JP6673563B2 - Method for producing distilled liquor, and processing member including metal-supported ion exchange resin - Google Patents
Method for producing distilled liquor, and processing member including metal-supported ion exchange resin Download PDFInfo
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- JP6673563B2 JP6673563B2 JP2015123198A JP2015123198A JP6673563B2 JP 6673563 B2 JP6673563 B2 JP 6673563B2 JP 2015123198 A JP2015123198 A JP 2015123198A JP 2015123198 A JP2015123198 A JP 2015123198A JP 6673563 B2 JP6673563 B2 JP 6673563B2
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- exchange resin
- ion exchange
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- beverage
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- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 title claims description 116
- 239000003456 ion exchange resin Substances 0.000 title claims description 93
- 229920003303 ion-exchange polymer Polymers 0.000 title claims description 93
- 238000004519 manufacturing process Methods 0.000 title claims description 29
- 238000012545 processing Methods 0.000 title claims description 19
- 229910052709 silver Inorganic materials 0.000 claims description 40
- 239000004332 silver Substances 0.000 claims description 40
- 239000003729 cation exchange resin Substances 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 31
- 229910052751 metal Inorganic materials 0.000 claims description 28
- 239000002184 metal Substances 0.000 claims description 28
- -1 silver ions Chemical group 0.000 claims description 28
- 150000003464 sulfur compounds Chemical class 0.000 claims description 20
- 235000015041 whisky Nutrition 0.000 claims description 18
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 17
- 150000002500 ions Chemical class 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- 150000001768 cations Chemical class 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 229910021645 metal ion Inorganic materials 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 230000032683 aging Effects 0.000 claims 1
- 230000001476 alcoholic effect Effects 0.000 claims 1
- 150000002739 metals Chemical class 0.000 claims 1
- 235000013361 beverage Nutrition 0.000 description 81
- 239000000243 solution Substances 0.000 description 22
- 238000004458 analytical method Methods 0.000 description 20
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- 235000020083 shōchū Nutrition 0.000 description 16
- 238000012360 testing method Methods 0.000 description 16
- 239000010457 zeolite Substances 0.000 description 16
- 229910021536 Zeolite Inorganic materials 0.000 description 13
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 13
- 238000011156 evaluation Methods 0.000 description 13
- GXCLVBGFBYZDAG-UHFFFAOYSA-N N-[2-(1H-indol-3-yl)ethyl]-N-methylprop-2-en-1-amine Chemical compound CN(CCC1=CNC2=C1C=CC=C2)CC=C GXCLVBGFBYZDAG-UHFFFAOYSA-N 0.000 description 12
- 238000010828 elution Methods 0.000 description 12
- 238000005342 ion exchange Methods 0.000 description 12
- 229910001961 silver nitrate Inorganic materials 0.000 description 10
- 238000000746 purification Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 8
- 235000013334 alcoholic beverage Nutrition 0.000 description 7
- 229940023913 cation exchange resins Drugs 0.000 description 7
- 229920001429 chelating resin Polymers 0.000 description 7
- 229910052717 sulfur Inorganic materials 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 235000019583 umami taste Nutrition 0.000 description 6
- 240000005979 Hordeum vulgare Species 0.000 description 5
- 235000007340 Hordeum vulgare Nutrition 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 235000013533 rum Nutrition 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 244000061456 Solanum tuberosum Species 0.000 description 4
- 235000002595 Solanum tuberosum Nutrition 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 230000001953 sensory effect Effects 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 description 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000796 flavoring agent Substances 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 229910001415 sodium ion Inorganic materials 0.000 description 3
- YZUPZGFPHUVJKC-UHFFFAOYSA-N 1-bromo-2-methoxyethane Chemical compound COCCBr YZUPZGFPHUVJKC-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QSJXEFYPDANLFS-UHFFFAOYSA-N Diacetyl Chemical group CC(=O)C(C)=O QSJXEFYPDANLFS-UHFFFAOYSA-N 0.000 description 2
- YWHLKYXPLRWGSE-UHFFFAOYSA-N Dimethyl trisulfide Chemical compound CSSSC YWHLKYXPLRWGSE-UHFFFAOYSA-N 0.000 description 2
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000003957 anion exchange resin Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000004434 sulfur atom Chemical group 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 240000008620 Fagopyrum esculentum Species 0.000 description 1
- 235000009419 Fagopyrum esculentum Nutrition 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
- 235000002678 Ipomoea batatas Nutrition 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 244000098338 Triticum aestivum Species 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000006359 acetalization reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 235000013524 arak Nutrition 0.000 description 1
- 235000020053 arrack Nutrition 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 235000020054 awamori Nutrition 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000013532 brandy Nutrition 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- VSGNNIFQASZAOI-UHFFFAOYSA-L calcium acetate Chemical compound [Ca+2].CC([O-])=O.CC([O-])=O VSGNNIFQASZAOI-UHFFFAOYSA-L 0.000 description 1
- 235000011092 calcium acetate Nutrition 0.000 description 1
- 229960005147 calcium acetate Drugs 0.000 description 1
- 239000001639 calcium acetate Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 235000013531 gin Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 235000013529 tequila Nutrition 0.000 description 1
- 235000013522 vodka Nutrition 0.000 description 1
Landscapes
- Distillation Of Fermentation Liquor, Processing Of Alcohols, Vinegar And Beer (AREA)
Description
本発明は、飲料に含まれる不要成分を除去する飲料の精製方法、及び該精製方法に用いられる飲料処理用金属担持イオン交換樹脂に関する。 The present invention relates to a beverage purification method for removing unnecessary components contained in a beverage, and a metal-supported ion-exchange resin for beverage treatment used in the purification method.
飲料、特に酒類のなかには、ウイスキーのように、短くて４〜６年、通常７〜１０年、長い場合には２０年近く樽に貯蔵されて、熟成されるものがある。
貯蔵の間に、硫黄化合物等の未熟成成分の蒸散及び消滅、ニューポット由来成分の反応（酸化反応、アセタール化反応、エステル化反応等）、樽の原材料由来成分の分解反応、樽内に溶出した原材料由来成分と原酒との反応、原酒を構成するエタノールと水との状態変化等が起こることにより、ウイスキーに特有の風味が引き出される。
しかし、貯蔵の間に原酒が樽に吸収されたり、樽を透過して揮発したりするため、原酒量は自然に減少する。このため、貯蔵期間の長期化は、製造効率の面では、製品ロスの増加を招いていた。
そこで、硫黄化合物等の未熟成成分、寒冷時における析出成分、不快な香り成分等の酒類にとっての不要成分を、貯蔵により自然に起こる変化を待たずに、積極的に除去する方法が考えられている。
Some beverages, especially alcoholic beverages, such as whiskey, are stored in barrels for a short period of 4 to 6 years, usually 7 to 10 years, and in the longest case, close to 20 years, and aged.
During storage, evaporation and disappearance of immature components such as sulfur compounds, reactions of components derived from new pots (oxidation reaction, acetalization reaction, esterification reaction, etc.), decomposition reactions of components derived from barrel raw materials, elution into barrels A reaction peculiar to the whiskey is brought out by the reaction between the raw material-derived components and the liquor, a change in the state of ethanol and water constituting the liquor, and the like.
However, during storage, the amount of the original sake naturally decreases because the original sake is absorbed into the barrel or evaporates through the barrel. For this reason, a prolonged storage period has caused an increase in product loss in terms of manufacturing efficiency.
Therefore, a method has been considered in which unnecessary components for liquor, such as unripened components such as sulfur compounds, precipitated components in cold weather, and unpleasant aroma components, are actively removed without waiting for changes that occur naturally by storage. I have.
