CN114753170A - Purple Lyocell fabric prepared by dyeing animal dye lacca and preparation method thereof - Google Patents
Purple Lyocell fabric prepared by dyeing animal dye lacca and preparation method thereof Download PDFInfo
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- CN114753170A CN114753170A CN202210425860.4A CN202210425860A CN114753170A CN 114753170 A CN114753170 A CN 114753170A CN 202210425860 A CN202210425860 A CN 202210425860A CN 114753170 A CN114753170 A CN 114753170A
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- 238000004043 dyeing Methods 0.000 title claims abstract description 87
- 229920000433 Lyocell Polymers 0.000 title claims abstract description 80
- 239000004744 fabric Substances 0.000 title claims abstract description 69
- 241001465754 Metazoa Species 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 100
- 108010059892 Cellulase Proteins 0.000 claims abstract description 37
- 229940106157 cellulase Drugs 0.000 claims abstract description 35
- 102000030523 Catechol oxidase Human genes 0.000 claims abstract description 30
- 108010031396 Catechol oxidase Proteins 0.000 claims abstract description 30
- 239000001057 purple pigment Substances 0.000 claims abstract description 27
- 102000004190 Enzymes Human genes 0.000 claims abstract description 14
- 108090000790 Enzymes Proteins 0.000 claims abstract description 14
- 229940088598 enzyme Drugs 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 9
- 230000000415 inactivating effect Effects 0.000 claims abstract description 7
- 239000008399 tap water Substances 0.000 claims abstract description 7
- 235000020679 tap water Nutrition 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- 239000000049 pigment Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- 239000000706 filtrate Substances 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 15
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000013078 crystal Substances 0.000 claims description 10
- 238000007865 diluting Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000008055 phosphate buffer solution Substances 0.000 claims description 10
- 239000007974 sodium acetate buffer Substances 0.000 claims description 10
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000001632 sodium acetate Substances 0.000 claims description 7
- 235000017281 sodium acetate Nutrition 0.000 claims description 7
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 5
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 5
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 5
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 5
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 claims description 5
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 5
- 235000011009 potassium phosphates Nutrition 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 241000238631 Hexapoda Species 0.000 claims description 4
- 230000009849 deactivation Effects 0.000 claims 1
- 229920002678 cellulose Polymers 0.000 abstract description 15
- 239000001913 cellulose Substances 0.000 abstract description 15
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 abstract description 8
- 102000003425 Tyrosinase Human genes 0.000 abstract description 4
- 108060008724 Tyrosinase Proteins 0.000 abstract description 4
- 238000010559 graft polymerization reaction Methods 0.000 abstract description 2
- 239000000975 dye Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 9
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- 230000000694 effects Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 241001516928 Kerria lacca Species 0.000 description 3
- 229930182559 Natural dye Natural products 0.000 description 3
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- 230000007547 defect Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000978 natural dye Substances 0.000 description 3
- 238000000643 oven drying Methods 0.000 description 3
- 239000000979 synthetic dye Substances 0.000 description 3
- 229920002994 synthetic fiber Polymers 0.000 description 3
- 229920003043 Cellulose fiber Polymers 0.000 description 2
- GUBGYTABKSRVRQ-CUHNMECISA-N D-Cellobiose Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-CUHNMECISA-N 0.000 description 2
- 229920000297 Rayon Polymers 0.000 description 2
- 229920001800 Shellac Polymers 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
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- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 235000013824 polyphenols Nutrition 0.000 description 2
- BBNQQADTFFCFGB-UHFFFAOYSA-N purpurin Chemical compound C1=CC=C2C(=O)C3=C(O)C(O)=CC(O)=C3C(=O)C2=C1 BBNQQADTFFCFGB-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
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- 239000004208 shellac Substances 0.000 description 2
