CN101431906B - Method for separating off coloring components from aqueous plant extracts - Google Patents
Method for separating off coloring components from aqueous plant extracts Download PDFInfo
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- CN101431906B CN101431906B CN2007800148134A CN200780014813A CN101431906B CN 101431906 B CN101431906 B CN 101431906B CN 2007800148134 A CN2007800148134 A CN 2007800148134A CN 200780014813 A CN200780014813 A CN 200780014813A CN 101431906 B CN101431906 B CN 101431906B
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- Prior art keywords
- plant extracts
- magnesium
- basic component
- extracts
- sediment
- Prior art date
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- 238000000034 method Methods 0.000 title claims abstract description 55
- 239000000419 plant extract Substances 0.000 title claims abstract description 35
- 239000006103 coloring component Substances 0.000 title claims abstract description 13
- 239000011777 magnesium Substances 0.000 claims abstract description 17
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001425 magnesium ion Inorganic materials 0.000 claims abstract description 9
- 239000000284 extract Substances 0.000 claims description 32
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 18
- 239000013049 sediment Substances 0.000 claims description 14
- 159000000003 magnesium salts Chemical class 0.000 claims description 13
- 239000000725 suspension Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 244000019459 Cynara cardunculus Species 0.000 claims description 9
- 235000019106 Cynara scolymus Nutrition 0.000 claims description 9
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 9
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 8
- 239000000920 calcium hydroxide Substances 0.000 claims description 8
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 7
- -1 alkali metal acetate Chemical class 0.000 claims description 6
- 235000016520 artichoke thistle Nutrition 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 4
- 239000001263 FEMA 3042 Substances 0.000 claims description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 4
- 229930003935 flavonoid Natural products 0.000 claims description 4
- 150000002215 flavonoids Chemical class 0.000 claims description 4
- 235000017173 flavonoids Nutrition 0.000 claims description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 4
- 229940033123 tannic acid Drugs 0.000 claims description 4
- 235000015523 tannic acid Nutrition 0.000 claims description 4
- 229920002258 tannic acid Polymers 0.000 claims description 4
- 150000001412 amines Chemical group 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 3
- 239000011654 magnesium acetate Substances 0.000 claims description 3
- 235000011285 magnesium acetate Nutrition 0.000 claims description 3
- 229940069446 magnesium acetate Drugs 0.000 claims description 3
- 238000004062 sedimentation Methods 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 2
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 235000011147 magnesium chloride Nutrition 0.000 claims description 2
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 239000002244 precipitate Substances 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 23
- 239000000203 mixture Substances 0.000 description 13
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 7
- 239000000347 magnesium hydroxide Substances 0.000 description 7
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 6
- 229920001202 Inulin Polymers 0.000 description 5
- 239000011575 calcium Substances 0.000 description 5
- 229940029339 inulin Drugs 0.000 description 5
- JYJIGFIDKWBXDU-MNNPPOADSA-N inulin Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)OC[C@]1(OC[C@]2(OC[C@]3(OC[C@]4(OC[C@]5(OC[C@]6(OC[C@]7(OC[C@]8(OC[C@]9(OC[C@]%10(OC[C@]%11(OC[C@]%12(OC[C@]%13(OC[C@]%14(OC[C@]%15(OC[C@]%16(OC[C@]%17(OC[C@]%18(OC[C@]%19(OC[C@]%20(OC[C@]%21(OC[C@]%22(OC[C@]%23(OC[C@]%24(OC[C@]%25(OC[C@]%26(OC[C@]%27(OC[C@]%28(OC[C@]%29(OC[C@]%30(OC[C@]%31(OC[C@]%32(OC[C@]%33(OC[C@]%34(OC[C@]%35(OC[C@]%36(O[C@@H]%37[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O%37)O)[C@H]([C@H](O)[C@@H](CO)O%36)O)[C@H]([C@H](O)[C@@H](CO)O%35)O)[C@H]([C@H](O)[C@@H](CO)O%34)O)[C@H]([C@H](O)[C@@H](CO)O%33)O)[C@H]([C@H](O)[C@@H](CO)O%32)O)[C@H]([C@H](O)[C@@H](CO)O%31)O)[C@H]([C@H](O)[C@@H](CO)O%30)O)[C@H]([C@H](O)[C@@H](CO)O%29)O)[C@H]([C@H](O)[C@@H](CO)O%28)O)[C@H]([C@H](O)[C@@H](CO)O%27)O)[C@H]([C@H](O)[C@@H](CO)O%26