酒類から不要成分を除去する方法としては、例えば、シリカを有機シラン化合物で処理してなる吸着剤に酒類を接触させる方法（特許文献１参照）、活性炭に酒類を接触させる方法（特許文献２参照）、金属粒と樹脂層とを用いる方法（特許文献３参照）、イオン交換樹脂を用いる方法（特許文献４参照）等が既に提案されている。
特許文献４には、内部に充填した強塩基性陰イオン交換樹脂を食塩で再生した後、更に亜硫酸水素ナトリウムで再生してなる単床式カラムと、内部に充填した強塩基性陰イオン交換樹脂を食塩のみで再生してなる亜硫酸トラップカラムとを使用して酒類の精製処理を行って、酒類に含まれる不快成分（ダイアセチル）を除去できることが記載されている。
しかし、酒類には、上述のように、硫黄化合物等の未熟成成分などのように、ダイアセチル以外の不要成分も含まれており、より高い品質の要求を満足する製品を提供するためには、更なる改良の余地が残されていた。
As a method for removing unnecessary components from liquor, for example, a method of contacting liquor with an adsorbent obtained by treating silica with an organic silane compound (see Patent Document 1) and a method of bringing liquor into contact with activated carbon (see Patent Document 2) ), A method using metal particles and a resin layer (see Patent Document 3), a method using an ion exchange resin (see Patent Document 4), and the like have already been proposed.
Patent Document 4 discloses a single-bed column in which a strongly basic anion exchange resin filled inside is regenerated with salt and then further regenerated with sodium bisulfite, and a strongly basic anion exchange resin filled inside is used. It is described that liquor can be purified using a sulfurous acid trap column in which liquor is regenerated only with salt to remove unpleasant components (diacetyl) contained in liquor.
However, as described above, liquors also contain unnecessary components other than diacetyl, such as unripened components such as sulfur compounds, and in order to provide products that satisfy higher quality requirements. There was room for further improvement.
本発明は、酒類のような飲料に含まれる不要成分を効率よく除去し得る飲料の精製方法、及び該精製方法に用いることのできる飲料処理用金属担持イオン交換樹脂を提供することを課題とする。 An object of the present invention is to provide a method for purifying a beverage that can efficiently remove unnecessary components contained in a beverage such as alcoholic beverages, and a metal-supported ion-exchange resin for beverage treatment that can be used in the purification method. .
本発明者らは、特定の金属担持イオン交換樹脂に飲料を通液することにより、飲料に含まれる不要成分を除去することができ、前記課題が解決できることを見出した。
すなわち、本発明の要旨は下記のとおりである。
［１］陽イオン交換樹脂の陽イオンの少なくとも一部が銀イオンに交換されてなる飲料処理用金属担持イオン交換樹脂に接触させる工程を包含する、飲料に含まれる不要成分を除去する飲料の精製方法。
［２］前記銀イオンの担持量が、乾燥換算の前記飲料処理用金属担持イオン交換樹脂全量に対して、銀質量換算で、１０質量％以上４０質量％以下である［１］に記載の飲料の精製方法。
［３］飲料を前記飲料処理用金属担持イオン交換樹脂に接触させる工程の後、前記飲料処理用金属担持イオン交換樹脂に接触させた飲料を、金属捕捉材料により金属イオンを除去する工程を、さらに有する［１］又は［２］に記載の飲料の精製方法。
［４］前記飲料が蒸留酒であることを特徴とする［１］〜［３］のいずれかに記載の飲料の精製方法。
［５］前記飲料が醸造酒であることを特徴とする［１］〜［３］のいずれかに記載の飲料の精製方法。
［６］陽イオン交換樹脂の陽イオンの少なくとも一部が銀イオンに交換されてなり、飲料に含まれる不要成分を除去する飲料処理用金属担持イオン交換樹脂。
［７］前記銀イオンの担持量が、乾燥換算の飲料処理用金属担持イオン交換樹脂全量に対して、銀質量換算で、１０質量％以上４０質量％以下であることを特徴とする［６］に記載の飲料処理用金属担持イオン交換樹脂。
The present inventors have found that by passing a beverage through a specific metal-supported ion exchange resin, unnecessary components contained in the beverage can be removed, and the above problem can be solved.
That is, the gist of the present invention is as follows.
[1] Purification of a beverage for removing unnecessary components contained in a beverage, the method including a step of contacting a metal-carrying ion-exchange resin for beverage treatment obtained by exchanging at least a part of cations of a cation exchange resin with silver ions. Method.
[2] The beverage according to [1], wherein the supported amount of the silver ion is 10% by mass or more and 40% by mass or less in terms of silver mass based on the total amount of the metal-supported ion-exchange resin for beverage treatment in terms of dryness. Purification method.
[3] After the step of bringing the beverage into contact with the beverage-treating metal-supported ion-exchange resin, the beverage contacted with the beverage-treating metal-supporting ion-exchange resin is further subjected to a step of removing metal ions with a metal capturing material. The method for purifying a beverage according to [1] or [2].
[4] The beverage purification method according to any one of [1] to [3], wherein the beverage is distilled liquor.
[5] The method for purifying a beverage according to any one of [1] to [3], wherein the beverage is brewed liquor.
[6] A metal-supported ion-exchange resin for beverage treatment, wherein at least a part of cations of the cation-exchange resin is exchanged with silver ions to remove unnecessary components contained in the beverage.
[7] The amount of the silver ion carried is 10% by mass or more and 40% by mass or less in terms of silver mass, based on the total amount of the metal ion-exchange resin for beverage processing in terms of dryness. 4. The metal-carrying ion exchange resin for beverage treatment according to 4.
本発明によれば、酒類のような飲料に含まれる不要成分を効率よく除去し得る飲料の精製方法、及び該精製方法に用いることのできる飲料処理用金属担持イオン交換樹脂を提供することができる。 ADVANTAGE OF THE INVENTION According to this invention, the refinement | purification method of the drink which can remove the unnecessary component contained in drinks, such as alcoholic beverage efficiently, and the metal carrying | support ion exchange resin for drink processing which can be used for the said refinement method can be provided. .
［飲料の精製方法］
本発明の実施形態に係る飲料の精製方法について、詳細に説明する。本実施形態に係る飲料の精製方法は、陽イオン交換樹脂の陽イオンの少なくとも一部が銀イオンに交換されてなる飲料処理用金属担持イオン交換樹脂に接触させる工程を包含し、飲料に含まれる不要成分を除去するものである。
本発明において対象とする飲料は、特に限定されるものではなく全ての飲料が適用できるが、以下では、飲料のなかでも酒類について説明する。
酒類としては、具体的には、ウイスキー、ブランデー、ジン、ウオッカ、テキーラ、ラム、白酒、アラック等の全ての蒸留酒が適用できる。また、清酒、ビール、ワイン、酒精強化ワイン、中国酒等の全ての醸造酒及び混成酒が適用できる。醸造酒及び混成酒のなかでは、清酒が好適に用いられる。さらに、麦焼酎、米焼酎、芋焼酎、黒糖酒、そば焼酎、コーン焼酎、粕取り焼酎、泡盛等の全ての焼酎が適用できる。
[Beverage purification method]
The method for purifying a beverage according to the embodiment of the present invention will be described in detail. The method for purifying a beverage according to the present embodiment includes a step of bringing at least a part of the cations of the cation exchange resin into contact with a metal-supported ion exchange resin for beverage treatment obtained by exchanging the cations with silver ions, and is included in the beverage. It removes unnecessary components.
The beverage targeted in the present invention is not particularly limited, and all beverages can be applied. In the following, alcoholic beverages will be described among the beverages.
As the liquor, specifically, all distilled liquors such as whiskey, brandy, gin, vodka, tequila, rum, white liquor, and arak can be applied. In addition, all brewed liquors and mixed liquors such as sake, beer, wine, refined wine, Chinese liquor and the like can be applied. Among brewed sake and mixed sake, sake is preferably used. Furthermore, all shochu such as barley shochu, rice shochu, potato shochu, brown sugar liquor, buckwheat shochu, corn shochu, lees shochu and awamori can be applied.
