JP2005137264A - Method for purifying distilled liquor - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for purifying distilled liquor, by which an unsaturated fatty acid to cause emission of oily smell in distilled liquor is reduced and occurrence of turbidity by a flocculent precipitate, fusel oil and an unsaturated fatty acid is prevented. <P>SOLUTION: Chitosan powder or a chitosan-coated material or chitosan powder or the chitosan-coated material and silica sol are added to distilled liquor and the distilled liquor is filtered by a filter to remove the unsaturated fatty acid, a compound of the unsaturated fatty acid and a metal ion or the fusel oil contained in the distilled liquor. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention relates to a method for purifying distilled liquor that removes unsaturated fatty acids, compounds of unsaturated fatty acids and metal ions, or fusel oil contained in distilled liquor.

  The ethyl ester of unsaturated fatty acid contained in distilled liquor oxidizes and generates an oily odor during storage or when exposed to direct sunlight. Unsaturated fatty acids, which are precursors of oily odor, are particularly increased in atmospheric distillation. When unsaturated fatty acid ethyl ester (especially ethyl linoleate) is oxidatively decomposed and converted into an oily odor component, the solubility of this component is several thousand times larger than that before decomposition, and thus it is not easy to remove.

  Further, higher fatty acid ethyl esters such as ethyl palmitate and ethyl linoleate give the taste of distilled liquor thick and round, but it not only causes the above-mentioned oily odor but also causes odor. In particular, when a metal ion reacts with a higher fatty acid ester, a compound of an unsaturated fatty acid and a metal ion is produced, which becomes a cottony precipitate. This metal ion is derived from the metal of the distiller (such as copper).

  In order to reduce the formation of such flocculent precipitates, a method of adding water as so-called split water to distilled liquor and allowing it to stand overnight to generate turbidity and then filtering to remove the turbidity is generally used. Has been done.

However, even if this method is used, the precursor of the orientation cannot be sufficiently removed. For this reason, after storing in a tank etc. after filtration, when further filtering, there was a problem that turbidity of fusel oil or unsaturated fatty acid, which is a higher alcohol, was generated. This turbidity occurs when water in the filter is mixed with distilled liquor and the alcohol content of the distilled alcohol decreases, or when the alcohol content in the filter is recovered by pushing the water at the end of filtration and the alcohol content decreases. To do.
JP-A-8-322547 U.S. Pat. No. 3,0078,778 JP-A-4-270107

  The purpose of the present invention is to reduce unsaturated fatty acids that cause oily odor in distilled liquor, and to prevent the occurrence of turbidity due to flocculent precipitates, fusel oil and unsaturated fatty acids. It is to provide a method for purifying sake.

  The method for purifying distilled liquor according to the first aspect of the present invention includes adding chitosan powder or chitosan coating to distilled liquor and filtering it with a filter to obtain unsaturated fatty acid and unsaturated fatty acid contained in distilled liquor. And a metal ion compound or fusel oil.

  Patent Document 1 discloses that silica sol and / or chitosan is used to remove proteins in sake and the like, but there is no description about removing unsaturated fatty acids contained in distilled sake. .

  The method for purifying distilled liquor according to the second aspect of the present invention includes the step of filtering distilled liquor using a filter having chitosan powder or chitosan coating attached to the filtration surface, thereby unsaturated fatty acid contained in distilled liquor. It is characterized by removing compounds of unsaturated fatty acids and metal ions, or fusel oil.

  The method for purifying distilled liquor according to the third aspect of the present invention comprises adding chitosan powder or chitosan coating and distilling liquor to the distilled liquor, thereby adding unsaturated fatty acids, unsaturated fatty acids and metal ions contained in the distilled liquor. It is characterized by removing compounds or fusel oil.

  The method for purifying distilled liquor according to the fourth aspect of the present invention includes adding unsaturated silica, a compound of unsaturated fatty acid and metal ion, or fusel oil contained in distilled liquor by adding a positively charged silica sol to the distilled liquor. It is characterized by removing.

  According to the method for purifying distilled liquor of the present invention, generation of oily odor of distilled liquor can be reduced, and turbidity in distilled liquor can be efficiently removed.

  The chitosan used in the present invention is known as a deacetylated product of chitin and is not particularly limited. However, the degree of deacetylation is preferably 70% or more, more preferably 85% or more. . Moreover, as a form, it is preferable that it is a fine powder form.

  The chitosan coating used in the present invention is prepared by dissolving chitosan in an acid solution such as lactic acid, acetic acid, and hydrochloric acid, and adding a core material such as activated carbon, cellulose, and diatomaceous earth, By adding an alkaline aqueous solution such as potassium, chitosan is deposited on the surface of the core material. Although there is no restriction | limiting in particular as a chitosan coating amount of a chitosan coating material, Usually, what was coated in the ratio of 5-300 weight part with respect to 100 weight part of core materials is used.

  In the first aspect of the present invention, the amount of chitosan powder or chitosan coating to be added to distilled liquor is preferably about 10 to 5000 g with respect to 1 ton of distilled liquor.

