CN115538195A - Color fixing finishing method and application thereof in pure cotton printing and dyeing - Google Patents
Color fixing finishing method and application thereof in pure cotton printing and dyeing Download PDFInfo
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- CN115538195A CN115538195A CN202211231371.1A CN202211231371A CN115538195A CN 115538195 A CN115538195 A CN 115538195A CN 202211231371 A CN202211231371 A CN 202211231371A CN 115538195 A CN115538195 A CN 115538195A
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- 238000000034 method Methods 0.000 title claims abstract description 30
- 229920000742 Cotton Polymers 0.000 title claims abstract description 25
- 238000007639 printing Methods 0.000 title abstract description 12
- 238000004043 dyeing Methods 0.000 title description 10
- 239000004744 fabric Substances 0.000 claims abstract description 68
- 229920002545 silicone oil Polymers 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- 239000011964 heteropoly acid Substances 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 238000007730 finishing process Methods 0.000 claims abstract description 5
- 238000002791 soaking Methods 0.000 claims abstract description 5
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- 229920013822 aminosilicone Polymers 0.000 claims description 16
- 239000003921 oil Substances 0.000 claims description 16
- 125000001302 tertiary amino group Chemical group 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- -1 N, N-diethylamine propyl methyl dimethoxy silane Chemical compound 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- XSFWXFNRRQJFKN-UHFFFAOYSA-N 1-chloro-2-ethenylsulfonylethane Chemical group ClCCS(=O)(=O)C=C XSFWXFNRRQJFKN-UHFFFAOYSA-N 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 5
- 239000002904 solvent Substances 0.000 claims description 5
- 150000001412 amines Chemical class 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 125000003277 amino group Chemical group 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000005956 quaternization reaction Methods 0.000 claims description 2
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- 238000012360 testing method Methods 0.000 description 17
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- 239000003795 chemical substances by application Substances 0.000 description 8
- 239000000975 dye Substances 0.000 description 8
- 239000000835 fiber Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000985 reactive dye Substances 0.000 description 4
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- 230000009471 action Effects 0.000 description 3
- 238000011161 development Methods 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
- 239000000047 product Substances 0.000 description 3
- 238000005160 1H NMR spectroscopy Methods 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 group 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
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 150000001450 anions Chemical class 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
- 238000005516 engineering process Methods 0.000 description 2
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- 125000001453 quaternary ammonium group Chemical group 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
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- 238000005096 rolling process Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 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
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 239000000022 bacteriostatic agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 229940095731 candida albicans Drugs 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
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- 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
- 238000001704 evaporation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
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- 239000003973 paint Substances 0.000 description 1
- 229920000768 polyamine Polymers 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
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 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
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000017550 sodium carbonate Nutrition 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
- 230000003068 static effect Effects 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Images
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- 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
Abstract
The invention discloses a color fixing finishing method, which comprises the steps of washing and drying a dyed cotton fabric, immersing the cotton fabric into a modified silicone oil solution, soaking the cotton fabric for 30min at 60 ℃, adding water-soluble heteropoly acid, continuing to keep the temperature and soak for 10min, adding alkali to adjust the pH to be 7-8, and keeping the temperature for 20min; and then the treated cotton fabric is subjected to baking, soaping and drying treatment. The color fixing and finishing processes are integrated under the technical scheme of the invention, so that the process flow is greatly shortened; by adopting the method, the jet printing effect of the fabric can be better. The color fixing finishing method provided by the invention is used for processing cotton fabrics, so that the fabrics with soft hand feeling, high friction color fastness and high soaping color fastness can be obtained, and the fabrics have lasting, effective and excellent antibacterial property.
Description
Technical Field
The invention belongs to the technical field of printing and dyeing, and particularly relates to a color fixing and finishing method and application thereof in pure cotton printing and dyeing.