)O)[C@H]([C@H](O)[C@@H](CO)O%25)O)[C@H]([C@H](O)[C@@H](CO)O%24)O)[C@H]([C@H](O)[C@@H](CO)O%23)O)[C@H]([C@H](O)[C@@H](CO)O%22)O)[C@H]([C@H](O)[C@@H](CO)O%21)O)[C@H]([C@H](O)[C@@H](CO)O%20)O)[C@H]([C@H](O)[C@@H](CO)O%19)O)[C@H]([C@H](O)[C@@H](CO)O%18)O)[C@H]([C@H](O)[C@@H](CO)O%17)O)[C@H]([C@H](O)[C@@H](CO)O%16)O)[C@H]([C@H](O)[C@@H](CO)O%15)O)[C@H]([C@H](O)[C@@H](CO)O%14)O)[C@H]([C@H](O)[C@@H](CO)O%13)O)[C@H]([C@H](O)[C@@H](CO)O%12)O)[C@H]([C@H](O)[C@@H](CO)O%11)O)[C@H]([C@H](O)[C@@H](CO)O%10)O)[C@H]([C@H](O)[C@@H](CO)O9)O)[C@H]([C@H](O)[C@@H](CO)O8)O)[C@H]([C@H](O)[C@@H](CO)O7)O)[C@H]([C@H](O)[C@@H](CO)O6)O)[C@H]([C@H](O)[C@@H](CO)O5)O)[C@H]([C@H](O)[C@@H](CO)O4)O)[C@H]([C@H](O)[C@@H](CO)O3)O)[C@H]([C@H](O)[C@@H](CO)O2)O)[C@@H](O)[C@H](O)[C@@H](CO)O1 JYJIGFIDKWBXDU-MNNPPOADSA-N 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000005418 vegetable material Substances 0.000 description 4
- 238000003809 water extraction Methods 0.000 description 4
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- ZGXJTSGNIOSYLO-UHFFFAOYSA-N 88755TAZ87 Chemical compound NCC(=O)CCC(O)=O ZGXJTSGNIOSYLO-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 229910019440 Mg(OH) Inorganic materials 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229940118199 levulan Drugs 0.000 description 2
- 238000011020 pilot scale process Methods 0.000 description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 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 description 1
- 235000016068 Berberis vulgaris Nutrition 0.000 description 1
- 241000335053 Beta vulgaris Species 0.000 description 1
- 241000219310 Beta vulgaris subsp. vulgaris Species 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 235000021536 Sugar beet Nutrition 0.000 description 1
- UVNKIYPMUDFRGV-UHFFFAOYSA-N [Mg].C(CC)(=O)O Chemical compound [Mg].C(CC)(=O)O UVNKIYPMUDFRGV-UHFFFAOYSA-N 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide 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
- 239000001639 calcium acetate Substances 0.000 description 1
- 235000011092 calcium acetate Nutrition 0.000 description 1
- 229960005147 calcium acetate Drugs 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000006187 pill Substances 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- 229960004109 potassium acetate Drugs 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 229960004249 sodium acetate Drugs 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
- A23L2/82—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter by flocculation
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/40—Colouring or decolouring of foods
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0051—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Fructofuranans, e.g. beta-2,6-D-fructofuranan, i.e. levan; Derivatives thereof
- C08B37/0054—Inulin, i.e. beta-2,1-D-fructofuranan; Derivatives thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Organic Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Extraction Or Liquid Replacement (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention relates to a method for separating off coloring components from aqueous plant extracts in which magnesium ions (Mg<2+>) are added to the plant extract, at least one alkaline component is added to the plant extract, a precipitate is formed, and the precipitate formed is separated off from the plant extract.
Description
The present invention relates to the method for separating off coloring components from aqueous plant extracts, also relate to magnesium salts for the purposes from the aqueous plant extracts separating off coloring components.
When from plant, separating valuable composition, usually use water extraction.In this case, usually vegetable material is ground and under agitation extracts with warm water.The extract of making thus is usually because its tannic acid and Flavonoid Content are dark brown yellow, in any case so can be from this class extract direct isolated composition do not meet the necessary requirement of centering color yet.
For example, the problems referred to above appear when separating inulin from arithoke.For the extract from beet, attempt decoloring method used when from sugar beet, separating sucrose, (add CO by adding chalk and then carbonization
2) decolour, but the method is carried out unsatisfactorily.Similarly, because it is required expensive, has got rid of and make spent ion exchange resin with the possibility of this extract decolouring.
