CN115538195B - Color fixation finishing method and application thereof in pure cotton printing and dyeing - Google Patents
Color fixation finishing method and application thereof in pure cotton printing and dyeing Download PDFInfo
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- CN115538195B CN115538195B CN202211231371.1A CN202211231371A CN115538195B CN 115538195 B CN115538195 B CN 115538195B CN 202211231371 A CN202211231371 A CN 202211231371A CN 115538195 B CN115538195 B CN 115538195B
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 229920000742 Cotton Polymers 0.000 title claims abstract description 21
- 238000007639 printing Methods 0.000 title abstract description 11
- 238000004043 dyeing Methods 0.000 title description 12
- 239000004744 fabric Substances 0.000 claims abstract description 61
- 229920002545 silicone oil Polymers 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000005406 washing Methods 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 19
- 229920013822 aminosilicone Polymers 0.000 claims description 19
- 125000001302 tertiary amino group Chemical group 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 9
- XSFWXFNRRQJFKN-UHFFFAOYSA-N 1-chloro-2-ethenylsulfonylethane Chemical group ClCCS(=O)(=O)C=C XSFWXFNRRQJFKN-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 6
- 150000001412 amines Chemical class 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- FHLZUEPKLGQEQP-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]-n,n-diethylpropan-1-amine Chemical compound CCN(CC)CCC[Si](C)(OC)OC FHLZUEPKLGQEQP-UHFFFAOYSA-N 0.000 claims description 2
- 125000003277 amino group Chemical group 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000000413 hydrolysate Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000004448 titration Methods 0.000 claims description 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 8
- 239000011964 heteropoly acid Substances 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 238000007730 finishing process Methods 0.000 abstract description 3
- 230000002045 lasting effect Effects 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 17
- 239000003921 oil Substances 0.000 description 12
- 239000003795 chemical substances by application Substances 0.000 description 9
- 239000000835 fiber Substances 0.000 description 8
- 239000000975 dye Substances 0.000 description 7
- 239000000985 reactive dye Substances 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- 239000002390 adhesive tape Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 description 3
- 238000005160 1H NMR spectroscopy Methods 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 2
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- DRRZZMBHJXLZRS-UHFFFAOYSA-N n-[3-[dimethoxy(methyl)silyl]propyl]cyclohexanamine Chemical compound CO[Si](C)(OC)CCCNC1CCCCC1 DRRZZMBHJXLZRS-UHFFFAOYSA-N 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229920000768 polyamine Polymers 0.000 description 2
- -1 quaternary ammonium ions Chemical class 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000222122 Candida albicans Species 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940095731 candida albicans Drugs 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 230000009615 deamination Effects 0.000 description 1
- 238000006481 deamination reaction Methods 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000005956 quaternization reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- TXROVKYTPPNNJW-UHFFFAOYSA-N silicon(4+) tetramethylazanium Chemical compound [Si+4].C[N+](C)(C)C TXROVKYTPPNNJW-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/08—After-treatment with organic compounds macromolecular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/26—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen nitrogen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
- C08G77/28—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen sulfur-containing groups
-
- 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
- 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
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Coloring (AREA)
Abstract
The invention discloses a fixation finishing method, which comprises the steps of washing dyed cotton fabric, drying, immersing in modified silicone oil solution, immersing at 60 ℃ for 30min, adding water-soluble heteropoly acid, continuing to keep the temperature for 10min, adding alkali to adjust pH=7-8, and keeping the temperature for 20min; and then baking, soaping and drying the treated cotton fabric. According to the technical scheme, the color fixation and finishing processes are integrated, so that the process flow is greatly shortened; by adopting the method, the jet printing effect of the fabric is better. The color fixing finishing method provided by the invention is used for treating cotton fabrics, so that fabrics with soft hand feeling, high rubbing color fastness and high soaping color fastness can be obtained, and the color fixing finishing method has lasting and effective excellent antibacterial property.
