CN100371310C - Method for separating ethyl ether, ethyl alcohol and acid water by combining rectifying and azeotropic distilling - Google Patents
Method for separating ethyl ether, ethyl alcohol and acid water by combining rectifying and azeotropic distilling Download PDFInfo
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- CN100371310C CN100371310C CNB2006100389570A CN200610038957A CN100371310C CN 100371310 C CN100371310 C CN 100371310C CN B2006100389570 A CNB2006100389570 A CN B2006100389570A CN 200610038957 A CN200610038957 A CN 200610038957A CN 100371310 C CN100371310 C CN 100371310C
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- ethanol
- ether
- water
- sour water
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 167
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 title claims abstract description 104
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000002253 acid Substances 0.000 title claims abstract description 12
- 235000019441 ethanol Nutrition 0.000 title abstract 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000004821 distillation Methods 0.000 claims abstract description 16
- 238000010533 azeotropic distillation Methods 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 241000282326 Felis catus Species 0.000 claims description 22
- 238000010992 reflux Methods 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 3
- 239000011260 aqueous acid Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 2
- 238000000605 extraction Methods 0.000 abstract 1
- 238000007599 discharging Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- PSLIMVZEAPALCD-UHFFFAOYSA-N ethanol;ethoxyethane Chemical compound CCO.CCOCC PSLIMVZEAPALCD-UHFFFAOYSA-N 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 210000000689 upper leg Anatomy 0.000 description 1
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Abstract
The present invention relates to a method for separating ethyl ether, ethyl alcohol and acid water by combining extraction and azeotropic distillation. Cyclohexane is used as an azeotropic agent for azeotropic distillation, and the method comprises: firstly, a mixed solution of ethyl alcohol, ethyl ether and acid water is separated by adopting a rectification apparatus, after separation, ethyl ether is obtained at tower top, and ethyl alcohol and acid water are obtained at tower bottom; ethyl ether and acid water at the tower bottom are introduced into a deacidification and rectification tower and separated, ethyl alcohol and water are obtained at the top of the deacidification and rectification tower, acid water is obtained at tower bottom, and the acid water is neutralized; and ethyl alcohol and water at the top of the deacidification and rectification tower are introduced into an azeotrpic distillation apparatus, cyclohexane (benzene and the like) is adopted as the azeotropic agent and circularly used in the azeotrpic distillation apparatus, the water content of ethyl alcohol can be reduced to lower than 0.2% by the azeotrpic distillation apparatus, and thus, ethyl alcohol can be returned to the raw materials for reuse. In the separation process, optimum technological conditions are adopted in all apparatuses, after separation, the water contents of ethyl ether and ethyl alcohol can be respectively reduced to lower than 1.5% and 0.2%, and thus, the requirement of circular use can be achieved.
Description
Technical field
The present invention relates to a kind of separating process of chemical industry, the rectifying of particularly a kind of ether, ethanol and sour water and the separation method that component distillation combines.
Technical background
Along with developing rapidly of China's economic construction, adopt ethanol constantly to increase as the demand of solvent, according to estimates, year demand is about 4,000,000 tons at present, and domestic annual production only is 200～3,000,000 tons, does not satisfy the demand in market far away, still needs the part import.Generally adopt ethanol as solvent in many building-up processes of medicine, chemical industry and pesticide intermediate, especially under acid (solid acid or mineral acid) catalyzer existence condition, ethanol is produced ether easily, so just form ethanol, ether and acidic aqueous solution easily, ethanol, ether and water all can form azeotrope, the azeotropic point and the composition that form azeotrope are shown in Table 1
| Material | The azeotropic point temperature (℃) | Azeotropic is formed |
| Water+ethanol | 78.17℃ | 4.4% (water) 95.6% (ethanol) |
| Water+ether | 34.15℃ | 1.3% (water) 98.7% (ether) |
Can the azeotrope that produce be (ethanol+water+ether), and therefore, can ethanol+water+ether effectively separate, be related to ethanol and reclaim and recycle.At present ethanol+ether+sour water separates general gap rectification method etc. and takes off ether earlier in the industrial production, steam ethanol then, adopt this method separating alcohol and ether, isolating ether and purity of alcohol is generally about 94% and 91%, and a yield only is about 87% and 80%, separate not thoroughly, can cause again the difficulty of removal process and energy consumption height.Simultaneously contain certain ethanol in the sour water and ether easily throws into question to environment.
Summary of the invention
The present invention will provide a kind of new separation method, adopt rectifying and the component distillation method separating alcohol+ether+sour water that combines, and separate back ethanol and recycle, and ether can be used as other solvent and uses, and ethanol and ether content are lower in the sour water simultaneously.