The objective of the invention is to develop a kind of effective plant extracts decoloring method, it can use inexpensive aids and carry out with low device and time expenditure, and can therefrom isolate the product of color neutrality.
In order to realize this purpose, the invention provides the method according to Patent right requirement 1.In the subordinate claim to a method, describe the concrete favourable embodiment of the method in detail.
The present invention includes the method for separating off coloring components from aqueous plant extracts, comprising:
A) with magnesium ion (Mg
2+) add in the plant extracts,
B) at least a basic component is added in the plant extracts,
C) form sediment, and
D) from plant extracts, isolate the sediment of formation.
This method can realize surprising effective decolouring of aqueous plant extracts.
The method is effective especially in from arithoke, the particularly decolouring from the extract of artichoke roots.But, the application that this instantiation does not limit the present invention in any way.
In addition, the method is characterised in that, and is adjuvant used, such as magnesium salts and alkali, is cheap.
Device when in addition, implementing the method and time expenditure are also low especially.
At last, by such decolouring, turbid material can also be from liquid extract, removed simultaneously, therefore the independent removal of turbid material need not be carried out.
Of the present invention from plant extracts the method for separating off coloring components usually be also referred to as decolouring, clarification or " purification " of plant extracts.These terms equate in the present invention.
Coloring components refer to plant extracts non-color neutrality and make plant extracts present any all the components that may color.Usually this relates to green, yellow and the mixing brown and this class color that is present in the plant extracts after the water extraction step of vegetable material.But the method is not limited to particular color.
Coloring components can exist with dissolving, suspension or emulsification form, or can be simultaneously exists with the two or more form of these forms.Preferably, they are compositions of dissolving.
The coloring components of plant extracts is preferably tannic acid and/or flavonoids, and they can be separated particularly well by method of the present invention.
Above-mentioned aqueous plant extracts for example separates by the water extraction of the vegetable material that grinds, and this extraction is carried out with warm water usually.Vegetable material can be for example be made of the mixture of root, stem, leaf, flower and fruit or these materials.
The method can with floristics be not particularly limited.For example, the method can be advantageously used in and wherein carry out water extraction to separate its composition and wherein to have all plants of corresponding tannic acid and flavonoids.
Have been found that method of the present invention particularly advantageously is applicable to the arithoke water extract, more particularly from the extract of artichoke roots.
Can from this cynara scolymus extracts, isolate levulan, particularly inulin.Therefore, the present invention is particularly suitable as and separates levulan, the intermediate steps when particularly separating inulin from arithoke from arithoke.
According to the present invention, with magnesium ion (Mg
2+) add in the aqueous plant extracts.In step variant a), magnesium salt solution can be added in the plant extracts.In another preferred variant, the magnesium salts of solid form is directly added plant extracts and be dissolved in wherein.
When adding magnesium salts, it is preferably because its high solubility product in water and the very easy salt of dissolving.Specially suitable magnesium salts is selected from the magnesium salts of magnesium chloride, magnesium sulfate, magnesium nitrate, other low carbon fatty acid, for example magnesium acetate and propionic acid magnesium, and composition thereof.
According to the present invention, basic component refers to contain hydroxide ion (OH
-) or merging the rear component that in this extract, forms hydroxide ion with plant extracts.Basic component can be liquid, solid-state or gaseous state.The liquid basic component of preferred use.
As the step of the method a) and b) described in when adding magnesium ion and basic component, form sediment by precipitation reaction.In the method, step a) and b) can carry out simultaneously in principle, particularly step use the solution of magnesium ion in a) and at step b) in during the use akaline liquid.But, preferably carry out method step a) first, then carry out step b).
For the method advantageously, magnesium ion and basic component all are evenly distributed in the extract as far as possible, so that the precipitation reaction in the extract also is uniformly and quantitative as far as possible.Therefore, preferred use can be sneaked into rapidly moisture alkali lye in the plant extracts equably as basic component, for example alkaline solution or alkaline suspension liquid.According to the present invention, alkaline solution or suspension contain hydroxide ion (OH
-) or after merging with plant extracts, form hydroxide ion.
In method variant very preferably, magnesium salts is solved homogeneously in the extract in a) in step first.Then, at step b) in, preferably under vigorous stirring, add alkaline aqueous solution or suspension.
In one embodiment, basic component is the aqueous solution or the suspension of alkali metal hydroxide or alkaline earth metal hydroxide.This hydroxide is preferably selected from lithium hydroxide, NaOH, potassium hydroxide, barium hydroxide and calcium hydroxide.
