CN104163752A - Technology for extracting high purity ethanol from wine - Google Patents
Technology for extracting high purity ethanol from wine Download PDFInfo
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- CN104163752A CN104163752A CN201410322406.1A CN201410322406A CN104163752A CN 104163752 A CN104163752 A CN 104163752A CN 201410322406 A CN201410322406 A CN 201410322406A CN 104163752 A CN104163752 A CN 104163752A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- Organic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a technology for extracting ethanol with high purity and high recovery rate from wine, which is characterized in that a fractionation apparatus is arranged by a sequence of a heating pot with controllable power, a flask with a circle bottom, a fractional column, a thermometer (an upper edge and a lower edge of a condenser tube are parallel), the condenser tube, a tail connection pipe and an accept ion bottle in order. The upper edge of the thermometer and the lower edge of the fractionating tube of a fractionation head are placed in a parallel mode, are heated at constant temperature with 180w power to an azeotropic temperature of 78.0-78.2 DEG C of ethanol and water, then collection is carried out, reflux ratio of ethanol is controlled at about 0.9, when the temperature of the thermometer exceeds 78.5 DEG C, collection is stopped for 5 minutes, when the temperature is returned to 78.0 DEG C, collection is carried out again, the collection is repeated until the temperature is kept at 78.5 DEG C after collection is stopped. The purpose for extracting ethanol with high purity and high recovery rate from wine can be realized by the most economic technology with simplest operation, SNIF-NMR analysis requirement can be better satisfied, and the technology provides powerful technical support for producing area division and quality grade of wine, and promotes the market standardization of the wine.
Description
Technical field
The present invention relates to a kind of processing method and device that extracts high purity high-recovery ethanol from grape wine, belong to technical field of chemical engineering.
Background technology
Grape wine is internationally recognized health drink, is one of industry most active in the national economic development, develops, expands employment, drives the aspects such as increasing peasant income to make significant contribution upgrading the living standards of both urban and rural residents, promote related industries.But consciousness that the current wine industry of China exists self-discipline is weak, the effectively shortcoming of supervision detection means of shortage, has badly influenced the sound development of wine industry.Selecting specificity natural isotopic fractionation nuclear magnetic resonance technique (SNIF-NMR) and isotope ratio mass spectrometer technology (IRMS) is a kind of international grape wine analytical procedure, and the countries use such as quilt France and Europe are in doping vinous detects.SNIF-NMR technology judges by analyzing the variation of deuterium isotopic content in ethanol the sugared biogenesis that becomes this ethanol molecule, so how to extract from grape wine sample, to isolate ethanolic soln be the first step of carrying out SNIF-NMR analysis.
In grape wine, 80% is moisture, 9.5-15% is ethanol, all the other are the materials such as acid, phenolic compound, residual sugar, aromatoising substance, amino acid, protein, trans-resveratrol and VITAMIN, often utilize ethanol to extract and separate from grape wine from different the making it of other boiling point substances.But due to heat effect, the movement rate of molecule, atom and the ion of different mass is directly proportional to its mass square root, lightweight particle has precedence over heavy amount Particles Moving, isotropic substance generation fractionation effect, and therefore the rate of recovery of ethanol directly affects the accuracy of SNIF-NMR detected result.In addition, carry out under deuterium natural abundance level because SNIF-NMR analyzes, higher alcohol concn is the prerequisite that obtains better resolution spectrogram, and purity is higher, and signal is stronger, and the time of detection will correspondingly shorten.Therefore, the extraction of high purity, high-recovery ethanol is to carry out one of the important step of SNIF-NMR analysis and difficult point.
The problem that the present invention solves is, the needs of analyzing for meeting SNIF-NMR, design and from grape wine, extracted the specific fractionation plant of high purity high-recovery ethanol, and each processing parameter is carried out to clear and definite regulation and strict restriction, finally obtain the highly purified ethanol of high-recovery, the design energy consumption of this technique is low, economically feasible and simple to operate.
In order to realize the object of the invention, the main technique means adopting is: pour the grape wine liquid of certain volume into round-bottomed flask, according to adding hot pot, round-bottomed flask, fractional column, still head, thermometer (the upper edge of its glass envelope is lower to concordant with still head fractionating tube), prolong, tail is taken over, the order of receiving flask is installed successively, open water of condensation, under 180w power, thermostatically heating is to 78.0 ~ 78.2 DEG C of the azeotropic points of ethanol and water, start to collect effluent liquid, control reflux ratio in 0.9 left and right, when exceeding 78.5 DEG C, thermometer displays temperature stops collecting 5 minutes, in the time that returning to 78.0 DEG C, temperature again collects, repeat this process and remain on 78.5 DEG C until stop collecting rear temperature, stop collecting.