Description
Technical Field
The invention belongs to the technical field of printing and dyeing, and particularly relates to a fixation finishing method and application thereof in pure cotton printing and dyeing.
Background
Cotton and other cellulosic fibers are often dyed with reactive dyes. In the reactive dye dyeing process, a large amount of salt is required to be added to promote dye-uptake, and fixation is required to be carried out under high-alkali conditions in the later dyeing period. In the fixation process, a part of reactive dye reacts with cellulose fiber under the action of alkali to form covalent bond combination; at the same time, the dye which does not react with the fiber is partially hydrolyzed under alkaline conditions and adsorbed on the fiber. These unfixed dyes directly lead to a decrease in the color fastness of the dyed fabric. Therefore, in practical production, a color fixing agent is commonly used for fixing the dyed fabric so as to improve color fastness. With the development of society, people are increasingly researching environment-friendly formaldehyde-free color fixing agents. The polyamine type color fixing agent is a high molecular compound formed by the reaction of diethylenetriamine and dicyandiamide and the steps of condensation, deamination, polycondensation and the like, and the structure of the polyamine type color fixing agent contains more reactive groups and can be combined with dye and fiber in a covalent bond way, so that the color fastness of the fabric is improved. However, a large amount of ammonia gas is generated during the reaction, which makes the production limited. The other is a polycation type color fixing agent (polydimethyldiallyl ammonium chloride, PDADMAC) which is prepared by polymerizing a cationic monomer of dimethyldiallyl ammonium chloride (DADMAC) in an aqueous solution through free radicals. PDADMAC has positive charges with higher density, can be combined with dye anions in an ionic bond way, and improves the color fastness of the fabric. However, due to the excellent water solubility of PDADMAC, the color-fixed fabrics have poor washing fastness, and most of the dye still enters the water phase through washing under the action of mechanical external force. Therefore, the development of a novel fixing agent and the application of the novel fixing agent to reactive dye cotton dyeing are of great significance.
Disclosure of Invention
Aiming at the technical current situation of dyeing cotton fixation, the invention provides a fixation finishing method, which adopts a one-pot method to fix and finish dyed cotton fabric simultaneously, shortens the process flow, simultaneously overcomes the problems of pollution emission and low friction color fastness of the fixation process in the prior art, simultaneously endows the cotton fabric with excellent antibacterial performance, has soft hand feeling and greatly improves the color depth.
The invention is realized in such a way that the invention provides the following technical scheme: the color fixing finishing method comprises the following steps:
(1) Preparing modified silicone oil: hydrolyzing N, N-diethyl amine propyl methyl dimethoxy silane with anhydrous diethyl ether as solvent under alkaline condition to prepare total grafted tertiary amino silicone oil; further, mixing N, N-diethyl amine propyl methyl dimethoxy silane with D4 and MM according to a metering ratio, and heating to react under the catalysis of tetramethylammonium silicon alkoxide hydroxide to prepare tertiary amino silicone oil; and (3) taking ethanol as a solvent, and carrying out quaternization reaction on tertiary amino silicone oil and (2-chloroethanesulfonyl) ethylene to obtain the modified silicone oil.
(2) Fixation and finishing: washing and drying dyed cotton fabric, immersing in modified silicone oil solution, immersing at 60 ℃ for 30min, adding water-soluble heteropoly acid, continuing to keep the temperature for 10min, adding alkali to adjust pH=7-8, and keeping the temperature for 20min.
(3) Baking, soaping and drying the treated cotton fabric.
Baking is carried out for 1-5 min at 60-80 ℃, then heating to 130-150 ℃ for baking for 3-8 min, then soaping for 20-40 min at 80-100 ℃, and finally drying.
(4) And (5) performing jet printing on the fabric.
Further, the modified silicone oil has the following molecular structure:
wherein m/n=1 to 5:1.
Further, in the step (2), the modified silicone oil solution is an aqueous solution, the bath ratio is 1:10, and the dosage is 5% o.w.f.
