CN111607249B - Preparation of organic plant dye and dyeing method thereof - Google Patents
Preparation of organic plant dye and dyeing method thereof Download PDFInfo
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- CN111607249B CN111607249B CN202010597804.XA CN202010597804A CN111607249B CN 111607249 B CN111607249 B CN 111607249B CN 202010597804 A CN202010597804 A CN 202010597804A CN 111607249 B CN111607249 B CN 111607249B
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- 238000000034 method Methods 0.000 title claims abstract description 60
- 238000004043 dyeing Methods 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000049 pigment Substances 0.000 claims abstract description 91
- 238000002414 normal-phase solid-phase extraction Methods 0.000 claims abstract description 87
- 238000000605 extraction Methods 0.000 claims abstract description 81
- 239000000047 product Substances 0.000 claims abstract description 45
- 238000002156 mixing Methods 0.000 claims abstract description 39
- 239000002904 solvent Substances 0.000 claims abstract description 35
- 239000000126 substance Substances 0.000 claims abstract description 34
- 238000001179 sorption measurement Methods 0.000 claims abstract description 33
- 230000000536 complexating effect Effects 0.000 claims abstract description 27
- 239000000284 extract Substances 0.000 claims abstract description 21
- 239000000706 filtrate Substances 0.000 claims abstract description 20
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 20
- 239000011707 mineral Substances 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 11
- 238000007873 sieving Methods 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 241000196324 Embryophyta Species 0.000 claims description 65
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 48
- 239000003208 petroleum Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- 235000010755 mineral Nutrition 0.000 claims description 19
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 18
- 238000003795 desorption Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000004744 fabric Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 235000013311 vegetables Nutrition 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 9
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 9
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 9
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 8
- 239000012752 auxiliary agent Substances 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- 239000004902 Softening Agent Substances 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 229930003935 flavonoid Natural products 0.000 claims description 7
- 235000017173 flavonoids Nutrition 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 229940037003 alum Drugs 0.000 claims description 6
- -1 flavonoid compounds Chemical class 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- 210000002268 wool Anatomy 0.000 claims description 4
- 244000144730 Amygdalus persica Species 0.000 claims description 3
- 235000006040 Prunus persica var persica Nutrition 0.000 claims description 3
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- 235000009984 Pterocarpus indicus Nutrition 0.000 claims description 3
- 229910000366 copper(II) sulfate Inorganic materials 0.000 claims description 3
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 3
- 235000018553 tannin Nutrition 0.000 claims description 3
- 239000001648 tannin Substances 0.000 claims description 3
- 229920001864 tannin Polymers 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- 235000016068 Berberis vulgaris Nutrition 0.000 claims description 2
- 241000335053 Beta vulgaris Species 0.000 claims description 2
- 235000011511 Diospyros Nutrition 0.000 claims description 2
- 244000157072 Hylocereus undatus Species 0.000 claims description 2
- 235000018481 Hylocereus undatus Nutrition 0.000 claims description 2
- 241000209035 Ilex Species 0.000 claims description 2
- 235000010254 Jasminum officinale Nutrition 0.000 claims description 2
- 240000005385 Jasminum sambac Species 0.000 claims description 2
- 240000000249 Morus alba Species 0.000 claims description 2
- 235000008708 Morus alba Nutrition 0.000 claims description 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 claims description 2
- 235000011613 Pinus brutia Nutrition 0.000 claims description 2
- 241000018646 Pinus brutia Species 0.000 claims description 2
- 244000294611 Punica granatum Species 0.000 claims description 2
- 235000014360 Punica granatum Nutrition 0.000 claims description 2
- 244000269722 Thea sinensis Species 0.000 claims description 2
- 240000007124 Brassica oleracea Species 0.000 claims 1
- 235000003899 Brassica oleracea var acephala Nutrition 0.000 claims 1
- 235000012905 Brassica oleracea var viridis Nutrition 0.000 claims 1
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- 235000015655 Crocus sativus Nutrition 0.000 claims 1
- 241000723267 Diospyros Species 0.000 claims 1
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- 235000002296 Ilex sandwicensis Nutrition 0.000 claims 1
- 235000002294 Ilex volkensiana Nutrition 0.000 claims 1
- 240000002853 Nelumbo nucifera Species 0.000 claims 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 claims 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 claims 1
- 241000123069 Ocyurus chrysurus Species 0.000 claims 1
- 235000004789 Rosa xanthina Nutrition 0.000 claims 1
- 241000109329 Rosa xanthina Species 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000004753 textile Substances 0.000 abstract description 5
- 239000000975 dye Substances 0.000 description 49
- 230000000052 comparative effect Effects 0.000 description 12
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- 239000003795 chemical substances by application Substances 0.000 description 5
- 235000013399 edible fruits Nutrition 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 229920000742 Cotton Polymers 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
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- 244000236655 Diospyros kaki Species 0.000 description 2
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 description 2
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- 238000001502 gel electrophoresis Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
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- NPHULPIAPWNOOH-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-3-(2,3-dihydroindol-1-ylmethyl)pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C(=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2)CN1CCC2=CC=CC=C12 NPHULPIAPWNOOH-UHFFFAOYSA-N 0.000 description 1
