CN115772812A - Environment-friendly mixed acid dye for mixed wool and production method thereof - Google Patents
Environment-friendly mixed acid dye for mixed wool and production method thereof Download PDFInfo
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- 239000000980 acid dye Substances 0.000 title claims abstract description 64
- 210000002268 wool Anatomy 0.000 title claims abstract description 58
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229920002472 Starch Polymers 0.000 claims abstract description 44
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 44
- 239000008107 starch Substances 0.000 claims abstract description 44
- 235000019698 starch Nutrition 0.000 claims abstract description 44
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000661 sodium alginate Substances 0.000 claims abstract description 39
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 39
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 39
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims abstract description 35
- 229920001353 Dextrin Polymers 0.000 claims abstract description 31
- 239000004375 Dextrin Substances 0.000 claims abstract description 31
- 235000019425 dextrin Nutrition 0.000 claims abstract description 31
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 229920001661 Chitosan Polymers 0.000 claims abstract description 22
- 239000000975 dye Substances 0.000 claims abstract description 21
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims abstract description 15
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims abstract description 15
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 15
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000001263 FEMA 3042 Substances 0.000 claims abstract description 15
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 15
- 229940047670 sodium acrylate Drugs 0.000 claims abstract description 15
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims abstract description 15
- 229940033123 tannic acid Drugs 0.000 claims abstract description 15
- 235000015523 tannic acid Nutrition 0.000 claims abstract description 15
- 229920002258 tannic acid Polymers 0.000 claims abstract description 15
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 14
- ZAWQXWZJKKICSZ-UHFFFAOYSA-N 3,3-dimethyl-2-methylidenebutanamide Chemical compound CC(C)(C)C(=C)C(N)=O ZAWQXWZJKKICSZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 60
- 238000003756 stirring Methods 0.000 claims description 49
- 238000000034 method Methods 0.000 claims description 44
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 33
- 238000010438 heat treatment Methods 0.000 claims description 29
- 238000005406 washing Methods 0.000 claims description 26
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- 239000010687 lubricating oil Substances 0.000 claims description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 13
- 239000004202 carbamide Substances 0.000 claims description 13
- 230000000149 penetrating effect Effects 0.000 claims description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 11
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000004108 freeze drying Methods 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 9
- 230000001376 precipitating effect Effects 0.000 claims description 9
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 11
- 239000003094 microcapsule Substances 0.000 abstract description 7
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 229920001864 tannin Polymers 0.000 abstract description 4
- 235000018553 tannin Nutrition 0.000 abstract description 4
- 239000001648 tannin Substances 0.000 abstract description 4
- SJEYSFABYSGQBG-UHFFFAOYSA-M Patent blue Chemical compound [Na+].C1=CC(N(CC)CC)=CC=C1C(C=1C(=CC(=CC=1)S([O-])(=O)=O)S([O-])(=O)=O)=C1C=CC(=[N+](CC)CC)C=C1 SJEYSFABYSGQBG-UHFFFAOYSA-M 0.000 abstract description 3
- 239000004744 fabric Substances 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 238000002845 discoloration Methods 0.000 abstract description 2
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- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 229940032147 starch Drugs 0.000 description 34
- 238000012360 testing method Methods 0.000 description 24
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- 239000000982 direct dye Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 6
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- -1 polypropylene Polymers 0.000 description 3
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
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- 241001330002 Bambuseae Species 0.000 description 1
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- 239000004677 Nylon Substances 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 125000003368 amide group Chemical group 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
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- 230000007717 exclusion Effects 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000000834 fixative Substances 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 230000007935 neutral effect Effects 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229940080313 sodium starch Drugs 0.000 description 1
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Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Coloring (AREA)
Abstract
The invention relates to the field of acid dyes, and discloses an environment-friendly mixed acid dye for mixed wool and a production method thereof; according to the invention, the acid dye fixing agent is prepared by taking t-butyl acrylamide sulfonic acid, acrylic acid and sodium acrylate as raw materials, so that the water solubility of the fixing agent is reduced, and the fixing effect is enhanced. The preparation method comprises the steps of preparing starch dextrin by grafting acrylamide and carboxymethyl starch, forming composite raw paste by microcapsules formed by coating tannin with a carboxymethyl chitosan solution and sodium alginate and a starch dextrin dye, coating the microcapsules to enable the dye to be attached to the surface of a fiber and release the tannin at the same time, and generating a layer of composite association body film on the surface of the fiber at the first time to block gaps and reduce the diffusion of the dye, so that various fastness is improved; the microcapsule can avoid the phenomenon that the fabric is yellowed or faded due to the oxidative discoloration of the tannic acid; the color fixing agent can fix color without causing color light change.
