CN102008831A - Rectification and recovery system of alcohol with high purity - Google Patents
Rectification and recovery system of alcohol with high purity Download PDFInfo
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- CN102008831A CN102008831A CN201010293728XA CN201010293728A CN102008831A CN 102008831 A CN102008831 A CN 102008831A CN 201010293728X A CN201010293728X A CN 201010293728XA CN 201010293728 A CN201010293728 A CN 201010293728A CN 102008831 A CN102008831 A CN 102008831A
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- condenser
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- tail gas
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- alcohol
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000011084 recovery Methods 0.000 title claims abstract description 18
- 239000000498 cooling water Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 3
- 238000011194 good manufacturing practice Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 3
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 25
- 238000000034 method Methods 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000002835 absorbance Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 238000004821 distillation Methods 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000004134 energy conservation Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000007812 deficiency Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a rectification and recovery system of alcohol with high purity. The system is characterized in that the top of a stripping tower (2) is connected with a fusel collector (3) which is connected with a rectifying tower (4) through a pipeline; the top of the rectifying tower (4) is connected with a finished product collector (5) the top of which is connected with the top of a condenser (6) through a pipeline; the lower end of the condenser (6) is connected with the upper part of the finished product collector (5) through a pipeline; the lower end of the finished product collector (5) is connected with a finished product cooler (8) through a pipeline; and the tail end of a tail gas condenser (7) is connected with a tail gas sorption pump (9). The invention has the beneficial effects that the problem that ultraviolet absorbency exceeds the standard is solved, real-time and exact monitoring is realized, the product quality is ensured, and the purity of the recycled product is high; the system is energy-saving and water-saving, has the characteristics of reasonable design and automated control, is simple and convenient to operate, and meets requirements of good manufacturing practice (GMP).
Description
Technical field
The present invention relates to a kind of the exceed standard new equipment of problem of recovered alcohol absorbance, particularly a kind of high-purity ethanol refinery recovery system of solving.
Background technology
Along with developing rapidly of China's traditional Chinese medicine cause, alcohol is as the main solvent that extracts, and consumption grows with each passing day.Therefore reclaiming discarded Diluted Alcohol, and guarantee the quality of recovered alcohol, make it reach the recycling standard and utilize once more, is that vast herbal pharmaceutical enterprise reduces production costs the main path of increasing economic efficiency.Alcohol distillation column is made up of tower still, body of the tower, condenser, cooler, surge tank, six parts of high-order basin, its operation principle is to utilize the alcohol boiling point to be lower than other solution boiling point, alcohol begins a large amount of volatilizations when reaching the boiling point of alcohol, and this moment, other compositions such as soup did not reach boiling point, basically non-volatile, alcohol just is separated like this, and cooling just obtains liquid alcohol to alcohol steam then, thereby reaches the purpose of recovered alcohol.Yet there is following problem in the existing alcohol distillation column of China at present:
(1) the alcohol rate of recovery is not high, and energy resource consumption is big.Because there is technological deficiency in rectification process itself, the liquid distribution inequality causes wall slide phenomenon serious, and energy resource consumption is big.
(2) recovered alcohol quality dissatisfaction, particularly the absorbance index is defective.Recovered alcohol, not only ethanol content and relative density should meet the requirements (under the normal temperature, ethanol content is not less than 95%, and relative density is not more than 0.8129), and its trap also wants the index up to specification (should be less than 0.08 during 240nm; Should be during 250-260nm less than 0.06; Should be during 270-340nm less than 0.02), but present alcohol recovery technology does not also reach this index.
(3) automation degree of equipment is not high.For the concentration of recovered alcohol, adopt off-line analysis, this just is difficult to guarantee that the concentration of recovered alcohol is accurate, and has hysteresis quality.
Rectifying has critical role as the core technology of alcohol recovery device in the alcohol removal process, rectification process has not only determined the quality of final recovered alcohol product, and is controlling product yield and public work consumption.Therefore, develop the rectifying equipment and the technical method efficient, low consumption that have independent intellectual property right,, have great realistic price for improving the quality of products and stability, improving modernization of Chinese medicine level and reduce enterprise's production cost and have profound significance.
Summary of the invention
At the defective of present alcohol distillation column, the invention provides a kind of high-purity ethanol refinery recovery system.
