WO1993016168A1 - Procedure and apparatus for producing whisky - Google Patents
Procedure and apparatus for producing whisky Download PDFInfo
- Publication number
- WO1993016168A1 WO1993016168A1 PCT/FI1992/000042 FI9200042W WO9316168A1 WO 1993016168 A1 WO1993016168 A1 WO 1993016168A1 FI 9200042 W FI9200042 W FI 9200042W WO 9316168 A1 WO9316168 A1 WO 9316168A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- column
- distillate
- mash
- conducted
- rectification
- Prior art date
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/001—Processes specially adapted for distillation or rectification of fermented solutions
- B01D3/003—Rectification of spirit
- B01D3/004—Rectification of spirit by continuous methods
- B01D3/005—Combined distillation and rectification
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
- C12H6/00—Methods for increasing the alcohol content of fermented solutions or alcoholic beverages
- C12H6/02—Methods for increasing the alcohol content of fermented solutions or alcoholic beverages by distillation
Definitions
- the present invention concerns a procedure for producing whisky and equivalent distilled alcoholic beverages, as defined in the preamble to Claim 1. Furt ⁇ hermore, the invention concerns apparatus for implemen ⁇ ting said procedure, as defined in the preamble to Claim 8.
- the invention concerns in particular a proce- dure and apparatus for producing whisky with low ethyl ⁇ carbamate concentration.
- Ethylcarbamate is inherently present in small quantities in all alcoholic beverages. This compound is formed as a result of microbial metabolism. However, certain distilled beverages, such as whisky, have been observed to contain significantly more ethylcarbamate than is formed in natural fermentation (Mildau,G. et al., Manual Lebensmittle-Rundschau,1987,vol.83,p. 69- 74). Ethylcarbamate is considered to be a carcino ⁇ gen. The principle is generally accepted that its con ⁇ centration in alcoholic beverages should be as low as possible. In Canada the maximum concentration limit of 150 ppb (150xl0 ⁇ 5 g/1) has been imposed on distilled alcoholic beverages such as whisky.
- the object of the present invention is to pro ⁇ vide a novel procedure for producing whisky and equiv ⁇ alent distilled alcoholic beverages yielding an alco- holic beverage with lowest possible ethylcarbamate con ⁇ centration.
- the invention is hereinafter descri ⁇ bed with specific reference to ethylcarbamate, it is to be understood that the principles of the invention are also applicable to produce an alcoholic beverage with low concentration of aldehydes, diacetyl and many vola- tile sulphur compounds like mercaptans, dimethyl sulp ⁇ hide, dimethyl disulphide and dimethyl trisulphide.
- the invention is based on the observed fact that fresh whisky distillate contains no significant amounts of ethylcarbamate.
- the ethylcarbamate concentration of barreled distillate has been found to increase during the first three months.
- the total cyanide concentration of the distillate has been found to diminish at the same time.
- the cyanides in the distillate appear to be con- verted to ethylcarbamate in the course of storage.
- the same phenomenon is known in distillates produced by continuous distillation as well as those made by pot distillation.
- cyanide compounds in the mash column can be enhanced by performing the distillation under reduced pressure, whereby the boiling temperature of the mash in the column, and on the bottom of the column, is significantly lower than 100°C. There will then be fewer thermal decomposition reactions, compared with a column under normal pressure, and the distillate obtained from the mash column will contain less cyanide compounds. It is thus understood that the use of sub- atmospheric pressure in the mash column reduces, on the whole, the formation of cyanide compounds in the dis ⁇ tilling system, and correspondingly the total cyanide concentration of the product will also be lower in that case. In later treatment steps only minor quantities of ethylcarbamate can then be formed in the product.
- Distillation in the rectification column may equally be carried out under subatmospheric pressure.
- the rectifica ⁇ tion column will operate under subatmospheric pressure and it will also maintain the mash column at subatmo ⁇ spheric pressure. Owing to this reduced pressure, dis ⁇ tillation takes place at subnormal temperature and the thermal decomposition reactions are less in the distil ⁇ ling process, whereby the forming of cyanide compounds is less in the distilling system, as was said in the foregoing.