- HVTQDSGGHBWVTR-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-3-phenylmethoxypyrazol-1-yl]-1-morpholin-4-ylethanone Chemical compound C(C1=CC=CC=C1)OC1=NN(C=C1C=1C=NC(=NC=1)NC1CC2=CC=CC=C2C1)CC(=O)N1CCOCC1 HVTQDSGGHBWVTR-UHFFFAOYSA-N 0.000 description 1
- VXZBYIWNGKSFOJ-UHFFFAOYSA-N 2-[4-[5-(2,3-dihydro-1H-inden-2-ylamino)pyrazin-2-yl]pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC=1N=CC(=NC=1)C=1C=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2 VXZBYIWNGKSFOJ-UHFFFAOYSA-N 0.000 description 1
- 240000005020 Acaciella glauca Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 235000007516 Chrysanthemum Nutrition 0.000 description 1
- 244000189548 Chrysanthemum x morifolium Species 0.000 description 1
- XDVZNDLANFJOQR-UHFFFAOYSA-N Coptisine Natural products O=Cc1c2OCOc2ccc1C=C3/NCCc4cc5OCOc5cc34 XDVZNDLANFJOQR-UHFFFAOYSA-N 0.000 description 1
- SEBIKDIMAPSUBY-ARYZWOCPSA-N Crocin Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)OC(=O)C(C)=CC=CC(C)=C\C=C\C=C(/C)\C=C\C=C(C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)O1)O)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O SEBIKDIMAPSUBY-ARYZWOCPSA-N 0.000 description 1
- 235000008597 Diospyros kaki Nutrition 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 235000003325 Ilex Nutrition 0.000 description 1
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- 241000972673 Phellodendron amurense Species 0.000 description 1
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- 240000003582 Platycodon grandiflorus Species 0.000 description 1
- 241000209504 Poaceae Species 0.000 description 1
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 description 1
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
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- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
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- 235000019864 coconut oil Nutrition 0.000 description 1
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- XYHOBCMEDLZUMP-UHFFFAOYSA-N coptisine Chemical compound C1=C2C=C(C3=C(C=C4OCOC4=C3)CC3)[N+]3=CC2=C2OCOC2=C1 XYHOBCMEDLZUMP-UHFFFAOYSA-N 0.000 description 1
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- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 1
- 235000012680 lutein Nutrition 0.000 description 1
- 239000001656 lutein Substances 0.000 description 1
- KBPHJBAIARWVSC-RGZFRNHPSA-N lutein Chemical compound C([C@H](O)CC=1C)C(C)(C)C=1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\[C@H]1C(C)=C[C@H](O)CC1(C)C KBPHJBAIARWVSC-RGZFRNHPSA-N 0.000 description 1
- 229960005375 lutein Drugs 0.000 description 1
- ORAKUVXRZWMARG-WZLJTJAWSA-N lutein Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=CC(O)CC2(C)C)C ORAKUVXRZWMARG-WZLJTJAWSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 235000005875 quercetin Nutrition 0.000 description 1
- 229960001285 quercetin Drugs 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000003499 redwood Nutrition 0.000 description 1
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- 238000011069 regeneration method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- KBPHJBAIARWVSC-XQIHNALSSA-N trans-lutein Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CC(O)CC1(C)C)C=CC=C(/C)C=CC2C(=CC(O)CC2(C)C)C KBPHJBAIARWVSC-XQIHNALSSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- FJHBOVDFOQMZRV-XQIHNALSSA-N xanthophyll Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CC(O)CC1(C)C)C=CC=C(/C)C=CC2C=C(C)C(O)CC2(C)C FJHBOVDFOQMZRV-XQIHNALSSA-N 0.000 description 1
- 239000001052 yellow pigment Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B68/00—Organic pigments surface-modified by grafting, e.g. by establishing covalent or complex bonds, in order to improve the pigment properties, e.g. dispersibility or rheology
- C09B68/20—Organic pigments surface-modified by grafting, e.g. by establishing covalent or complex bonds, in order to improve the pigment properties, e.g. dispersibility or rheology characterised by the process features
- C09B68/28—Complexing
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/34—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using natural dyestuffs
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/653—Nitrogen-free carboxylic acids or their salts
- D06P1/6533—Aliphatic, araliphatic or cycloaliphatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/673—Inorganic compounds
- D06P1/67333—Salts or hydroxides
- D06P1/6735—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Inorganic Chemistry (AREA)
- Coloring (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a preparation method of an organic plant dye and a dyeing method thereof, wherein the preparation method comprises the following steps: (1) mixing the extraction raw materials with a solvent, preserving heat, and performing countercurrent extraction; (2) performing centrifugal separation on the primary extract to obtain a first filtrate, and performing adsorption treatment on the first filtrate under ultrasonic waves; (3) respectively returning the first filter residue and the first effluent to countercurrent extraction equipment for countercurrent extraction, and then treating according to the step (2); (4) treating the second filter residue and the second effluent according to the step (3); respectively desorbing the three solid phase extraction columns; (5) conveying the pigment extracting solution into a vacuum reaction kettle, adding mineral substances and organic substances, and stirring and complexing; (6) and drying, sieving and grinding the complex primary product for 3-10 h. The preparation method has the characteristics of high pigment extraction rate, low solvent consumption, low energy consumption, high yield and high quality, the obtained dye can improve the color fastness of textiles, and the energy consumption and the production cost of the dyeing method are low.
Description
Technical Field
The invention relates to the technical field of dye extraction and dyeing, in particular to a preparation method and a dyeing method of an organic vegetable dye.
Background
At present, the application of dyes is very wide and is an indispensable part in modern life, but substances which cause serious harm to human bodies and the environment, such as chromium, arsenic, twenty-four aromatic amines and the like, exist in the chemical dye technology, and the dyes have the defects of complex synthesis process, high production cost, great environmental pollution and the like.