除去される不要成分とは、飲料の風味を妨げる成分であり、主として、不味成分が挙げられる。不味成分としては、酒類においては、ジメチルサルファイド、ジメチルジサルファイド、ジメチルトリサルファイド等の硫黄化合物が挙げられる。また、ピリジン等の窒素化合物が挙げられる。
酒類の精製方法の場合は、酒類に含まれる上述した不要成分を除去する一方で、高級アルコール類、フーゼル類、エステル類等の旨味成分を酒類中に残すことができる。
飲料が酒類である場合には、処理前の酒類に含まれる硫黄化合物の濃度が１００質量ｐｐｍ以下であることが好ましい。この範囲であれば、上述した飲料処理用金属担持イオン交換樹脂にて脱硫処理することが可能である。硫黄化合物の濃度は、より好ましくは、１０質量ｐｐｍ以下である。
処理温度の範囲は、−５０℃以上１５０℃以下であり、より好ましくは０℃以上１００℃以下であり、さらに好ましくは１０℃以上６０℃以下である。
上述した飲料処理用金属担持イオン交換樹脂に、飲料を通液させる際の条件は、流速（ＬＨＳＶ）範囲が０．１ｈ−１以上１００ｈ−１以下であり、より好ましくは０．５以上５０ｈ−１以下であり、さらに好ましくは１以上３０ｈ−１以下である。また、液の流れ方向はアップフロー又はダウンフローのどちらでも構わない。
The unnecessary components to be removed are components that hinder the flavor of the beverage, and mainly include unpleasant components. Examples of the unpleasant components include, in alcoholic beverages, sulfur compounds such as dimethyl sulfide, dimethyl disulfide, and dimethyl trisulfide. Further, a nitrogen compound such as pyridine may be used.
In the case of a method for purifying liquor, while removing the above-mentioned unnecessary components contained in liquor, umami components such as higher alcohols, fusels, and esters can be left in the liquor.
When the beverage is liquor, the concentration of the sulfur compound contained in the liquor before the treatment is preferably 100 ppm by mass or less. Within this range, desulfurization treatment can be performed using the above-described metal-supported ion-exchange resin for beverage treatment. The concentration of the sulfur compound is more preferably 10 ppm by mass or less.
The range of the treatment temperature is from −50 ° C. to 150 ° C., more preferably from 0 ° C. to 100 ° C., and even more preferably from 10 ° C. to 60 ° C.
The above-described beverage processing metal supported ion exchange resins, conditions for which passed through the beverage, the flow rate (LHSV) range is at 0.1 h -1 or more 100h -1 or less, more preferably 0.5 or more 50h - It is 1 or less, More preferably, it is 1 or more and 30h- 1 or less. Further, the flow direction of the liquid may be either upflow or downflow.
上記条件によれば、飲料が酒類であれば、酒類中に高級アルコール類、フーゼル類、エステル類等の旨味成分を保持しながら、不要成分を除去することができる。
本発明の実施形態に係る飲料の精製方法は、飲料を飲料処理用金属担持イオン交換樹脂に接触させる工程の後、飲料処理用金属担持イオン交換樹脂に接触させた飲料を、金属捕捉材料により金属イオンを除去する工程を、さらに有することが好ましい。
本実施形態に係る飲料の精製方法では、後述する、銀イオンが担持されたイオン交換樹脂を用いるため、該イオン交換樹脂に通液した後の飲料には、銀イオンが溶出していることがある。
そこで、金属捕捉材料により、通液後の飲料に許容量を超える銀イオンが流出することを防止することができる。
According to the above conditions, if the beverage is liquor, unnecessary components can be removed while retaining umami components such as higher alcohols, fusels, and esters in the liquor.
The method for purifying a beverage according to the embodiment of the present invention comprises, after the step of bringing the beverage into contact with the metal-supported ion-exchange resin for beverage treatment, the beverage that has been brought into contact with the metal-supported ion-exchange resin for beverage treatment, the metal capturing material It is preferable to further include a step of removing ions.
In the method for purifying a beverage according to the present embodiment, which will be described later, since an ion exchange resin carrying silver ions is used, silver ions are eluted in the beverage after passing through the ion exchange resin. is there.
Therefore, it is possible to prevent the silver ions exceeding the permissible amount from flowing out into the beverage after passing through the liquid by the metal capturing material.
［飲料処理用金属担持イオン交換樹脂］
本発明の実施形態に係る飲料処理用金属担持イオン交換樹脂は、陽イオン交換樹脂の陽イオンの少なくとも一部が銀イオンに交換されたものである。この飲料処理用金属担持イオン交換樹脂は、飲料に含まれる不要成分を除去することができる。
＜陽イオン交換樹脂＞
本実施形態に係る飲料処理用金属担持イオン交換樹脂に適用可能な陽イオン交換樹脂は、強酸性陽イオン交換樹脂、弱酸性陽イオン交換樹脂等の種類に限定されず、適用可能である。陽イオン交換樹脂のイオン型は、特に限定されず、水素型であってもよいし、カルシウム型、ナトリウム型等の塩型であってもよい。
陽イオン交換樹脂の構造として、スチレンやアクリルといった母体構造は、特に問わない。また、架橋密度などの樹脂物性によって特に限定されず、種々の陽イオン交換樹脂が使用できる。例えば、多孔質型又はゲルタイプの陽イオン交換樹脂が使用でき、特により表面積が高い多孔質型の陽イオン交換樹脂が好ましい。これらの陽イオン交換樹脂は、単独で用いてもよく、２種以上の陽イオン交換樹脂を組み合わせて用いてもよい。
[Metal-supported ion exchange resin for beverage processing]
The metal-supported ion-exchange resin for beverage processing according to the embodiment of the present invention is obtained by exchanging at least a part of the cations of the cation-exchange resin with silver ions. This metal-supporting ion-exchange resin for beverage treatment can remove unnecessary components contained in the beverage.
<Cation exchange resin>
The cation exchange resin applicable to the metal-carrying ion exchange resin for beverage processing according to the present embodiment is not limited to a strongly acidic cation exchange resin, a weakly acidic cation exchange resin, and the like, and can be applied. The ion type of the cation exchange resin is not particularly limited, and may be a hydrogen type or a salt type such as a calcium type and a sodium type.
The structure of the cation exchange resin is not particularly limited to a parent structure such as styrene or acrylic. Further, there is no particular limitation on the resin properties such as the crosslink density, and various cation exchange resins can be used. For example, a porous or gel type cation exchange resin can be used, and a porous cation exchange resin having a higher surface area is particularly preferable. These cation exchange resins may be used alone, or two or more cation exchange resins may be used in combination.
イオン交換樹脂の粒径は、０．３ｍｍ未満では通液時の差圧が高くなり、１．０ｍｍを超えると拡散性が悪くなる、又は破砕しやすくなるといった弊害が起きやすい。この観点から、イオン交換樹脂の粒径は０．３〜１．０ｍｍの粒径であることが好ましい。
本実施形態に係る飲料処理用金属担持イオン交換樹脂に適用可能な陽イオン交換樹脂の市販品としては、銀イオンの担持の容易性や、その後の飲料の精製効率を高める観点から、例えば、Ｒｏｈｍ ａｎｄ Ｈａａｓ株式会社製のＡｍｂｅｒｌｉｔｅを用いることができる。
また、上述した陽イオン交換樹脂は、本実施形態に係る飲料の精製方法において、飲料を飲料処理用金属担持イオン交換樹脂に接触させる工程の後、飲料処理用金属担持イオン交換樹脂に接触させた飲料を、陽イオン交換樹脂により金属イオンを除去する工程を有するものとした場合に、該金属イオンを除去する工程で使用される陽イオン交換樹脂としても適用可能である。
When the particle size of the ion-exchange resin is less than 0.3 mm, the differential pressure at the time of passing the liquid increases, and when it exceeds 1.0 mm, adverse effects such as poor diffusibility or easy crushing are likely to occur. From this viewpoint, the particle size of the ion exchange resin is preferably 0.3 to 1.0 mm.
Commercially available cation exchange resins applicable to the metal-supported ion exchange resin for beverage processing according to the present embodiment include, for example, Rohm from the viewpoint of easiness of silver ion loading and enhancement of subsequent beverage purification efficiency. and Amberlite manufactured by Haas Co., Ltd. can be used.
Further, the above-described cation exchange resin was brought into contact with the metal ion-exchange resin for beverage treatment after the step of bringing the beverage into contact with the metal-ion exchange resin for beverage treatment in the method for purifying a beverage according to the present embodiment. When the beverage has a step of removing metal ions with a cation exchange resin, the beverage can also be applied as a cation exchange resin used in the step of removing the metal ions.