- the total cyanide concentration of the distillate is also suc ⁇ cessfully lowered by conducting the distillate into a separator column and removing from its head an impurity fraction containing cyanide compounds in abundance, whereby the low-cyanide product gained as bottom pro- duct of the separator column can be conducted, as it is, to further processing steps.
- the distillate con ⁇ ducted to the separator column may be produced by con ⁇ tinuous distillation or by pot distillation (batch process) .
- the reflux ratio of the separator column is advantageously made high, i.e., in the separation step a very small fraction should be withdrawn.
- the reflux ratio is greater than 5, advantageously greater than 10.
- Cyanide compounds present high relative volatility compared with ethanol, and it is therefore possible to remove an impurity fraction concentrated in respect of cyanide compounds, from the head of the column. Thanks to the invention, it becomes possible with the aid of a separator column to remove cyanide compounds from the distilling system in controlled manner and to leave, all the same, those compounds in the product which have an influence on the whisky flavor.
- Removal of cyanide compounds by using a sep ⁇ arator column may for in ⁇ stance be implemented in that the distillate coming from the mash column is conducted into the separator column and the bottom product of the separator column is further conducted to a rectification column, to be concentrated to desired strength.
- the procedure of the invention may equally be implemented in that the distillate obtained from the head of the mash column is conducted to the rectification column, the distillate from the latter being conducted to a separate separator column for re ⁇ moval of cyanide compounds after the rectification col- umn. The actual product is then gained as the bottom product of the separator column.
- Scotch whisky is understood in this context to mean an alcoholic beverage which has been produced in Scotland by distillation, from mash derived from grain and saccharified by malt diastases, and sto ⁇ red in casks three years at a minimum.
- American whisky is understood to be an alcohol distillate obtained by distilling mash produced from fermented grain to distillate concentration less than 95% (190° proof) in such manner that the distillate has the taste, flavor and other properties of whisky.
- Bour ⁇ bon whisky, rye whisky, wheat whisky, malt whisky or rye-malt whisky are understood to be whiskeys obtained by distilling mash produced from grain by fermentation to less than 80% (160° proof) and stored at a concen ⁇ tration not over 62.5% (125° proof) in new oak casks.
- Neutral grain spirit or alcohol is alcohol distilled from any kind of cereal, concentration 95% (190° proof) or higher, either at reduced concentration or as it is.
- Blended whisky is understood to be a mixture containing at least 20% whisky proper (50%, 100° proof) and, sepa ⁇ rately or in combination, whisky or neutral grain spir ⁇ it.
- Canadian whisky is understood to be an alco- holic beverage which has been produced in compliance with Canadian law and contains no distilled spirits younger than three years.
- Irish whisky is understood to be whisky pro ⁇ substituted in the Republic of Ireland or in North Ireland in compliance with Irish law, for consumption, containing no distilled spirits of age less than three years.
- the apparatus of the invention comprises a particular separator column for eliminating a fraction containing cyanide compounds.
- the separator column has been disposed in such manner that the distillate, ob ⁇ tained by continuous distillation or by pot distilling, is conducted to said separator column.
- the sepa- rator column is advantageously disposed so that the distillate from a conventional, e.g. multi-plate or packed column is conducted directly to the separator column.
- the rectification column may then be disposed in conjunction with the separator column in that the bottom product of the separator column is conducted directly to the rectification column.
- the separator column is disposed in conjunction with the distillate line of the rectification column so that the distillate of the rec ⁇ tification column is carried to the separator column, the bottom product of the latter constituting the pro ⁇ duct for further processing, in this case.
- Fig. 1 presents in a schematic diagram the relationship between cyanide compounds and ethylcarbamate during storage of distillate
- Fig. 2 presents an embodiment of the procedure and apparatus of the invention, in which concentration takes place after cyanide compound separation
- Fig. 3 presents another embodiment of the procedure and apparatus of the invention, in which separation of cya- nide compounds is effected after concentration
- Fig. 4 displays the dependence of cyanide compounds on distilling temperature.