Description
Technical Field
The invention relates to the field of environment-friendly mixed acid dyes for mixed wool, in particular to an environment-friendly mixed acid dye for mixed wool and a production method thereof.
Background
Bamboo charcoal, cotton-like fiber, nylon, polypropylene fiber and other synthetic fiber mixed wool clothes and various complex components of mixed wool and the like are often dyed by acid dyes. However, the traditional acid dye dyed plants are easily dissolved out in water during water washing or physical friction overcharging, so that the fabrics fade or other clothes washed together are dyed. Because the color fastness of the acid dye in the wet treatment process is poor and is difficult to meet the market requirements, the acid dye fixing agent is required to be used for further fixing the dye and the fiber so as to enhance the color fastness of the dye and the fiber. Most of the acid dye fixing agents in the market adopt phenols and aldehydes, and the problem of environmental protection exists.
Therefore, the preparation of the environment-friendly mixed acid dye for the mixed wool has important significance.
Disclosure of Invention
The invention aims to provide an environment-friendly mixed acid dye for mixed wool and a production method thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a production method of an environment-friendly mixed acid dye for mixed wool comprises the following steps:
s1: adding starch paste and sodium alginate paste into water, heating and stirring uniformly, and standing to obtain a composite paste solution;
s2: adding the dye, the penetrating agent, the lubricating oil, the urea and the color fixing agent into the composite paste solution, adding water, and uniformly stirring to obtain the environment-friendly mixed acid dye for the mixed wool.
Further, in the step S1, the starch-based paste is prepared by the following steps:
under the nitrogen atmosphere, adding carboxymethyl starch into water, heating and pasting to obtain a paste; adjusting the pH value of the paste, sequentially adding potassium persulfate and acrylamide, and stirring while keeping the temperature; precipitating, filtering and drying to obtain the starch dextrin.
Further, the heating gelatinization temperature is 75-85 ℃, and the gelatinization time is 30-60 min; carboxymethyl starch: acrylamide: the mass ratio of the potassium persulfate is (1-1.5): (1.5-3): (0.05-0.06); adjusting the pH value of the paste to 7.5-9.5; the temperature of the heat preservation and the stirring is 45 to 55 ℃, and the time is 2 to 2.5 hours.
Further, in the step S1, the sodium alginate dextrin is prepared as follows:
and dripping the sodium alginate solution and the tannic acid into the carboxymethyl chitosan solution, stirring, solidifying, washing, and freeze-drying to obtain the sodium alginate dextrin.
Further, the carboxymethyl chitosan solution is a mixed solution of calcium chloride and carboxymethyl chitosan, wherein the weight ratio of carboxymethyl chitosan: the mass ratio of calcium chloride is 1:10.
further, the sodium alginate solution: carboxymethyl chitosan solution: the mass ratio of the tannic acid is (2-4): 1: (0.2-0.4).
Further, the mass fraction of the sodium alginate solution is 2%, the mass fraction of the carboxymethyl chitosan solution is 0.2%, and the mass fraction of the solvent is 1% of acetic acid solution.
Further, in the step S2, the fixing agent is prepared by the following method:
adding acrylic acid into absolute ethyl alcohol, adding sodium acrylate, t-butyl acrylamide sulfonic acid and deionized water, and uniformly stirring; and introducing nitrogen, adding an ammonium persulfate solution, and carrying out heat preservation reaction to obtain the color fixing agent.
Further, the acrylic acid: sodium acrylate: the mass ratio of the t-butyl acrylamide sulfonic acid is 6:1: (1-3), the adding amount of the ammonium persulfate solution is 0.8-1% of the total mass of the acrylic acid, the sodium acrylate and the t-butyl acrylamide sulfonic acid; the reaction temperature is kept at 65-75 ℃ and the reaction time is 3-4 h.