＜飲料処理用金属担持イオン交換樹脂の製造方法＞
本発明の実施形態に係る飲料処理用金属担持イオン交換樹脂の製造方法は、陽イオン交換樹脂の陽イオンの少なくとも一部に、銀イオンを含有する溶液を用いてイオン交換法により、銀イオンを担持させる工程を有する。
イオン交換法では、上述したイオン交換樹脂の内部に、銀イオンを含有する溶液を用いて、イオン交換樹脂の内部のイオン、例えば、Ｈ＋イオン又はＮａ＋イオンを銀イオンで交換し、イオン交換樹脂の内部に銀イオンを担持させる。
本実施形態では、銀イオンを含有する溶液として、硝酸銀など水溶性の金属塩を用いることができる。
また、本実施形態では、銀イオンを含有する溶液を用いて銀イオンを担持させる工程の前に、硝酸アンモニウム溶液や塩化アンモニウム溶液、硫酸アンモニウム溶液、アンモニア水等のＮＨ４ ＋イオンを含む水溶液を用いて、陽イオン交換樹脂の陽イオンをＮＨ４ ＋イオンで置き換える工程を有することが好ましい。
<Method for producing metal-supported ion exchange resin for beverage treatment>
The method for producing a metal-carrying ion-exchange resin for beverage treatment according to the embodiment of the present invention comprises, in at least a part of the cations of the cation-exchange resin, silver ions by an ion exchange method using a solution containing silver ions. It has a step of carrying.
In the ion exchange method, ions inside the ion exchange resin, for example, H + ions or Na + ions are exchanged with silver ions by using a solution containing silver ions inside the above ion exchange resin, and ion exchange is performed. Silver ions are supported inside the resin.
In this embodiment, a water-soluble metal salt such as silver nitrate can be used as the solution containing silver ions.
In the present embodiment, an aqueous solution containing NH 4 + ions, such as an ammonium nitrate solution, an ammonium chloride solution, an ammonium sulfate solution, or ammonia water, is used before the step of supporting silver ions using a solution containing silver ions. It is preferable to have a step of replacing cations of the cation exchange resin with NH 4 + ions.
本実施形態においては、ＮＨ４ ＋イオンを含む水溶液を用いることにより、イオン交換樹脂のＨ＋イオン又はＮａ＋イオンの少なくとも一部がＮＨ４ ＋イオンに置き換えられる。この後、硝酸銀溶液で処理すると、飲料処理用金属担持イオン交換樹脂中における銀イオンの分散性を高めることができる。
これは、アンモニウムイオンが銀イオンを取り囲んだ銀アンミン錯体が形成されることにより、銀イオン同士の凝集が抑制されることによるものと推察される。
本実施形態に係る飲料処理用金属担持イオン交換樹脂において、イオン交換樹脂に担持された銀の総担持量は、乾燥換算の飲料処理用金属担持イオン交換樹脂全量に対して、１０質量％以上４０質量％以下であることが好ましく、より好ましくは、１５質量％以上３５質量％以下であり、さらに好ましくは、２０質量％以上３５質量％以下である。銀の担持量が１０質量％未満であると飲料に含まれる不要成分を十分に除去できず、４０質量％を超えると、銀がイオン交換され難くなるため、銀が凝集し、金属当たりの不要成分の除去効率が低下する。
In the present embodiment, by using an aqueous solution containing NH 4 + ions, at least a portion of the ion exchange resin H + ions or Na + ions are replaced by NH 4 + ions. After that, when treated with a silver nitrate solution, the dispersibility of silver ions in the metal-supported ion exchange resin for beverage processing can be increased.
This is presumed to be due to formation of a silver ammine complex in which ammonium ions surround silver ions, thereby suppressing aggregation of silver ions.
In the metal ion-exchange resin for beverage processing according to the present embodiment, the total amount of silver supported on the ion-exchange resin is 10% by mass or more and 40% or more of the total amount of the metal ion-exchange resin for beverage processing on a dry basis. It is preferably at most 15 mass%, more preferably at least 15 mass% and at most 35 mass%, even more preferably at least 20 mass% and at most 35 mass%. If the supported amount of silver is less than 10% by mass, unnecessary components contained in the beverage cannot be sufficiently removed, and if the amount exceeds 40% by mass, silver is hardly ion-exchanged, so that silver is aggregated and unnecessary per metal. The efficiency of removing components is reduced.
＜金属捕捉材料＞
飲料のなかの不要成分の除去効率を高めるためには、上述した飲料処理用金属担持イオン交換樹脂中の金属の担持量を増大させる必要がある。しかし、飲料を飲料処理用金属担持イオン交換樹脂に接触させる場合、飲料処理用金属担持イオン交換樹脂に担持されている金属が飲料に溶出することがあり、金属の溶出量は、飲料処理用金属担持イオン交換樹脂に担持されている金属の担持量に比例して増大する。
そこで、本実施形態においては、飲料を飲料処理用金属担持イオン交換樹脂に接触させる工程の後、飲料処理用金属担持イオン交換樹脂に接触させた飲料を、金属捕捉材料により金属イオンを除去する工程を、さらに有していることが好ましい。飲料処理用金属担持イオン交換樹脂に接触させた飲料を金属捕捉材料に接触させることにより、飲料処理用金属担持イオン交換樹脂から溶出した金属が除去される。
<Metal capture material>
In order to increase the efficiency of removing unnecessary components in the beverage, it is necessary to increase the amount of the metal carried in the above-described metal-supported ion-exchange resin for beverage treatment. However, when a beverage is brought into contact with a metal-supported ion-exchange resin for beverage processing, the metal supported on the metal-supported ion-exchange resin for beverage processing may be eluted into the beverage, and the amount of metal eluted may vary from the metal for beverage processing. It increases in proportion to the amount of metal supported on the supported ion exchange resin.
Therefore, in the present embodiment, after the step of bringing the beverage into contact with the metal-supported ion-exchange resin for beverage processing, the step of removing the metal ions from the beverage that has been brought into contact with the metal-supported ion-exchange resin for beverage processing with a metal capturing material. It is preferable to further have The metal eluted from the metal-supported ion-exchange resin for beverage treatment is removed by bringing the beverage in contact with the metal-exchange resin for beverage treatment into contact with the metal capture material.
金属捕捉材料としては、公知の陽イオン交換樹脂、ゼオライトなどのイオン交換能を示す材料が使用できる。金属捕捉材料のイオン交換可能な陽イオンとしては、特に限定されず、Ｈ＋イオンであってもよいし、Ｃａ２＋イオン、Ｎａ＋イオン等であってもよい。 As the metal capturing material, a material having an ion exchange ability such as a known cation exchange resin or zeolite can be used. The ion exchangeable cation of the metal capturing material is not particularly limited, and may be H + ion, Ca 2+ ion, Na + ion, or the like.
金属捕捉材料用陽イオン交換樹脂としては、強酸性陽イオン交換樹脂、弱酸性陽イオン交換樹脂等の種類に限定されず、適用可能である。
陽イオン交換樹脂の構造として、スチレンやアクリルといった母体構造は、特に問わない。また、架橋密度などの樹脂物性によって特に限定されず、種々の陽イオン交換樹脂が使用できる。例えば、多孔質型又はゲルタイプの陽イオン交換樹脂が使用でき、特により表面積が高い多孔質型の陽イオン交換樹脂が好ましい。これらの陽イオン交換樹脂は、単独で用いてもよく、２種以上の陽イオン交換樹脂を組み合わせて用いてもよい。
The cation exchange resin for the metal capture material is not limited to a strong acid cation exchange resin, a weakly acidic cation exchange resin, and the like, and is applicable.
The structure of the cation exchange resin is not particularly limited to a parent structure such as styrene or acrylic. Further, there is no particular limitation on the resin properties such as the crosslink density, and various cation exchange resins can be used. For example, a porous or gel type cation exchange resin can be used, and a porous cation exchange resin having a higher surface area is particularly preferable. These cation exchange resins may be used alone, or two or more cation exchange resins may be used in combination.