In the second aspect of the present invention, distilled liquor is filtered using a filter having a chitosan powder or chitosan coating adhered to the filtration surface. As a method of affixing chitosan powder or chitosan coating to the filtration surface of the filter, mix water and chitosan powder or chitosan coating into a half-cut piece (a 200-500 liter tub-like container) in advance and filter this. Apply chitosan powder or chitosan coating uniformly on the filtration surface while circulating in the machine. The amount of chitosan powder and chitosan coating applied is preferably about 50 to 400 g per 1 m ^{2 of} filtration area.

  In the third aspect of the present invention, chitosan powder or chitosan coating and silica sol are added to distilled liquor. As the silica sol, either a negatively charged silica sol or a positively charged silica sol can be used. A typical common silica sol is a negatively charged silica sol. The positively charged silica sol will be described in detail later.

  In the third aspect of the present invention, the amount of chitosan powder or chitosan coating added to distilled liquor is preferably 10 to 5000 g of chitosan powder or chitosan coating added to 1 ton of distilled liquor. Moreover, as addition amount of a silica sol, it is preferable to add so that it may become a density | concentration of 50 ppm-2000 ppm with respect to distilled liquor. By setting these addition amounts, unsaturated fatty acids, unsaturated fatty acid and metal ion compounds, and fusel oil can be efficiently removed.

  In the fourth aspect of the present invention, a positively charged silica sol is added to distilled liquor. The amount of positively charged silica sol added is preferably 50 ppm to 2000 ppm with respect to the distilled liquor. By adding at such a concentration, unsaturated fatty acids, compounds of unsaturated fatty acids and metal ions, and fusel oil can be efficiently removed. In particular, the method according to the fourth aspect is preferably employed to remove white turbidity caused by adding so-called split water to distilled liquor. This turbidity is turbidity caused by fusel oil or unsaturated fatty acid, and such turbidity can be efficiently removed.

  The positively charged silica sol used in the present invention is a colloidal silica sol having a positively charged particle surface. Generally, since colloidal silica is an acidic oxide, its particle surface is negatively charged. For example, the particle surface of this negatively charged colloidal silica is coated with a fine metal compound having a positive charge. Thus, a positive charge can be imparted to the colloidal silica. Examples of such a metal compound having a positive charge include basic metal oxides such as alumina (aluminum oxide), iron oxide, zirconia (zirconium oxide), and titanium oxide. Alumina is most preferred from a practical and economical viewpoint.

  Examples of the method for coating the particle surface of the negatively charged colloidal silica with a fine metal compound having a positive charge include methods such as a spray method, a vacuum deposition method, an impregnation heating method, and a hydrolysis method. As a coating method, the surface of the negatively charged silica sol is mixed with one or two or more of a negatively charged silica sol and an aqueous solution of a basic metal chloride, and the pH of the negatively charged silica sol is adjusted appropriately with an acid and / or alkali. Examples of the method include depositing a metal salt hydrolyzate and the like to coat. As the basic metal chloride salt used, in the case of alumina, basic aluminum chloride is used. In the case of iron oxide, basic iron chloride is used. In the case of zirconia, basic zirconium chloride is used. In this case, basic titanium chloride is used. Details of the coating by hydrolysis are described in, for example, Patent Document 2 and Patent Document 3. The metal oxide precipitated by hydrolysis is preferably a fine amorphous hydrate.

  The coating amount of the colloidal silica with the metal compound such as a metal oxide having a positive charge is preferably about 2 to 40% by weight with respect to the colloidal silica. When the coating amount is less than 2% by weight, a sufficient positive charge may not be imparted. When the coating amount exceeds 40% by weight, a part of the basic metal oxide or the like does not adhere to the silica sol surface. May occur or may be economically disadvantageous.

The average particle size of the positively charged silica sol used in the present invention is preferably about 3 to 100 nm, more preferably about 5 to 50 nm. The silica (SiO ₂ ) content in the positively charged silica sol is preferably about 15 to 45% by weight, more preferably about 15 to 30% by weight.

  The average particle size of the negatively charged silica sol used in the present invention is preferably about 3 to 100 nm, more preferably about 5 to 50 nm. The silica content in the negatively charged silica sol is preferably 10 to 50% by weight, more preferably about 15 to 45% by weight.

  As a commercial product of the positively-charged silica sol, trade name “COPOLOK 200” (manufactured by Otsuka Foods Co., Ltd.) and the like can be mentioned. Moreover, as a commercial item of negatively charged silica sol, a trade name “COPOLOK 300” (manufactured by Otsuka Foods Co., Ltd.) can be exemplified.

  In the purification method of the present invention, gelatin, collagen, fish gelatin, protein derived from milk, protein such as wheat protein, pea protein, polysaccharides such as sodium alginate, carrageenan, agar, etc., as long as the effects of the present invention are not impaired. , Tannins such as tannic acid, PVPP (polyvinyl polypyrrolidone), silica dioxide such as silica gel, filter aids such as diatomaceous earth, perlite, and cellulose, adsorbents such as bentonite, activated carbon, acid clay, and ion exchange resin be able to. These may use 1 type (s) or 2 or more types.