- ZLGIYFNHBLSMPS-ATJNOEHPSA-N shellac Chemical compound OCCCCCC(O)C(O)CCCCCCCC(O)=O.C1C23[C@H](C(O)=O)CCC2[C@](C)(CO)[C@@H]1C(C(O)=O)=C[C@@H]3O ZLGIYFNHBLSMPS-ATJNOEHPSA-N 0.000 description 2
- 229940113147 shellac Drugs 0.000 description 2
- 235000013874 shellac Nutrition 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- PKTBUSPVTXIOCN-QHIUXXQWSA-N 4-{[4-(dimethylamino)phenyl]diazenyl}phenyl-beta-lactoside Chemical compound C1=CC(N(C)C)=CC=C1N=NC(C=C1)=CC=C1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)[C@@H](O)[C@@H](CO)O2)O)[C@@H](CO)O1 PKTBUSPVTXIOCN-QHIUXXQWSA-N 0.000 description 1
- RHAXKFFKGZJUOE-UHFFFAOYSA-N 7-acetyl-6-ethyl-3,5,8-trihydroxy-9,10-dioxoanthracene-1,2-dicarboxylic acid Chemical compound O=C1C2=CC(O)=C(C(O)=O)C(C(O)=O)=C2C(=O)C2=C1C(O)=C(CC)C(C(C)=O)=C2O RHAXKFFKGZJUOE-UHFFFAOYSA-N 0.000 description 1
- 108010084185 Cellulases Proteins 0.000 description 1
- 102000005575 Cellulases Human genes 0.000 description 1
- 108010008885 Cellulose 1,4-beta-Cellobiosidase Proteins 0.000 description 1
- 241000732800 Cymbidium Species 0.000 description 1
- 101710112457 Exoglucanase Proteins 0.000 description 1
- 241000237858 Gastropoda Species 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
- 108090000604 Hydrolases Proteins 0.000 description 1
- 102000004157 Hydrolases Human genes 0.000 description 1
- 229930192967 Laccaic acid Natural products 0.000 description 1
- 244000208060 Lawsonia inermis Species 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 108010047754 beta-Glucosidase Proteins 0.000 description 1
- 102000006995 beta-Glucosidase Human genes 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 150000004676 glycans Polymers 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000025 natural resin Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000010908 plant waste Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 150000004804 polysaccharides Polymers 0.000 description 1
- 239000001047 purple dye Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
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Classifications
-
- 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
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
-
- 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
-
- 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
-
- 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
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Coloring (AREA)
Abstract
The invention relates to purple Lyocell fabric prepared by dyeing animal dye lacca and a preparation method thereof. The purple pigment of the lacca is extracted from the lacca through an aqueous solution to prepare the purple pigment of the lacca, a phenol oxidase solution and a cellulase solution are prepared, and the purple pigment of the lacca, the phenol oxidase solution, the cellulase solution and H are mixed2O2Preparing a dyeing solution from the solution and the like, putting manganese dioxide, the Lyocell fabric and the dyeing solution into a dyeing machine for dyeing, inactivating enzyme of the dyed Lyocell fabric, washing with tap water, and drying to obtain purple Lyocell fabric. According to the invention, cellulose and purple pigment are respectively activated by selecting cellulase and polyphenol oxidase, so that the graft polymerization reaction of the cellulose and the purple pigment is realized. The dyeing condition of the invention is mild, and the pollution to the environment is small; the dyed purple lyocell fabric has a high K/S value and high soaping fastness and dry rubbing fastness grades.
Description
Technical Field
The invention belongs to the technical field of fabric preparation, and particularly relates to a purple Lyocell fabric prepared by dyeing with animal dye lacca and a preparation method thereof.
Background
It has been known for thousands of years to obtain colors from animals and plants to decorate one's own garments. The animal dye represents ancient purple, and the ancient purple is a beautiful purple dye obtained by oxidizing yellow liquid secreted by bone snails along the coast of the Mediterranean Xiaotenia; further, as the dye plant, henna, cymbidium and the like are known. Since the recent times, the synthetic dye gradually replaces the natural animal and plant dye due to its colorful, cheap and durable properties, and the natural dye slowly exits the history stage. Since the 21 st century, people have increasingly pursued health, environmental protection and ecological consciousness, and the synthetic dye can release toxic and harmful gas and harm human health under certain conditions, so that people have transferred attention to the natural dye again.