Background
Cotton and other cellulosic fibers are commonly dyed with reactive dyes. A large amount of salt is required to be added in the dyeing process of the reactive dye to promote the dye to be dyed, and the color fixation is required to be carried out under the condition of high alkali in the later dyeing stage. In the color fixing process, a part of reactive dye reacts with cellulose fiber under the action of alkali to form covalent bond combination; meanwhile, the dye which does not react with the fiber is partially hydrolyzed under the alkaline condition and is adsorbed on the fiber. These unfixed dyes directly lead to a reduction in the fastness of the dyed fabric. Therefore, in actual production, a color fixing agent is commonly used for fixing the dyed fabric so as to improve the color fastness. With the development of society, people have more and more researches on environment-friendly formaldehyde-free color fixing agents. The polyamine color fixing agent is a macromolecular compound formed by reacting diethylenetriamine with dicyandiamide and performing condensation, deamination, polycondensation and other steps, has a structure containing more reactive groups, can be combined with dyes and fibers by covalent bonds, and improves the color fastness of fabrics. However, a large amount of ammonia gas is generated in the reaction process, so that the production is limited. The other is a polycation color fixing agent (PDADMAC), which is prepared by polymerizing cationic monomer dimethyl diallyl ammonium chloride (DADMAC) in water solution through free radicals. PDADMAC has higher-density positive charges, can be combined with dye anions through ionic bonds, and improves the color fastness of the fabric. However, because PDADMAC has excellent water solubility, the fastness to washing of the fixed fabric is not good, and most of the dye still enters the water phase through the washing action especially under the action of mechanical external force. Therefore, the development of a novel color fixing agent and the application of the color fixing agent in dyeing cotton by using reactive dyes are of great significance.
Disclosure of Invention
Aiming at the technical current situation of color fixation of dyed cotton, the invention provides a color fixation finishing method, which adopts a one-pot method to simultaneously fix and finish the color of the dyed cotton fabric, shortens the process flow, overcomes the problems of pollution discharge and low friction color fastness of the color fixation process in the prior art, 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, and provides the following technical scheme: the color fixing finishing method comprises the following steps:
(1) Preparing modified silicone oil: using anhydrous ether as a solvent, and hydrolyzing N, N-diethylamine propyl methyl dimethoxy silane under an alkaline condition to prepare fully grafted tertiary amino silicone oil; further, mixing N, N-diethylamine propyl methyl dimethoxy silane with D4 and MM according to a metering ratio, and heating to react under the catalysis of tetramethylammonium hydroxide silicon alkoxide to prepare tertiary amino silicone oil; the modified silicone oil is prepared by quaternization reaction of tertiary amino silicone oil and (2-chloroethanesulfonyl) ethylene by using ethanol as a solvent.
(2) Fixation and finishing: washing and drying the dyed cotton fabric, immersing the cotton fabric into a modified silicone oil solution, soaking the cotton fabric for 30min at 60 ℃, adding water-soluble heteropoly acid, keeping the temperature for soaking for 10min, adding alkali to adjust the pH to be 7-8, and keeping the temperature for 20min.
(3) And (3) baking, soaping and drying the treated cotton fabric.
The baking is carried out for 1-5 min at 60-80 ℃, then the temperature is raised to 130-150 ℃ for baking 3-8 min, and then the product is soaped for 20-40 min at 80-100 ℃, and finally the product is dried.
(4) And (4) carrying out jet printing on the fabric.
Further, the modified silicone oil has the following molecular structure:
wherein m/n =1 to 5: 1.
Further, the modified silicone oil solution in the step (2) was an aqueous solution, the bath ratio was 1: 10, and the amount was 5% by volume o.w.f.
Further, the water-soluble heteropoly acid in the step (2) is preferably nano phosphotungstic acid; the amount is 1 to 2% by weight.
Further, in the step (2), the alkali is NaOH or Na 2 CO 3 One or more of (a).
The color fixing and finishing process principle comprises the following steps:
the heteropoly acid is a metal oxide cluster with a sub-nanometer structure, can be combined with quaternary ammonium ions through electrostatic acting force, and a Keggin type heteropoly acid can be compounded with quaternary ammonium to form a cross-linked structure. On the other hand, the research shows that the heteropoly acid is a good bacteriostatic agent, the anion of the heteropoly acid and the quaternary ammonium cation of the heteropoly acid can exert the synergistic antibacterial performance through the combination of the electrostatic acting force, and the heteropoly acid is a novel antibacterial agent.
On the other hand, after the metal oxide clusters with the sub-nanometer structures and the silicone oil chain segments are combined 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 under SEM observation, and meanwhile, as the heteropoly acid has extremely strong hydrophilicity, the fiber after fixation and finishing has both hydrophilicity and roughness, 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. Before prebaking, padding in a cross-linking agent aqueous solution can improve the rubbing fastness.
Furthermore, after the pH value is adjusted to be alkaline, the 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, the fabric is endowed with lasting antibiosis and flexibility, and the color fastness is improved.