Further, in the step (2), the water-soluble heteropolyacid is preferably nano phosphotungstic acid; the dosage is 1-2% o.w.f.
Further, in the step (2), the alkali is NaOH or Na 2 CO 3 One or more of the following.
Color fixation finishing process principle:
the heteropoly acid is a metal oxide cluster with a sub-nano structure, can be combined with quaternary ammonium ions through electrostatic acting force, and can be compounded with quaternary ammonium to form a cross-linked structure. On the other hand, research shows that the heteropolyacid is a good antibacterial agent, and anions and quaternary ammonium cations of the heteropolyacid can exert synergistic antibacterial performance through electrostatic acting force combination, so that the heteropolyacid is a novel antibacterial agent.
On the other hand, after the metal oxide clusters with the sub-nano structure are combined with the silicone oil chain segments through electrostatic acting force, the metal oxide clusters are fixed on the polymer and attached to the surface of the fiber, the roughness of the surface of the fiber is obviously improved when observed under an SEM, and meanwhile, the fiber after fixation and finishing has hydrophilicity and roughness at the same time because the hydrophilicity of the heteropoly acid is extremely strong, so that good conditions are improved for the spray printing of subsequent fabrics.
The color development efficiency of the dye is improved, and the color of the dyed fabric is deepened. Padding in an aqueous solution of a cross-linking agent before prebaking can improve the rubbing fastness.
Further, after the pH is regulated to be alkaline, hydroxyl groups of the cotton fabric are protonated and crosslinked with vinyl groups in the silicone oil, so that the silicone oil is bonded on the fabric, the adhesion rate of the curing finishing agent is improved, and the fabric is endowed with lasting antibacterial property, flexibility and color fastness.
The invention has the following advantages and beneficial effects:
(1) The color fixation finishing method integrates the color fixation and finishing processes, so that the process flow is greatly shortened; by adopting the method, the jet printing effect of the fabric is better.
(2) The color fixing finishing method provided by the invention is used for treating cotton fabrics, so that fabrics with soft hand feeling, high rubbing color fastness and high soaping color fastness can be obtained, and the color fixing finishing method has lasting and effective excellent antibacterial property.
Drawings
FIG. 1 is a tertiary amino silicone oil 1 H-NMR。
FIG. 2 is a modified silicone oil 1 H-NMR。
Fig. 3 is an SEM image of cotton fabric fibers (a base fabric, b fabric sample 4, c fabric sample 1, d fabric sample 2, e fabric sample 3).
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art.
The invention tests:
(1) Antibacterial test: the evaluation was carried out according to GB/T20944.3-2008 vibration method for antibacterial properties. Test instrument: a spectrophotometer. Experimental strain: staphylococcus aureus (ATCC 6538), escherichia coli (ATCC 25922), candida albicans (ATCC 10231).
The testing method comprises the following steps: 0.75+ -0.05 g of the cloth sample was weighed into a Erlenmeyer flask, and 70mL of PBS buffer was added. Into a Erlenmeyer flask, 4×10 was added 5 CFU/mL of bacterial liquid 5mL is placed in a constant temperature oscillator for shake culture at 24+/-1 ℃ for 18h. Measuring absorbance of the culture solution, obtaining the concentration of viable bacteria according to a standard curve, and calculating the bacteriostasis rate according to the following formula:
blank refers to no cloth added.
(2) Softness test: the effect of the finishing agent on the treated fabric is evaluated by feeling the combination factors such as the bulk, softness, rebound resilience and smoothness of the treated fabric by touching with hands, and the hand feeling is classified into 5 grades, the higher the grade is, the better the grade is, the 5 grades are the best, and the grade 1 is the lowest.
(3) Color fastness testing:
the fastness to soaping is determined according to the method of GB/T3921-2008 "fastness to soaping for textile color fastness test".
The rubbing fastness was determined according to GB/T3920-2008 "rubbing fastness to fabric fastness test".