The organic plant dye is pigment extracted from flowers, grasses, trees, stems, leaves, fruits, seeds, peels, roots and the like in the nature, for example, leftover materials and wood chips after the production of redwood furniture are rich in a large amount of polyphenol pigment, has the advantages of no toxicity, no harm, no pollution, reproducibility and the like, is used for dyeing textiles, can improve the secondary and additional values, and realizes ecological protection on the environment, so that how to extract the natural plant pigment and obtain the organic plant dye which realizes zero emission, zero pollution and good color fastness is a problem which is urgently needed to be solved at present.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of an organic vegetable dye and a dyeing method thereof, wherein the preparation method has the characteristics of high pigment extraction rate, low solvent consumption, low energy consumption, high yield and high quality, the obtained dye can obviously improve the color fastness of textiles when used for dyeing, and the dyeing method is practical and easy to implement, greatly reduces the energy consumption and saves the production cost.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an organic plant dye comprises the following steps:
(1) mixing the components in a mass ratio of 1: 3, mixing the extraction raw material and the solvent in a countercurrent extraction device, heating to 40-95 ℃, preserving heat for 1h, and then carrying out countercurrent extraction to obtain a primary extract;
(2) carrying out centrifugal separation on the primary extract to obtain a first filtrate and a first filter residue, and carrying out adsorption treatment on the first filtrate by a first solid-phase extraction column under an ultrasonic state to obtain a first effluent;
(3) respectively returning the first filter residue and the first effluent to a countercurrent extraction device, carrying out countercurrent extraction again at 40-95 ℃, then treating according to the method in the step (2) to obtain a second filter residue and a second effluent, and carrying out adsorption treatment by using a second solid-phase extraction column in the step;
(4) treating the second filter residue and the second effluent according to the method in the step (3) to obtain a third filter residue and a third effluent, wherein the third effluent is used as a solvent for next pigment extraction and is kept for standby application, and in the step, a third solid-phase extraction column is used for adsorption treatment; respectively carrying out desorption treatment on the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column by using petroleum ether, and then mixing liquids obtained by desorption to obtain a pigment extracting solution;
(5) conveying the pigment extracting solution into a vacuum reaction kettle, adding mineral substances and organic substances, uniformly stirring, complexing at 60-90 ℃ for 2 hours, vacuumizing to remove petroleum ether after complexing is finished, and obtaining a complex primary product, wherein the using amounts of the mineral substances and the organic substances are 0.1-10% and 10-30% of the mass of the pigment extracting solution respectively;
(6) and drying the complex primary product at 65-85 ℃, sieving the product by a 325-mesh sieve, and conveying the product to a nano grinder for grinding for 3-10 h to obtain the nano organic plant dye.
The first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column are all prepared by mixing and filling alkaline alumina and kieselguhr according to the mass ratio of 1: 1.5.
The extraction raw material is plant root, stem, leaf, flower, fruit or rosewood sawdust. Wherein the plant root, stem, leaf, and fruit include folium Ilicis Pubescentis, folium Mori, folium Pini, folium Camelliae sinensis, fructus kaki, dragon fruit peel, pericarpium Granati, Carthami flos, stigma croci Sativi, flos Rosae Rugosae, radix Rubiae, radix Arnebiae, folium Isatidis, folium Nelumbinis, flos Jasmini sambac, caulis et folium Ipomoeae, and petiolus Citri Tangerinae.
The solvent is ethanol or deionized water or sodium bicarbonate solution with the concentration of 0.5 g/L.
The mineral is selected from one of alum, blue vitriol, titanium dioxide and magnesium oxide, and the organic is selected from one of tannin, peach gum, acetic acid and flavonoid compounds. Wherein the flavonoids include gardenia yellow pigment, chrysanthemum yellow pigment, coptisin, phellodendron amurense, quercetin, lutein, etc.
In the step (5), the pigment extracting solution is conveyed to a vacuum reaction kettle and then is subjected to heat preservation for 3-8 hours, so that the complexing rate of the pigment, mineral substances and organic substances can be improved.
The pigment extraction purity has an important influence on the subsequent pigment complexing yield, and the pigment extraction method comprises gel electrophoresis separation, resin separation and purification, membrane separation, countercurrent extraction and other methods, but the gel electrophoresis separation is suitable for the condition of small laboratory treatment capacity, and the industrial production can adopt the resin separation and purification and the membrane separation technology, but the resin separation and purification has the defects of difficult regeneration, more generated waste deionized water, and larger membrane separation investment in the early stage, while the traditional countercurrent extraction has the problems of large solvent consumption, low extraction rate, large energy consumption in the subsequent concentration process and the like. Therefore, the method adopts the method of combining countercurrent extraction and physical adsorption to extract the pigment, reduces the dosage of the solvent, improves the extraction rate of the pigment, omits the subsequent concentration process and reduces the energy consumption.
In the step (1), the solubility of the plant pigment is improved by heat preservation, particularly the solubility of lipophilic pigment in hot deionized water can be improved, and in addition, when sodium bicarbonate solution is used as a solvent, the sodium bicarbonate solution can promote the dissolution rate of the plant pigment, accelerate the extraction of the pigment and can also carry out extraction in a low-temperature environment.
Separating the filter residue containing impurities and the pigment dissolved in the solvent by the centrifugal separation operation in the step (2) because the initial extract obtained in the step (1) still contains the impurities such as fiber, protein and the like; the first solid phase extraction column can adsorb the pigment dissolved in the solvent, so that the solvent and the pigment are separated, the solvent can be recycled, and the dosage of the solvent is reduced; the first solid phase extraction column takes alkaline alumina and diatomite as fillers, so that the first solid phase extraction column can adsorb hydrophilic and lipophilic pigments at the same time, the pure pigments are collected in the solid phase extraction column completely and intensively, and the extraction method is favorable for reducing energy consumption; in addition, the adsorption capacity of the solid phase extraction column can be promoted by ultrasonic-assisted adsorption, because the activity of the adsorbent is increased by the interface effect of an ultrasonic field, and the diffusion of the pigment is enhanced.
