CN1091414A - The extraction rectification technique that ethanol concentrates and reclaims - Google Patents
The extraction rectification technique that ethanol concentrates and reclaims Download PDFInfo
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- CN1091414A CN1091414A CN 93110577 CN93110577A CN1091414A CN 1091414 A CN1091414 A CN 1091414A CN 93110577 CN93110577 CN 93110577 CN 93110577 A CN93110577 A CN 93110577A CN 1091414 A CN1091414 A CN 1091414A
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Abstract
What the present invention relates to is the extracting rectifying novel process that a kind of ethanol concentrates and reclaims, and this processing method is applicable to that grain distillery's ethanol reclaims and purification, also is applicable to the recovery of other factory's waste alcohol.This process using primary tower purifies to 60%～66%mol with ethanol in the fermented liquid, is extraction agent with ethylene glycol, adopts extractive distillation column ethanol to be concentrated into 89%～99.1% (mol) again, and ethylene glycol uses through the regenerator column reprocessing cycle.This technology stability is good, separate back purity of alcohol height, and it is big to have changed conventional production methods (distillation method and azeotropic distn) energy consumption, and purity of alcohol is subjected to boiling point to limit this defective.It is low to separate the required energy consumption of the used conventional distillation of energy loss-rate.
Description
What the present invention relates to is the extracting rectifying novel process that a kind of ethanol concentrates and reclaims, and this processing method is applicable to that grain distillery's ethanol reclaims and purification, also is applicable to the recovery of other factory's waste alcohol.
At present, China produces ethanol still based on fermentation method, reclaims ethanol still based on traditional azeotropic distn that is distilled into from fermented liquid.Because distillation method commonly used and azeotropic distn separating alcohol and water consumption are big, and alcohol concn is restricted, and therefore, seeks a kind of new effective separation method, and recovery or concentrated ethanol are necessary from fermentation method.The heat energy that distillation is consumed is equivalent to 50～70% of full scale production process.It is generally acknowledged, produce the energy that 1 liter of required heat of ethanol is obtained greater than burning 1kg ethanol,, just be devoted to the research of ethanol and water sepn in the world in view of distillation method (or azeotropic distn) separating alcohol and big this drawback of water consumption.
German Hoechest company of connection group has developed the ethanol distillation new technology, can be reduced to the required energy of distillation ethanol originally about 1/3rd, but this technology needs carry out new arrangement and complicated operations control techniques to distillation tower; Japan is a kind of separatory membrane of invention recently, uses this membrane sepn second alcohol and water, energy consumption can reduce by 1/2nd to three minutes this two, separate back alcoholic acid purity height, but equipment miniaturization, industrial scale is restricted; With siccative (Cao etc.) or molecular sieve adsorption, this method production cycle is long, and produces and to obtain high purity ethanol, and institute's energy requirement surpasses the used heat of distillation; The saline extraction distillation is (as CaCl
2, NaCl etc.), can improve purity of alcohol, but the salt solution of discharging at the bottom of the tower, need through concentrating, just can returning after the crystallization and reuse, salt is being carried, difficulty and problems such as obstruction, corrosion in the reinforced process are used the saline extraction distillatory and are limited to restriction.
The objective of the invention is weak point at above-mentioned processing method existence, adopt the method for ethylene glycol distillation and extracting rectifying, concentrate and reclaim ethanol, this technology is separated used distillation and extraction rectification technique good stability, separate back purity of alcohol height, separates that used can loss-rate conventional to distill required energy consumption low.
The extraction rectification technique that ethanol concentrates and reclaims takes following scheme to realize: at first adopt primary tower that ethanol in the fermented liquid is purified to 60%～66%(mol), be extraction agent then with ethylene glycol, adopt extractive distillation column again ethanol to be concentrated into 89%～99.1%(mol).The regenerator column reprocessing cycle is used.Ethylene glycol adopts industrial goods, and content is more than 96%.
Ethanol concentrates and reclaims and carry out continuously in primary tower, extraction tower, and device is operated interior dress Stainless Steel Helices under normal pressure.The electrically heated of tower still, solvent and raw material adopt spinner survey, and whole device energy expenditure adopts power electric meter to measure.Regenerator column is used for ethylene glycol regeneration, so that recycle.