(4) Scanning electron microscope test: and (3) spreading the test sample subjected to metal spraying on a conductive double-sided adhesive tape by adopting a scanning electron microscope manufactured by Smart Lab Japan, adhering the double-sided adhesive tape on a test sample stage, and then purging the sample stage on which the sample is adhered with nitrogen for a plurality of times, and then testing.
(5) Static water contact angle test: the sample was placed on a test bench using a DSA 100 contact angle measuring instrument manufactured by Kruss, germany, fixed with a double sided adhesive tape, kept flat, and tested in three different areas of the same sample using a contact angle measuring instrument, and the results were averaged. The volume of the water droplet used in the measurement was 5. Mu.L.
(6) The color effect of the fabric is evaluated by K/S, the color is measured by a Datacolor SF650 color measuring and matching instrument, a D65 light source and a 10-degree visual angle are selected, the K/S value at the maximum absorption wavelength of the dyed fabric is measured, each sample is measured for 4 times at different positions, and the average value is obtained.
Example 1
Preparing modified silicone oil.
S1: preparation of tertiary amino silicone oil
100mL of anhydrous diethyl ether and 60g of N, N-diethylaminopropyl methyl dimethoxy silane are added into a three-neck flask equipped with an electric stirrer, a thermometer and a reflux condenser, the mixture is stirred and heated to 40 ℃, 17g of 20wt% NaOH aqueous solution is slowly added dropwise, the hydrolysate is poured into a separating funnel after 4 hours, the mixture is washed with water until the pH value is 8, and an ether layer is prepared by using anhydrous MgSO 4 Drying, filtering and evaporating diethyl ether to obtain the full-grafted tertiary amino silicone oil, wherein the amine value measured by a non-aqueous titration method is 4.24mmol/g.
Is provided with N 2 Adding full-grafted tertiary amino silicone oil into a four-neck flask of a protection device, an electric stirrer, a thermometer and a condenser tube, and D 4 And (2) the MM and the tetramethylammonium hydroxide accounting for 1 weight percent of the total mass of the raw materials are heated to 90 ℃ to react for 9 hours, then heated to 150 ℃ and stirred for 30 minutes to decompose the catalyst. And (3) removing small molecular low-boiling substances by rotary evaporation at 120 ℃ to obtain the target product tertiary amino silicone oil.
The amount of tertiary amino silicone oil (PtAMS) charged, the amine number and the molecular weight are shown in the following table.
TABLE 1
The number average molecular weight (Mn) was measured by using a Waters 515-2414 type gel permeation chromatograph, chloroform as the mobile phase, a flow rate of 1mL/min, a detector temperature of 35℃and a column temperature of 40℃and a narrow distribution of Polystyrene (PS) as the standard.
S2: preparation of modified silicone oil
Adding tertiary amino silicone oil, absolute ethyl alcohol and heating to 90 ℃ into a three-port reaction bottle provided with a thermometer, a stirring device and a condenser tube, starting to dropwise add an ethanol solution of (2-chloroethanesulfonyl) ethylene, carrying out heat preservation reflux reaction for 30h, removing a solvent by evaporation, dissolving and dialyzing for 3d again by water to remove (2-chloroethanesulfonyl) ethylene, and drying to obtain the modified silicone oil. The ratio of the amine group molar quantity of the tertiary amino silicone oil to the molar quantity of the (2-chloroethanesulfonyl) ethylene is 1:3.
Example 2
The cotton fabric adopts bleached and mercerized pure cotton knitted fabric (21 counts, 180 g/m) 2 And (3) cargo number: DM1, manufacturer: guangzhou Fuguang Kongya textile dyeing and finishing plant), cotton fabrics are dyed using the following conditions: the dye is active scarlet 3BS (purchased from Zhejiang leap soil Co., ltd.) with the dosage of 3% o.w.f, the bath ratio of 1:10, the temperature of 60 ℃ and the time of 60min; washing with water (bath ratio 1:10, temperature 60 deg.C, time 10 min); drying (120 ℃ C., 20 min) was performed.