The lac insect is an important resource insect, lives on host plants, absorbs plant juice, and female insects secrete a purely natural resin lac through glands. The lac is an important chemical raw material and is widely applied to various industries. During the production of shellac, pigment is required to be precipitated, and this precipitated purpurin can be used as a by-product of shellac production as a natural dye. The laccaic acid has phenolic hydroxyl group in its structure, so that it has good antibacterial, antiviral, anticancer and antioxidant effects.
Lyocell fiber is a brand-new variety of artificial cellulose fiber, and compared with the lyocell fiber which is formed in Europe and America in the last 90 s, the lyocell fiber has the characteristics of comfortableness, good hand feeling, easy dyeing and the like of natural cellulose fiber, and also has the environmental protection advantage which is not possessed by the traditional viscose fiber production. The raw material is inexhaustible cellulose in nature, the production process of the fiber is simple, the production process has no chemical reaction, and the plant waste can be biologically and naturally degraded, so the fiber is a green chemical fiber. The manufacturing process of the lyocell fiber is different from other artificial fibers such as viscose fiber and the like, the production process is less, the time consumption is very short, no powerful chemical agent is used in the production process, only the recyclable organic solvent is used, no intermediate compound is formed in the whole production process, and no pollutant is discharged. Lyocell fibers have a higher index of physical and mechanical properties than other man-made fibers.
Because the performance of the lyocell fiber combines the advantages of the artificial fiber and the synthetic fiber, the fabric is comfortable to wear, good in color and luster, strong in wrinkle resistance, firm and durable, and is favored by the market. Meanwhile, researches on dyeing processes of lyocell fibers are more and more, but most of the researches on dyeing lyocell fibers by using chemical synthetic dyes and dyeing the lyocell fibers by using natural animal dyes are only reported and need to be further researched.
Disclosure of Invention
The chemically synthesized dye has strong reactivity and is combined with the lyocell fabric through chemical bonds, while the purple pigment of the animal dye lacca is relatively stable and has poor reactivity, so that the dye is not easily combined with the lyocell fabric; under the auxiliary action of the printing and dyeing auxiliary agent, the animal dye lacca can be used for dyeing the lyocell fabric. The dyeing process of the lyocell fabric by the lac dye with the assistance of the printing and dyeing auxiliary agent can cause environmental pollution and large consumption of resources; in addition, the lyocell fabric prepared by the dyeing process has low color fastness, washing resistance and weather fastness. Aiming at the defects in the prior art, the invention aims to provide the purple Lyocell fabric prepared by dyeing animal dye lacca and the preparation method thereof.
The invention aims to provide a purple Lyocell fabric prepared by dyeing animal dye lacca sinensis, which has a high K/S value and excellent soaping color change fastness and dry rubbing color fastness.
The invention aims to provide a purple lyocell fabric prepared by dyeing animal dye lacca, which can be prepared by the following preparation method: extracting purple pigment from Lacca by water solution to obtain purple pigment, preparing phenol oxidase solution and cellulase solution, mixing purple pigment, phenol oxidase solution, cellulase solution and H 2O2Preparing a dyeing solution from the solution and the like, putting manganese dioxide, the Lyocell fabric and the dyeing solution into the dyeing solution for dyeingAnd (3) dyeing by using a machine, inactivating enzyme of the dyed lyocell fabric, washing with tap water, and drying to obtain the purple lyocell fabric.
The invention also aims to provide a preparation method of the purple lyocell fabric prepared by dyeing animal dye lacca, which comprises the following steps:
(1) and (3) extraction of the pigment: grinding the lacca sinensis and water, wherein the material-liquid ratio is 1: 2-4 (g/mL); extracting for 2-3 times by using 5-10 times of water, centrifuging the extract liquor to remove residues, adding a mixed solution of 0.1-0.3 mol/L sodium hydroxide and 0.1-0.3 mol/L calcium chloride into the extract liquor, adding 3 wt% hydrochloric acid to adjust the pH value to 2.0-3.0, standing for 3-4 hours, filtering and collecting filtrate; adding 10 wt% of sulfuric acid into the filtrate until no pigment crystals are separated out, filtering with filter paper, standing the filtrate for 2-3 d to separate out pigment crystals, filtering and washing for 3 times, and drying at 50-60 ℃ to obtain the purple lacca purpurea pigment.