Furthermore, in the environment-friendly mixed acid dye for the mixed wool, the components of the environment-friendly mixed acid dye comprise, by mass, 15-65% of starch dextrin, 15-65% of sodium alginate dextrin, 0.5-1.5% of dye, 0.5-1% of penetrating agent, 0.5-1% of lubricating oil, 3-5% of urea, 0.5-1.5% of citric acid, 1-3% of color fixing agent and the balance of water.
Further, the dye is any one or more of a direct dye, a neutral dye and an acid dye.
The invention has the following beneficial effects: the acid dye fixing agent is prepared by taking t-butyl acrylamide sulfonic acid, acrylic acid and sodium acrylate as raw materials; unsaturated double bonds at alpha and beta positions of three monomer carbonyls are utilized to form a stable copolymer in a free radical solution polymerization mode, carboxylate radicals and sulfur radicals on the side faces of the surfaces of the stable copolymer form anions in water, and the stable copolymer and the anions form electrostatic mutual exclusion with acid dye anions, so that the acid dye can be organized to diffuse into a dye bath; the main structure of the copolymer is a carbon-carbon double bond, so that the water solubility of the color fixing agent is reduced, the color fixing agent is not easy to fall off in the wet treatment process, and the color fixing effect is enhanced.
According to the invention, the starch dextrin is prepared by grafting the acrylamide and the carboxymethyl starch, the surface of the starch dextrin contains a large number of amino and hydroxyl groups, the amino and hydroxyl groups can adsorb and fully disperse the dye, the amide group on the side chain has excellent affinity to the fiber, and can form hydrogen bonds with the fiber to be combined together, so that the dye can be better dispersed on the surface of the fiber. The method comprises the following steps of forming composite raw paste by microcapsules formed by coating tannin with carboxymethyl chitosan solution and sodium alginate and starch dextrin dye, coating the microcapsules to enable the dye to be distributed on the surface of fiber and release the tannin at the same time, and generating a layer of composite association body film on the surface of the fiber at the first time to block gaps and reduce the diffusion of the dye, so that various fastness is improved; the microcapsule can avoid the phenomenon that tannic acid is excessively adsorbed at the white part without pattern patterns, and the fabric is yellowed or faded due to the oxidative discoloration of the tannic acid; the color fixing agent can fix color without causing color light change.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples, carboxymethyl starch is provided by Shandongda cellulose Co., ltd, carboxymethyl chitosan is provided by Beijing Sorley Tech Co., ltd, and the penetrant is S-C degassing penetrant provided by Kekai Fine chemical engineering (Shanghai) Co., ltd; the lubricating oil is PN brightening lubricating oil and is provided by Hensman chemical trade (Shanghai) Co., ltd; the acid dye is Lannacolong BLACK N-BGL, provided by Hensman chemical trade (Shanghai) Inc.; the direct dye is EVERCION BLUE P-3R, supplied by Taiwan Yongphotochemistry industries, inc.
Example 1
S1: under the nitrogen atmosphere, adding 10g of carboxymethyl starch into 20mL of water, heating to 85 ℃, and gelatinizing for 1h to obtain a paste; adjusting the pH value of the paste to 7.5, sequentially adding 10g of potassium persulfate and 0.5g of acrylamide, keeping the temperature at 45 ℃, and stirring for 2 hours; precipitating, filtering, and drying at 60 deg.C for 24 hr to obtain starch dextrin;
s2: dripping 20g of sodium alginate solution and 2g of tannic acid into 10g of carboxymethyl chitosan solution, stirring, solidifying for 30min, washing, and freeze-drying for 24h to obtain sodium alginate dextrin;
s3: adding 12g of acrylic acid into 50mL of absolute ethyl alcohol, adding 2g of sodium acrylate, 2 gt-butyl acrylamide sulfonic acid and 25mL of deionized water, and uniformly stirring; introducing nitrogen, adding 0.14g of 10% ammonium persulfate solution, and reacting for 3 hours at the temperature of 70 ℃ to obtain a color fixing agent;
s4: adding 150g of starch paste and 150g of sodium alginate paste into water, heating to 50 ℃, uniformly stirring, and standing for 1h to obtain a composite paste solution;
s5: adding 5g of acid dye, 5g of direct dye, 5g of penetrating agent, 5g of lubricating oil, 30g of urea, 5g of citric acid and 10g of fixing agent into the composite paste solution, adding water, and uniformly stirring to obtain the environment-friendly mixed acid dye for the mixed wool.