Technical process: grain distillery contains ethanol 13%～20%(mol) fermented liquid and delivers to primary tower and carry out fore-running, produce waste liquid at the bottom of the fore-running Tata, overhead distillate contains ethanol 60～66%(mol), deliver to extractive distillation column, extraction tower is extraction agent with ethylene glycol, the ratio 1～4: 1 of extraction agent and extraction tower inlet amount, temperature in is controlled at 370K～373K, and reflux ratio (R) gets 2～3, and seat is got separating alcohol and water, overhead distillate contains the second alcohol and water, overhead distillate contains ethanol 89%～99.1%(mol), and the tower bottom flow fluid is delivered to solvent regeneration tower, and the regenerator column overhead distillate is a waste liquid, tower bottom flow goes out not contain the extraction solvent of second alcohol and water and delivers to extraction tower, circulation.
The extraction rectification technique that ethanol concentrates and reclaims, the method that adopts ethylene glycol distillation and extracting rectifying to combine, separate used distillation and extraction rectification technique good stability, the pure end of ethanol, separation back, reach the 99.7%(mass content) time, separate the required energy consumption of the used conventional distillation of energy loss-rate and hang down more than 20% approximately; Obtain the 95.5%(mass content if separate) ethanol compares with conventional still-process, and it is about more than 35% to save energy consumption.It is big that the present invention has changed conventional production methods (distillation method and azeotropic distn) energy consumption, and purity of alcohol is subjected to azeotropic point to limit this defective.The provincial-level appraisal of this technology.Its success will produce tangible economic benefit and social benefit, has general promotional value.
Below with reference to accompanying drawing, table is to this bright being described further.
Fig. 1 is distillation of the present invention and the extracting rectifying technological process of production synoptic diagram that combines.
Fig. 2 is that extractant feed amount of the present invention is to extractive distillation column (Q) cat head ethanol content influence curve figure.
Fig. 3 is that extraction tower trim the top of column of the present invention influences (molar content) synoptic diagram than (R) to the cat head ethanol content.
Subordinate list 2 is test-results that distillation of the present invention and extracting rectifying combine.
Subordinate list 3 is that 2 kinds of flow processs of the present invention obtain the about 58ml of 1mol() ethanol consumption of calorie etc. is relatively.
With reference to accompanying drawing and subordinate list, the extraction rectification technique process that ethanol concentrates and reclaims, the fermented liquid (stream strand 1) that grain distillery contains ethanol 13%～20%mol is delivered to primary tower P and is carried out fore-running, produce waste liquid at the bottom of the P Tata, overhead distillate (stream thigh 9) contains ethanol 60～66%(mol) and delivers to extractive distillation column Q, the Q tower is extraction solvent (stream thigh 4) with ethylene glycol, ethylene glycol adopts the industrial goods of content 96%, ratio 1～4: 1 volume ratio of extraction agent and extractive distillation column charging, inlet (stream thigh 4) temperature is controlled at 370K～373K, reflux ratio (R) gets 2～3, extracting and separating second alcohol and water, Q Tata underflow fluid (stream thigh 5) is delivered to solvent regeneration tower R, and R column overhead distillate (stream thigh 7) is a waste liquid, tower bottom flow goes out not contain the extraction solvent of second alcohol and water and delivers to extraction tower, recycles.
When extraction agent and extractive distillation column Q raw material inlet amount ratio get 3.8: in the time of the 1(volume ratio), separating resulting sees attached list 1, separates the back ethanol content and reaches 99.1%(mol); When extraction agent and extractive distillation column Q material quantity than getting 1 approximately: in the time of the 1(volume ratio), the results are shown in subordinate list 2, separate back ethanol mass content and reach 89.4%mol.
In order to compare, adopting primary tower P is device, and fractionation by distillation second alcohol and water with technical process separating alcohol and water shown in the accompanying drawing 1, obtains each tower consumption of calorie of 1mol ethanol, and the ethanol rate of recovery, separation back purity of alcohol see attached list 3.
