CN119162834A - A preparation process of comfortable skin-friendly fabric - Google Patents
A preparation process of comfortable skin-friendly fabric Download PDFInfo
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- CN119162834A CN119162834A CN202411414073.5A CN202411414073A CN119162834A CN 119162834 A CN119162834 A CN 119162834A CN 202411414073 A CN202411414073 A CN 202411414073A CN 119162834 A CN119162834 A CN 119162834A
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- quaternary ammonium
- ammonium salt
- fabric
- salt modified
- comfortable skin
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- 239000004744 fabric Substances 0.000 title claims abstract description 95
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- -1 3-aminoethyl-4-aminobutyric acid Chemical compound 0.000 claims abstract description 61
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 56
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 239000000835 fiber Substances 0.000 claims abstract description 20
- KEZMLECYELSZDC-UHFFFAOYSA-N 3-chloropropyl-diethoxy-methylsilane Chemical compound CCO[Si](C)(OCC)CCCCl KEZMLECYELSZDC-UHFFFAOYSA-N 0.000 claims abstract description 11
- WBJINCZRORDGAQ-UHFFFAOYSA-N ethyl formate Chemical compound CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 239000008367 deionised water Substances 0.000 claims description 33
- 229910021641 deionized water Inorganic materials 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 27
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 21
- 239000002904 solvent Substances 0.000 claims description 21
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 18
- 239000013067 intermediate product Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- FDTLQXNAPKJJAM-UHFFFAOYSA-N 2-(3-hydroxyquinolin-2-yl)indene-1,3-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C1C1=NC2=CC=CC=C2C=C1O FDTLQXNAPKJJAM-UHFFFAOYSA-N 0.000 claims description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 239000003995 emulsifying agent Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 229920000728 polyester Polymers 0.000 claims description 13
- 229920002334 Spandex Polymers 0.000 claims description 10
- 239000004759 spandex Substances 0.000 claims description 10
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 235000009518 sodium iodide Nutrition 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000005096 rolling process Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 4
- ONJQDTZCDSESIW-UHFFFAOYSA-N polidocanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO ONJQDTZCDSESIW-UHFFFAOYSA-N 0.000 claims description 4
- 238000007493 shaping process Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 10
- XGYCWCIGCYGQFU-UHFFFAOYSA-N 1,2-thiazolidine 1,1-dioxide Chemical compound O=S1(=O)CCCN1 XGYCWCIGCYGQFU-UHFFFAOYSA-N 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000004043 dyeing Methods 0.000 abstract 1
- 230000001276 controlling effect Effects 0.000 description 22
- 230000001105 regulatory effect Effects 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 229910002808 Si–O–Si Inorganic materials 0.000 description 2
- 210000000170 cell membrane Anatomy 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000007730 finishing process Methods 0.000 description 2
- FSSPGSAQUIYDCN-UHFFFAOYSA-N 1,3-Propane sultone Chemical compound O=S1(=O)CCCO1 FSSPGSAQUIYDCN-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 210000000805 cytoplasm Anatomy 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
-
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- 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
- D06P3/34—Material containing ester groups
- D06P3/52—Polyesters
- D06P3/54—Polyesters using dispersed dyestuffs
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Dispersion Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Silicon Polymers (AREA)
Abstract
The invention relates to the technical field of fabrics and discloses a preparation process of comfortable skin-friendly fabrics, which takes 3-aminoethyl-4-aminobutyric acid, bromoacetic acid, 1, 3-propane sultone lactone, chloropropyl methyl diethoxy silane, octamethyl cyclo-tetrasiloxane, N-beta- (aminoethyl) -gamma-aminopropyl methyl dimethoxy silane and the like as raw materials, and the preparation process comprises the steps of obtaining quaternary ammonium salt modified polysiloxane through a series of reactions, preparing the quaternary ammonium salt modified polysiloxane into quaternary ammonium salt modified polysiloxane finishing liquid, finishing the fiber fabrics by the finishing liquid, and finally obtaining the comfortable skin-friendly fabrics through dyeing process. According to the invention, the antibacterial performance of the fabric is improved by utilizing the antibacterial quaternary ammonium salt group contained in the finishing liquid, and the hydrophilic and hygroscopic performances of the fabric are improved by utilizing the polar group contained in the finishing liquid. The fabric prepared by the invention has comfortable skin-friendly performance and antibacterial performance.