Preferably, the dosage of the mixed solution is 4-6% of the dosage of the extraction liquid.
(2) Preparing an enzyme solution: preparing a polyphenol oxidase solution: dissolving polyphenol oxidase in a phosphate buffer solution with the pH value of 6.3-6.7 to prepare a polyphenol oxidase solution of 20-30 mg/mL; preparing a cellulase solution: and dissolving cellulase in an acetic acid-sodium acetate buffer solution with the pH value of 4.6-5.0 to prepare 20-30 mg/mL cellulase solution.
Preferably, the preparation method of the phosphate buffer solution is as follows: taking 0.6-0.7 g of monopotassium phosphate, adding 15-16 mL of 0.08-0.12 mol/L sodium hydroxide solution, and diluting with water to 80-120 mL to obtain the potassium phosphate.
Preferably, the preparation method of the acetic acid-sodium acetate buffer solution comprises the following steps: and (3) taking 5.0-6.0 g of sodium acetate, adding 40-60 mL of water for dissolving, adjusting the pH value to 4.6-5.0 by using glacial acetic acid, and adding water for diluting to 80-120 mL to obtain the sodium acetate.
(3) Preparing a dyeing liquid: mixing purple pigment of Lacca, polyphenol oxidase solution, cellulase solution, and 10 wt% of H2O2Adding distilled water into the aqueous solution, stirring and mixing to prepare a dyeing solution, and regulating the pH value of the dyeing solution to 6-7 by using 28-32 wt% NaOH alkali liquor.
Preferably, the purple pigment (g) of the lac insect, a polyphenol oxidase solution (mL), a cellulase solution (mL) and 8-12 wt% of H2O2The dosage ratio of the solution (mL) and the distilled water (mL) is as follows: 1: 0.2-0.6: 0.1-0.3: 1.0-1.4: 50-70.
(4) Dyeing: MnO of2And putting the lyocell fabric and the dyeing solution into a dyeing machine for dyeing, wherein the bath ratio is 1: 20-30, the dyeing time is 60-90 minutes, the dyeing temperature is 40-50 ℃, and the lyocell fabric is taken out after dyeing is finished.
Preferably, the MnO 2The dosage (g) of the dye liquor is the ratio of the dosage (mL) of the dye liquor: 0.02 to 0.06 percent.
(5) And (3) post-treatment: and inactivating enzyme of the dyed lyocell fabric in boiling water for 15-30 min, washing the enzyme-inactivated lyocell fabric with tap water for 2-4 times, and drying to obtain the purple lyocell fabric.
The dyeing mechanism analysis of the invention comprises the following steps:
in the dyeing process, H2O2In MnO2Under the condition of being used as a catalyst, oxygen is continuously and slowly generated, and the reaction equation is shown as follows.
Polyphenol Oxidase (PPO) is an enzyme specific to phenolic compounds, which catalyzes the oxidation of purple pigment of lacca to purple pigment with active free radicals in the presence of oxygen, and the reaction is schematically shown below:
cellulases are a multicomponent enzyme system comprising a plurality of members of the group of hydrolases, generally classified into the following 3 classes: (a) endoglucanase, which hydrolyzes beta-1, 4 glycosidic bonds in amorphous regions inside cellulose molecules, cuts long-chain cellulose molecules into short chains, and generates a large amount of small-molecule cellulose; (b) exoglucanases, also known as cellobiohydrolases, which act on the ends of polysaccharide chains to hydrolyze the beta-1, 4 glycosidic linkages, cleaving one cellobiose molecule at a time from a non-reducing end; (c) beta-glucosidase, which hydrolyzes cellobiose to glucose molecules. It can be seen that the chemical bonds (e.g.. beta. -1, 4 glycosidic bonds) associated with cellulose, the major component of lyocell, are slowly broken by the action of cellulase enzymes.