To achieve these goals, the technical solution used in the present invention is:
A kind of high-purity ethanol refinery recovery system, comprise reboiler, carry and heat up in a steamer tower, rectifying column, condenser, tail gas condenser and finished product cooler, carry and heat up in a steamer tower and be connected reboiler, condenser is connected with tail gas condenser, carry the top of heating up in a steamer tower and be connected with the fusel gatherer, the fusel gatherer links to each other with rectifying column by pipeline, the rectifying column top is connected with product collector, the product collector top is connected with the top of condenser by pipeline, the lower end of condenser links to each other with the top of product collector by pipeline, the lower end of product collector is connected with the finished product cooler by pipeline, and the end of tail gas condenser is connected with the tail gas suction pump;
Be connected with triple valve between described finished product cooler and the condenser, one end of triple valve links to each other with the finished product cooler, the other end of triple valve links to each other with the ultraviolet-visible spectrophotometer that is connected with recorder by rubber tube, and the 3rd end of triple valve is connected with the alcohol concentration detector;
Described tail gas suction pump is a variable frequency pump, and the setting range of its flow is 0～1m
3/ h;
Described cooling device is a frequency conversion cooling water flow regulative mode;
Described pipeline is a rubber tube.
Beneficial effect of the present invention: solved the problem that recovered alcohol finished product ultraviolet absorptivity exceeds standard, the recovered alcohol absorbance is monitored in real time, guaranteed that recovered alcohol reaches quality requirement; Accurately detect alcohol concentration, guarantee constant product quality, reliable; Possess multiple spot impurity and get rid of function, the product purity height of recovery; Whole ethanol refinery system's evaporation rate and condensation rate are in stable state, reach water saving, energy-conservation effect; Method and reasonable in design has automation control function, and is easy and simple to handle, more meets GMP requirements such as environmental protection, energy-conservation, safety and equipment long-time running.
Description of drawings
Fig. 1, structural representation of the present invention.
The specific embodiment
A kind of high-purity ethanol refinery recovery system, comprise reboiler 1, carry and heat up in a steamer tower 2, rectifying column 4, condenser 6, tail gas condenser 7 and finished product cooler 8, carry and heat up in a steamer tower 2 and be connected reboiler 1, condenser 6 is connected with tail gas condenser 7, carry the top of heating up in a steamer tower 2 and be connected with fusel gatherer 3, fusel gatherer 3 links to each other with rectifying column 4 by pipeline, rectifying column 4 tops are connected with product collector 5, product collector 5 tops are connected by the top of pipeline with condenser 6, the lower end of condenser 6 links to each other by the top of pipeline with product collector 5, the lower end of product collector 5 is connected with finished product cooler 8 by pipeline, and the end of tail gas condenser 7 is connected with tail gas suction pump 9; Be connected with triple valve 11 between described finished product cooler 8 and the condenser 6, one end of triple valve 11 links to each other with finished product cooler 8, the other end of triple valve 11 links to each other with the ultraviolet-visible spectrophotometer 10 that is connected with recorder 13 by rubber tube, and the 3rd end of triple valve 11 is connected with alcohol concentration detector 12; Described tail gas suction pump 9 is a variable frequency pump, and the setting range of its flow is 0～1m
3/ h; Described cooling device is a frequency conversion cooling water flow regulative mode; Described pipeline is a rubber tube.
During system works, heated mixed vapour moves upward through reboiler 1, Diluted Alcohol heats up in a steamer tower 2 tops and moves downwards from carrying, during through fusel gatherer 3, most of liquid redistribution continues operation downwards, small part is taken out as fusel, gas, liquid carries out matter in running, can exchange, carry and heat up in a steamer tower 2 top gases and send rectifying column 4 bottoms to through pipeline, and upwards operation, entering condenser 6 from rectifying column 4 tops, most of gas is condensed into liquid, small part gas enters tail gas condenser 7 as tail gas and carries out condensation, and uncooled tail gas enters tail gas suction pump 9 discharge systems.The liquid of condenser 6 lower ends returns operation downwards behind rectifying column 4 tops, during through product collector 5, the gas that a part continues operation downwards and upwards operation carries out matter, can exchange, another part carries out the online detection of absorbance and alcohol concentration through finished product cooler 8, treats that sample reaches qualified requirement back taking-up and so finishes the whole recovery process as finished product.