Description
Technical Field
The invention relates to the technical field of fabrics, in particular to a preparation process of a comfortable skin-friendly fabric.
Background
The comfort and skin-friendly performance is an integrated index, and for the fabric of the textile clothing, the comfort and skin-friendly performance is mainly determined by factors such as hygroscopicity and softness, and for the fabric directly contacting the skin, the fabric has soft hand feeling, and the hydrophilic moisture absorption function is an important part of the comfort of the fabric.
Polyester fabric and spandex fabric have many excellent performances, but have poor hygroscopicity and poor comfort when worn next to the skin, so hydrophilic finishing of the polyester fabric and spandex fabric is one of important ways for improving the comfort of the fabric.
The organic silicon fabric softening finishing agent not only can endow soft and comfortable and skin-friendly smooth hand feeling to the fabric, but also has good air permeability and wear resistance, can be used for finishing various textiles, has wide application prospect, but has poor hydrophilic performance and does not have good comprehensive use performance, so that the application of the organic silicon fabric softening finishing agent in high-grade textiles is limited to a certain extent.
Disclosure of Invention
The invention aims to provide a preparation process of a comfortable skin-friendly fabric, which is characterized in that a modified organic silicon finishing agent is prepared to endow the fiber fabric with good hydrophilic and antibacterial properties and expand the application field of the fiber fabric.
The technical scheme adopted by the invention is as follows:
A preparation process of a comfortable skin-friendly fabric comprises the following steps:
Adding deionized water into quaternary ammonium salt modified polysiloxane finishing liquid at room temperature to prepare a solution with the concentration of 20-30g/L, soaking the fiber fabric in the solution for 20-60s, performing one-dip-rolling on a vertical rolling mill, controlling the rolling residual rate to be 60-80%, drying at 100 ℃, shaping at 150 ℃ for 1-2min to obtain finished fiber fabric, placing the fiber fabric into deionized water, adding disperse yellow 54 and disperse leveling agent 2119 into the fiber fabric, controlling the bath ratio to be 1:10, heating to 130 ℃ at the rate of 2 ℃ per min, preserving heat for 1h, cooling to 90 ℃ at the rate of 2 ℃ per min after finishing, preserving heat for 10-20min, taking out and drying to obtain the comfortable skin-friendly fabric.
According to the above technical scheme, the concentration of the disperse yellow 54 is preferably 3-5g/L, and the concentration of the disperse leveling agent 2119 is preferably 1-3g/L.
According to the technical scheme, under the preferable condition, the fiber fabric is one of polyester fabric and spandex fabric.
According to the technical scheme, preferably, the preparation process of the quaternary ammonium salt modified polysiloxane finishing liquid comprises the following steps of:
(1) Adding 3-aminoethyl-4-aminobutyric acid into an ethanol solvent, stirring and mixing uniformly, adding bromoacetic acid into the mixture, heating to 60-80 ℃, reacting for 24-48 hours, performing reduced pressure distillation, washing with diethyl ether, and recrystallizing to obtain an intermediate product 1;
(2) Adding the intermediate product 1, 3-propane sulfonic acid lactone into a methanol solvent under the nitrogen atmosphere, stirring and mixing uniformly, heating to 60-70 ℃, reacting for 24-48h, adding sodium carbonate into the mixture, continuing stirring and reacting for 1-3h, filtering, distilling under reduced pressure after the reaction is finished, and recrystallizing to obtain an intermediate product 2;
(3) Adding an intermediate product 2, chloropropyl methyl diethoxy silane and sodium iodide into an ethanol solvent under the nitrogen atmosphere, stirring and dispersing, heating to 70-80 ℃, stirring and reacting for 24-36h, filtering after the reaction is finished, and distilling the filtrate under reduced pressure to obtain quaternary ammonium salt modified siloxane;
(4) Under the nitrogen atmosphere, octamethyl cyclotetrasiloxane and tetramethylammonium hydroxide are added into a flask, stirred and heated to 65-75 ℃, then N-beta- (aminoethyl) -gamma-aminopropyl methyldimethoxy silane and quaternary ammonium salt modified siloxane are added into the flask, the temperature is raised to 100-110 ℃, the reaction is carried out for 3-5 hours, the temperature is continuously raised to 130-140 ℃, the reaction is carried out for 1-2 hours, and after the reaction is finished, the reduced pressure distillation is carried out to obtain quaternary ammonium salt modified polysiloxane;
(5) Adding the quaternary ammonium salt modified polysiloxane into deionized water, adding an emulsifier into the deionized water, uniformly mixing, adding ethylene glycol monobutyl ether into the mixture, adjusting the pH to 6-7 by using 3g/L acetic acid aqueous solution, and uniformly stirring and mixing to obtain the quaternary ammonium salt modified polysiloxane finishing liquid.