Through the gradual operation of step (3) and step (4), can fully gather the pigment that remains in the filter residue in each step on the one hand, guarantee the purity of the pigment of adsorbing on the extraction column, improve the extraction yield, on the other hand, can retrieve the solvent again and use repeatedly, greatly reduced the consumption of solvent, also there is not the discharge problem of solvent, reduce environmental pollution.
In the step (5), the vegetable pigment is eluted by petroleum ether, on one hand, the vegetable pigment is eluted by the petroleum ether on the basis of the consideration that hydrophilic water pigment and lipophilic pigment can be eluted by the petroleum ether and the elution effect is good, on the other hand, the boiling point of the petroleum ether is 90-120 ℃ and is easy to volatilize, the liquid can still be kept when the pigment is complexed with mineral substances and organic substances, the complexing rate is ensured, and after the complexing, the vegetable pigment can be directly removed and recycled through extraction, so that the solvent concentration process in the traditional countercurrent extraction is omitted, and the energy consumption is greatly reduced.
A dyeing method of organic plant dye comprises the following steps of dyeing a fabric to be dyed according to a bath ratio of 1: 10 adding the mixture into a loose wool dyeing machine, heating to 60 ℃, adding the prepared organic plant dye and the auxiliary agent, and keeping the temperature for 20min, wherein the use amounts of the organic plant dye and the auxiliary agent are respectively 8% and 6% of the mass of the fabric to be dyed; adding organic acid to adjust pH to 5, heating to 95 deg.C at a rate of 1 deg.C/min, maintaining for 20min, adding softening agent, maintaining for 20min, and discharging deionized water when the temperature is increased to room temperature, wherein the amount of the softening agent is 1.8% of the amount of the dye.
The auxiliary agent is anhydrous sodium sulphate, and the organic acid is citric acid.
The bath ratio is 1: 10, dyeing cotton fabrics by using a traditional organic plant dye method, wherein the traditional organic plant dye method comprises the following steps: and (3) mixing the fabric to be dyed according to the bath ratio of 1: 10 adding the mixture into a loose wool dyeing machine, adding a dyeing pretreatment agent with the dosage of 20% of the fabric to be dyed, heating to 100 ℃, preserving the temperature for 90min, and discharging deionized water; washing with deionized water for 2 times, adding dye, dyeing auxiliary agent and deionized water with the same mass as that of the cotton fabric, wherein the use amounts of the dye and the auxiliary agent are respectively 8% and 10% of the mass of the fabric to be dyed, and discharging the deionized water after heat preservation at 100 ℃ for 60 min; then washing for 3-5 times by using deionized water, adding a color fixing agent, keeping the temperature at 65 ℃ for 20min, and discharging the deionized water, wherein the dosage of the color fixing agent is 1.6% of that of the dye; and finally adding a softening agent, keeping the temperature at 45 ℃ for 20min, discharging deionized water again, removing the deionized water, and drying to obtain the dyed fabric.
Compared with the traditional method, the dyeing method of the invention omits the repeated operations of temperature rise, heat preservation and water washing, thereby greatly reducing the energy consumption and saving the production cost. Like dyeing 100kg cotton fabric, the traditional method is adopted, deionized water is used for at least 1 ton, steam is used for 5 tons, electricity is used for 400 degrees, and labor cost is 700 yuan/ton, while the method of the invention is adopted, the dosage of the deionized water is about 150kg, steam is used for 2.6 tons, electricity is used for 150 degrees, and labor cost is 200 yuan/ton.
The invention has the beneficial effects that:
(1) the plant pigment is dissolved by alcohol, deionized water or sodium bicarbonate solution under heating, especially the sodium bicarbonate solution can accelerate extraction speed and can extract at low temperature, thus realizing primary extraction of the plant pigment.
(2) Through step-by-step repeated filter residue and steps such as filtrating centrifugal separation, phytochrome ultrasonic adsorption, dissolving reflux, countercurrent extraction, make the pigment that remains in the filter residue in each step carry out abundant collection on the one hand and get, guarantee the pigment purity of absorption on the extraction column, improved and extracted purity, and then improve the end product income, on the other hand can retrieve the solvent again and use repeatedly, the consumption of the solvent that has significantly reduced also does not have the discharge problem of solvent, does not have environmental pollution.
(3) The extracted plant pigment is complexed by mineral substances and organic substances, so that the stability of the product can be improved, and the color fastness of the textile fabric is improved.
(4) The petroleum ether is used for eluting the plant pigment, so that the complexing rate of the pigment, mineral substances and organic matters can be ensured, the complex can be directly removed by vacuumizing for recycling, the solvent concentration process in the traditional countercurrent extraction is omitted, and the energy consumption is greatly reduced.
(5) The dyeing process is improved, the plant pigment extracted from the plant is used for dyeing, the obtained textile does not harm human bodies, and meanwhile, the fabric can also have the performances of resisting bacteria and inflammation, resisting ultraviolet radiation, protecting skin and the like; in addition, the process can also greatly reduce energy consumption and save production cost.
Detailed Description
The invention is further described below with reference to specific embodiments:
example 1
The preparation method of the organic plant dye comprises the following steps:
(1) mixing the components in a mass ratio of 1: 3, mixing the plant leaves and the ethanol in a countercurrent extraction device, heating to 70 ℃, preserving the heat for 1h, and then carrying out countercurrent extraction to obtain a primary extract; the plant leaves are selected from tea leaves or Chinese ilex leaves or mulberry leaves or pine needles and the like;
(2) carrying out centrifugal separation on the primary extract to obtain a first filtrate and a first filter residue, and carrying out adsorption treatment on the first filtrate by a first solid-phase extraction column under an ultrasonic state to obtain a first effluent;
(3) respectively returning the first filter residue and the first effluent to a countercurrent extraction device, carrying out countercurrent extraction again at 70 ℃, then treating according to the method in the step (2) to obtain a second filter residue and a second effluent, and carrying out adsorption treatment by using a second solid-phase extraction column in the step;
(4) treating the second filter residue and the second effluent according to the method in the step (3) to obtain a third filter residue and a third effluent, wherein the third effluent is used as a solvent for next pigment extraction and is kept for standby application, and in the step, a third solid-phase extraction column is used for adsorption treatment; respectively carrying out desorption treatment on the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column by using petroleum ether, and then mixing liquids obtained by desorption to obtain a pigment extracting solution; the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column are all prepared by mixing and filling alkaline alumina and kieselguhr according to the mass ratio of 1: 1.5.