And (3) testing: the color fixing process comprises the following steps:
and (3) placing the prepared mixed acidic dye into a 500mL conical flask, heating to 80 ℃ in a water bath, placing the mixed wool sample into the conical flask, shaking and preserving heat for 30min, washing with hot water at 60 ℃, washing with cold water, and drying to obtain a sample to be detected.
Soaping color fastness: according to GB/T3921-2008 textile color fastness test: measuring by a soaping fastness method;
color fastness to rubbing: according to GB/T3920-2008 textile color fastness test: measuring by a rubbing color fastness method;
fastness to perspiration: measured according to the method of GB/T3922-1995.
Example 2
S1: under the nitrogen atmosphere, adding 10g of carboxymethyl starch into 20mL of water, heating to 85 ℃, and gelatinizing for 1h to obtain a paste; adjusting the pH value of the paste to 7.5, sequentially adding 10g of potassium persulfate and 0.5g of acrylamide, keeping the temperature at 45 ℃, and stirring for 2 hours; precipitating, filtering, and drying at 60 deg.C for 24 hr to obtain starch dextrin;
s2: dripping 20g of sodium alginate solution and 2g of tannic acid into 10g of carboxymethyl chitosan solution, stirring, solidifying for 30min, washing, and freeze-drying for 24h to obtain sodium alginate dextrin;
s3: adding 12g of acrylic acid into 50mL of absolute ethyl alcohol, adding 2g of sodium acrylate, 2 gt-butyl acrylamide sulfonic acid and 25mL of deionized water, and uniformly stirring; introducing nitrogen, adding 0.14g of 10% ammonium persulfate solution, and reacting for 3 hours at the temperature of 70 ℃ to obtain a color fixing agent;
s4: adding 150g of starch paste and 650g of sodium alginate paste into water, heating to 50 ℃, uniformly stirring, and standing for 1h to obtain a composite paste solution;
s5: adding 5g of acid dye, 5g of direct dye, 5g of penetrating agent, 5g of lubricating oil, 30g of urea, 5g of citric acid and 10g of fixing agent into the composite paste solution, adding water, and uniformly stirring to obtain the environment-friendly mixed acid dye for the mixed wool.
And (3) testing: the color fixing process comprises the following steps:
and (3) placing the prepared mixed acidic dye into a 500mL conical flask, heating to 80 ℃ in a water bath, placing the mixed wool sample into the conical flask, shaking and preserving heat for 30min, washing with hot water at 60 ℃, washing with cold water, and drying to obtain a sample to be detected.
Soaping color fastness: according to GB/T3921-2008 textile color fastness test: measuring by a soaping fastness method;
color fastness to rubbing: according to GB/T3920-2008 textile color fastness test: measuring by a rubbing color fastness method;
fastness to perspiration: measured according to the method of GB/T3922-1995.
Example 3
S1: under the nitrogen atmosphere, adding 10g of carboxymethyl starch into 20mL of water, heating to 85 ℃, and gelatinizing for 1h to obtain a paste; adjusting the pH value of the paste to 7.5, sequentially adding 10g of potassium persulfate and 0.5g of acrylamide, keeping the temperature at 45 ℃, and stirring for 2 hours; precipitating, filtering, and drying at 60 deg.C for 24 hr to obtain starch dextrin;
s2: dripping 20g of sodium alginate solution and 2g of tannic acid into 10g of carboxymethyl chitosan solution, stirring, solidifying for 30min, washing, and freeze-drying for 24h to obtain sodium alginate dextrin;
s3: adding 12g of acrylic acid into 50mL of absolute ethyl alcohol, adding 2g of sodium acrylate, 2 gt-butyl acrylamide sulfonic acid and 25mL of deionized water, and uniformly stirring; introducing nitrogen, adding 0.14g of 10% ammonium persulfate solution, and reacting for 3 hours at the temperature of 70 ℃ to obtain a color fixing agent;
s4: adding 650g of starch paste and 150g of sodium alginate paste into water, heating to 50 ℃, uniformly stirring, and standing for 1h to obtain a composite paste solution;
s5: adding 5g of acid dye, 5g of direct dye, 5g of penetrating agent, 5g of lubricating oil, 30g of urea, 5g of citric acid and 10g of fixing agent into the composite paste solution, adding water, and uniformly stirring to obtain the environment-friendly mixed acid dye for the mixed wool.