  In addition to distilled spirits such as shochu shellfish, shochu oysters, shochu cocoon mixed products, awamori, brandy, whiskey, bourbon, scotch, etc., these distilled spirits were stored in shochu barrels. These include those in which plants such as plums, ginseng, and herbs are soaked in these spirits, and those in which animals such as viper and hub are soaked in these spirits.

  Hereinafter, the present invention will be described in detail with specific examples, but the present invention is not limited to the following examples.

<Example 1>
200 ml of 2-year-old rice shochu (alcohol 31%) with an oily odor was placed in a beaker, and 1 g of chitosan powder (average molecular weight by viscosity method: 150,000, mesh size: 40 mesh pass) was added and stirred.

<Comparative Example 1>
In the above, Comparative Example 1 was obtained without adding chitosan powder.

  The rice shochu of Example 1 and Comparative Example 1 was No. The turbidity of the filtrate filtered through 5C filter paper was measured with a turbidimeter (Nippon Denshoku Industries Co., Ltd .: NDH-20D type), and the results of examining the presence or absence of oily odor are shown in Table 1.

表１に示すように、本発明の精製方法により、濁度を低減でき、油臭を除去できることがわかる。

As shown in Table 1, it can be seen that the purification method of the present invention can reduce turbidity and remove oily odor.

<Example 2>
200 ml of commercially available rice shochu (alcohol content 25%) is taken in a beaker, 0.2 g of chitosan powder (average molecular weight by viscosity method: 150,000, mesh size: 40 mesh pass) and silica sol (trade name “Otsuka Foods Co., Ltd. Copolok 200 ") 800 ppm was added and stirred.

<Comparative example 2>
In the above, Comparative Example 2 was obtained without adding chitosan powder and silica sol.

  The rice shochus of Example 2 and Comparative Example 2 were allowed to stand for 24 hours, and the amount of sediment that had settled and the turbidity were measured using the turbidimeter. The measurement results are shown in Table 2.

表２に示すように、本発明の精製方法により、濁度を低減できることがわかる。

As shown in Table 2, turbidity can be reduced by the purification method of the present invention.

<Example 3>
Rice shochu with an alcohol content of 35% is divided into water with an alcohol content of 25%, and 200 ml of white turbidity is taken into a beaker, and a positively charged silica sol (trade name “COPOLOK 200”, manufactured by Otsuka Foods Co., Ltd.) (Silica content 20% by weight) 1000 ppm was added and stirred.

<Comparative Example 3>
In the above, Comparative Example 3 was obtained without adding silica sol.

  The rice shochus of Example 3 and Comparative Example 3 were allowed to stand for 24 hours, and the amount of sediment that had settled and the turbidity were measured using the turbidimeter. Table 3 shows the measurement results.

表３に示すように、本発明の精製方法により、濁度を低減できることがわかる。

As shown in Table 3, turbidity can be reduced by the purification method of the present invention.

<Example 4>
A rice shochu with an alcohol content of 35% was split to give an alcohol content of 25%, and white turbidity was obtained. Diatomaceous earth (trade name: Celite Hyflo Supercell, manufactured by Celite, USA) was pre-coated on 5C filter paper and filtered with Nutsche. Add 1 g of chitosan powder (average molecular weight by viscosity method: 150,000, mesh size: 40 mesh pass) to 200 ml of water that has been hydrated to this filtrate, the alcohol concentration is 3%, and an increase in turbidity is observed. did.

<Comparative example 4>
In the above, Comparative Example 4 was obtained without adding chitosan powder.

  The rice shochu of Example 4 and Comparative Example 4 was No. Table 4 shows the results of measuring the turbidity of the filtrate filtered through 5C filter paper.

表４に示すように、本発明の精製方法により、濁度を低減できることがわかる。

As shown in Table 4, turbidity can be reduced by the purification method of the present invention.

Claims (4)

  It is characterized by removing unsaturated fatty acids, compounds of unsaturated fatty acids and metal ions, or fusel oil contained in distilled liquor by adding chitosan powder or chitosan coating to the distilled liquor and filtering it with a filter. A method for purifying distilled spirits.   Unsaturated fatty acids, unsaturated fatty acid and metal ion compounds, or fusel oil contained in distilled liquor are removed by filtering distilled liquor using a filter with chitosan powder or chitosan coating applied to the filtration surface. A method for purifying distilled liquor, characterized in that:   Distilled liquor characterized by removing unsaturated fatty acid, compound of unsaturated fatty acid and metal ion, or fusel oil contained in distilled liquor by adding chitosan powder or chitosan coating and silica sol to the distilled liquor Purification method. A method for purifying distilled liquor, comprising adding unsaturated silica sol to distilled liquor to remove unsaturated fatty acids, compounds of unsaturated fatty acids and metal ions, or fusel oil contained in distilled liquor.