In the process of decomposing cellulose by cellulase, when chemical bonds of the cellulose are broken, the purple lac-worm pigment with active free radicals is encountered, and at the moment, the purple lac-worm pigment with active free radicals attacks the chemical bond groups of the cellulose which is just broken, and the purple lac-worm pigment and the chemical bond groups are subjected to chemical reaction, so that the purple lac-worm pigment is grafted on the cellulose.
The invention has the following remarkable advantages:
(1) aiming at the characteristic of low reactivity of the lyocell, the method selects the cellulase to activate the reactivity of the lyocell, and in the process, the method properly selects the low-dose cellulase, so that the method not only realizes the activation of the reactivity of the lyocell, but also does not damage the molecular structure of the cellulose.
(2) Aiming at the characteristics of stable structure and low reaction activity of the purple pigment of the lacca, the polyphenol oxidase is selected to activate the reaction activity of the purple pigment, so that the anthraquinone derivative with reactive free radicals is generated.
(3) Aiming at the defect of poor reaction activity of purple pigment of lacca and cellulose in Lyocell fabric, the inventor of the application unexpectedly finds that cellulose and purple pigment with reaction activity are respectively activated by selecting cellulase and polyphenol oxidase, so that the graft polymerization reaction of the cellulose and the purple pigment is realized.
(4) The purple lyocell fabric prepared by dyeing the animal dye lacca prepared by the method has a slightly higher K/S value than that of the purple lyocell fabric purchased in the market, and the grades of the fastness to soaping and discoloration and the fastness to dry rubbing are slightly higher than those of the purple lyocell fabric purchased in the market.
(5) Aiming at the defects of large environmental pollution and large resource consumption of chemical dye dyeing, the invention adopts cellulase and polyphenol oxidase for dyeing, the dyeing condition is mild, and the environmental pollution is small.
Detailed Description
The examples and comparative examples described below illustrate the present invention in detail.
The main raw material sources are as follows: polyphenol oxidase (870U/mg) was purchased from Worthington Biotech development, Inc., and cellulase (40U/mg) was purchased from Shanghai-derived leaf Biotech, Inc.
Example 1
The preparation method of the purple Lyocell fabric prepared by dyeing animal dye lacca comprises the following steps:
(1) and (3) extraction of the pigment: grinding the lacca sinensis and water, wherein the ratio of material to liquid is 1: 3 (g/mL); extracting with 7 times of water for 2 times, centrifuging the extractive solution to remove residue, adding mixed solution of 0.2mol/L sodium hydroxide and 0.2mol/L calcium chloride into the extractive solution, wherein the amount of the mixed solution is 5% of the amount of the extractive solution, adding 3 wt% hydrochloric acid to adjust pH to 2.5, standing for 3.5h, filtering, and collecting filtrate; adding 10 wt% sulfuric acid into the filtrate until no pigment crystal is separated out, filtering with filter paper, standing the filtrate for 2.5d to separate out pigment crystal, filtering and washing with water for 3 times, and oven drying at 55 deg.C to obtain purple pigment of Lacca.
(2) Preparing an enzyme solution: preparing a polyphenol oxidase solution: dissolving polyphenol oxidase in phosphate buffer solution with pH of 6.5 to obtain 25mg/mL polyphenol oxidase solution; preparing a cellulase solution: dissolving cellulase in acetic acid-sodium acetate buffer solution with the pH value of 4.8 to prepare 25mg/mL cellulase solution; the preparation method of the phosphate buffer solution comprises the following steps: taking 0.68g of monopotassium phosphate, adding 15.2mL of 0.1mol/L sodium hydroxide solution, and diluting with water to 100mL to obtain the potassium phosphate; the preparation method of the acetic acid-sodium acetate buffer solution comprises the following steps: dissolving sodium acetate 5.4g in water 50mL, adjusting pH to 4.8 with glacial acetic acid, and diluting with water to 100 mL.
(3) Preparing a dyeing solution: 1g purple pigment of lacca, 0.4mL polyphenol oxidase solution, 0.2mL cellulase solution, 1.2mL10 wt% H2O2Adding 60mL of distilled water into the aqueous solution, stirring and mixing to prepare a dyeing solution, and regulating the pH value of the dyeing solution to be 6.5 by using 30 wt% NaOH alkali liquor.