And (3) testing: the color fixing process comprises the following steps:
and (3) placing the prepared mixed acid dye into a 500mL conical flask, heating the mixed acid dye to 80 ℃ in a water bath, placing the mixed wool sample into the conical flask, oscillating and preserving heat for 30min, washing the mixed wool sample with hot water at 60 ℃, washing the mixed wool sample with cold water, and drying the washed mixed wool sample to obtain a sample to be detected.
Soaping color fastness: according to GB/T3921-2008 textile color fastness test: measuring by a soaping fastness method;
color fastness to rubbing: according to GB/T3920-2008 textile color fastness test: measuring by a rubbing color fastness method;
fastness to perspiration: measured according to the method of GB/T3922-1995.
Example 4
S1: under the nitrogen atmosphere, adding 10g of carboxymethyl starch into 20mL of water, heating to 85 ℃, and gelatinizing for 1h to obtain a paste; adjusting the pH value of the paste to 7.5, sequentially adding 10g of potassium persulfate and 0.5g of acrylamide, keeping the temperature at 45 ℃, and stirring for 2 hours; precipitating, filtering, and drying at 60 deg.C for 24 hr to obtain starch dextrin;
s2: dripping 20g of sodium alginate solution and 2g of tannic acid into 10g of carboxymethyl chitosan solution, stirring, solidifying for 30min, washing, and freeze-drying for 24h to obtain sodium alginate dextrin;
s3: adding 12g of acrylic acid into 50mL of absolute ethyl alcohol, adding 2g of sodium acrylate, 2 gt-butyl acrylamide sulfonic acid and 25mL of deionized water, and uniformly stirring; introducing nitrogen, adding 0.14g of 10% ammonium persulfate solution, and reacting for 3 hours at the temperature of 70 ℃ to obtain a color fixing agent;
s4: adding 400g of starch paste and 400g of sodium alginate paste into water, heating to 50 ℃, uniformly stirring, and standing for 1h to obtain a composite paste solution;
s5: adding 7.5g of acid dye, 7.5g of direct dye, 10g of penetrating agent, 10g of lubricating oil, 50g of urea, 10g of citric acid and 30g of color fixing agent into the composite paste solution, adding water, and uniformly stirring to obtain the environment-friendly mixed acid dye for the mixed wool.
And (3) testing: the color fixing process comprises the following steps:
and (3) placing the prepared mixed acid dye into a 500mL conical flask, heating the mixed acid dye to 80 ℃ in a water bath, placing the mixed wool sample into the conical flask, oscillating and preserving heat for 30min, washing the mixed wool sample with hot water at 60 ℃, washing the mixed wool sample with cold water, and drying the washed mixed wool sample to obtain a sample to be detected.
Soaping color fastness: according to GB/T3921-2008 textile color fastness test: measuring by a soaping fastness method;
color fastness to rubbing: according to GB/T3920-2008 textile color fastness test: measuring by a rubbing color fastness method;
fastness to perspiration: measured according to the method of GB/T3922-1995.
Example 5
S1: under the nitrogen atmosphere, adding 10g of carboxymethyl starch into 20mL of water, heating to 85 ℃, and gelatinizing for 1h to obtain a paste; adjusting the pH value of the paste to 7.5, sequentially adding 10g of potassium persulfate and 0.5g of acrylamide, keeping the temperature at 45 ℃, and stirring for 2 hours; precipitating, filtering, and drying at 60 deg.C for 24 hr to obtain starch dextrin;
s2: dripping 20g of sodium alginate solution and 2g of tannic acid into 10g of carboxymethyl chitosan solution, stirring, solidifying for 30min, washing, and freeze-drying for 24h to obtain sodium alginate dextrin;
s3: adding 12g of acrylic acid into 50mL of absolute ethyl alcohol, adding 2g of sodium acrylate, 2 gt-butyl acrylamide sulfonic acid and 25mL of deionized water, and uniformly stirring; introducing nitrogen, adding 0.14g of 10% ammonium persulfate solution, and reacting for 3 hours at the temperature of 70 ℃ to obtain a color fixing agent;
s4: adding 300g of starch paste and 300g of sodium alginate paste into water, heating to 50 ℃, uniformly stirring, and standing for 1h to obtain a composite paste solution;
s5: adding 7.5g of acid dye, 7.5g of direct dye, 10g of penetrating agent, 10g of lubricating oil, 50g of urea, 10g of citric acid and 30g of color fixing agent into the composite paste solution, adding water, and uniformly stirring to obtain the environment-friendly mixed acid dye for the mixed wool.