(5) Conveying the pigment extracting solution into a vacuum reaction kettle, preserving the heat of the pigment extracting solution for 5 hours, adding alum and tannin, uniformly stirring, complexing at 70 ℃ for 2 hours, vacuumizing to remove petroleum ether after complexing is finished, and obtaining a complex primary product, wherein the using amounts of mineral substances and organic substances are 4% and 20% of the mass of the pigment extracting solution respectively;
(6) and drying the complex primary product at 65 ℃, sieving the product by a 325-mesh sieve, and conveying the product to a nano grinder for grinding for 10 hours to obtain the nano organic plant dye.
A dyeing method of organic plant dye comprises the following steps of dyeing a fabric to be dyed according to a bath ratio of 1: 10 adding the mixture into a loose wool dyeing machine, heating to 60 ℃, adding the prepared organic plant dye and anhydrous sodium sulphate, and keeping the temperature for 20min, wherein the use amounts of the organic plant dye and the anhydrous sodium sulphate are respectively 8% and 6% of the mass of the fabric to be dyed; adding citric acid to adjust pH to 5, heating to 95 deg.C at a rate of 1 deg.C/min, maintaining for 20min, adding a softening agent, maintaining for 20min, and discharging deionized water when the temperature is increased to room temperature, wherein the amount of the softening agent is 1.8% of the dye.
The soft and solid agent is prepared by the following method: (a) 0.1kg of alum, 1kg of stearic acid and 60kg of deionized water are poured into a reaction kettle; raising the temperature by 1 ℃ per minute, stirring while raising the temperature, stopping heating when the temperature is raised to 80 ℃, and preserving the heat for 20 minutes; (b) after the heat preservation is finished, pouring 3kg of coconut oil amide, 3kg of palm wax, 1kg of glycerol, 3kg of glucose and 300kg of deionized water into the reaction kettle; stirring uniformly, keeping the temperature at 80 ℃, and keeping the temperature for 100 minutes; (c) after the heat preservation in the step (b) is finished, completely emulsifying the materials in the reaction kettle into mercerized bright thick liquid; and (5) placing the mixture at normal temperature to reduce the temperature to obtain the softening and solidifying agent.
Example 2
The preparation method of the organic plant dye comprises the following steps:
(1) mixing the components in a mass ratio of 1: 3, mixing the plant fruits and the deionized water in a countercurrent extraction device, heating to 60 ℃, preserving heat for 1h, and then carrying out countercurrent extraction to obtain a primary extract; the plant fruit is selected from pomegranate pericarp or persimmon or dragon pericarp, etc.;
(2) carrying out centrifugal separation on the primary extract to obtain a first filtrate and a first filter residue, and carrying out adsorption treatment on the first filtrate by a first solid-phase extraction column under an ultrasonic state to obtain a first effluent;
(3) respectively returning the first filter residue and the first effluent to a countercurrent extraction device, carrying out countercurrent extraction again at 60 ℃, then treating according to the method in the step (2) to obtain a second filter residue and a second effluent, and carrying out adsorption treatment by using a second solid-phase extraction column in the step;
(4) treating the second filter residue and the second effluent according to the method in the step (3) to obtain a third filter residue and a third effluent, wherein the third effluent is used as a solvent for next pigment extraction and is kept for standby application, and in the step, a third solid-phase extraction column is used for adsorption treatment; respectively carrying out desorption treatment on the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column by using petroleum ether, and then mixing liquids obtained by desorption to obtain a pigment extracting solution; the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column are all prepared by mixing and filling alkaline alumina and kieselguhr according to the mass ratio of 1: 1.5.
(5) And conveying the pigment extracting solution into a vacuum reaction kettle, and keeping the temperature of the pigment extracting solution for 6 hours. Adding magnesium oxide and peach gum, stirring, complexing at 80 deg.C for 2 hr, vacuumizing to remove petroleum ether to obtain complex primary product, wherein the amount of mineral and organic substances is 0.1% and 130% of the pigment extractive solution;
(6) and drying the complex primary product at 70 ℃, sieving the product by a 325-mesh sieve, and conveying the product to a nano grinder for grinding for 6 hours to obtain the nano organic plant dye.
A method for dyeing an organic plant dye, which comprises the following steps of example 1.
Example 3
The preparation method of the organic plant dye comprises the following steps:
(1) mixing the components in a mass ratio of 1: 3, mixing the rosewood sawdust and a sodium bicarbonate solution with the concentration of 0.5g/L in a countercurrent extraction device, heating to 50 ℃, preserving the heat for 1h, and then carrying out countercurrent extraction to obtain a primary extract;
(2) carrying out centrifugal separation on the primary extract to obtain a first filtrate and a first filter residue, and carrying out adsorption treatment on the first filtrate by a first solid-phase extraction column under an ultrasonic state to obtain a first effluent;
(3) respectively returning the first filter residue and the first effluent to a countercurrent extraction device, carrying out countercurrent extraction again at 50 ℃, then treating according to the method in the step (2) to obtain a second filter residue and a second effluent, and carrying out adsorption treatment by using a second solid-phase extraction column in the step;
(4) treating the second filter residue and the second effluent according to the method in the step (3) to obtain a third filter residue and a third effluent, wherein the third effluent is used as a solvent for next pigment extraction and is kept for standby application, and in the step, a third solid-phase extraction column is used for adsorption treatment; respectively carrying out desorption treatment on the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column by using petroleum ether, and then mixing liquids obtained by desorption to obtain a pigment extracting solution; the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column are all prepared by mixing and filling alkaline alumina and kieselguhr according to the mass ratio of 1: 1.5.