(4) Dyeing: adding 0.04g MnO2And putting the lyocell fabric and 100mL of dyeing solution into a dyeing machine for dyeing, wherein the bath ratio is 1: 25, the dyeing time is 75 minutes, the dyeing temperature is 45 ℃, and taking out the lyocell fabric after dyeing is finished.
(5) And (3) post-treatment: and (3) inactivating enzyme of the dyed lyocell fabric in boiling water for 25min, washing the enzyme-inactivated lyocell fabric with tap water for 3 times, and drying to obtain the purple lyocell fabric.
Example 2
The preparation method of the purple Lyocell fabric prepared by dyeing animal dye lacca comprises the following steps:
(1) and (3) extraction of the pigment: grinding the lacca sinensis and water, wherein the ratio of material to liquid is 1: 2 (g/mL); extracting with 5 times of water for 2 times, centrifuging the extractive solution to remove residue, adding mixed solution of 0.1mol/L sodium hydroxide and 0.1mol/L calcium chloride into the extractive solution, wherein the amount of the mixed solution is 4% of the amount of the extractive solution, adding 3 wt% hydrochloric acid to adjust pH to 2.0, standing for 3 hr, filtering, and collecting filtrate; adding 10 wt% sulfuric acid into the filtrate until no pigment crystal is separated out, filtering with filter paper, standing the filtrate for 2d to separate out pigment crystal, filtering and washing with water for 3 times, and oven drying at 50 deg.C to obtain purple pigment of Lacca.
(2) Preparing an enzyme solution: preparing a polyphenol oxidase solution: dissolving polyphenol oxidase in phosphate buffer solution with pH of 6.5 to obtain 20mg/mL polyphenol oxidase solution; preparing a cellulase solution: dissolving cellulase in acetic acid-sodium acetate buffer solution with the pH value of 4.8 to prepare 20mg/mL cellulase solution; the preparation method of the phosphate buffer solution comprises the following steps: taking 0.68g of monopotassium phosphate, adding 15.2mL of 0.1mol/L sodium hydroxide solution, and diluting with water to 100mL to obtain the potassium phosphate; the preparation method of the acetic acid-sodium acetate buffer solution comprises the following steps: dissolving sodium acetate 5.4g in water 50mL, adjusting pH to 4.8 with glacial acetic acid, and diluting with water to 100 mL.
(3) Preparing a dyeing liquid: dissolving 1g purple pigment of lacca and 0.2mL polyphenol oxidaseLiquid, 0.1mL cellulase solution, 1.0mL10 wt% H2O2Adding 60mL of distilled water into the aqueous solution, stirring and mixing to prepare a dyeing solution, and regulating the pH value of the dyeing solution to be 6.0 by using 30 wt% NaOH alkali liquor.
(4) Dyeing: adding 0.02g of MnO2And putting the lyocell fabric and 100mL of dyeing solution into a dyeing machine for dyeing, wherein the bath ratio is 1: 20, the dyeing time is 60 minutes, the dyeing temperature is 40 ℃, and taking out the lyocell fabric after dyeing is finished.
(5) And (3) post-treatment: and (3) inactivating enzyme of the dyed lyocell fabric in boiling water for 15min, washing the enzyme-inactivated lyocell fabric with tap water for 2 times, and drying to obtain the purple lyocell fabric.
Example 3
The preparation method of the purple Lyocell fabric prepared by dyeing animal dye lacca comprises the following steps:
(1) and (3) extraction of the pigment: grinding the lacca sinensis and water, wherein the ratio of material to liquid is 1: 4 (g/mL); extracting with 10 times of water for 2 times, centrifuging the extractive solution to remove residue, adding mixed solution of 0.3mol/L sodium hydroxide and 0.3mol/L calcium chloride into the extractive solution, wherein the amount of the mixed solution is 6% of the amount of the extractive solution, adding 3 wt% hydrochloric acid to adjust pH to 3.0, standing for 4 hr, filtering, and collecting filtrate; adding 10 wt% sulfuric acid into the filtrate until no pigment crystal is separated out, filtering with filter paper, standing the filtrate for 3d to separate out pigment crystal, filtering and washing with water for 3 times, and oven drying at 60 deg.C to obtain purple pigment of lac insect.