And (3) testing: the color fixing process comprises the following steps:
and (3) placing the prepared mixed acid dye into a 500mL conical flask, heating the mixed acid dye to 80 ℃ in a water bath, placing the mixed wool sample into the conical flask, oscillating and preserving heat for 30min, washing the mixed wool sample with hot water at 60 ℃, washing the mixed wool sample with cold water, and drying the washed mixed wool sample to obtain a sample to be detected.
Soaping color fastness: according to GB/T3921-2008 textile color fastness test: measuring by a soaping fastness method;
color fastness to rubbing: according to GB/T3920-2008 textile color fastness test: measuring by a rubbing color fastness method;
fastness to perspiration: measured according to the method of GB/T3922-1995.
Comparative example 1
S1: dripping 20g of sodium alginate solution and 2g of tannic acid into 10g of carboxymethyl chitosan solution, stirring, solidifying for 30min, washing, and freeze-drying for 24h to obtain sodium alginate dextrin;
s2: adding 12g of acrylic acid into 50mL of absolute ethyl alcohol, adding 2g of sodium acrylate, 2 gt-butyl acrylamide sulfonic acid and 25mL of deionized water, and uniformly stirring; introducing nitrogen, adding 0.14g of 10% ammonium persulfate solution, and reacting for 3 hours at the temperature of 70 ℃ to obtain a color fixing agent;
s3: adding 150g of starch paste and 150g of sodium alginate paste into water, heating to 50 ℃, uniformly stirring, and standing for 1h to obtain a composite paste solution;
s4: adding 5g of acid dye, 5g of direct dye, 5g of penetrating agent, 5g of lubricating oil, 30g of urea, 5g of citric acid and 10g of fixing agent into the composite paste solution, adding water, and uniformly stirring to obtain the environment-friendly mixed acid dye for the mixed wool.
And (3) testing: the color fixing process comprises the following steps:
and (3) placing the prepared mixed acid dye into a 500mL conical flask, heating the mixed acid dye to 80 ℃ in a water bath, placing the mixed wool sample into the conical flask, oscillating and preserving heat for 30min, washing the mixed wool sample with hot water at 60 ℃, washing the mixed wool sample with cold water, and drying the washed mixed wool sample to obtain a sample to be detected.
Soaping color fastness: according to GB/T3921-2008 textile color fastness test: measuring by a soaping fastness method;
color fastness to rubbing: according to GB/T3920-2008 textile color fastness test: measuring by a rubbing color fastness method;
fastness to perspiration: measured according to the method of GB/T3922-1995.
Comparative example 2
S1: under the nitrogen atmosphere, adding 10g of carboxymethyl starch into 20mL of water, heating to 85 ℃, and gelatinizing for 1h to obtain a paste; adjusting the pH value of the paste to 7.5, sequentially adding 10g of potassium persulfate and 0.5g of acrylamide, keeping the temperature at 45 ℃, and stirring for 2 hours; precipitating, filtering, and drying at 60 deg.C for 24 hr to obtain starch dextrin;
s2: adding 12g of acrylic acid into 50mL of absolute ethyl alcohol, adding 2g of sodium acrylate, 2 gt-butyl acrylamide sulfonic acid and 25mL of deionized water, and uniformly stirring; introducing nitrogen, adding 0.14g of 10% ammonium persulfate solution, and reacting for 3 hours at the temperature of 70 ℃ to obtain a color fixing agent;
s3: adding 150g of starch paste and 150g of sodium alginate paste into water, heating to 50 ℃, uniformly stirring, and standing for 1h to obtain a composite paste solution;
s4: adding 5g of acid dye, 5g of direct dye, 5g of penetrating agent, 5g of lubricating oil, 30g of urea, 5g of citric acid and 10g of fixing agent into the composite paste solution, adding water, and uniformly stirring to obtain the environment-friendly mixed acid dye for the mixed wool.