- Fig. 1 illustrates the formation of ethylcar ⁇ bamate during the first four months of storing distil- late made from grain. During the same period the cya ⁇ nide concentration in the distillate goes down in equivalent amount. The distillate is meant to be used in producing whisky.
- Fig. 2 is depicted the principle diagram of a distilling procedure and process according to an em ⁇ bodiment of the invention.
- the figure reveals a dis ⁇ tilling apparatus 1 meant for mash distilling, compris- ing in the embodiment here shown, a conventional mash column 1.
- the distillate obtained from the mash column is conducted to a special separator column 2, the pro ⁇ duct from the bottom thereof being conducted towards further processing, in the present embodiment to a rec ⁇ tification column 3.
- the distillate obtained from the head of the rectification column is carried onwards to further process steps, in the present embodiment to barreling and warehousing.
- Fig. 1 the principle diagram of a distilling procedure and process according to an em ⁇ bodiment of the invention.
- the figure reveals a dis ⁇ tilling apparatus 1 meant for mash distilling, compris- ing in the embodiment here shown, a conventional mash column 1.
- the distillate obtained from the mash column is conducted to a special separator column 2,
- the mash is supplied through a feed line 6 to the first condenser connected to the head of the mash column 1, and which serves as mash pre-heater at the same time.
- the preheated mash is further con ⁇ ducted by the line 6 to the mash column 1.
- the mash column contains about 20 plates below, and 0-10 plates above the feed input.
- a condenser 8 which is connected to a vacuum system 4, by means of which the pressure in the mash column is maintained lower than the ambient pressure.
- a condenser 8 which is connected to a vacuum system 4, by means of which the pressure in the mash column is maintained lower than the ambient pressure.
- a mash col ⁇ umn under subatmospheric pressure reduces the formation of cyanide compounds in the distilling system on the whole, and correspondingly the product will then also have a low total concentration of cyanide compounds. In that case very little ethylcarbamate can be produced in the product in any later process steps.
- the distillate obtained from the mash column 1 is conducted by the line 9 to a separate separator col ⁇ umn 2.
- the head of the separator column is provided with a reflux condenser 10, and the column works with a high reflux ratio, reflux ratio greater than 5.
- Cyanide compounds have high volatility relative to ethanol, whereby it becomes possible to remove from the head of the separator, an impurity fraction 11 concentrated in cyanide compounds.
- the bottom product from the separator column is conducted by the line 12 to a rectification column 3 and concentrated to requisite concentration.
- the pro ⁇ duct proper is withdrawn as head product from the rec ⁇ tification column, line 20.
- Fig. 3 is depicted an alternative procedure for an under-pressurized mash column.
- the apparatus depicted in Fig. 3 comprises a mash column 1, a recti ⁇ fication column 3 and a separator column 2.
- the distil ⁇ late from the mash column is fed as a vapor directly to the rectification column, and the distillate from the rectification column is fed to the separator column.
- the mash column of Fig. 3 contains, typically, about 20 plates.
- the product is conducted by the line 6, through pre-heating 16, into the mash column 1.
- the pre-heating consists of the con- denser 16 on the head of the rectification column 3.
- the vapor departing from the head of the mash column is conducted in vapor form by the line 15 to the rectifi ⁇ cation column 3.
- the head of the rectification column is provided with condensers 16 and 17; the condensers are connected to a vacuum system 5.
- the rectification column 3 operating under subatmospheric pressure also maintains subatmospheric pressure in the mash column 1. The effect is the same as that of the procedure illustrated by Fig. 2.
- distilling systems presented in Figs 2 and 3 have been depicted as plate columns.
- the systems can equally be implemented using columns with random pack ⁇ ing or high efficiency packing or with any combinations of plate columns and packed columns.
- the distilling columns shown in the figures are generally provided with boilers, e.g. the boilers 21, 22 and 23 in, respectively, the distilling column 1, separator column 2 and rectification column 3.
- the distilling apparatus comprised a distill ⁇ ing flask 3 1, a packed column with packing made of stainless steel, a reflux condenser, cooled by means of a refrigerating liquid circulation at -2°C, and cont ⁇ rols for the reflux ratio.