The dyed cloth is soaked into modified silicone oil solution for fixation, soaked for 30min at 60 ℃ (the bath ratio is 1:10, the dosage is 5% o.w.f.), then phosphotungstic acid (the dosage is 0% -3% o.w.f, purchased from Shanghai Ala Latin Biochemical technology Co., ltd.) is added, after the mixture is stirred for 10min at 200rmp, naOH solid is added to adjust pH to 7-8, the mixture is kept for 20min, the fabric is fished out for prebaking (60 ℃ for 3 min), then the mixture is heated to baking (140 ℃ for 6 min), then soaping (2 g/L DB-5, the bath ratio is 1:10, the temperature is 90 ℃ for 20 min), and finally drying (the temperature is 120 ℃ for 20 min) is carried out.
The treatment recipe for the swatches is shown in table 2 below.
TABLE 2
| Sample of | The dosage of phosphotungstic acid,% o.w.f |
| Sample cloth 1 | 2 |
| Sample cloth 2 | 1 |
| Sample cloth 3 | 3 |
| Cloth sample 4 | 0 |
Comparative example 1
The cotton fabric is dyed, fixed and finished in a conventional manner and is marked as sample 5.
The specific flow is as follows: padding dyeing, drying (80 ℃), impregnating fixation, steaming (100 ℃,70 seconds), washing (bath ratio 1:10, 60 ℃,10 minutes), soaping (2 g/L DB-5, bath ratio 1:10, 90 ℃,20 minutes), washing (bath ratio 1:10, 60 ℃,10 minutes), drying (80 ℃), padding finishing liquor, drying (10 minutes pre-baking at 90 ℃,5 minutes baking at 120 ℃).
Padding and dyeing: active scarlet 3BS (the dosage is 3% o.w.f), anhydrous sodium sulphate 50g/L; the rolling surplus rate is 65 percent.
Color fixing liquid: 6g/L sodium hydroxide, 20g/L sodium carbonate and 200g/L sodium chloride; the bath ratio is 1:10, the temperature is 60 ℃, and the time is 60min.
Finishing liquid: amino silicone oil (amine value 0.6mmol/g, viscosity 5000cP, purchased from Jinan Xinglong chemical industry Co., ltd.) 30%, emulsifier 5% (TO-5/TO-7=1:1), and water in balance; the rolling surplus rate is 80 percent.
The results of each test of the finished fabric are shown in tables 3 to 4.
Table 3:
table 4: antibacterial rate (machine washing)%, percent
Washing: the type B agitator washing machine and washing program 8B were selected as specified in GB 8629-2001 "household washing and drying program for textile test".
Example 4
And carrying out digital printing on the fabric and carrying out color depth testing.
The fabric is directly immersed into modified silicone oil solution without dyeing, immersed for 30min at 60 ℃ (bath ratio is 1:10, dosage is 5% o.w.f.), then phosphotungstic acid (dosage is 0-3% o.w.f.) is added, stirring is carried out for 10min at 200rmp under heat preservation, naOH solid is added to adjust pH=7-8, heat preservation is carried out for 20min, the fabric is fished out for prebaking (60 ℃ for 3 min), then heating to baking (140 ℃ for 6 min), then soaping (2 g/L DB-5, bath ratio is 1:10, temperature is 90 ℃ for 20 min), and finally drying (temperature 120 ℃ for 20 min) is carried out.
The dried fabric was digital printed using water-based paint ink for strapdown textile, purchased from digital technologies, inc. of Hongsheng Zhengzhou, and used in four colors of C (cyan), M (red), Y (yellow) and K (black). The adopted digital printer is an HJ-RCT8460 digital printer manufactured by Shishihong color fly digital technology Co., ltd, a single-channel Beijing ceramic nozzle is adopted, the printing precision is 720dpi multiplied by 2160dpi, and the highest printing speed is 550m 2 And/h. Baking the fabric subjected to the ink-jet printing at the temperature of 140 ℃ for 3min; then washing with water (30 ℃ C., 10min, bath ratio 1:10), and soaping (2 g/L DB-5, bath ratio 1:10, temperature 90 ℃ C., time 20 min).