In a variant very particularly preferably, basic component is the suspension of calcium hydroxide.Use the advantage of calcium hydroxide to be, at the step c of the method) in a small amount of especially centrifugation thing of acquisition.In addition, precipitate in the time of by magnesium hydroxide and calcium sulfate, realized the sediment compactibility of the higher rate of settling and Geng Gao.Sediment shows low especially gel-like consistency.Therefore, in this method variant, the binding capacity of unnecessary composition such as inulin is low especially in the sediment.
Another available basic component is ammonia, is preferably aqueous solution form.Do not get rid of in principle the use gaseous ammonia yet, but not as using the aqueous solution preferred.
In another embodiment, basic component is the aqueous solution, emulsion or the suspension of amine (such as ethylenediamine and triethanolamine).
Also can use the salt of weak organic acid, such as alkali metal acetate and alkaline-earth metal acetate, particularly sodium acetate, potassium acetate, calcium acetate and magnesium acetate.
Formed magnesium hydroxide, as the sediment of the inventive method.In this case, according to the present invention, the coloring components of water extract is stayed in the sediment, and so and liquid phase separation.Obtain the extract of basic decolouring.The quantitative extent of this decolouring especially depends on Mg
2+The amount of ion and used basic component, therefore and depend on the sedimentary amount of formation.The optimization of the amount of reactant is in those skilled in the art's limit of power.
If necessary, according to claim 1 whole decoloring method or its substep also can be arranged to the multistage.
In the method for the invention, the mol ratio OH of hydroxide ion and magnesium ion
-: Mg
2+Be preferably 2.2: 1 to 1.8: 1.This ratio most preferably is fully stoichiometric, i.e. OH
-: Mg
2+=2: 1.Therefore, select the amount of basic component, in order to there is the hydroxide ion of respective amount with respect to magnesium ion.
According to claims, the present invention also comprises the combination of using above-mentioned magnesium salts.Similarly, the present invention includes the combination of using above-mentioned basic component.
Method step a) and b) in, the dissolving of magnesium salts and the interpolation of basic component are preferably under agitation carried out, to realize the fastest as far as possible dissolving or homogenizing and therefore to realize fast reaction.But, hybrid technology is had no particular limits.For example, other hybrid technology that also can for example be familiar with by those skilled in the art of the method is carried out.
In order to accelerate the method, the step of the method a) is preferably carried out 60-80 ℃ temperature.Reaction time behind the interpolation basic component is typically about 1 to 15 minute, average about 10 minutes.
The separating step d of the inventive method) preferably by sedimentation, filtration or centrifugal, undertaken by separator (for example except pulp separator).But, other isolation technics that also can use those skilled in the art to be familiar with.
The below describes the present invention based on specific embodiments, and still, these specific embodiments in no case are the restrictions to General Principle of the present invention.
Embodiment
Embodiment 1-decolours with magnesium sulfate and NaOH
According to following chemical formula, form magnesium hydroxide with magnesium sulfate and NaOH:
MgSO
47H
2O+2NaOH → Mg (OH)
2+ Na
2SO
4+ 7H
2O (Chemical formula 1)
Table 1 has shown bitter salt that the amount that forms per 100 milliliters of extract 0.1-10 gram magnesium hydroxide is required and the amount of NaOH.
Table 1: be used to form Mg (OH
2) the stoichiometric amount of reactant
| Mg(OH) 2[g/100ml] (theoretical value) | 0.10 | 0.20 | 0.30 | 0.40 | 0.50 | 0.60 | 0.70 | 0.80 | 0.90 | 1.00 |
| MgSO 4·7H 2O[g/L] | 4.23 | 8.46 | 12.68 | 16.91 | 21.14 | 25.37 | 29.60 | 33.83 | 38.05 | 42.28 |
| NaOH[g/L] | 1.37 | 2.74 | 4.12 | 5.49 | 6.86 | 8.23 | 9.61 | 10.98 | 12.35 | 13.72 |
By form 0.5 gram Mg (OH) with laboratory scale
2/ 100 milliliters of decolorization experiments that extract carries out:
● 400 milliliters of dark brown extract from artichoke roots are warming up to 60 ℃, and under agitation with 8.4 gram MgSO
47H
2O is dissolved in wherein.
● to the NaOH that wherein adds 8.0 grams, 33% concentration, and with this mixture stirring 10 minutes.Obtain 9.7 pH value.
● with this mixture in beaker centrifuge at 5500g centrifugal 10 minutes.