- the distilling apparatus was connected to a vacuum control system enabling the pressure in the dis ⁇ tilling column to be regulated within ⁇ 10 mbar.
- the reflux ratio was 2 in the distilling tests.
- the boiling rate was adjusted so that each dis ⁇ tillation took 20+1 min.
- About 70 g of distillate were collected in the distilling test.
- EXAMPLE 2 Operation of the cyanide compound separator The distillates described in Example 1 were lumped to- gether and redistilled with the distilling apparatus described in Example 1.
- the distilling pressure was 1050 mbar in the test and the reflux ratio was 20. 10 g of distillate were recovered.
- the ethanol, methanol and MC concentra ⁇ tions of the solution to be distilled, the distillate and the bottom product of the distillation were deter ⁇ mined by analysis. The results are presented in Table 1.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Food Science & Technology (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU12774/92A AU1277492A (en) | 1992-02-14 | 1992-02-14 | Procedure and apparatus for producing whisky |
JP4504981A JPH07503360A (en) | 1992-02-14 | 1992-02-14 | Whiskey manufacturing method and manufacturing equipment |
GB9416450A GB2278849B (en) | 1992-02-14 | 1992-02-14 | Procedure and apparatus for producing whisky |
CA002130097A CA2130097A1 (en) | 1992-02-14 | 1992-02-14 | Procedure and apparatus for producing whisky |
PCT/FI1992/000042 WO1993016168A1 (en) | 1992-02-14 | 1992-02-14 | Procedure and apparatus for producing whisky |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA002130097A CA2130097A1 (en) | 1992-02-14 | 1992-02-14 | Procedure and apparatus for producing whisky |
PCT/FI1992/000042 WO1993016168A1 (en) | 1992-02-14 | 1992-02-14 | Procedure and apparatus for producing whisky |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1993016168A1 true WO1993016168A1 (en) | 1993-08-19 |
Family
ID=25677430
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/FI1992/000042 WO1993016168A1 (en) | 1992-02-14 | 1992-02-14 | Procedure and apparatus for producing whisky |
Country Status (2)
Country | Link |
---|---|
AU (1) | AU1277492A (en) |
WO (1) | WO1993016168A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008046633A1 (en) * | 2006-10-18 | 2008-04-24 | Gea Wiegand Gmbh | Installation for the distillation of drinking alcohol, especially whiskey |
CN104630014A (en) * | 2015-02-12 | 2015-05-20 | 江南大学 | Method for reducing content of ethyl carbamate in white spirit through reduced pressure secondary distillation |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0243535A1 (en) * | 1986-04-29 | 1987-11-04 | Thomas Alfred Ziegler | Method and apparatus for the batchwise production of spirits |
EP0266088A1 (en) * | 1986-10-14 | 1988-05-04 | Takeda Chemical Industries, Ltd. | Quality improvement of alcoholic liquors |
DE3734400A1 (en) * | 1987-02-25 | 1989-04-27 | Norbert Dr Christoph | Process for purifying fruit brandies and spirits |
EP0320275A1 (en) * | 1987-12-11 | 1989-06-14 | Takeda Chemical Industries, Ltd. | Quality improvement of alcoholic liquors |
EP0343260A1 (en) * | 1988-05-02 | 1989-11-29 | Firma Arnold Holstein | Process and device for the treatment of fruit spirits |
EP0459310A1 (en) * | 1990-05-25 | 1991-12-04 | Firma Arnold Holstein | Process and device for the treatment of fruit spirits |
-
1992
- 1992-02-14 AU AU12774/92A patent/AU1277492A/en not_active Abandoned
- 1992-02-14 WO PCT/FI1992/000042 patent/WO1993016168A1/en active Application Filing
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0243535A1 (en) * | 1986-04-29 | 1987-11-04 | Thomas Alfred Ziegler | Method and apparatus for the batchwise production of spirits |
EP0266088A1 (en) * | 1986-10-14 | 1988-05-04 | Takeda Chemical Industries, Ltd. | Quality improvement of alcoholic liquors |
US4844911A (en) * | 1986-10-14 | 1989-07-04 | Takeda Chemical Industries | Quality improvement of alcoholic liquors |