Determine to concern between ethylene glycol inlet amount and the extracting rectifying column overhead purity of alcohol.Under following condition:
Raw material (raw material is a primary tower top of tower distillate, stream strand 9): flow 5, ml/s, form and close the about 65%(mol of ethanol), temperature in 351K～356K.
Extraction agent (stream thigh 4): flow 5.1ml/s～20ml/s, temperature in 370K～373K,
Extracting rectifying Tata still temperature: 411K～417K,
Extractive distillation column tower top temperature: 351.4K～352.5K,
Trim the top of column is than (R): R=3
Overhead distillate (stream thigh 3): flow 4.5ml/s,
The extractant feed amount influences accompanying drawing 2 to extracting rectifying column overhead purity of alcohol, the result show contain 65%(mol approximately in the raw material) ethanol, extraction agent ethylene glycol is 1～4: 1 o'clock with the ratio of raw material inlet amount, separates the back purity of alcohol and reaches 89%～99.1%mol.
The extractive distillation column trim the top of column is than concerning between (R) and the cat head purity of alcohol.Under following condition:
Raw material (stream thigh 9): flow 5.1ml/s, form and contain the about 65%mol of ethanol, temperature in 351K,
Extraction agent (stream thigh 4): flow 10.0ml/s, temperature in 372K,
Extracting rectifying Tata still temperature: 413K～417K,
Extractive distillation column tower top temperature: 351.6K.
Reflux ratio (R) influences extracting rectifying column overhead ethanol content sees accompanying drawing 3.The result shows that under the higher situation of cat head ethanol content, it is influential slightly to ethanol content to change reflux ratio, but influence is little, therefore selects R=2～3 as the separation processes parameter.
Bonded test-results room temperature is heated up in a steamer in table 1 distillation and extraction clearly: 13.5 ℃
| The stream thigh | Flow (ml/s) | Temperature (K) | Form (mol%) | ||
| Water | | Ethylene glycol | |||
| 1 | 11.0 | 347.6 | 86.20 | 13.80 | / |
| 2 | 13.6 | 351.4 | 0.94 | 99.06 | / |
| 3 | 3.4 | 315.1 | 0.94 | 99.06 | / |
| 4 | 15.1 | 371.1 | / | / | 100.00 |
| 5 | 15.6 | 373.1 | |||
| 6 | 1.0 | 372.1 | 98.22 | 1.78 | / |
| 7 | 0.5 | 316.1 | 98.22 | 1.78 | / |
| 8 | 8.0 | 355.1 | 34.75 | 65.25 | / |
| 9 | 4.0 | 356.1 | 34.75 | 65.25 | / |
| 10 | 6.9 | 375.2 | 99.83 | 0.17 | / |
Bonded test-results room temperature is heated up in a steamer in table 2 distillation and extraction clearly: 9 ℃
| The stream thigh | Flow (ml/s) | Temperature (K) | Form (mol%) | ||
| Water | | Ethylene glycol | |||
| 1 | 11.0 | 347.6 | 86.36 | 13.64 | / |
| 2 | 10.5 | 351.7 | 10.60 | 89.40 | / |
| 3 | 3.5 | 315.1 | 10.60 | 89.40 | / |
| 4 | 4.1 | 373.1 | / | / | 100.00 |
| 5 | 4.6 | 374.1 | |||
| 6 | 0.8 | 372.1 | 98.25 | 1.75 | / |
| 7 | 0.4 | 315.1 | 98.25 | 1.75 | / |
| 8 | 8.0 | 355.1 | 37.43 | 62.57 | / |
| 9 | 4.0 | 354.1 | 37.43 | 62.57 | / |
| 10 | 6.9 | 374.2 | 99.06 | 0.94 | / |
Claims (3)
1, a kind of ethanol extraction rectification technique of concentrating and reclaiming, it is characterized in that adopting primary tower that ethanol in the fermented liquid is purified to 60%～66% (mol), with ethylene glycol is extraction agent, adopts extractive distillation column ethanol to be concentrated into 89%～99.1% (mol) again, and ethylene glycol uses through the regenerator column reprocessing cycle.