In the course of work, when having one to surpass setting value in reboiler temperature, rectifying tower top temperature, rectifying steam pressure and the rectifying column pressure, close the heating steam control valve, when all being no more than setting value, enter pid loop, the aperture of steam regulation control valve, control rectifying steam pressure is controlled tower top temperature simultaneously and is no more than setting value about the steam pressure of setting.The ratio of water is very big in reboiler after the rectifying for a long time, presses the button, and stops fluid infusion automatically, stops rectifying, and the steam off control valve is opened atmospheric valve, opens blowoff valve and carries out draining.In the cooling device, when cooling water inlet temperature and cooling water outlet temperature difference during greater than 15 ℃, show the chilled(cooling) water supply (CWS) deficiency, the variable frequency pump frequency increases automatically increases cooling water flow, guarantees cooling effect; When cooling water inlet temperature and cooling water outlet temperature difference during less than 15 ℃, the variable frequency pump frequency reduces automatically reduces cooling water flow, reaches the water saving purpose.
Embodiment one
Investigate the influence of tail gas suction to rectification effect,
Untreated Diluted Alcohol is squeezed in the distillation still with pump, minimumly must not be lower than steam-heating pipe in the still, the highlyest must not exceed the tower still
Footpath 2/3,, open cold condenser and cooler water intaking valve, and confirm to have had the water proper flow,
The return valve standard-sized sheet is opened the tail gas suction pump then, opens steam valve and heats.In implementation process, instrument parameters such as record available machine time, feed time, stabilization time, tower top temperature, condensation outlet temperature, condenser return water temperature, the results are shown in Table 1, after alcohol to be recycled reaches stable state, get a sample in per 10 minutes, get six samples altogether, sample number into spectrum is respectively A1, A2, A3, A4, A5, measure its ethanol content, relative density, absorbance respectively, the record experimental data, experimental result sees Table 1.
The suction of table 1 tail gas is to the experimental result of rectification effect influence
Embodiment two
Investigate of the influence of tail gas pumping velocity to rectification effect,
Untreated Diluted Alcohol is squeezed in the distillation still with pump, minimumly must not be lower than steam-heating pipe in the still, the highlyest must not exceed the tower still
Footpath 2/3, open cold condenser and cooler water intaking valve, and confirm to have had the water proper flow,
The return valve standard-sized sheet is opened steam valve then and is heated.Concrete implementation step is identical with embodiment one, in implementation process, gets first sample when finished product concentration meets the requirements, and per hour gets a sample later on, and (exhaust flow is 0.8m to first three sample
3/ h) to have got the back to regulate exhaust flow, still (exhaust flow is 0.5m to sample by per hour getting one and carrying out
3/ h), sample number into spectrum is respectively B1, B2, B3, B4, B5, B6, B7, measures its ethanol content, relative density, absorbance respectively, the record experimental data, and experimental result sees Table 2.
Table 2 tail gas aspiration rate is to the experimental result of rectification effect influence
Beneficial effect of the present invention: utilize normal pressure tail gas to deviate from technology and solve the problem that recovered alcohol finished product ultraviolet absorptivity exceeds standard, and increased UV, visible light absorbance on-line monitoring equipment, the recovered alcohol absorbance is monitored in real time, guarantee that recovered alcohol reaches quality requirement; Adopt online alcohol content tester that alcohol concentration is carried out online measuring technique research, accurately detect alcohol concentration, guarantee constant product quality, reliable; Owing to increased fusel gatherer, product collector, got rid of function, the product purity height of recovery, production efficiency thereby make this device possess multiple spot impurity
Improve 10%, the recovered alcohol that obtains at normal temperatures, ethanol content can reach more than 98%, relative density is also less than 0.8129; By frequency conversion cooling water flow regulative mode, make whole ethanol refinery system's evaporation rate and condensation rate be in stable state, cooling water amount is saved more than 20%, reaches water saving, energy-conservation effect; Method and reasonable in design has automation control function, and is easy and simple to handle, more meets GMP requirements such as environmental protection, energy-conservation, safety and equipment long-time running.
The alcohol that native system is not only applicable to the herbal pharmaceutical production process reclaims, and also is applicable to the alcohol removal process of industries such as other chemical industry, food.
Simple replacement of those skilled in the art and replacing all are within this patent protection domain in this area.