(2) Preparing an enzyme solution: preparing a polyphenol oxidase solution: dissolving polyphenol oxidase in phosphate buffer solution with pH of 6.5 to obtain 30mg/mL polyphenol oxidase solution; preparing a cellulase solution: dissolving cellulase in acetic acid-sodium acetate buffer solution with the pH value of 4.8 to prepare 30mg/mL cellulase solution; the preparation method of the phosphate buffer solution comprises the following steps: taking 0.68g of monopotassium phosphate, adding 15.2mL of 0.1mol/L sodium hydroxide solution, and diluting with water to 100mL to obtain the potassium phosphate; the preparation method of the acetic acid-sodium acetate buffer solution comprises the following steps: dissolving sodium acetate 5.4g in water 50mL, adjusting pH to 4.8 with glacial acetic acid, and diluting with water to 100 mL.
(3) Of dyeing liquorsPreparation: 1g of purple pigment of lacca, 0.6mL of polyphenol oxidase solution, 0.3mL of cellulase solution and 1.4mL of 10 wt% H2O2Adding 60mL of distilled water into the aqueous solution, stirring and mixing to prepare a dyeing solution, and regulating the pH value of the dyeing solution to be 7.0 by using 30 wt% NaOH alkali liquor.
(4) Dyeing: adding 0.06g MnO2And putting the lyocell fabric and 100mL of dyeing solution into a dyeing machine for dyeing, wherein the bath ratio is 1: 30, the dyeing time is 90 minutes, the dyeing temperature is 50 ℃, and taking out the lyocell fabric after dyeing is finished.
(5) And (3) post-treatment: and (3) inactivating enzyme of the dyed lyocell fabric in boiling water for 30min, washing the enzyme-inactivated lyocell fabric with tap water for 4 times, and drying to obtain the purple lyocell fabric.
Comparative example 1
In this comparative example, only the polyphenol oxidase solution was added in the step (2) and the cellulase solution was not added, and the other preparation method was performed as in example 1, by way of comparison with example 1.
Comparative example 2
In this comparative example, only the cellulase solution and not the polyphenol oxidase solution were added in step (2) by way of comparison with example 1, and the other preparation methods were carried out as in example 1.
Performance evaluation:
the performance of the purple lyocell fabric obtained in the above examples 1 to 3 and comparative examples 1 to 2 and the purple lyocell fabric purchased in the market, which was purchased from Jiangsu Huaye textile Co., Ltd. The K/S value is measured by a computer color measuring and matching instrument; the soaping-resistant color change fastness value test refers to GB/T3921-2008 'textile color fastness test soaping-resistant color fastness'; the dry rubbing fastness value test refers to GB/T3920-2008 'color fastness to rubbing' of textile color fastness test, and the specific data are shown in Table 1.
TABLE 1
| Sample (I) | K/S value | Fastness to soaping change/grade | Color fastness to dry rubbing/grade |
| Example 1 | 12.77 | 5 | 4-5 |
| Example 2 | 12.36 | 5 | 5 |
| Example 3 | 12.18 | 5 | 5 |
| Comparative example 1 | 5.34 | 3 | 3-4 |
| Comparative example 2 | 5.39 | 3 | 3 |
| Market procurement | 11.26 | 4-5 | 4-5 |
As can be seen from Table 1, the K/S values, the soaping color fastness resistance and the dry rubbing color fastness of examples 1-3 are better than those of comparative examples 1-2; in addition, the K/S value of the purple lyocell fabric prepared by the method is slightly higher than that of the purple lyocell fabric purchased in the market.