And (3) testing: the color fixing process comprises the following steps:
and (3) placing the prepared mixed acid dye into a 500mL conical flask, heating the mixed acid dye to 80 ℃ in a water bath, placing the mixed wool sample into the conical flask, oscillating and preserving heat for 30min, washing the mixed wool sample with hot water at 60 ℃, washing the mixed wool sample with cold water, and drying the washed mixed wool sample to obtain a sample to be detected.
Soaping color fastness: according to GB/T3921-2008 textile color fastness test: measuring by a soaping fastness method;
color fastness to rubbing: according to GB/T3920-2008 textile color fastness test: measuring by a rubbing color fastness method;
fastness to perspiration: measured according to GB/T3922-1995.
Comparative example 3
S1: under the nitrogen atmosphere, adding 10g of carboxymethyl starch into 20mL of water, heating to 85 ℃, and gelatinizing for 1h to obtain a paste; adjusting the pH value of the paste to 7.5, sequentially adding 10g of potassium persulfate and 0.5g of acrylamide, keeping the temperature at 45 ℃, and stirring for 2 hours; precipitating, filtering, and drying at 60 deg.C for 24 hr to obtain starch dextrin;
s2: dripping 20g of sodium alginate solution and 2g of tannic acid into 10g of carboxymethyl chitosan solution, stirring, solidifying for 30min, washing, and freeze-drying for 24h to obtain sodium alginate dextrin;
s3: adding 150g of starch paste and 150g of sodium alginate paste into water, heating to 50 ℃, uniformly stirring, and standing for 1h to obtain a composite paste solution;
s4: adding 5g of acid dye, 5g of direct dye, 5g of penetrating agent, 5g of lubricating oil, 30g of urea and 5g of citric acid into the composite paste solution, adding water, and uniformly stirring to obtain the environment-friendly mixed acid dye for the mixed wool.
And (3) testing: the color fixing process comprises the following steps:
and (3) placing the prepared mixed acid dye into a 500mL conical flask, heating the mixed acid dye to 80 ℃ in a water bath, placing the mixed wool sample into the conical flask, oscillating and preserving heat for 30min, washing the mixed wool sample with hot water at 60 ℃, washing the mixed wool sample with cold water, and drying the washed mixed wool sample to obtain a sample to be detected.
Soaping color fastness: according to GB/T3921-2008 textile color fastness test: measuring by a soaping fastness method;
color fastness to rubbing: according to GB/T3920-2008 textile color fastness test: measuring by a rubbing color fastness method;
fastness to perspiration: measured according to the method of GB/T3922-1995.
Examples 1-5 show that the color fastness of the sample is best when the mixed acid dye component comprises 30% of starch dextrin, 30% of sodium alginate dextrin, 1.5% of dye, 1% of penetrant, 1% of lubricating oil, 5% of urea, 1.5% of citric acid and 3% of fixing agent, and 27% of water. In comparative example 1 no acrylamide grafted starch was used; in comparative example 2, no chitosan/sodium alginate/tannic acid was used to prepare microcapsules, and in comparative example 3, no polymeric dye fixative was used resulting in a dyed sample having poor color fastness.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A production method of an environment-friendly mixed acid dye for mixed wool is characterized by comprising the following steps: the method comprises the following steps:
s1: adding starch paste and sodium alginate paste into water, heating and stirring uniformly, and standing to obtain a composite paste solution;
s2: adding the dye, the penetrating agent, the lubricating oil, the urea and the color fixing agent into the composite paste solution, adding water, and uniformly stirring to obtain the environment-friendly mixed acid dye for the mixed wool.
2. The method for producing the environment-friendly mixed acid dye for the mixed wool according to claim 1, wherein the method comprises the following steps: in step S1, the starch-based paste is prepared by the steps of:
under the nitrogen atmosphere, adding carboxymethyl starch into water, heating and pasting to obtain a paste; adjusting the pH value of the paste, sequentially adding potassium persulfate and acrylamide, and stirring while keeping the temperature; precipitating, filtering and drying to obtain the starch dextrin.
3. The method for producing the environment-friendly mixed acid dye for the mixed wool according to claim 2, wherein the method comprises the following steps: heating and pasting at 75-85 deg.c for 30-60 min; carboxymethyl starch: acrylamide: the mass ratio of the potassium persulfate is (1-1.5): (1.5-3): (0.05-0.06); adjusting the pH value of the paste liquid to 7.5-9.5; the temperature of the heat preservation and the stirring is 45 to 55 ℃, and the time is 2 to 2.5 hours.