(5) And conveying the pigment extracting solution into a vacuum reaction kettle, and preserving the temperature of the pigment extracting solution for 3 hours. Adding alum and flavonoid compounds, uniformly stirring, complexing at 60 ℃ for 2h, vacuumizing to remove petroleum ether after complexing is finished, and obtaining a complex primary product, wherein the using amounts of mineral substances and organic substances are 8% and 12% of the mass of the pigment extracting solution respectively;
(6) and drying the complex primary product at 80 ℃, sieving the product by a 325-mesh sieve, and conveying the product to a nano grinder for grinding for 3 hours to obtain the nano organic plant dye.
A method for dyeing an organic plant dye, which comprises the following steps of example 1.
Example 4
The preparation method of the organic plant dye comprises the following steps:
(1) mixing the components in a mass ratio of 1: 3, mixing the plant roots with a sodium bicarbonate solution with the concentration of 0.5g/L in a countercurrent extraction device, heating to 40 ℃, preserving heat for 1h, and then carrying out countercurrent extraction to obtain a primary extract; the plant root is selected from radix Rubiae;
(2) carrying out centrifugal separation on the primary extract to obtain a first filtrate and a first filter residue, and carrying out adsorption treatment on the first filtrate by a first solid-phase extraction column under an ultrasonic state to obtain a first effluent;
(3) respectively returning the first filter residue and the first effluent to a countercurrent extraction device, carrying out countercurrent extraction again at 40 ℃, then treating according to the method in the step (2) to obtain a second filter residue and a second effluent, and carrying out adsorption treatment by using a second solid-phase extraction column in the step;
(4) treating the second filter residue and the second effluent according to the method in the step (3) to obtain a third filter residue and a third effluent, wherein the third effluent is used as a solvent for next pigment extraction and is kept for standby application, and in the step, a third solid-phase extraction column is used for adsorption treatment; respectively carrying out desorption treatment on the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column by using petroleum ether, and then mixing liquids obtained by desorption to obtain a pigment extracting solution; the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column are all prepared by mixing and filling alkaline alumina and kieselguhr according to the mass ratio of 1: 1.5.
(5) And conveying the pigment extracting solution into a vacuum reaction kettle, and keeping the temperature of the pigment extracting solution for 6 hours. Adding blue vitriol and acetic acid, stirring, complexing at 70 deg.C for 2 hr, vacuumizing to remove petroleum ether to obtain complex primary product, wherein the amount of mineral and organic substances is 10% and 10% of the pigment extractive solution;
(6) and drying the complex primary product at 85 ℃, sieving the product by a 325-mesh sieve, and conveying the product to a nano grinder for grinding for 8 hours to obtain the nano organic plant dye.
A method for dyeing an organic plant dye, which comprises the following steps of example 1.
Example 5
The preparation method of the organic plant dye comprises the following steps:
(1) mixing the components in a mass ratio of 1: 3, mixing the plant leaves and the ethanol in a countercurrent extraction device, heating to 77 ℃, preserving heat for 1h, and then carrying out countercurrent extraction to obtain a primary extract; the plant leaf is selected from herba Kalimeridis leaf or folium Isatidis or folium Nelumbinis;
(2) carrying out centrifugal separation on the primary extract to obtain a first filtrate and a first filter residue, and carrying out adsorption treatment on the first filtrate by a first solid-phase extraction column under an ultrasonic state to obtain a first effluent;
(3) respectively returning the first filter residue and the first effluent to a countercurrent extraction device, carrying out countercurrent extraction again at 77 ℃, then treating according to the method in the step (2) to obtain a second filter residue and a second effluent, wherein in the step, a second solid-phase extraction column is used for adsorption treatment;
(4) treating the second filter residue and the second effluent according to the method in the step (3) to obtain a third filter residue and a third effluent, wherein the third effluent is used as a solvent for next pigment extraction and is kept for standby application, and in the step, a third solid-phase extraction column is used for adsorption treatment; respectively carrying out desorption treatment on the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column by using petroleum ether, and then mixing liquids obtained by desorption to obtain a pigment extracting solution; the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column are all prepared by mixing and filling alkaline alumina and kieselguhr according to the mass ratio of 1: 1.5.
(5) And conveying the pigment extracting solution into a vacuum reaction kettle, and preserving the temperature of the pigment extracting solution for 7 hours. Adding titanium dioxide and flavonoid compounds, uniformly stirring, complexing at 80 ℃ for 2h, vacuumizing to remove petroleum ether after complexing is finished, and obtaining a complex primary product, wherein the using amounts of mineral substances and organic substances are 5% and 15% of the mass of the pigment extracting solution respectively;
(6) and drying the complex primary product at 80 ℃, sieving the product by a 325-mesh sieve, and conveying the product to a nano grinder for grinding for 5 hours to obtain the nano organic plant dye.
A method for dyeing an organic plant dye, which comprises the following steps of example 1.