2, the extraction rectification technique that ethanol according to claim 1 concentrates and reclaims, it is characterized in that containing in the technical process ethanol 13%～20%(mol) fermented liquid delivers to primary tower and carries out fore-running, produce waste liquid at the bottom of the fore-running Tata, overhead distillate contains ethanol 60～66%(mol), deliver to extractive distillation column, extraction tower is extraction solvent with ethylene glycol, ratio 1～4: 1 volume ratio of extraction agent and extraction tower inlet amount, temperature in is controlled at 370K～373K, reflux ratio (R) gets 2～3, extracting and separating second alcohol and water, overhead distillate contains the second alcohol and water, and overhead distillate contains ethanol 89%～99.1%(mol), the tower bottom flow fluid is delivered to solvent regeneration tower, the regenerator column overhead distillate is a waste liquid, and tower bottom flow goes out not contain the extraction solvent of second alcohol and water and delivers to extraction tower, recycles.
3, the ethanol according to claim 1 extraction rectification technique that concentrates and reclaim is characterized in that extraction agent ethylene glycol adopts industrial goods, and content is more than 96%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93110577 CN1091414A (en) | 1993-02-24 | 1993-02-24 | The extraction rectification technique that ethanol concentrates and reclaims |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93110577 CN1091414A (en) | 1993-02-24 | 1993-02-24 | The extraction rectification technique that ethanol concentrates and reclaims |
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| CN1091414A true CN1091414A (en) | 1994-08-31 |
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| CN 93110577 Pending CN1091414A (en) | 1993-02-24 | 1993-02-24 | The extraction rectification technique that ethanol concentrates and reclaims |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092309C (en) * | 1997-07-18 | 2002-10-09 | Smc株式会社 | Valve guide structure |
| CN102126924A (en) * | 2011-01-05 | 2011-07-20 | 安徽科立华化工有限公司 | Recycling method of waste ethanol obtained through recrystallization of oxadiazon |
| CN102399130A (en) * | 2011-12-13 | 2012-04-04 | 西南化工研究设计院 | Method for simplifying rectification process for preparing ethanol through hydrogenation of acetic acid |
| CN103130610A (en) * | 2011-11-23 | 2013-06-05 | 四川制药制剂有限公司 | Ethanol purification device with accurate temperature control |
| CN108046991A (en) * | 2017-12-07 | 2018-05-18 | 佛山手心制药有限公司 | A kind of method that edestan recycling ethyl alcohol recycles |
| CN110433516A (en) * | 2019-05-23 | 2019-11-12 | 河南莱帕克物联装备技术股份有限公司 | A kind of dehydrated alcohol Refining tests device and technique |
-
1993
- 1993-02-24 CN CN 93110577 patent/CN1091414A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092309C (en) * | 1997-07-18 | 2002-10-09 | Smc株式会社 | Valve guide structure |
| CN102126924A (en) * | 2011-01-05 | 2011-07-20 | 安徽科立华化工有限公司 | Recycling method of waste ethanol obtained through recrystallization of oxadiazon |
| CN102126924B (en) * | 2011-01-05 | 2013-06-05 | 安徽科立华化工有限公司 | Recycling method of waste ethanol obtained through recrystallization of oxadiazon |
| CN103130610A (en) * | 2011-11-23 | 2013-06-05 | 四川制药制剂有限公司 | Ethanol purification device with accurate temperature control |
| CN102399130A (en) * | 2011-12-13 | 2012-04-04 | 西南化工研究设计院 | Method for simplifying rectification process for preparing ethanol through hydrogenation of acetic acid |
| CN102399130B (en) * | 2011-12-13 | 2014-07-02 | 西南化工研究设计院 | Method for simplifying rectification process for preparing ethanol through hydrogenation of acetic acid |
| CN108046991A (en) * | 2017-12-07 | 2018-05-18 | 佛山手心制药有限公司 | A kind of method that edestan recycling ethyl alcohol recycles |
| CN108046991B (en) * | 2017-12-07 | 2020-07-28 | 佛山手心制药有限公司 | Method for recycling ethanol from fructus cannabis |
| CN110433516A (en) * | 2019-05-23 | 2019-11-12 | 河南莱帕克物联装备技术股份有限公司 | A kind of dehydrated alcohol Refining tests device and technique |
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