● after this separates, obtain about 350 milliliters of extracts that water sample is limpid, this extract is lurid in 5 cm thick layer.As centrifugate, obtain 55.1 gram gel pills.
Embodiment 2-decolours with magnesium sulfate and calcium hydroxide
Form magnesium hydroxide according to following chemical formula with magnesium sulfate and calcium hydroxide:
MgSO
47H
2O+Ca (OH)
2→ Mg (OH)
2+ CaSO
4+ 7H
2O (Chemical formula 2)
Table 2 has shown bitter salt that the amount that forms per 100 milliliters of extract 0.1-10 gram magnesium hydroxide is required and the amount of calcium hydroxide.
Table 2: be used to form Mg (OH
2) the stoichiometric amount of reactant
| Mg(OH) 2[g/100ml] (theoretical value) | 0.10 | 0.20 | 0.30 | 0.40 | 0.50 | 0.60 | 0.70 | 0.80 | 0.90 | 1.00 |
| MgSO 4·7H 2O[g/L] | 4.23 | 8.46 | 12.68 | 16.91 | 21.14 | 25.37 | 29.60 | 33.83 | 38.05 | 42.28 |
| Ca(OH) 2[g/L] | 1.27 | 2.55 | 3.82 | 5.09 | 6.36 | 7.64 | 8.91 | 10.18 | 11.45 | 12.73 |
By form 0.5 gram Mg (OH) with laboratory scale
2/ 100 milliliters of decolorization experiments that extract carries out
● 400 milliliters of dark brown extract from artichoke roots are warming up to 60 ℃, and under agitation with 8.4 gram MgSO
47H
2O is dissolved in wherein.
● to wherein adding the Ca (OH) of 2.63 grams as 96% concentration of the suspension in 5 ml waters
2, and with this mixture stirring 10 minutes.Obtain 9.5 pH value.
● with this mixture in beaker centrifuge at 5500g centrifugal 10 minutes.
● after this separates, in 5 cm thick layer, obtain about 375 milliliters of extracts that light yellow water sample is limpid.As centrifugate, obtain 28.3 gram thick-pasty pellet.
Obvious relatively large centrifugation phase ratio during with use NaOH, the centrifugation thing of centrifugal rear small amount have clearly show and have used calcium hydroxide as the advantage (referring to embodiment 1 and 2) of alkali.Because precipitation (comparative chemistry formula 2) has realized the higher rate of settling and higher sediment compactibility in the time of magnesium hydroxide and calcium sulfate.Sedimentary gel-like consistency is less obvious.Therefore, purifying the loss of inulin that causes reduces.Under pilot-scale, can easily isolate sediment by disc separator.
Embodiment 3-0.7 restrains Mg (OH) by forming altogether under pilot-scale
2/ 100 milliliters of extracts and two stages of carrying out decolouring
● with 3400 gram MgSO
47H
2O (is equivalent to 0.5 gram Mg (OH)
2/ 100 milliliters of extracts) be dissolved in about 170 liters of dark brown extract from artichoke roots, and stirred 10 minutes.
● to wherein adding the Ca (OH) of 1015 grams as 96% concentration of the suspension in 3 premium on currency
2And stirred 10 minutes.Obtain 9.4 pH value.
● in disc separator, through 120 minutes whole precipitation mixture is quantitatively clarified.The extraction solution (150 liters) of decolouring does not have light yellow and does not have turbid material.As the sludge part, obtain the solid phase of 20 liters of thick-pasty.
● use gained to extract solution (150 liters), use 1350 gram MgSO
47H
2O (is equivalent to 0.2 gram Mg (OH)
2/ 100 milliliters of extracts) and 410 grams as the Ca (OH) of 96% concentration of suspension in 1.5 premium on currency
2Repeat whole decolouring step.
● in disc separator, through 30 minutes whole precipitation mixture is quantitatively clarified.PH value is that the extraction solution (145 liters) of 9.4 decolouring is that water sample is limpid, lurid and do not have a turbid material.As the sludge part, obtain the centrifugation thing of 7 liters of thick-pasty.
Claims (19)
1. the method for separating off coloring components from aqueous plant extracts comprises:
A) with magnesium ion (Mg
2+) add in the described plant extracts,
B) at least a basic component is added in the described plant extracts,
C) form sediment, and
D) from described plant extracts, isolate the sediment of formation,
The coloring components of wherein said plant extracts is tannic acid and/or flavonoids.
2. the method for claim 1, wherein step a) and b) under agitation carry out.