Claims (5)
1. high-purity ethanol refinery recovery system, comprise reboiler (1), carry and heat up in a steamer tower (2), rectifying column (4), condenser (6), tail gas condenser (7) and finished product cooler (8), carry and heat up in a steamer tower (2) and be connected reboiler (1), condenser (6) is connected with tail gas condenser (7), it is characterized in that: carry the top of heating up in a steamer tower (2) and be connected with fusel gatherer (3), fusel gatherer (3) links to each other with rectifying column (4) by pipeline, rectifying column (4) top is connected with product collector (5), product collector (5) top is connected by the top of pipeline with condenser (6), the lower end of condenser (6) links to each other by the top of pipeline with product collector (5), the lower end of product collector (5) is connected with finished product cooler (8) by pipeline, and the end of tail gas condenser (7) is connected with tail gas suction pump (9).
2. a kind of high-purity ethanol refinery recovery system according to claim 1, it is characterized in that: be connected with triple valve (11) between described finished product cooler (8) and the condenser (6), one end of triple valve (11) links to each other with finished product cooler (8), the other end of triple valve (11) links to each other with the ultraviolet-visible spectrophotometer that is connected with recorder (13) (10) by rubber tube, and the 3rd end of triple valve (11) is connected with alcohol concentration detector (12).
3. a kind of high-purity ethanol refinery recovery system according to claim 1 and 2 is characterized in that: described tail gas suction pump (9) is a variable frequency pump, and the setting range of its flow is 0～1m
3/ h.
4. a kind of high-purity ethanol refinery recovery system according to claim 3 is characterized in that: described cooling device adopts frequency conversion cooling water flow regulative mode.
5. a kind of high-purity ethanol refinery recovery system according to claim 4, it is characterized in that: described pipeline is a rubber tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010293728XA CN102008831A (en) | 2010-09-27 | 2010-09-27 | Rectification and recovery system of alcohol with high purity |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010293728XA CN102008831A (en) | 2010-09-27 | 2010-09-27 | Rectification and recovery system of alcohol with high purity |
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| CN102008831A true CN102008831A (en) | 2011-04-13 |
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ID=43839279
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| CN201010293728XA Pending CN102008831A (en) | 2010-09-27 | 2010-09-27 | Rectification and recovery system of alcohol with high purity |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636003A (en) * | 2012-05-16 | 2012-08-15 | 唐山三友氯碱有限责任公司 | Energy-saving device for rectification tail gas condensation system |
| CN105080173A (en) * | 2015-09-29 | 2015-11-25 | 广西新龙制药有限责任公司 | Alcohol recovery tower |
| CN106807096A (en) * | 2015-11-28 | 2017-06-09 | 衡阳春天医药化工设备有限公司 | A kind of alcohol recovery device |
| CN111474971A (en) * | 2020-04-28 | 2020-07-31 | 宁波奥克斯电气股份有限公司 | Control method for preventing excessive low water flow and water supply machine |
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| CN2571758Y (en) * | 2002-07-24 | 2003-09-10 | 林明刚 | External circulation evaporation low position back flow alcohol distillation equipment |
| CN1802194A (en) * | 2003-04-25 | 2006-07-12 | 2S－精密系统有限公司 | Distillation method |
| CN101235392A (en) * | 2008-01-16 | 2008-08-06 | 柏晓东 | Cellulose fuel ethanol and preparation method thereof |
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2010
- 2010-09-27 CN CN201010293728XA patent/CN102008831A/en active Pending
Patent Citations (7)
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| US4306942A (en) * | 1980-06-27 | 1981-12-22 | Raphael Katzen Associates International, Inc. | Hydrous alcohol distillation method and apparatus |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636003A (en) * | 2012-05-16 | 2012-08-15 | 唐山三友氯碱有限责任公司 | Energy-saving device for rectification tail gas condensation system |
| CN102636003B (en) * | 2012-05-16 | 2014-09-10 | 唐山三友氯碱有限责任公司 | Energy-saving device for rectification tail gas condensation system |
| CN105080173A (en) * | 2015-09-29 | 2015-11-25 | 广西新龙制药有限责任公司 | Alcohol recovery tower |
| CN106807096A (en) * | 2015-11-28 | 2017-06-09 | 衡阳春天医药化工设备有限公司 | A kind of alcohol recovery device |
| CN111474971A (en) * | 2020-04-28 | 2020-07-31 | 宁波奥克斯电气股份有限公司 | Control method for preventing excessive low water flow and water supply machine |
| CN111474971B (en) * | 2020-04-28 | 2021-08-24 | 宁波奥克斯电气股份有限公司 | Control method for preventing excessive low water flow and water supply machine |
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Application publication date: 20110413 |