The beneficial effect that the present invention obtains is: the present invention has developed the technique of extracting high purity high-recovery ethanol from grape wine, adopt the fractionation plant of a set of particular design, the length of this device to fractional column, heating power, the position of thermometer, the parameters such as the starting point of collecting have clearly strict regulation, final with most economical, the simplest technique of operation has realized the object of extracting high purity high-recovery ethanol from grape wine, the needs that SNIF-NMR analyzes are well met, determine strong technical support is provided for time qualification vinous and quality grade, promote China's Wine Market Normalization.
Summary of the invention
The problem that the present invention solves is, the needs of analyzing for meeting SNIF-NMR, design and from grape wine, extracted the specific fractionation plant of high purity high-recovery ethanol, and each processing parameter is carried out to clear and definite regulation and strict restriction, finally obtain the highly purified ethanol of high-recovery, the design energy consumption of this technique is low, economically feasible and simple to operate.
In order to realize the object of the invention, the main technique means adopting is: pour the grape wine liquid of certain volume into round-bottomed flask, according to adding hot pot, round-bottomed flask, fractional column, still head, thermometer (the upper edge of its glass envelope is lower to concordant with still head fractionating tube), prolong, tail is taken over, the order of receiving flask is installed successively, open water of condensation, under 180w power, thermostatically heating is to 78.0 ~ 78.2 DEG C of the azeotropic points of ethanol and water, start to collect effluent liquid, control reflux ratio in 0.9 left and right, when exceeding 78.5 DEG C, thermometer displays temperature stops collecting 5 minutes, in the time that returning to 78.0 DEG C, temperature again collects, repeat this process and remain on 78.5 DEG C until stop collecting rear temperature, stop collecting.
The beneficial effect that the present invention obtains is: the present invention has developed the technique of extracting high purity high-recovery ethanol from grape wine, adopt the fractionation plant of a set of particular design, the length of this device to fractional column, heating power, the position of thermometer, the parameters such as the starting point of collecting have clearly strict regulation, final with most economical, the simplest technique of operation has realized the object of extracting high purity high-recovery ethanol from grape wine, the needs that SNIF-NMR analyzes are well met, determine strong technical support is provided for time qualification vinous and quality grade, promote China's Wine Market Normalization.
Brief description of the drawings
Fig. 1 is the specific fractionation plant (water distilling apparatus) that extracts high purity ethanol from used in the present invention from grape wine.
embodiment
Describe as example to extract 12 ° of ethanol in (V/V) dry red winew:
1. the impact that the position of thermometer is measured boiling point
| Thermometer position | Solution boiling temperature | Remarks |
| Under thermometer along with under prolong along parallel | 84℃ | Measurement temperature is inaccurate |
| On thermometer along with under prolong along parallel | 78.15℃ | Measurement temperature is accurate |
Thermometer installation site: when the lower edge of thermometer with under prolong when parallel, most of steam has proceeded in the prolong of side, causes the temperature drift of the upper reaction of thermometer bulb bubble, therefore the temperature of solution boiling is apparently higher than its theoretical temperatures; When the upper edge of thermometer with under prolong when parallel, ensure that the steam rising enters prolong at once when all bubble by thermometer bulb, react more accurately the boiling temperature of this solution, therefore selected lower to parallel placement by the upper edge of thermometer and prolong.
2. the impact of the length of fractional column on fractionation result
| Post is high | Purity of alcohol | The ethanol rate of recovery | Distillation time (min) |
| 50 centimetres | ＜80° | ＞90% | 30 |
| 70 centimetres | ＞88° | ＞92% | 50 |
| 100 centimetres | ＞90° | ＜80% | 90 |
The common thorn type fractional column that 50cm is long, because post falls short of, separation purity is not high; In the time adopting the fractional column of 100cm, under identical heating intensity, the overlong time of ethanol distillation, due to the cooling effect of air, a small amount of gas in distillation later stage does not reach fractionation capital and is just condensed into liquid return to matrass, makes the ethanol rate of recovery not high; The pillar of 70cm is selected in compromise, and without lagging material in the situation that, the ethanolic soln concentration of collection also can reach more than 88%, and when distillation time obviously shortens, the rate of recovery also obtains larger raising.
3. add the impact of hot pot power on fractionation result
| Add hot pot power | Rate of yield | Purity | The rate of recovery | Distillation time | Remarks |
| 150w | Gas cannot reach tower top | ||||
| 180w | 1/3-5 second | 88—93° | 90-98% | 55min | Adopt |
| 210w | 1/1-2 second | 70-85° | 92-98% | 30min |
Because fractional column is longer, under the power of 150w, heat, heating intensity is inadequate, and low-boiling point material steam by air cooling, cannot reach tower top in fractional column uphill process, thereby cannot realize separation; Strengthen heating intensity, heat with the power of 210w, the rate of yield of ethanol is 1/1-2 second, the rate of recovery is very high, substantially can intactly ethanol be recycled to from grape wine to receiving flask, but because rate of yield is very fast, and ethanol and very approaching some materials of water azeotropic point separated well, cause the purity of ethanol not high; Suitably control heating power, while being down to 180w, rate of yield becomes 1/3-5 second, and the rate of recovery of ethanol and purity are all higher, is respectively 90-98% and 88-93 °
4. collect the selection of temperature: be 78.15 DEG C (101.3kPa, azeotropic consists of 95.5% ethanol and 4.5% water) according to the azeotropic point of the azeotropic system of ethanol and water formation, while selecting temperature to be 78.0～78.2 DEG C, start to collect.