3. the method for claim 1 is wherein isolated the sediment of formation by sedimentation or filtration from described plant extracts.
4. method as claimed in claim 2 is wherein isolated the sediment of formation by sedimentation or filtration from described plant extracts.
5. such as each described method among the claim 1-4, wherein step a) in, add magnesium salts.
6. method as claimed in claim 5, wherein said magnesium salts is selected from magnesium chloride, magnesium sulfate, magnesium acetate and magnesium nitrate.
7. method as claimed in claim 5, wherein said magnesium salts is magnesium sulfate.
8. such as each described method among the claim 1-4, wherein step a) is carried out 60 to 80 ℃ temperature.
9. method as claimed in claim 5, wherein step a) is carried out 60 to 80 ℃ temperature.
10. such as each described method among the claim 1-4, wherein select the amount of basic component, thereby with mol ratio OH
-: Mg
2+Be set as 2.2: 1 to 1.8: 1.
11. such as each described method among the claim 1-4, wherein said basic component is the aqueous solution or the water slurry of alkali metal hydroxide or alkaline earth metal hydroxide.
12. method as claimed in claim 11, wherein said basic component are the suspension of calcium hydroxide.
13. such as each described method among the claim 1-4, wherein said basic component is ammoniacal liquor.
14. such as each described method among the claim 1-4, wherein said basic component is the aqueous solution or the water slurry of the salt of weak organic acid.
15. method as claimed in claim 14, wherein said salt are selected from alkali metal acetate and alkaline-earth metal acetate.
16. such as each described method among the claim 1-4, wherein said basic component is amine.
17. method as claimed in claim 16, wherein said amine are ethylenediamine or triethanolamine.
18. such as each described method among the claim 1-4, wherein said plant extracts is cynara scolymus extracts.
19. method as claimed in claim 18, wherein said cynara scolymus extracts are the extracts of artichoke roots.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP06090065.1 | 2006-04-28 | ||
| EP06090065 | 2006-04-28 | ||
| US79683806P | 2006-05-02 | 2006-05-02 | |
| US60/796,838 | 2006-05-02 | ||
| PCT/EP2007/004027 WO2007128558A1 (en) | 2006-04-28 | 2007-04-27 | Method for separating off coloring components from aqueous plant extracts |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101431906A CN101431906A (en) | 2009-05-13 |
| CN101431906B true CN101431906B (en) | 2013-01-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007800148134A Active CN101431906B (en) | 2006-04-28 | 2007-04-27 | Method for separating off coloring components from aqueous plant extracts |
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| Country | Link |
|---|---|
| CN (1) | CN101431906B (en) |
| AT (1) | ATE500750T1 (en) |
| BR (1) | BRPI0711067B1 (en) |
| DE (1) | DE602007013030D1 (en) |
| DK (1) | DK2015646T3 (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1816394A (en) * | 1929-02-09 | 1931-07-28 | Muller Oskar Albert | Process for working up materials containing lignin and cellulose |
| CN1740341A (en) * | 2005-09-15 | 2006-03-01 | 陈秀恋 | Decolour and refining apparatus for ion exchange method of sugar cane juice |
-
2007
- 2007-04-27 DK DK07724951.4T patent/DK2015646T3/en active
- 2007-04-27 CN CN2007800148134A patent/CN101431906B/en active Active
- 2007-04-27 AT AT07724951T patent/ATE500750T1/en not_active IP Right Cessation
- 2007-04-27 DE DE602007013030T patent/DE602007013030D1/en active Active
- 2007-04-27 BR BRPI0711067A patent/BRPI0711067B1/en active IP Right Grant
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1816394A (en) * | 1929-02-09 | 1931-07-28 | Muller Oskar Albert | Process for working up materials containing lignin and cellulose |
| CN1740341A (en) * | 2005-09-15 | 2006-03-01 | 陈秀恋 | Decolour and refining apparatus for ion exchange method of sugar cane juice |
Non-Patent Citations (2)
| Title |
|---|
| 等.镁盐对印染废水脱色处理研究.《工业水处理》.2002,(第6期),37－39. * |
| 路平 * |
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|---|---|
| ATE500750T1 (en) | 2011-03-15 |
| DK2015646T3 (en) | 2011-06-27 |
| BRPI0711067B1 (en) | 2016-05-17 |
| CN101431906A (en) | 2009-05-13 |
| DE602007013030D1 (en) | 2011-04-21 |
| BRPI0711067A2 (en) | 2011-08-23 |
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