Example 6
The preparation method of the organic plant dye comprises the following steps:
(1) mixing the components in a mass ratio of 1: 3, mixing the plant flowers and the deionized water in a countercurrent extraction device, heating to 95 ℃, preserving heat for 1h, and then carrying out countercurrent extraction to obtain a primary extract; the plant flower is selected from Carthami flos or stigma croci Sativi or flos Rosae Rugosae;
(2) carrying out centrifugal separation on the primary extract to obtain a first filtrate and a first filter residue, and carrying out adsorption treatment on the first filtrate by a first solid-phase extraction column under an ultrasonic state to obtain a first effluent;
(3) respectively returning the first filter residue and the first effluent to a countercurrent extraction device, carrying out countercurrent extraction again at 95 ℃, then treating according to the method in the step (2) to obtain a second filter residue and a second effluent, and carrying out adsorption treatment by using a second solid-phase extraction column in the step;
(4) treating the second filter residue and the second effluent according to the method in the step (3) to obtain a third filter residue and a third effluent, wherein the third effluent is used as a solvent for next pigment extraction and is kept for standby application, and in the step, a third solid-phase extraction column is used for adsorption treatment; respectively carrying out desorption treatment on the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column by using petroleum ether, and then mixing liquids obtained by desorption to obtain a pigment extracting solution; the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column are all prepared by mixing and filling alkaline alumina and kieselguhr according to the mass ratio of 1: 1.5.
(5) And conveying the pigment extracting solution into a vacuum reaction kettle, and keeping the temperature of the pigment extracting solution for 8 hours. Adding magnesium oxide and flavonoid compounds, uniformly stirring, complexing at 90 deg.C for 2 hr, vacuumizing to remove petroleum ether to obtain complex primary product, wherein the amount of mineral and organic substances is 1% and 25% of the pigment extractive solution;
(6) and drying the complex primary product at 85 ℃, sieving the product by a 325-mesh sieve, and conveying the product to a nano grinder for grinding for 4 hours to obtain the nano organic plant dye.
A method for dyeing an organic plant dye, which comprises the following steps of example 1.
Example 7
The preparation method of the organic plant dye comprises the following steps:
(1) mixing the components in a mass ratio of 1: 3, mixing the plant stems with the sodium bicarbonate solution in a countercurrent extraction device, heating to 90 ℃, preserving heat for 1h, and then carrying out countercurrent extraction to obtain a primary extract; the plant stem is selected from jasmine flower diameter, beet stem or balloonflower stem;
(2) carrying out centrifugal separation on the primary extract to obtain a first filtrate and a first filter residue, and carrying out adsorption treatment on the first filtrate by a first solid-phase extraction column under an ultrasonic state to obtain a first effluent;
(3) respectively returning the first filter residue and the first effluent to a countercurrent extraction device, carrying out countercurrent extraction again at 90 ℃, then treating according to the method in the step (2) to obtain a second filter residue and a second effluent, and carrying out adsorption treatment by using a second solid-phase extraction column in the step;
(4) treating the second filter residue and the second effluent according to the method in the step (3) to obtain a third filter residue and a third effluent, wherein the third effluent is used as a solvent for next pigment extraction and is kept for standby application, and in the step, a third solid-phase extraction column is used for adsorption treatment; respectively carrying out desorption treatment on the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column by using petroleum ether, and then mixing liquids obtained by desorption to obtain a pigment extracting solution; the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column are all prepared by mixing and filling alkaline alumina and kieselguhr according to the mass ratio of 1: 1.5.
(5) And conveying the pigment extracting solution into a vacuum reaction kettle, and keeping the temperature of the pigment extracting solution for 8 hours. Adding alum and flavonoid compounds, uniformly stirring, complexing at 88 ℃ for 2h, vacuumizing to remove petroleum ether after complexing is finished, and obtaining a complex primary product, wherein the using amounts of mineral substances and organic substances are 5% and 22% of the mass of the pigment extracting solution respectively;
(6) and drying the complex primary product at 85 ℃, sieving the product by a 325-mesh sieve, and conveying the product to a nano grinder for grinding for 4 hours to obtain the nano organic plant dye.
A method for dyeing an organic plant dye, which comprises the following steps of example 1.
Comparative examples 1 to 7
According to the types and the amounts of the extraction raw materials and the solvents corresponding to the embodiments 1 to 7, the extraction raw materials and the solvents are conveyed to a countercurrent extraction device to be mixed, the temperature is raised to the same heat preservation temperature corresponding to the embodiments 1 to 7 and is kept for 1 hour, then, the countercurrent extraction is carried out for 3 times to obtain pigment extracting solution, the pigment extracting solution is conveyed to a vacuum reaction kettle, the mineral substances and the organic substances corresponding to the embodiments 1 to 7 are added, the mixture is uniformly stirred and then concentrated, then, the complexing is carried out for 2 hours at the temperature corresponding to the embodiments 1 to 7, after the complexing is finished, the solvents are drained to obtain a complexing primary product, the complexing primary product is dried at the temperature corresponding to the embodiments 1 to 7, the complexing primary product is sieved by a 325-mesh sieve and conveyed to a nanometer grinder to be ground for corresponding time, and the nanoscale organic plant dye is also obtained.
The yields of the organic plant dyes obtained in examples 1-7 and comparative examples 1-7 are weighed and calculated, and as shown in table 1, the results show that the product yields in examples 1-7 are all higher than those in comparative examples 1-7, which shows that the extraction rate of the plant pigment is improved by the method of combining physical adsorption and countercurrent extraction, and further the yield of the final product is improved.
TABLE 1
Comparative examples 8 to 14
Preparing pigment extracting solutions respectively according to the methods of the embodiments 1 to 7, conveying the pigment extracting solutions into a vacuum reaction kettle, preserving the heat of the pigment extracting solutions for corresponding time, vacuumizing to remove petroleum ether to obtain a primary product, drying the primary product at 65 ℃, sieving by a 325-mesh sieve, conveying the primary product into a nano-grinder for grinding for corresponding time to obtain nano-scale organic plant dyes, and dyeing by the dyeing method of the embodiment 1.