5. the judgement of temperature variation and terminal
| Temperature variation | Purity of alcohol | The ethanol rate of recovery | Distillation time | Remarks |
| When temperature declines | 91．89° | 76．49% | 45min | |
| Temperature rises suddenly | 92．98° | 95．95% | 55min | Terminal |
In the time that test proceeds to a certain degree, the temperature that thermometer shows, declines suddenly, doubts the arriving into terminal, stops distillation at once, and recording purity of alcohol in receiving flask and be 91.89 °, the rate of recovery is 76.49%.The recovery of ethanol is sufficiently complete, consider the length of fractional column, heating intensity, after the problems such as vessel are residual, again test with same sample, after declining suddenly, temperature continues distillation, after several minutes, finding occasionally has several ethanol to reach tower top, enter prolong by thermometer, thermometer temperature declines again at once afterwards, ball bubble around absence of liquid suspends, continue heating, even again have several ethanol to flow out, after repeating several times, ethanol is fewer and feweri, under same temperature, heat, the time that reaches boiling point is more and more longer, finally even cannot reach tower top just flows back in matrass.In order to ensure the rate of recovery, strengthen a little electric heating cooker power, allow to drive remaining ethanol to reach tower top, temperature stops distillation while suddenly rising.Both in the time that distillation proceeds to a certain degree, thermometer displays temperature exceeded 78.5 DEG C and stops collecting 5 minutes, in the time that temperature is returned to 78.0 DEG C, again collected, and repeated this process until stop collecting rear temperature and remained on 78.5 DEG C.The rate of recovery of ethanol reaches 95.95%, 92.98 ° of purity, has accomplished that high recovery of high purity isolate ethanol.
6. the results of measuring to purity of alcohol and the rate of recovery after extracting:
By processing method of the present invention, the purity that finally obtains ethanol is greater than 92.0 ° (m/m), the rate of recovery more than 95%, economically feasible, simple to operate, and well met the needs that SNIF-NMR analyzes.
Claims (3)
1. from grape wine, extract a process unit for high purity ethanol, comprise the erection sequence of fractionation plant, the installation position of thermometer, the aspects such as the length of fractional column, is characterized in that:
(1) fractionation plant is installed according to the order that adds hot pot, round-bottomed flask, fractional column, still head, thermometer, prolong, tail adapter, receiving flask of power-adjustable successively;
(2) fractionation plant is for the boiling temperature of reaction soln more accurately, selects lower to concordant placement by the upper edge of thermometer glass bubble and still head fractionating tube;
(3), in fractionation plant, the length of choosing fractional column is 50-100cm.
2. from grape wine, extract a technique for high purity ethanol, to the power of electric heating cooker, start to collect temperature and distillation end point has strict control, it is characterized in that:
(1) in extraction process, the heating power of electric heating cooker is 180w, and control of reflux ratio is in 0.9 left and right;
(2), in extraction process, be to collect cut between 78.0～78.2 DEG C in temperature;
(3) in extraction process, stop collecting 5 minutes when thermometer displays temperature exceedes 78.5 DEG C, in the time that temperature is returned to 78.0 DEG C, again collect, repeat this process until stop collecting rear temperature and remain on 78.5 DEG C.
3. as claimed in claim 1,, when in fractionation plant, the length optimization of fractional column is 70cm, now the rate of recovery of ethanol reaches 95.95%, purity is 92.98%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410322406.1A CN104163752A (en) | 2014-07-09 | 2014-07-09 | Technology for extracting high purity ethanol from wine |
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| CN201410322406.1A CN104163752A (en) | 2014-07-09 | 2014-07-09 | Technology for extracting high purity ethanol from wine |
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| CN201410322406.1A Pending CN104163752A (en) | 2014-07-09 | 2014-07-09 | Technology for extracting high purity ethanol from wine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104897442A (en) * | 2015-05-12 | 2015-09-09 | 中国科学院地球环境研究所 | Method used for identifying aged liquor, and vacuum freezing transferring device |
-
2014
- 2014-07-09 CN CN201410322406.1A patent/CN104163752A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 蒋露等: "SNIF -NMR 和 IRMS技术在葡萄酒质量评价中的初步研究", 《食品与发酵工业》 * |
| 赵建庄等: "《有机化学实验》", 31 October 2007, 高等教育出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104897442A (en) * | 2015-05-12 | 2015-09-09 | 中国科学院地球环境研究所 | Method used for identifying aged liquor, and vacuum freezing transferring device |
| CN104897442B (en) * | 2015-05-12 | 2017-09-19 | 中国科学院地球环境研究所 | The authentication method and vacuum refrigeration transfer device of a kind of time white wine |
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Application publication date: 20141126 |