金属捕捉材料用ゼオライトとしては、イオン交換可能な陽イオンを有するゼオライトであって、特に、フォージャサイト、Ｘ型ゼオライト、Ｙ型ゼオライト、Ａ型ゼオライト、ＺＳＭ−５ゼオライト、モルデンフッ石、ベータ型ゼオライトの中のいずれか１構造を有するゼオライトである。中でも好ましいゼオライトはＸ型ゼオライト、Ｙ型ゼオライトである。 The zeolite for a metal capturing material is a zeolite having an ion-exchangeable cation. Is a zeolite having any one of the following structures: Among them, preferred zeolites are X-type zeolites and Y-type zeolites.
以下、本発明を実施例によりさらに詳細に説明する。本発明は、以下の実施例に限定されるものではない。
［評価方法］
＜飲料処理用金属担持イオン交換樹脂の銀担持量の定量＞
後述する供試イオン交換樹脂における銀担持量は、ＩＣＰ発光分光分析装置（アジレントテクノロジー株式会社製 ７２０−ＥＳ）を用いて定量した。ここで、銀担持量とは、乾燥換算の供試イオン交換樹脂全質量に対する金属換算の質量％である。
希硝酸を用いて、供試イオン交換樹脂から銀を溶出させる処理を２回行って、抽出された液の分析結果から、供試イオン交換樹脂の銀担持量を算出した。
Hereinafter, the present invention will be described in more detail with reference to Examples. The present invention is not limited to the following examples.
[Evaluation methods]
<Quantification of the amount of silver supported on the metal-supported ion exchange resin for beverage processing>
The amount of silver supported on the test ion exchange resin described below was quantified using an ICP emission spectrometer (720-ES, manufactured by Agilent Technologies). Here, the amount of silver carried is the mass% in terms of metal relative to the total mass of the test ion exchange resin in terms of dryness.
The treatment for eluting silver from the test ion exchange resin was performed twice using dilute nitric acid, and the amount of silver carried on the test ion exchange resin was calculated from the analysis result of the extracted liquid.
＜酒類の硫黄成分分析＞
後述する供試イオン交換樹脂を封入したカラムの通液前の供試酒と、通液後の供試酒中の硫黄化合物（硫化水素（Ｈ２Ｓ）、メチルメルカプタン（ＣＨ３ＳＨ）、ジメチルスルフィド（ＤＭＳ）、及びジメチルジスルフィド（ＤＭＤＳ））の濃度を、ＧＣ−ＳＣＤ装置（化学発光硫黄検出器付ガスクロマトグラフィー、アレジレントテクノロジー株式会社製、ＧＣ：６８９０Ｎ／ＳＣＤ：３５５）を用いて分析した。なお、ここでの硫黄化合物の濃度は、化合物濃度ではなく、硫黄原子濃度である。
また、供試酒中に含まれている全硫黄濃度を、紫外蛍光法硫黄分析計（三菱化学アナルテック株式会社製、型番ＴＳ−１００）を使用して、燃焼−紫外蛍光法により測定した。なお、全硫黄濃度とは、化合物濃度ではなく、硫黄原子濃度である。
<Sulfur component analysis of alcoholic beverages>
A sample liquor before passing through a column in which a test ion exchange resin described below is sealed and a sulfur compound (hydrogen sulfide (H 2 S), methyl mercaptan (CH 3 SH), dimethyl) in the sample liquor after passing through the column The concentration of sulfide (DMS) and dimethyl disulfide (DMDS) is analyzed using a GC-SCD device (gas chromatography with a chemiluminescent sulfur detector, manufactured by Resilient Technology, GC: 6890N / SCD: 355). did. Here, the concentration of the sulfur compound is not a compound concentration but a sulfur atom concentration.
The concentration of total sulfur contained in the test liquor was measured by a combustion-ultraviolet fluorescence method using an ultraviolet fluorescence sulfur analyzer (manufactured by Mitsubishi Chemical Analtech Co., Ltd., model number TS-100). In addition, the total sulfur concentration is not a compound concentration but a sulfur atom concentration.
＜酒類の香気成分等の分析＞
後述する供試イオン交換樹脂を封入したカラムの通液前の供試酒と、通液後の供試酒中の香気成分等の分析は、ヘッドスペースガスクロマトグラフ質量分析計（ヘッドスペースインジェクター「ＭｕｌｔｉＰｕｒｐｏｓｅ Ｓａｍｐｌｅｒ ＭＰＳ２」 Ｇｅｒｓｔｅｌ株式会社製）を用いて行った。ここでの濃度は、化合物濃度である。
<Analysis of flavor components of alcoholic beverages>
The analysis of the sample liquor before passing through the column in which the test ion exchange resin is sealed and the fragrance component in the test liquor after passing through the column were performed using a headspace gas chromatograph mass spectrometer (headspace injector “MultiPurpose”). Sampler MPS2 "manufactured by Gerstel, Inc.). The concentration here is the compound concentration.
＜銀の溶出量の定量＞
後述する供試イオン交換樹脂を封入したカラムの通液後の供試酒に、硫酸処理と、灰化処理とを施した後、アルカリ溶解法を実施することにより均一な水溶液を得た。この水溶液に含まれる銀の量を、ＩＣＰ発光分光分析装置 アジレントテクノロジー株式会社製 ７２０−ＥＳを用いて定量し、これを溶出量とした。
<Quantification of silver elution amount>
After a sample liquor passed through a column in which a sample ion exchange resin described below was sealed, the sample liquor was subjected to a sulfuric acid treatment and an ashing treatment, and then an alkaline dissolution method was performed to obtain a uniform aqueous solution. The amount of silver contained in this aqueous solution was quantified using an ICP emission spectrometer 720-ES manufactured by Agilent Technologies, Inc., and this was used as the elution amount.
＜官能評価試験＞
実施例１及び比較例１，２の方法にて通液処理したウイスキー、および未処理のウイスキー（未処理）に対し、１２名のパネラーにより、最低１点〜最高７点による７段階で行った。その結果を第４表に示す。
<Sensory evaluation test>
The whiskey passed through the method of Example 1 and Comparative Examples 1 and 2, and the untreated whiskey (untreated) were evaluated by 12 panelists in 7 steps from a minimum of 1 point to a maximum of 7 points. . Table 4 shows the results.
［供試イオン交換樹脂の製造例］
＜製造例１＞
硝酸アンモニウム２６４ｇを水３．３Ｌに溶解し、市販のＮａ型イオン交換樹脂（Ｒｏｈｍ ａｎｄ Ｈａａｓ株式会社製、商品名：Ａｍｂｅｒｌｉｔｅ ２００）を、乾燥重量で１ｋｇ投入し、液を３時間撹拌し、イオン交換処理を行ってＮＨ４型イオン交換樹脂を得た。水洗の後、水３Ｌに硝酸銀７８８ｇを溶解して得られた硝酸銀溶液に、ＮＨ４型イオン交換樹脂１ｋｇを投入し、液を３時間撹拌し、Ａｇイオン交換を行い、さらに、濾過及び水洗を行った。この後、６０℃で１２時間の乾燥を行い、Ａｇ型イオン交換樹脂１を得た。
[Production example of test ion exchange resin]
<Production Example 1>
264 g of ammonium nitrate was dissolved in 3.3 L of water, 1 kg of a commercially available Na-type ion exchange resin (manufactured by Rohm and Haas Co., Ltd., trade name: Amberlite 200) was added by dry weight, and the solution was stirred for 3 hours and ion-exchanged. By performing the treatment, an NH 4 type ion exchange resin was obtained. After washing with water, 1 kg of an NH 4 type ion exchange resin was added to a silver nitrate solution obtained by dissolving 788 g of silver nitrate in 3 L of water, and the solution was stirred for 3 hours to perform Ag ion exchange, followed by filtration and washing with water. went. Thereafter, drying was performed at 60 ° C. for 12 hours to obtain an Ag-type ion exchange resin 1.