The color depth of the printed fabric is assessed, the color depth is measured by a Datacolor SF650 color measuring and matching instrument, a D65 light source and a 10-degree visual angle are selected, the K/S value at the maximum absorption wavelength of the dyed fabric is measured, each sample is measured for 4 times at different positions, and the average value is obtained, so that the result is as follows:
table 5:
the above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (6)
1. The color fixing finishing method is characterized by comprising the following steps of:
(1) Fixation and finishing: washing and drying the dyed fabric, immersing the dyed fabric in a modified silicone oil solution, immersing the dyed fabric at 60 ℃ for 30min, adding phosphotungstic acid, continuously preserving heat and immersing for 10min, adding alkali to adjust pH=7-8, and preserving heat for 20min;
(2) Baking, soaping and drying the treated fabric
Baking specifically, pre-baking at 60-80 ℃ for 1-5 min, then heating to 130-150 ℃ for 3-8 min, soaping at 80-100 ℃ for 20-40 min, and finally drying;
the preparation method of the modified silicone oil comprises the following steps:
s1: preparation of tertiary amino silicone oil
100mL of anhydrous diethyl ether and 60g of N, N-diethylaminopropyl methyl dimethoxy silane are added into a three-neck flask equipped with an electric stirrer, a thermometer and a reflux condenser, the mixture is stirred and heated to 40 ℃, 17g of 20wt% NaOH aqueous solution is slowly added dropwise, the hydrolysate is poured into a separating funnel after 4 hours, the mixture is washed with water until the pH value is 8, and the ether layer is prepared by using anhydrous MgSO 4 Drying, filtering and evaporating diethyl ether to obtain the full-grafted tertiary amino silicone oil, wherein the amine value measured by a non-water titration method is 4.24 mmol/g;
is provided with N 2 Protection device, electric stirrer, thermometer and condenser were added with 23.02g of full-grafted tertiary amino silicone oil, 21.72. 21.72g D 4 1.24g of MM and tetramethyl ammonium hydroxide accounting for 1wt% of the total mass of the raw materials are heated to 90 ℃ for reaction for 9 hours, then heated to 150 ℃ and stirred for 30min to decompose the catalyst; spin-evaporating at 120deg.C to remove small molecular low-boiling substances to obtain tertiary amino silicone oil; the tertiary amino silicone oil has a number average molecular weight of 5125g/mol and an amine value of 2.56mmol/g;
s2: preparation of modified silicone oil
Adding tertiary amino silicone oil, absolute ethyl alcohol and heating to 90 ℃ into a three-port reaction bottle provided with a thermometer, a stirring device and a condenser tube, starting to dropwise add an ethanol solution of (2-chloroethanesulfonyl) ethylene, carrying out heat preservation reflux reaction for 30h, removing a solvent by evaporation, dissolving and dialyzing for 3d again by water to remove (2-chloroethanesulfonyl) ethylene, and drying to obtain modified silicone oil; the ratio of the amine group molar quantity of the tertiary amino silicone oil to the molar quantity of the (2-chloroethanesulfonyl) ethylene is 1:3.
2. the color fixing finishing method according to claim 1, wherein the dosage of the phosphotungstic acid is 1-2% o.w.f.
3. The color fixing finishing method according to claim 1, wherein the modified silicone oil solution in the step (1) is an aqueous solution, the bath ratio is 1:10, and the dosage is 5% o.w.f.
4. The color fixing finishing method according to claim 1, wherein the alkali in the step (1) is NaOH or Na 2 CO 3 One or more of the following.
5. The color fixing finishing method according to claim 1, wherein the fabric is printed after baking, soaping and drying.
6. The color fixing finishing method according to any one of claims 1 to 5, wherein the fabric is a pure cotton fabric.
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