The technical scheme of finishing the foregoing invention task is: the method for Separated ether by rectification and azeotropic distillation, ethanol and sour water, and step is as follows:
At first adopt rectifier unit separating alcohol+ether+sour water mixing solutions, after the separation, cat head is an ether, is ethanol+sour water at the bottom of the tower;
Ethanol+sour water at the bottom of the tower is delivered to the depickling rectifying tower and is separated, and the depickling rectifying tower top is ethanol+water, is sour water at the bottom of the tower;
Sour water neutralizing treatment at the bottom of the tower;
Ethanol+the water of depickling rectifying tower top is delivered to the component distillation device, and adds entrainer and carry out component distillation, and entrainer recycles in the azeotropic device;
Ethanol is returned to raw material and re-uses.
Above-described entrainer can adopt hexanaphthene, benzene or toluene etc.
Separating apparatus adopts optimizes processing condition, and separated ethyl ether and ethyl, ethanol water content can be taken off respectively to below 2% and 0.2%, can reach the requirement that recycles.
Refluxing in the sepn process, when stage number is as follows to the influence of each device, other condition of T-1 tower is constant in the table 1, reflux ratio (R) to the influence of ethanol at the bottom of the tower and cat head ether content is: when reflux ratio is increased to 5 gradually by 1, ether concentration reduces very fast at the bottom of the tower, when R=2, cat head ether content reaches more than 98%, does not have ether at the bottom of the tower and exists, when R increased again, ethanol content changed less; Other condition of T-1 tower is constant in the table 1, stage number (N) to the influence of ethanol content at the bottom of the tower and cat head ether is: when stage number is increased to 16 gradually by 10, alcohol concn begins to increase very fast, when N=12, cat head ether content reaches more than 98%, do not had ether at the bottom of the tower, when N increased again, ethanol and ether content were less;
Other condition of T-2 tower is constant in the table 1, and reflux ratio (R) to the influence of cat head ethanol content is: when reflux ratio was increased to 8 gradually by 2, alcohol concn began to increase very fast, and when R=4, ethanol content reaches more than 95%, and when R increased again, ethanol content changed less; Other condition of T-2 tower is constant in the table 1, and stage number (N) to the influence of ethanol content at the bottom of the tower is: when stage number was increased to 40 gradually by 25, alcohol concn began to increase very fast, when N=35, ethanol content reaches more than 95%, and when N increased again, ethanol content changed less;
Other condition of T-3 tower is constant in the table 1, and reflux ratio (R) to the influence of ethanol content at the bottom of the tower is: when reflux ratio was increased to 6 gradually by 2, alcohol concn began to increase very fast, when R=4, ethanol content reaches more than 99.8%, and when R increased again, ethanol content changed less; Other condition of T-3 tower is constant in the table 1, and stage number (N) to the influence of ethanol content at the bottom of the tower is: when stage number was increased to 37 gradually by 25, alcohol concn began to increase very fast, when N=31, ethanol content reaches more than 99.8%, and when N increased again, ethanol content changed less;
Other condition of T-4 tower is constant in the table 1, and reflux ratio (R) to the influence of ethanol content at the bottom of the tower is: when reflux ratio is increased to 6 gradually by 2, contains alcohol concn at the bottom of the tower in the water and reduce very fast, when R=4, ethanol content is lower than 0.2%, and when R increased again, ethanol content changed less; Other condition of T-4 tower is constant in the table 1, and stage number (N) to the influence of ethanol content at the bottom of the tower is: when stage number is increased to 45 gradually by 30, at the bottom of the tower in the water alcohol concn begin to reduce very fast, when N=37, ethanol content is lower than 0.2%, and when N increased again, ethanol content changed less.
Described " optimization processing condition " are: raw material F1 is ether+ethanol+sour water mixed solution, the mass content (Xf1, Xf2, Xf3) of ether (1), ethanol (2) and sour water (3) is respectively 2%, 93%, 5%, pH=1～2, flow is 110Kg/h, through being preheated to 33 ℃, when precise rectification tower T-1 top, end temperature are respectively 34.5 ℃ and 78-81 ℃, top, low flow are respectively 2.24Kg/h, 107.76Kg/h, the pH value is respectively 5～6 and 1～2, precise distillation cat head reflux ratio (R1) is controlled at 2～3, forms (x at the bottom of the cat head
Di, x
Wi) x
D1=0.9810, x
D2=0.0055, x
D3=0.0135, x
W1=0.0000, x
W2=0.9485, x
W3=0.0515; Component is delivered to depickling rectifier unit T-2 processing at the bottom of the tower, and trim the top of column is controlled at 3～4 than (R2), and rectifying tower top can get 95.12% ethanol, and the pH value is 5～6, is rich in the aqueous acid neutralizing treatment at the bottom of the tower; Precise distillation cat head stream part is delivered to azeotropic device T-3, adopt benzene as entrainer, blend column overhead distillate is after condenser condenses, layering in liquid liquid separator tank, the benzene layer refluxes, water layer is delivered to azeotrope column T-4 and is handled, and can get the ethanol more than 99.8% at the bottom of the azeotropic Tata, and cat head, end cut pH value are 5～6; Azeotrope column T-4 top, end pH value are 6～7, and water-content is 99.84% at the bottom of the tower.