＜製造例２＞
硝酸銀７８８ｇを水３Ｌに溶解し、市販のＮａ型イオン交換樹脂（Ｒｏｈｍ ａｎｄ Ｈａａｓ株式会社製、商品名：Ａｍｂｅｒｌｉｔｅ ２００）を乾燥重量で１ｋｇ投入し、液を３時間撹拌し、Ａｇイオン交換を行い、さらに、濾過及び水洗を行った。この後、６０℃で１２時間の乾燥を行い、Ａｇ型イオン交換樹脂２を得た。
<Production Example 2>
788 g of silver nitrate is dissolved in 3 L of water, and 1 kg of a commercially available Na-type ion exchange resin (manufactured by Rohm and Haas Co., Ltd., trade name: Amberlite 200) is added by dry weight, and the solution is stirred for 3 hours to carry out Ag ion exchange. Further, filtration and washing with water were performed. Thereafter, drying was performed at 60 ° C. for 12 hours to obtain an Ag-type ion exchange resin 2.
＜製造例３＞
硝酸銀３９４ｇを水３Ｌに溶解し、市販のＮａ型イオン交換樹脂（Ｒｏｈｍ ａｎｄ Ｈａａｓ株式会社製、商品名：Ａｍｂｅｒｌｉｔｅ ２００）を乾燥重量で１ｋｇ投入し、液を３時間撹拌し、Ａｇイオン交換を行い、さらに、濾過及び水洗を行った。この後、６０℃で１２時間の乾燥を行い、Ａｇ型イオン交換樹脂３を得た。
<Production Example 3>
394 g of silver nitrate was dissolved in 3 L of water, and 1 kg of a commercially available Na-type ion exchange resin (manufactured by Rohm and Haas Co., Ltd., trade name: Amberlite 200) was added by dry weight, and the solution was stirred for 3 hours to perform Ag ion exchange. Further, filtration and washing with water were performed. Thereafter, drying was performed at 60 ° C. for 12 hours to obtain an Ag-type ion exchange resin 3.
＜製造例４＞
硝酸銀３９４ｇを水３Ｌに溶解し、市販のＨ型イオン交換樹脂（Ｒｏｈｍ ａｎｄ Ｈａａｓ株式会社製、商品名：Ａｍｂｅｒｌｙｓｔ １５）を乾燥重量で１ｋｇ投入し、液を３時間撹拌し、Ａｇイオン交換を行い、さらに、濾過及び水洗を行った。この後、６０℃で１２時間の乾燥を行い、Ａｇ型イオン交換樹脂４を得た。
<Production Example 4>
394 g of silver nitrate was dissolved in 3 L of water, 1 kg of a commercially available H-type ion exchange resin (manufactured by Rohm and Haas Co., trade name: Amberlyst 15) was added by dry weight, and the solution was stirred for 3 hours to carry out Ag ion exchange. Further, filtration and washing with water were performed. Thereafter, drying was performed at 60 ° C. for 12 hours to obtain an Ag-type ion exchange resin 4.
＜製造例５＞
硝酸アンモニウム２６４ｇを水３．３Ｌに溶解し、市販のＨ型イオン交換樹脂（Ｒｏｈｍ ａｎｄ Ｈａａｓ株式会社製、商品名：Ａｍｂｅｒｌｙｓｔ １５）を乾燥重量で１ｋｇ投入し、液を３時間撹拌し、イオン交換処理を行ってＮＨ４型イオン交換樹脂を得た。水洗の後、水３Ｌに硝酸銀３９４ｇを溶解して得られた硝酸銀溶液に、ＮＨ４型イオン交換樹脂１ｋｇを投入し、液を３時間撹拌し、Ａｇイオン交換を行い、さらに、濾過及び水洗を行った。この後、６０℃で１２時間の乾燥を行い、Ａｇ型イオン交換樹脂５を得た。
<Production Example 5>
264 g of ammonium nitrate was dissolved in 3.3 L of water, and 1 kg of a commercially available H-type ion exchange resin (manufactured by Rohm and Haas Co., Ltd., trade name: Amberlyst 15) was added thereto by dry weight, and the solution was stirred for 3 hours to perform ion exchange treatment. Was performed to obtain an NH 4 type ion exchange resin. After washing with water, 394 g of silver nitrate was dissolved in 3 L of water, 1 kg of an NH 4 type ion exchange resin was added to the silver nitrate solution, and the solution was stirred for 3 hours to perform Ag ion exchange, followed by filtration and washing with water. went. Thereafter, drying was performed at 60 ° C. for 12 hours to obtain an Ag-type ion exchange resin 5.
＜製造例６＞
市販のナトリウムＹ型ゼオライト成型体（東ソー株式会社製 ＨＳＺ−３２０ＮＡＤ１Ａ）を砕いて平均粒径を１．０〜１．５ｍｍに揃えた。硝酸アンモニウム２６４ｇを水３．３Ｌに溶解し、上記ゼオライト１ｋｇを投入し、液を３時間撹拌し、イオン交換処理を行ってＮＨ４Ｙ型ゼオライトを得た。水洗及び乾燥の後、ＮＨ４Ｙ型ゼオライト１ｋｇを硝酸銀３９４ｇ及びアンモニア（３０％）３３０ｇを水２．５Ｌに溶解した銀アンミン錯イオン溶液に投入し、液を３時間撹拌し、Ａｇイオン交換を行い、さらに、水洗及び乾燥を行った。この後、４００℃で３時間の焼成を行い、ＡｇＹ型ゼオライト１を得た。
<Production Example 6>
A commercially available sodium Y-type zeolite molded product (HSZ-320NAD1A manufactured by Tosoh Corporation) was crushed to adjust the average particle size to 1.0 to 1.5 mm. 264 g of ammonium nitrate was dissolved in 3.3 L of water, 1 kg of the above zeolite was added, the solution was stirred for 3 hours, and an ion exchange treatment was performed to obtain an NH 4 Y-type zeolite. After washing and drying, 1 kg of NH 4 Y zeolite was put into a silver ammine complex ion solution in which 394 g of silver nitrate and 330 g of ammonia (30%) were dissolved in 2.5 L of water, and the solution was stirred for 3 hours to carry out Ag ion exchange. Then, washing and drying were performed. Thereafter, calcination was carried out at 400 ° C. for 3 hours to obtain AgY-type zeolite 1.
＜比較製造例１＞
直径１ｃｍのカラムに、市販のＮａ型イオン交換樹脂（Ｒｏｈｍ ａｎｄ Ｈａａｓ株式会社製、商品名：Ａｍｂｅｒｌｉｔｅ ２００）を１８ｃｍ３封入し、濃硫酸（純正化学株式会社製）を用いて調製した３質量％硫酸水溶液１．８Ｌを１時間通液し、Ｈ型イオン交換樹脂を作製した。
<Comparative Production Example 1>
18 cm 3 of a commercially available Na-type ion exchange resin (manufactured by Rohm and Haas Co., Ltd., trade name: Amberlite 200) was sealed in a column having a diameter of 1 cm, and 3 mass% prepared using concentrated sulfuric acid (manufactured by Junsei Chemical Co., Ltd.). 1.8 L of an aqueous sulfuric acid solution was passed for 1 hour to prepare an H-type ion exchange resin.
［実施例及び比較例］
（１）供試酒として、モルトウイスキー（アルコール分６２％）を用いたときの評価
＜実施例１＞
直径１ｃｍの第１カラムに、製造例１により得られたＡｇ型イオン交換樹脂１を１８ｃｍ３封入した。また、直径１ｃｍの第２カラムに、市販のＮａ型イオン交換樹脂（Ｒｏｈｍ ａｎｄ Ｈａａｓ株式会社製、商品名：Ａｍｂｅｒｌｉｔｅ ２００）を１８ｃｍ３封入した。第１カラムと第２カラムとを直列に接続し、供試酒として、モルトウイスキー（アルコール分６２％）２．５Ｌを、通液温度３０℃，通液条件ＬＨＳＶ＝２０ｈ−１で通液させた。
通液前の供試酒と、通液後の供試酒とを、上述の方法により分析した。なお、通液後の供試酒とは、通液開始から７時間後に流出した供試酒である。
供試酒のモルトウイスキーには、ＤＭＳが１．０４７ｐｐｍ、ＤＭＤＳが０．２４８ｐｐｍ含まれていた。第１カラム及び第２カラムからのＡｇ溶出量を第１表に、硫黄化合物の分析結果を第２表に、香気成分の分析結果を第３表に、官能評価試験の結果を第４表に示す。なお、Ａｇ溶出量は、第１カラム通液後と第２カラム通液後の双方について確認した。
[Examples and Comparative Examples]
(1) Evaluation when malt whiskey (alcohol content: 62%) was used as the sample sake <Example 1>
18 cm 3 of the Ag-type ion exchange resin 1 obtained in Production Example 1 was sealed in a first column having a diameter of 1 cm. Further, 18 cm 3 of a commercially available Na-type ion exchange resin (manufactured by Rohm and Haas Co., trade name: Amberlite 200) was sealed in the second column having a diameter of 1 cm. The first column and the second column are connected in series, and 2.5 L of malt whiskey (alcohol content: 62%) is passed as a sample liquor at a flowing temperature of 30 ° C. under flowing conditions of LHSV = 20 h −1. Was.