The invention has the following advantages and beneficial effects:
(1) The color fixing finishing method integrates the color fixing and finishing processes, so that the process flow is greatly shortened; by adopting the method, the jet printing effect of the fabric can be better.
(2) The color fixing finishing method provided by the invention is used for treating cotton fabrics, so that the fabrics with soft hand feeling, high friction color fastness and high soaping color fastness can be obtained, and the fabric has lasting, effective and excellent antibacterial property.
Drawings
FIG. 1 shows tertiary amino silicone oil 1 H-NMR。
FIG. 2 shows modified silicone oil 1 H-NMR。
FIG. 3 is SEM image of cotton fabric fibers (a original cloth, b cloth sample 4, c cloth sample 1, d cloth sample 2 and e cloth sample 3).
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited to these examples in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
The test of the invention comprises the following steps:
(1) And (3) antibacterial testing: and evaluating according to a GB/T20944.3-2008 antibacterial performance oscillation method. Testing an instrument: a spectrophotometer is provided. Experimental strains: staphylococcus aureus (ATCC 6538), escherichia coli (ATCC 25922), candida albicans (ATCC 10231).
The test method comprises the following steps: 0.75. + -. 0.05g of the cloth sample was weighed into a Erlenmeyer flask, and 70mL of PBS buffer was added. Into a Erlenmeyer flask, 4X 10 5 5mL of CFU/mL bacterial solution is placed in a constant temperature oscillator to be subjected to shake culture for 18h at the temperature of 24 +/-1 ℃. Measuring the absorbance of the culture solution, obtaining the viable bacteria concentration according to a standard curve, and calculating the bacteriostasis rate according to the following formula:
blank group means no swatches added.
(2) Flexibility test: the effect of the finishing agent on the treated fabric is evaluated by feeling comprehensive factors such as bulkiness, softness, resilience, smoothness and the like of the treated fabric in a manner of touching by hands, the hand feeling is totally divided into 5 grades, the higher grade is better, the 5 grade is best, and the 1 grade is lowest.
(3) And (3) testing color fastness:
the soaping color fastness is measured according to the method of GB/T3921-2008 soaping color fastness resistance test for textiles.
The color fastness to rubbing is determined according to GB/T3920-2008 'color fastness to rubbing test for fabrics'.
(4) And (3) testing a scanning electron microscope: a scanning electron microscope manufactured by Smart Lab Japan science company is adopted, a test sample after being sprayed with gold is tiled and adhered on a conductive double-sided adhesive, the double-sided adhesive is adhered on a test sample table, the sample table adhered with the sample is blown by nitrogen for a plurality of times, and then the test is carried out.
(5) Static water contact angle test: a DSA 100 contact angle measuring instrument manufactured by Germany Kruss company is adopted, a sample is placed on a test bench, a double-sided adhesive tape is used for fixing, the surface is kept flat, the contact angle measuring instrument is used for testing three different areas of the same sample, and the results are averaged. The water drop volume used for the measurement was 5. Mu.L.
(6) The color obtaining effect of the fabric is evaluated by K/S, a Datacolor SF650 color measuring and matching instrument is adopted for measuring, 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 at different positions for 4 times, and the average value of the K/S values is taken.
Example 1
And preparing the modified silicone oil.
S1: preparation of tertiary amino silicone oil
Adding anhydrous ether 100mL and N, N-diethylamine propyl methyldimethoxysilane 60g into a three-neck flask equipped with electric stirrer, thermometer and reflux condenser, stirring and heating to 40 deg.C, slowly adding dropwise NaOH aqueous solution 17g,4h, pouring the hydrolysate into a separating funnel, washing with water to pH =8, and collecting ether layer with anhydrous MgSO 2 4 Drying, filtering and distilling to remove ether to obtain the full-grafted tertiary amino silicone oil, wherein the amine value is 4.24mmol/g by a non-aqueous titration method.
In the presence of N 2 Adding full-grafted tertiary amino silicone oil D into a four-neck flask with a protection device, an electric stirrer, a thermometer and a condenser pipe 4 Heating MM and tetramethylammonium hydroxide accounting for 1wt% of the total mass of the raw materials to 90 ℃ for reaction for 9 hours, then heating to 150 ℃, and continuously stirring for 30min to decompose the catalyst. And (3) carrying out rotary evaporation at 120 ℃ to remove small-molecule low-boiling-point substances to obtain the target product tertiary amino silicone oil.