Claims (10)
1. The preparation method of the purple Lyocell fabric prepared by dyeing animal dye laccai is characterized by comprising the following steps:
(1) preparing a dyeing solution: mixing purple pigment of Lacca, polyphenol oxidase solution, cellulase solution, and 10 wt% of H2O2Adding distilled water into the aqueous solution, stirring and mixing to prepare a dyeing solution, and regulating the pH value of the dyeing solution to 6-7 by using 28-32 wt% NaOH alkali liquor;
(2) dyeing: MnO of2The Lyocell fabric and the dyeing solution are placed into a dyeing machine for dyeing, the bath ratio is 1: 20-30, the dyeing time is 60-90 minutes, the dyeing temperature is 40-50 ℃, and the Lyocell fabric is taken out after dyeing is finished;
(3) and (3) post-treatment: and (3) inactivating enzyme of the dyed lyocell fabric in boiling water, washing the enzyme-inactivated lyocell fabric for 2-4 times by using tap water, and drying to obtain the purple lyocell fabric.
2. The preparation method of the purple lyocell fabric dyed by the animal dye lacca according to claim 1, wherein the preparation method of the lacca purple pigment in the step (1) comprises the following steps: grinding lacca and water, wherein the material-liquid ratio is 1g to (2-4) mL; extracting for 2-3 times by using 5-10 times of water, centrifuging the extract liquor to remove residues, and adding a mixed solution of 0.1-0.3 mol/L sodium hydroxide and 0.1-0.3 mol/L calcium chloride into the extract liquor, wherein the amount of the mixed solution is 4-6% of that of the extract liquor; adding 3 wt% of hydrochloric acid to adjust the pH value to 2.0-3.0, standing for 3-4 h, filtering and collecting filtrate; adding 10 wt% of sulfuric acid into the filtrate until no pigment crystals are separated out, filtering with filter paper, standing the filtrate for 2-3 d to separate out pigment crystals, filtering and washing for 3 times, and drying at 50-60 ℃ to obtain the purple lacca purpurea pigment.
3. The method for preparing the purple lyocell fabric dyed by the animal dye laccai according to claim 1, wherein the preparation method of the polyphenol oxidase solution in the step (1) comprises the following steps: and dissolving polyphenol oxidase in a phosphate buffer solution with the pH value of 6.3-6.7 to prepare a 20-30 mg/mL polyphenol oxidase solution.
4. The method for preparing the purple lyocell fabric dyed by the animal dye lacca according to claim 3, wherein the phosphate buffer solution is prepared by the following steps: taking 0.6-0.7 g of monopotassium phosphate, adding 15-16 mL of 0.08-0.12 mol/L sodium hydroxide solution, and diluting with water to 80-120 mL to obtain the potassium phosphate.
5. The method for preparing the purple lyocell fabric dyed by the animal dye lacca according to claim 1, wherein the preparation method of the cellulase solution in the step (1) comprises the following steps: and dissolving cellulase in an acetic acid-sodium acetate buffer solution with the pH value of 4.6-5.0 to prepare 20-30 mg/mL cellulase solution.
6. The method for preparing the purple lyocell fabric dyed by the animal dye lacca according to claim 5, wherein the preparation method of the acetic acid-sodium acetate buffer solution comprises the following steps: and (3) taking 5.0-6.0 g of sodium acetate, adding 40-60 mL of water for dissolving, adjusting the pH value to 4.6-5.0 by using glacial acetic acid, and adding water for diluting to 80-120 mL to obtain the sodium acetate.
7. The method for preparing purple lyocell fabric dyed by animal dye lacca according to claim 1, wherein the lacca purple pigment in step (1), polyphenol oxidase solution, cellulase solution, and 8-12 wt% of H2O2The dosage ratio of the water solution to the distilled water is 1g to (0.2-0.6) mL to (0).1～0.3)mL∶(1.0～1.4)mL∶(50～70)mL。
8. The method for preparing purple lyocell fabric dyed with the animal dye lacca according to claim 1, wherein said MnO in step (2) 2The dosage of the dye liquor accounts for 0.02 to 0.06 percent g/mL of the dyeing liquor.
9. The preparation method of the purple lyocell fabric dyed by the animal dye lacca according to claim 1, wherein the enzyme deactivation time in the step (3) is 15-30 min.
10. The purple lyocell fabric dyed by the animal dye laccai insect is characterized by being prepared by the preparation method of the purple lyocell fabric dyed by the animal dye laccai insect according to any one of claims 1 to 9.
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