbent is 101 ~ 150 DEG C.
4. the absorption method as described in claim 1 and 2 prepares alcohol fuel technique, it is characterised in that: adsorbent is the Si-Al molecular sieve that ethanol, water can carry out selective absorption.
CN201610463499.9A 2016-06-24 2016-06-24 Technology for preparing fuel ethanol through adsorption method Pending CN105967977A (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109776266A (en) * 2019-02-28 2019-05-21 肥城金塔酒精化工设备有限公司 A kind of energy-saving equipment and its power-economizing method producing absolute alcohol
CN112923601A (en) * 2019-12-05 2021-06-08 中粮生物科技股份有限公司 Ethanol steam waste heat recovery method and device, ethanol steam dehydration method and system

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1328987A (en) * 2001-05-17 2002-01-02 天津大学 Production process of anhydrous ethyl alcohol by using several adsorbers
CN1348942A (en) * 2001-06-21 2002-05-15 北京迈胜普技术有限公司 Molecular sieve adsorbing and dewatering process of producing absolute alcohol
CN1686986A (en) * 2005-04-13 2005-10-26 天津大学 Method for producting absolute ethyl alcohol
CN102992954A (en) * 2013-01-05 2013-03-27 四川亚连科技有限责任公司 High-yield technology for preparing absolute ethyl alcohol
CN104289008A (en) * 2014-08-11 2015-01-21 肥城金塔机械科技有限公司 Preparation apparatus for anhydrous alcohol

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1328987A (en) * 2001-05-17 2002-01-02 天津大学 Production process of anhydrous ethyl alcohol by using several adsorbers
CN1348942A (en) * 2001-06-21 2002-05-15 北京迈胜普技术有限公司 Molecular sieve adsorbing and dewatering process of producing absolute alcohol
CN1686986A (en) * 2005-04-13 2005-10-26 天津大学 Method for producting absolute ethyl alcohol
CN102992954A (en) * 2013-01-05 2013-03-27 四川亚连科技有限责任公司 High-yield technology for preparing absolute ethyl alcohol
CN104289008A (en) * 2014-08-11 2015-01-21 肥城金塔机械科技有限公司 Preparation apparatus for anhydrous alcohol

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109776266A (en) * 2019-02-28 2019-05-21 肥城金塔酒精化工设备有限公司 A kind of energy-saving equipment and its power-economizing method producing absolute alcohol
CN112923601A (en) * 2019-12-05 2021-06-08 中粮生物科技股份有限公司 Ethanol steam waste heat recovery method and device, ethanol steam dehydration method and system

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Application publication date: 20160928