4. The production method of the environment-friendly mixed acid dye for mixed wool according to claim 1, characterized in that: in step S1, the sodium alginate dextrin is prepared by the following method:
and dripping the sodium alginate solution and the tannic acid into the carboxymethyl chitosan solution, stirring, solidifying, washing, and freeze-drying to obtain the sodium alginate dextrin.
5. The method for producing the environment-friendly mixed acid dye for the mixed wool according to claim 4, wherein the method comprises the following steps:
the carboxymethyl chitosan solution is a mixed solution of calcium chloride and carboxymethyl chitosan, wherein the weight ratio of carboxymethyl chitosan: the mass ratio of calcium chloride is 1:10; sodium alginate solution: carboxymethyl chitosan solution: the mass ratio of the tannic acid is (2-4): 1: (0.2-0.4).
6. The method for producing the environment-friendly mixed acid dye for the mixed wool according to claim 1, wherein the method comprises the following steps: in step S2, the fixing agent is prepared by the following method:
adding acrylic acid into absolute ethyl alcohol, adding sodium acrylate, t-butyl acrylamide sulfonic acid and deionized water, and uniformly stirring; and introducing nitrogen, adding an ammonium persulfate solution, and carrying out heat preservation reaction to obtain the color fixing agent.
7. The method for producing the environment-friendly mixed acid dye for the mixed wool according to claim 6, wherein the method comprises the following steps: acrylic acid: sodium acrylate: the mass ratio of the t-butyl acrylamide sulfonic acid is 6:1: (1-3), the adding amount of the ammonium persulfate solution is 0.8-1% of the total mass of the acrylic acid, the sodium acrylate and the t-butyl acrylamide sulfonic acid; the reaction temperature is kept at 65-75 ℃ and the reaction time is 3-4 h.
8. The method for producing the environment-friendly mixed acid dye for the mixed wool according to claim 1, wherein the method comprises the following steps: the environment-friendly mixed acid dye for the mixed wool comprises, by mass, 15-65% of starch dextrin, 15-65% of sodium alginate dextrin, 0.5-1.5% of dye, 0.5-1% of penetrating agent, 0.5-1% of lubricating oil, 3-5% of urea, 0.5-1.5% of citric acid, 1-3% of color fixing agent and the balance of water.
9. The environment-friendly mixed acid dye for mixed wool, which is prepared by the production method of the environment-friendly mixed acid dye for mixed wool according to any one of claims 1 to 8.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101245563A (en) * | 2008-03-12 | 2008-08-20 | 徐辉 | High-efficiency environment protection acidic color fixing agent and manufacture method thereof |
| CN102838898A (en) * | 2012-09-26 | 2012-12-26 | 长胜纺织科技发展(上海)有限公司 | Acidic dye ink for cold transfer printing and application method thereof |
| US20200315168A1 (en) * | 2017-03-26 | 2020-10-08 | The American University In Cairo | Aroma-Loaded Microcapsules with Antibacterial Activity for Eco-friendly Applications |
| CN112323520A (en) * | 2020-11-16 | 2021-02-05 | 五邑大学 | Nylon, nylon/spandex acid dye printing anti-staining soaping agent and preparation method thereof |
| CN112941931A (en) * | 2021-01-29 | 2021-06-11 | 浙江金典印染有限公司 | Printing process of polyester fabric |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101245563A (en) * | 2008-03-12 | 2008-08-20 | 徐辉 | High-efficiency environment protection acidic color fixing agent and manufacture method thereof |
| CN102838898A (en) * | 2012-09-26 | 2012-12-26 | 长胜纺织科技发展(上海)有限公司 | Acidic dye ink for cold transfer printing and application method thereof |
| US20200315168A1 (en) * | 2017-03-26 | 2020-10-08 | The American University In Cairo | Aroma-Loaded Microcapsules with Antibacterial Activity for Eco-friendly Applications |
| CN112323520A (en) * | 2020-11-16 | 2021-02-05 | 五邑大学 | Nylon, nylon/spandex acid dye printing anti-staining soaping agent and preparation method thereof |
| CN112941931A (en) * | 2021-01-29 | 2021-06-11 | 浙江金典印染有限公司 | Printing process of polyester fabric |
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