The dyed fabrics obtained in examples 1 to 7 and comparative examples 8 to 14 were subjected to the color fastness test, as shown in Table 2. The results show that the color fastness to washing, rubbing and sunlight of the examples 1 to 7 are enhanced, and especially the color fastness to sunlight is greatly increased, because after the mineral substances and the organic substances are added, the milky liquid with the network structure is generated to play a role in coating, precipitating and complexing, so that the plant pigment is converted into the natural complex dye, and the color fastness to dyeing is improved.
| Categories | Color fastness to washing | Colour fastness to rubbing | Color fastness to sunlight |
| Example 1 | Grade 5 | Grade 5 | Grade 5 |
| Example 2 | Grade 5 | Grade 5 | 4 stage |
| Example 3 | Grade 5 | 4 stage | Grade 5 |
| Example 4 | Grade 5 | Grade 5 | Grade 5 |
| Example 5 | Grade 5 | Grade 5 | Grade 5 |
| Example 6 | 4 stage | 4 stage | Grade 5 |
| Example 7 | 4 stage | 4 stage | 4 stage |
| Comparative example 8 | 4 stage | 4 stage | 4 stage |
| Comparative example 9 | 4 stage | 4 stage | Grade 3 |
| Comparative example 10 | 4 stage | Grade 3 | 4 stage |
| Comparative example 11 | 4 stage | 4 stage | 4 stage |
| Comparative example 12 | 4 stage | 4 stage | 4 stage |
| Comparative example 13 | Grade 3 | Grade 3 | 4 stage |
| Comparative example 14 | Grade 3 | Grade 3 | Grade 3 |
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A preparation method of an organic plant dye is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing the components in a mass ratio of 1: 3, mixing the extraction raw material and the solvent in a countercurrent extraction device, heating to 40-95 ℃, preserving heat for 1h, and then carrying out countercurrent extraction to obtain a primary extract; the extraction raw materials are one or more of tea leaves, holly leaves, mulberry leaves, pine needles, pomegranate peels, persimmons, dragon fruit peels, rosewood sawdust, madder roots, kale leaves, folium isatidis, green lotus leaves, safflower, crocus sativus, roses, jasmine flower diameters, beet stems and orange stem;
(2) carrying out centrifugal separation on the primary extract to obtain a first filtrate and a first filter residue, and carrying out adsorption treatment on the first filtrate by a first solid-phase extraction column under an ultrasonic state to obtain a first effluent;
(3) respectively returning the first filter residue and the first effluent to a countercurrent extraction device, carrying out countercurrent extraction again at 40-95 ℃, then treating according to the method in the step (2) to obtain a second filter residue and a second effluent, and carrying out adsorption treatment by using a second solid-phase extraction column in the step;
(4) treating the second filter residue and the second effluent according to the method in the step (3) to obtain a third filter residue and a third effluent, wherein the third effluent is used as a solvent for next pigment extraction and is kept for standby application, and in the step, a third solid-phase extraction column is used for adsorption treatment; respectively carrying out desorption treatment on the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column by using petroleum ether, and then mixing liquids obtained by desorption to obtain a pigment extracting solution;
(5) conveying the pigment extracting solution into a vacuum reaction kettle, adding mineral substances and organic substances, uniformly stirring, complexing at 60-90 ℃ for 2 hours, vacuumizing to remove petroleum ether after complexing is finished, and obtaining a complex primary product, wherein the using amounts of the mineral substances and the organic substances are 0.1-10% and 10-30% of the mass of the pigment extracting solution respectively;
(6) and drying the complex primary product at 65-85 ℃, sieving the product by a 325-mesh sieve, and conveying the product to a nano grinder for grinding for 3-10 h to obtain the nano organic plant dye.
2. A process for the preparation of an organic vegetable dye according to claim 1, characterized in that: the first solid-phase extraction column, the second solid-phase extraction column and the third solid-phase extraction column are all prepared by mixing and filling alkaline alumina and kieselguhr according to the mass ratio of 1: 1.5.
3. A process for the preparation of an organic vegetable dye according to claim 1, characterized in that: the solvent is ethanol or deionized water or sodium bicarbonate solution with the concentration of 0.5 g/L.
4. A process for the preparation of an organic vegetable dye according to claim 1, characterized in that: the mineral is selected from one of alum, blue vitriol, titanium dioxide and magnesium oxide, and the organic is selected from one of tannin, peach gum, acetic acid and flavonoid compounds.
5. A process for the preparation of an organic vegetable dye according to claim 1, characterized in that: in the step (5), the pigment extracting solution is conveyed to a vacuum reaction kettle and then is subjected to heat preservation for 3-8 hours.
6. A method of dyeing an organic vegetable dye prepared according to any one of claims 1 to 5, characterized in that: and (3) mixing the fabric to be dyed according to the bath ratio of 1: 10 adding the mixture into a loose wool dyeing machine, heating to 60 ℃, adding the prepared organic plant dye and the auxiliary agent, and keeping the temperature for 20min, wherein the use amounts of the organic plant dye and the auxiliary agent are respectively 8% and 6% of the mass of the fabric to be dyed; adding organic acid to adjust pH to 5, heating to 95 deg.C at a rate of 1 deg.C/min, maintaining for 20min, adding softening agent, maintaining for 20min, and discharging deionized water when the temperature is increased to room temperature, wherein the amount of the softening agent is 1.8% of the amount of the dye.
7. A method of dyeing an organic vegetable dye as claimed in claim 6, characterized in that: the auxiliary agent is anhydrous sodium sulphate, and the organic acid is citric acid.
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