The test liquor before passing the liquid and the test liquor after passing the liquid were analyzed by the above-described method. In addition, the sample liquor after the passage is the sample liquor that has flowed out 7 hours after the start of the passage.
The test sake malt whiskey contained 1.047 ppm of DMS and 0.248 ppm of DMDS. Table 1 shows the amounts of Ag eluted from the first and second columns, Table 2 shows the analysis results of sulfur compounds, Table 3 shows the analysis results of odor components, and Table 4 shows the results of sensory evaluation tests. Show. The Ag elution amount was confirmed both after the passage through the first column and after the passage through the second column.
＜実施例２＞
直径１ｃｍのカラムに、製造例２により得られたＡｇ型イオン交換樹脂２を１８ｃｍ３封入した。このカラムに、供試酒としてモルトウイスキー（アルコール分６２％）２．５Ｌを、通液温度３０℃，通液条件ＬＨＳＶ＝２０ｈ−１で通液させた。Ａｇ溶出量を第１表に、硫黄化合物の分析結果を第２表に示す。
<Example 2>
18 cm 3 of the Ag type ion exchange resin 2 obtained in Production Example 2 was sealed in a column having a diameter of 1 cm. 2.5 L of malt whiskey (alcohol content: 62%) as a sample liquor was passed through this column at a flowing temperature of 30 ° C. under flowing conditions of LHSV = 20 h −1 . The elution amount of Ag is shown in Table 1, and the analysis results of sulfur compounds are shown in Table 2.
＜実施例３＞
直径１ｃｍのカラムに、製造例３により得られたＡｇ型イオン交換樹脂３を１８ｃｍ３封入した。このカラムに、供試酒としてモルトウイスキー（アルコール分６２％）２．５Ｌを、通液温度３０℃，通液条件ＬＨＳＶ＝２０ｈ−１で通液させた。Ａｇ溶出量を第１表に、硫黄化合物の分析結果を第２表に示す。
<Example 3>
18 cm 3 of the Ag type ion exchange resin 3 obtained in Production Example 3 was sealed in a column having a diameter of 1 cm. 2.5 L of malt whiskey (alcohol content: 62%) as a sample liquor was passed through this column at a flowing temperature of 30 ° C. under flowing conditions of LHSV = 20 h −1 . The elution amount of Ag is shown in Table 1, and the analysis results of sulfur compounds are shown in Table 2.
＜実施例４＞
直径１ｃｍの第１カラムに、製造例４により得られたＡｇ型イオン交換樹脂４を１８ｃｍ３封入した。このカラムに、供試酒として、モルトウイスキー（アルコール分６２％）２．５Ｌを、通液温度３０℃，通液条件ＬＨＳＶ＝２０ｈ−１で通液させた。Ａｇ溶出量を第１表に、硫黄化合物の分析結果を第２表に示す。
<Example 4>
18 cm 3 of the Ag type ion exchange resin 4 obtained in Production Example 4 was sealed in a first column having a diameter of 1 cm. 2.5 L of malt whiskey (alcohol content: 62%) as a sample liquor was passed through this column at a flowing temperature of 30 ° C. under flowing conditions of LHSV = 20 h −1 . The elution amount of Ag is shown in Table 1, and the analysis results of sulfur compounds are shown in Table 2.
＜実施例５＞
直径１ｃｍの第１カラムに、製造例５により得られたＡｇ型イオン交換樹脂５を１８ｃｍ３封入した。このカラムに、供試酒として、モルトウイスキー（アルコール分６２％）２．５Ｌを、通液温度３０℃，通液条件ＬＨＳＶ＝２０ｈ−１で通液させた。Ａｇ溶出量を第１表に、硫黄化合物の分析結果を第２表に示す。
<Example 5>
18 cm 3 of the Ag type ion exchange resin 5 obtained in Production Example 5 was sealed in a first column having a diameter of 1 cm. 2.5 L of malt whiskey (alcohol content: 62%) as a sample liquor was passed through this column at a flowing temperature of 30 ° C. under flowing conditions of LHSV = 20 h −1 . The elution amount of Ag is shown in Table 1, and the analysis results of sulfur compounds are shown in Table 2.
＜参考例１＞
直径１ｃｍの第１カラムに、製造例６により得られたＡｇＹ型ゼオライト1を１８ｃｍ３封入した。また、市販のナトリウムＹ型ゼオライト成型体（東ソー株式会社製 ＨＳＺ−３２０ＮＡＤ１Ａ）を砕いて平均粒径を１．０〜１．５ｍｍに揃えて、これを直径１ｃｍの第２カラムに１８ｃｍ３封入した。第１カラムと第２カラムとを直列に接続し、供試酒として、モルトウイスキー（アルコール分６２％）２．５Ｌに酢酸カルシウム（和光純薬社製）０．１０ｇを加え、これを通液温度３０℃，通液条件ＬＨＳＶ＝２０ｈ−１で通液させた。Ａｇ溶出量を第１表に示す。
<Reference Example 1>
18 cm 3 of the AgY-type zeolite 1 obtained in Production Example 6 was sealed in a first column having a diameter of 1 cm. Also, a commercially available sodium Y-type zeolite molded product (HSZ-320NAD1A manufactured by Tosoh Corporation) was crushed to adjust the average particle size to 1.0 to 1.5 mm, and this was sealed in a second column having a diameter of 1 cm in an amount of 18 cm 3 . . The first column and the second column were connected in series, and 0.10 g of calcium acetate (manufactured by Wako Pure Chemical Industries, Ltd.) was added to 2.5 L of malt whiskey (alcohol content: 62%) as a sample liquor. The solution was passed at a temperature of 30 ° C. and under a flowing condition of LHSV = 20 h −1 . Table 1 shows the elution amount of Ag.
＜比較例１＞
直径１ｃｍのカラムに、市販のＮａ型イオン交換樹脂（Ｒｏｈｍ ａｎｄ Ｈａａｓ株式会社製、商品名：Ａｍｂｅｒｌｉｔｅ ２００）を１８ｃｍ３封入した。このカラムに、供試酒として、モルトウイスキー（アルコール分６２％）２．５Ｌを、通液温度３０℃，通液条件ＬＨＳＶ＝２０ｈ−１で通液させた。硫黄化合物の分析結果を第２表に、香気成分の分析結果を第３表に、官能評価試験の結果を第４表に示す。
<Comparative Example 1>
18 cm 3 of a commercially available Na-type ion exchange resin (manufactured by Rohm and Haas Co., trade name: Amberlite 200) was sealed in a column having a diameter of 1 cm. 2.5 L of malt whiskey (alcohol content: 62%) as a sample liquor was passed through this column at a flowing temperature of 30 ° C. under flowing conditions of LHSV = 20 h −1 . Table 2 shows the analysis results of the sulfur compounds, Table 3 shows the analysis results of the aroma components, and Table 4 shows the results of the sensory evaluation test.