Advantage of the present invention: adopt technology shown in Figure 1 and optimized parameters, raw material (ethanol+ether+sour water) at first separates T-1 through rectifying tower, tower is low then separates with device T-4 with azeotropic device T-3 through rectifier unit T-2, and separated ethyl ether and ethyl and ethanol content can reach more than 98% and 99.8% respectively; Separate and to contain ethanol in the water of back and the ether amount all is lower than below 1.5% and 0.05%, compare with present method therefor, once ether can be separated, one time yield reaches more than 99.9%, and the ethanol that rectifying is separated+water azeotrope separates through the azeotropic device, and alcoholic acid purity reaches more than 99.8%, can be recycled, one time yield reaches 99.4%, and alcohol concn is lower than 1.5% in the sour water, is difficult for throwing into question to environment.
Description of drawings
Fig. 1 rectifying and component distillation process combined flow process.
Embodiment
With reference to parameter shown in technology shown in Figure 1 and the table 2, raw material (F1) is ether+ethanol+sour water mixed solution, the mass content (Xf1, Xf2, Xf3) of ether (1), ethanol (2) and sour water (3) is respectively 2%, 93%, 5%, pH=1～2, flow is 110Kg/h, through being preheated to 33 ℃, when precise rectification tower T-1 top, low temperature are respectively 34.5 ℃ and 78-81 ℃, top, low flow are respectively 2.24Kg/h, 107.76Kg/h, the pH value is respectively 5～6 and 1～2, precise distillation cat head reflux ratio (R1) is controlled at 2～3, forms (x at the bottom of the cat head
Di, x
Wi) x
D1=0.9810, x
D2=0.0055, x
D3=0.0135, x
W1=0.0000, x
W2=0.9485, x
W3=0.0515; Component is delivered to depickling rectifier unit T-2 processing at the bottom of the tower, and trim the top of column is controlled at 3～4 than (R2), and rectifying tower top can get 95.12% ethanol, and the pH value is 5～6, is rich in the aqueous acid neutralizing treatment at the bottom of the tower; Precise distillation cat head stream part is delivered to azeotropic device T-3, adopt benzene as entrainer, blend column overhead distillate is after condenser condenses, layering in liquid liquid separator tank, the benzene layer refluxes, water layer is delivered to azeotrope column T-4 and is handled, and can get the ethanol more than 99.8% at the bottom of the azeotropic Tata, and cat head, end cut pH value branch are 5～6; Azeotrope column T-4 top, end pH value are 6～7, and water-content is 99.84% at the bottom of the tower.
Each tower process condition of table 1
| The T-1 tower | The T-2 tower | The T-3 tower | The T-4 |
||||
| 1. feed entrance point reflux ratio (R1) stage number tower top temperature ℃ column |
5 2-3 12 34.5 78-81 | 2. feed entrance point reflux ratio (R2) stage number tower top temperature ℃ column bottom temperature ℃ | 18 3-4 35 76-79 97-102 | 3. feed entrance point reflux ratio (R3) stage number tower top temperature ℃ column |
7 4-5 31 64-66 78-79 | 4. feed entrance point reflux ratio stage number tower top temperature ℃ column |
10 3-4 37 64-66 99-102 |
Table 2 separating resulting
| The stream thigh | Title | Flow (Kg/h) | Form (mass content) | ||||
| Ether | Ethanol | Water | | PH value | |||
| ① ② ③ ④ ⑤ ⑥ ⑦ ⑧ ⑨ ⑩ | Stock liquid (F 1) tower T-1 ejects at the bottom of the material tower T-1 discharging tower T-2 and eject material tower T-3 and eject material tower T-4 and eject discharging at the bottom of the discharging tower T-4 at the bottom of the discharging tower T-3 at the bottom of the material layering bottom land discharging tower T-2 | 110 2.24 107.76 107.45 210.15 70.54 73.14 0.31 102.29 5.16 | 0.0200 0.9810 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 | 0.9300 0.0055 0.9485 0.9512 0.1850 0.1850 0.5300 0.0126 0.9991 0.0016 | 0.0500 0.0135 0.0515 0.0488 0.0740 0.0740 0.3600 0.9874 0.0009 0.9984 | 0.0000 0.0000 0.0000 0.0000 0.7410 0.7410 0.1100 0.0000 0.0000 0.0000 | 1-2 5-6 1-2 5-6 5-6 6-7 6-7 0-1 5-6 6-7 |
Claims (3)
1. the method for a Separated ether by rectification and azeotropic distillation, ethanol and sour water, step is as follows:
At first adopt rectifier unit separating alcohol+ether+sour water mixing solutions, after the separation, cat head is an ether, is ethanol+sour water at the bottom of the tower;
Ethanol+sour water at the bottom of the tower is delivered to the depickling rectifying tower and is separated, and the depickling rectifying tower top is ethanol+water, is sour water at the bottom of the tower;
Sour water neutralizing treatment at the bottom of the tower;
Ethanol+the water of depickling rectifying tower top is delivered to the component distillation device, and adds entrainer and carry out component distillation, and entrainer recycles in the azeotropic device;
Ethanol is returned to raw material and re-uses.