The charge, amine number and molecular weight of the tertiary amino silicone oil (PtAMS) are shown in the table below.
TABLE 1
The number average molecular weight (Mn) is measured by Waters 515-2414 type gel permeation chromatograph, the mobile phase is chloroform, the flow rate is 1mL/min, the detector temperature is 35 ℃, the column temperature is 40 ℃, and the standard sample is narrow-distribution Polystyrene (PS).
S2: preparation of modified Silicone oils
Adding tertiary amino silicone oil and absolute ethyl alcohol into a three-mouth reaction bottle provided with a thermometer, a stirring device and a condenser tube, heating to 90 ℃, starting to dropwise add an ethanol solution of (2-chloroethanesulfonyl) ethylene, carrying out heat preservation reflux reaction for 30 hours, evaporating to remove the solvent, dissolving again in water, dialyzing for 3d to remove the (2-chloroethanesulfonyl) ethylene, and drying to obtain the modified silicone oil. The molar ratio of the amine group molar weight of the tertiary amine silicone oil to the molar weight of the (2-chloroethanesulfonyl) ethylene is 1: 3.
Example 2
The cotton fabric is made of bleached and mercerized pure cotton knitted fabric (specification: 21, 180 g/m) 2 And the goods number: DM1, manufacturer: guangzhou buddha shun ya textile dyeing and finishing factory), cotton fabric is dyed by adopting the following conditions: the dye is active scarlet 3BS (available from Rgawa GmbH, zhejiang, leap soil Co., ltd.) in an amount of 3% o.w.f, a bath ratio of 1: 10, a temperature of 60 deg.C, and a time of 60min; washing with water (bath ratio 1: 10, temperature 60 deg.C, time 10 min); drying (temperature 120 ℃ C., time 20 min) was carried out.
Immersing the dyed cloth in a modified silicone oil solution for fixation, immersing for 30min at 60 ℃ (the bath ratio is 1: 10, the using amount is 5% o.w.f), then adding phosphotungstic acid (the using amount is 0% -3% o.w.f, purchased from Shanghai Aladdin Biotechnology Co., ltd.), keeping the temperature and stirring for 10min at 200rmp, adding NaOH solid to adjust the pH = 7-8, keeping the temperature for 20min, fishing out the fabric for pre-baking (60 ℃,3 min), then heating to baking (140 ℃,6 min), then soaping (2 g/L DB-5, the bath ratio is 1: 10, the temperature is 90 ℃, the time is 20 min), and finally drying (the temperature is 120 ℃, the time is 20 min).
The treating recipe for the sample cloths is shown in table 2 below.
TABLE 2
| Sample (I) | The dosage of phosphotungstic acid is percent |
| Sample cloth | |
| 1 | 2 |
| |
1 |
| |
3 |
| |
0 |
Comparative example 1
The cotton fabric is dyed, fixed and finished according to the traditional method and is marked as a sample cloth 5.
The specific process is as follows: padding dyeing → drying (80 ℃) → impregnating fixing solution → steam (100 ℃,70 s) → water washing (bath ratio 1: 10, 60 ℃,10 min) → soaping (2 g/L DB-5, bath ratio 1: 10, 90 ℃,20 min) → water washing (bath ratio 1: 10, 60 ℃,10 min) → drying (80 ℃) → padding finishing solution → drying (90 ℃ prebaking 10min,120 ℃ baking 5 min).
Padding and dyeing: active scarlet 3BS (the dosage is 3 percent), anhydrous sodium sulphate 50g/L; the rolling allowance rate is 65 percent.
Color fixing liquid: 6g/L of sodium hydroxide, 20g/L of soda ash and 200g/L of sodium chloride; the bath ratio is 1: 10, the temperature is 60 deg.C, and the time is 60min.
Finishing liquid: 30% of amino silicone oil (amine value is 0.6mmol/g, viscosity is 5000cP, purchased from Jinan Xinglong chemical Co., ltd.), 5% of emulsifier (TO-5/TO-7 = 1: 1), and the balance of water; the rolling residue rate is 80%.
The test results of the finished fabric are shown in tables 3-4.
Table 3:
table 4: bacteriostasis rate (machine washing)%
Machine washing: according to the regulation of GB 8629-2001, domestic washing and drying program adopted in textile test, a B-type stirring type washing machine and a washing program 8B are selected.