＜比較例２＞
比較製造例１によって得られたＨ型イオン交換樹脂に、供試酒として、モルトウイスキー（アルコール分６２％）２．５Ｌを、通液温度３０℃，通液条件ＬＨＳＶ＝２０ｈ−１で通液させた。硫黄化合物の分析結果を第２表に、香気成分の分析結果を第３表に、官能評価試験の結果を第４表に示す。
<Comparative Example 2>
2.5 L of malt whiskey (alcohol content: 62%) was passed through the H-type ion-exchange resin obtained in Comparative Production Example 1 as a sample liquor at a flowing temperature of 30 ° C. under flowing conditions of LHSV = 20 h −1. I let it. Table 2 shows the analysis results of the sulfur compounds, Table 3 shows the analysis results of the aroma components, and Table 4 shows the results of the sensory evaluation test.
＜モルトウイスキーの評価結果＞
第４表に示すように、未処理品の評点の平均が４．００点であるのに対して、比較例１は４．００点、比較例２は４．０８点であり、比較例のものは、未処理品と同等の未熟感を有していた。
一方、実施例１は４．５０点であり、未処理品に比べて未熟感の少ない良好な香味を有していた。
上記結果から、モルトウイスキー（アルコール分６２％）を、本実施例に係る金属担持イオン交換樹脂に通液すると、旨味成分を残しながら、不要成分を除去できることがわかった。
また、実施例１のように、Ａｇ型イオン交換樹脂のカラムと、Ｎａ型イオン交換樹脂のカラムとを直列に接続したシステムでは、上記不要成分の除去とともに、溶出した銀イオン量も十分に低減できることがわかった。
<Evaluation results of malt whiskey>
As shown in Table 4, the average of the scores of the untreated products was 4.00, whereas Comparative Example 1 had 4.00 points and Comparative Example 2 had 4.08 points. The product had the same immaturity as the untreated product.
On the other hand, Example 1 had 4.50 points, and had a good flavor with less immaturity compared to the untreated product.
From the above results, it was found that when malt whiskey (alcohol content: 62%) was passed through the metal-supported ion exchange resin according to the present example, unnecessary components could be removed while leaving umami components.
Further, in the system in which the Ag-type ion exchange resin column and the Na-type ion exchange resin column are connected in series as in Example 1, the amount of eluted silver ions is sufficiently reduced along with the removal of the unnecessary components. I knew I could do it.
（２）供試酒として、麦焼酎を用いたときの評価
＜実施例６＞
直径１ｃｍの第１カラムに、製造例１により得られたＡｇ型イオン交換樹脂1を１８ｃｍ３封入した。このカラムに、供試酒として、麦焼酎（常圧蒸溜（アルコール分２５％））２．５Ｌを、通液温度３０℃，通液条件ＬＨＳＶ＝２０ｈ−１で通液させた。Ａｇ溶出量を第５表に、硫黄化合物の分析結果を第６表に、香気成分の分析結果を第７表に示す。
＜参考例２＞
直径１ｃｍの第１カラムに、製造例６により得られたＡｇＹ型ゼオライト1を１８ｃｍ３封入した。また、市販のナトリウムＹ型ゼオライト成型体（東ソー株式会社製 ＨＳＺ−３２０ＮＡＤ１Ａ）を砕いて平均粒径を１．０〜１．５ｍｍに揃えて、これを直径１ｃｍの第２カラムに１８ｃｍ３封入した。第１カラムと第２カラムとを直列に接続し、供試酒として、麦焼酎（常圧蒸溜（アルコール分２５％））２．５Ｌを、通液温度３０℃，通液条件ＬＨＳＶ＝２０ｈ−１で通液させた。Ａｇ溶出量を第５表に示す。
(2) Evaluation when barley shochu was used as sample sake <Example 6>
18 cm 3 of the Ag-type ion exchange resin 1 obtained in Production Example 1 was sealed in a first column having a diameter of 1 cm. As a sample liquor, 2.5 L of barley shochu (distilled at normal pressure (alcohol content: 25%)) was passed through this column at a flow-through temperature of 30 ° C. under flow-through conditions of LHSV = 20 h −1 . The Ag elution amount is shown in Table 5, the analysis results of sulfur compounds are shown in Table 6, and the analysis results of aroma components are shown in Table 7.
<Reference Example 2>
18 cm 3 of the AgY-type zeolite 1 obtained in Production Example 6 was sealed in a first column having a diameter of 1 cm. Also, a commercially available sodium Y-type zeolite molded product (HSZ-320NAD1A manufactured by Tosoh Corporation) was crushed to adjust the average particle size to 1.0 to 1.5 mm, and this was sealed in a second column having a diameter of 1 cm in an amount of 18 cm 3 . . The first column and the second column are connected in series, and as a sample liquor, 2.5 L of barley shochu (distilled at normal pressure (alcohol content: 25%)) is passed at a passing temperature of 30 ° C. and passing conditions LHSV = 20 h − 1 was passed. Table 5 shows the Ag elution amount.
＜麦焼酎の評価結果＞
上記結果から、麦焼酎を、製造例１の金属担持イオン交換樹脂に通液すると、旨味成分を残しながら、不要成分を除去できることがわかった。
<Evaluation results of wheat shochu>
From the above results, it was found that when barley shochu was passed through the metal-supported ion exchange resin of Production Example 1, unnecessary components could be removed while leaving umami components.
（２）供試酒として、芋焼酎を用いたときの評価
＜実施例７＞
直径１ｃｍの第１カラムに、製造例１により得られたＡｇ型イオン交換樹脂1を１８ｃｍ３封入した。このカラムに、供試酒として、芋焼酎（常圧蒸溜（アルコール分３９％））２．５Ｌを、通液温度３０℃，通液条件ＬＨＳＶ＝２０ｈ−１で通液させた。Ａｇ溶出量を第８表に、硫黄化合物の分析結果を第９表に、香気成分の分析結果を第１０表に示す。
(2) Evaluation when potato shochu was used as sample sake <Example 7>
18 cm 3 of the Ag-type ion exchange resin 1 obtained in Production Example 1 was sealed in a first column having a diameter of 1 cm. As a sample liquor, 2.5 L of potato shochu (distilled at normal pressure (alcohol content: 39%)) was passed through this column at a flow-through temperature of 30 ° C. under flow-through conditions of LHSV = 20 h −1 . Table 8 shows the amount of Ag eluted, Table 9 shows the analysis results of sulfur compounds, and Table 10 shows the analysis results of aroma components.
＜芋焼酎の評価結果＞
上記結果から、芋焼酎を、製造例１の金属担持イオン交換樹脂に通液すると、旨味成分を残しながら、不要成分を除去できることがわかった。
<Evaluation results of potato shochu>
From the above results, it was found that when the sweet potato shochu was passed through the metal-supported ion exchange resin of Production Example 1, unnecessary components could be removed while leaving umami components.
（３）供試酒として、ラム酒を用いたときの評価
＜実施例８＞
直径１ｃｍの第１カラムに、製造例２により得られたＡｇ型イオン交換樹脂２を１８ｃｍ３封入した。このカラムに、供試酒として、ラム酒（アルコール分６２％）２．５Ｌを、通液温度３０℃，通液条件ＬＨＳＶ＝２０ｈ−１で通液させた。Ａｇ溶出量を第１１表に、硫黄化合物の分析結果を第１２表に、香気成分の分析結果を第１３表に示す。
(3) Evaluation when rum was used as the sample sake <Example 8>
18 cm 3 of the Ag-type ion exchange resin 2 obtained in Production Example 2 was sealed in a first column having a diameter of 1 cm. As a sample liquor, 2.5 L of rum (alcohol content: 62%) was passed through the column at a flow-through temperature of 30 ° C. under a flow-through condition of LHSV = 20 h −1 . The elution amount of Ag is shown in Table 11, the analysis results of sulfur compounds are shown in Table 12, and the analysis results of aroma components are shown in Table 13.
＜ラム酒の評価結果＞
上記結果から、ラム酒を、製造例２の金属担持イオン交換樹脂に通液すると、旨味成分を残しながら、不要成分を除去できることがわかった。
<Rum evaluation results>
From the above results, it was found that when rum was passed through the metal-supported ion exchange resin of Production Example 2, unnecessary components could be removed while leaving umami components.
Claims (6)
Supported amount of the silver ions, to the alcoholic liquor processing metal supported ion exchange resin the total amount of drying terms of silver mass conversion, at least 10 wt% 40 wt% or less, metallic carrying ions of claim 5 Processing member containing exchange resin.
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