2. according to the method for the described Separated ether by rectification and azeotropic distillation of claim 1, ethanol and sour water, it is characterized in that described entrainer is selected from hexanaphthene, benzene or toluene.
3. according to the method for claim 1 or 2 described Separated ether by rectification and azeotropic distillation, ethanol and sour water, it is characterized in that described processing condition are:
Raw material F1 is ether+ethanol+sour water mixed solution, ether, the mass content of ethanol and sour water is respectively 2%, 93%, 5%, pH=1～2, flow is 110Kg/h, through being preheated to 33 ℃, precise rectification tower T-1 top, when low temperature is respectively 34.5 ℃ and 78-81 ℃, the top, the underflow amount is respectively 2.24Kg/h, 107.76Kg/h, the pH value is respectively 5～6 and 1～2, precise distillation cat head reflux ratio R1 is controlled at 2～3, forms at the bottom of the cat head: mass content=0.9810 of accurate fractionate cat head ether, accurate fractionate cat head alcoholic acid mass content=0.0055, mass content=0.0135 of accurate fractionate cat head sour water, mass content=0.0000 of ether at the bottom of the accurate fractionate tower, alcoholic acid mass content=0.9485 at the bottom of the accurate fractionate tower, mass content=0.0515 of sour water at the bottom of the accurate fractionate tower; Component is delivered to depickling rectifier unit T-2 processing at the bottom of the tower, and trim the top of column is controlled at 3～4 than R2, and rectifying tower top can get 95.12% ethanol, and the pH value is 5～6, is rich in the aqueous acid neutralizing treatment at the bottom of the tower; Precise distillation cat head stream part is delivered to azeotropic device T-3, adopt benzene as entrainer, blend column overhead distillate is after condenser condenses, layering in liquid liquid separator tank, the benzene layer refluxes, water layer is delivered to azeotrope column T-4 and is handled, and can get the ethanol more than 99.8% at the bottom of the azeotropic Tata, and cat head, end cut pH value branch are 5～6; Azeotrope column T-4 top, end pH value are 6～7, and water-content is 99.84% at the bottom of the tower.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100389570A CN100371310C (en) | 2006-03-21 | 2006-03-21 | Method for separating ethyl ether, ethyl alcohol and acid water by combining rectifying and azeotropic distilling |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100389570A CN100371310C (en) | 2006-03-21 | 2006-03-21 | Method for separating ethyl ether, ethyl alcohol and acid water by combining rectifying and azeotropic distilling |
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|---|---|
| CN1821199A CN1821199A (en) | 2006-08-23 |
| CN100371310C true CN100371310C (en) | 2008-02-27 |
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| CN102321013B (en) * | 2011-09-06 | 2013-06-05 | 天津大学 | Piperidone continuous refining production method and device capable of continuously recovering acetone |
| CN105036437B (en) * | 2015-07-09 | 2017-03-08 | 西南化工研究设计院有限公司 | A kind of handling process of producing ethylene from dehydration of ethanol high-concentration waste water |
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Assignee: Jiangsu Longchang Chemical Co., Ltd. Assignor: Nanjing Normal University Contract fulfillment period: 2008.5.9 to 2017.5.9 contract change Contract record no.: 2009320000742 Denomination of invention: Method for separating ethyl ether, ethyl alcohol and acid water by combining rectifying and azeotropic distilling Granted publication date: 20080227 License type: Exclusive license Record date: 2009.5.4 |
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