DE3734400A1 (en) * | 1987-02-25 | 1989-04-27 | Norbert Dr Christoph | Process for purifying fruit brandies and spirits |
EP0320275A1 (en) * | 1987-12-11 | 1989-06-14 | Takeda Chemical Industries, Ltd. | Quality improvement of alcoholic liquors |
EP0343260A1 (en) * | 1988-05-02 | 1989-11-29 | Firma Arnold Holstein | Process and device for the treatment of fruit spirits |
EP0459310A1 (en) * | 1990-05-25 | 1991-12-04 | Firma Arnold Holstein | Process and device for the treatment of fruit spirits |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008046633A1 (en) * | 2006-10-18 | 2008-04-24 | Gea Wiegand Gmbh | Installation for the distillation of drinking alcohol, especially whiskey |
GB2457187A (en) * | 2006-10-18 | 2009-08-12 | Gea Wiegand Gmbh | Installation for the distillation of drinking alcohol, especially whiskey |
GB2457187B (en) * | 2006-10-18 | 2011-05-04 | Gea Wiegand Gmbh | Installation for the distillation of drinking alcohol, especially whiskey |
CN104630014A (en) * | 2015-02-12 | 2015-05-20 | 江南大学 | Method for reducing content of ethyl carbamate in white spirit through reduced pressure secondary distillation |
Also Published As
Publication number | Publication date |
---|---|
AU1277492A (en) | 1993-09-03 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US4784868A (en) | Potable spirit production | |
Guymon | Chemical aspects of distilling wines into brandy | |
Medeiros et al. | Cachaça and rum | |
EP0160442B1 (en) | Production of alcoholic beverages | |
Pyke | The manufacture of Scotch grain whisky | |
US4889805A (en) | Continuous process of optimized fermentation for the production of alcohol | |
WO1993016168A1 (en) | Procedure and apparatus for producing whisky | |
Greenshields | Volatiles in home‐brewed beers and wines | |
US3821418A (en) | Preparation of alcoholic malt beverages | |
US5897904A (en) | Method for the production of high proof liquor | |
US2050908A (en) | Process of purifying distilled alcomolic spirits | |
US419332A (en) | Alcoholic distillation | |
US2358272A (en) | Art of distilling spirituous liquors | |
US2182550A (en) | Method of producing alcohols | |
IE920564A1 (en) | Procedure and apparatus for producing whisky | |
CA2130097A1 (en) | Procedure and apparatus for producing whisky | |
US4374859A (en) | Method for reducing fusel oil in alcoholic beverages and yeast strain useful in that method | |
Swan et al. | V The development of flavour in potable spirits | |
US2868645A (en) | Processes for producing distilled potable alcoholic liquors | |
US2099864A (en) | Process for manufacture of distilled spirits | |
KR20220100650A (en) | Distilled liquor, manufacturing method thereof, and use thereof | |
JP5891505B2 (en) | Yeast and method for producing alcoholic fermentation broth from beet molasses using this yeast | |
US2386924A (en) | Production of heavy bums | |
Riponi et al. | Influence of yeast strain on the composition of wines for the production of brandy | |
EP0756011B1 (en) | Process for the treatment of molasses |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
AK | Designated states |
Kind code of ref document: A1 Designated state(s): AT AU BR CA CH DE DK ES FI GB HU JP KR LU NL NO PL RO RU SE US |
|
AL | Designated countries for regional patents |
Kind code of ref document: A1 Designated state(s): AT BE CH DE DK ES FR GB GR IT LU MC NL SE |
|
DFPE | Request for preliminary examination filed prior to expiration of 19th month from priority date (pct application filed before 20040101) | ||
WWE | Wipo information: entry into national phase |
Ref document number: 2130097 Country of ref document: CA |
|
ENP | Entry into the national phase |
Ref document number: 1994 284649 Country of ref document: US Date of ref document: 19940928 Kind code of ref document: A |
|
REG | Reference to national code |
Ref country code: DE Ref legal event code: 8642 |
|
122 | Ep: pct application non-entry in european phase |