Example 4
And (4) carrying out digital printing on the fabric, and carrying out color depth test.
The fabric was not dyed, immersed directly in a modified silicone oil solution, soaked at 60 ℃ for 30min (bath ratio 1: 10, amount 5% o.w.f), then phosphotungstic acid (amount 0-3% o.w.f) was added, stirred at 200rmp for 10min, naOH solids were added to adjust pH = 7-8, the temperature was maintained for 20min, the fabric was fished out for prebaking (60 ℃,3 min), then warmed to baking (140 ℃,6 min), then soaped (2 g/L DB-5, bath ratio 1: 10, temperature 90 ℃, time 20 min), and finally dried (temperature 120 ℃, time 20 min).
The dried fabric is subjected to digital printing, and the fabric is made of Jietesi textile water-based paint ink purchased from Zhengzhou Hongsheng digital science and technology limited company and adopts four colors of C (cyan), M (red), Y (yellow) and K (black). The adopted digital printer is a HJ-RCT8460 digital printer produced by Shishi hongcai Feiyang digital technology Limited company, a single-channel Jing porcelain spray head is adopted, the printing precision is 720dpi multiplied by 2160dpi, and the highest printing speed is 550m 2 H is used as the reference value. Baking the fabric subjected to ink-jet printing at the temperature of 140 ℃ for 3min; then washing with water (30 deg.C, 10min, bath ratio 1: 10) and soaping (2 g/L DB-5, bath ratio 1: 10, temperature 90 deg.C, time 20 min).
Evaluating the color depth of the printed fabric, adopting a Datacolor SF650 color measuring and matching instrument for measurement, selecting a D65 light source and a 10-degree visual angle, measuring the K/S value at the maximum absorption wavelength of the dyed fabric, measuring each sample at different positions for 4 times, and taking the average value, wherein the result is as follows:
table 5:
the above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such modifications are intended to be included in the scope of the present invention.
Claims (9)
1. The color fixing finishing method is characterized by comprising the following steps:
(1) Fixation and finishing: washing and drying the dyed fabric, immersing the fabric into a modified silicone oil solution, soaking the fabric for 30min at 60 ℃, adding water-soluble heteropoly acid, keeping the temperature for soaking for 10min, adding alkali to adjust the pH to be 7-8, and keeping the temperature for 20min;
(2) And (4) baking, soaping and drying the treated fabric.
The baking is specifically pre-baked at 60-80 ℃ for 1-5 min, then the temperature is raised to 130-150 ℃ for 3-8 min, and then soaping is carried out at 80-100 ℃ for 20-40 min, and finally drying is carried out;
further, the modified silicone oil has the following molecular structure:
wherein m/n =1 to 5: 1.
2. The fixing finishing method according to claim 1, characterized in that the modified silicone oil is prepared by the following steps:
hydrolyzing N, N-diethylamine propyl methyl dimethoxy silane under alkaline condition by using anhydrous ether as solvent to prepare full-grafted tertiary amino silicone oil; further, N, N-diethylamine propyl methyl dimethoxy silane is mixed with D according to the metering ratio 4 Mixing with MM, and heating to react under the catalysis of tetramethylammonium hydroxide silicon alkoxide to prepare tertiary amino silicone oil;
the modified silicone oil is prepared by quaternization reaction of tertiary amino silicone oil and (2-chloroethanesulfonyl) ethylene by using ethanol as a solvent.
3. A fixation finishing process as claimed in claim 1, wherein the heteropolyacid is phosphotungstic acid, used in an amount of 1-2% o.w.f. .
4. The fixing finishing process according to claim 1, characterized in that in step (1) the modified silicone oil solution is an aqueous solution with a bath ratio of 1: 10 in an amount of 5% o.w.f.
5. The fixation finishing method according to claim 1, wherein the alkali in step (1) is NaOH or Na 2 CO 3 One or more of (a).
6. The fixation finishing method as claimed in claim 1, wherein the fabric is printed after being baked, soaped, dried.
7. The color fixing finishing method according to claim 2, characterized in that the amine value of the tertiary amino silicone oil is 1.6-3.5 mmol/g.
8. The fixing finishing method according to claim 2, wherein the molar ratio of the amine group molar amount of the tertiary amino silicone oil to the molar amount of the (2-chloroethanesulfonyl) ethene is 1: 3.
9. The fixation finishing method according to any one of claims 1 to 8, wherein the fabric is a pure cotton fabric.
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