According to the above technical scheme, in the preferred case, in the (1), the mass ratio of the 3-aminoethyl-4-aminobutyric acid to the bromoacetic acid is 1:1.8-2.2.
According to the above technical scheme, in the preferred case, in the (2), the mass ratio of the intermediate product 1, 3-propane sultone is 1:0.8-1.4.
According to the above technical scheme, in the preferred case, in the (3), the mass ratio of the intermediate product 2, the chloropropyl methyldiethoxysilane and the sodium iodide is 1:0.6-1:0.5-0.8.
According to the above technical scheme, in the preferred case, in the (4), the mass ratio of octamethyl cyclotetrasiloxane, tetramethylammonium hydroxide, N-beta- (aminoethyl) -gamma-aminopropyl methyldimethoxy silane and quaternary ammonium salt modified siloxane is 100:0.05-0.1:5-10:5-25.
According to the technical scheme, in the preferred case, in the (4), the mass ratio of the quaternary ammonium salt modified polysiloxane, the emulsifier and the ethylene glycol monobutyl ether is 100:15-40:4-7.
According to the above technical solution, in the preferred embodiment (4), the emulsifier is one of the emulsifiers AEO-3 and AEO-9.
The beneficial effects of the invention are as follows:
According to the invention, 3-aminoethyl-4-aminobutyric acid, bromoacetic acid, 1, 3-propane sulfonic acid lactone, chloropropyl methyl diethoxy silane, octamethyl cyclo-tetrasiloxane, N-beta- (aminoethyl) -gamma-aminopropyl methyl dimethoxy silane and the like are used as raw materials, quaternary ammonium salt modified polysiloxane is obtained through a series of reactions, and is emulsified to prepare quaternary ammonium salt modified polysiloxane finishing liquid, and the fiber fabric is finished by the finishing liquid and is dyed to finally obtain the comfortable skin-friendly fabric.
The finishing liquid prepared by the invention contains antibacterial quaternary ammonium salt particles which have positive charges, can be adsorbed on the surfaces of microorganisms with negative charges through electrostatic attraction and are combined with the negative charges on cell membranes to destroy the cell membranes to cause cytoplasm outflow, so that the aim of sterilizing and resisting bacteria is achieved.
The finishing liquid prepared by the invention contains amino, carboxyl, sulfonic acid and other hydrophilic groups, can generate hydrogen bonds with water molecules, has better hydrophilicity, and the fiber fabric has poor hydrophilic performance, and can improve the hydrophilic and hygroscopic performances of the fiber fabric after finishing by the finishing liquid, thereby improving the comfortable and skin-friendly performances of the fabric.
The polysiloxane skeleton prepared by the invention is composed of a Si-O-Si structure, the Si-O-Si bond angle is larger, the bond length is long, the degree of freedom is high, the fiber fabric is finished by the finishing liquid, the polysiloxane can form a film on the surface of the fiber fabric and cover the gaps and rough parts on the surface of the fiber, so that the friction coefficient of the surface of the fiber is reduced, the fabric has excellent smooth hand feeling, and the comfortable skin-friendly performance of the fabric is further improved.
Drawings
FIG. 1 is a reaction scheme for quaternary ammonium salt modified siloxanes.
Detailed Description
The present invention will be described more fully hereinafter in order to facilitate an understanding of the present invention, and preferred embodiments of the present invention are set forth. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Example 1
(1) 15G of 3-aminoethyl-4-aminobutyric acid is added into ethanol solvent, stirred and mixed uniformly, 27g of bromoacetic acid is added into the mixture, the temperature is raised to 70 ℃, the reaction is carried out for 48 hours, and after the reaction is completed, the mixture is distilled under reduced pressure, washed by diethyl ether and recrystallized, thus obtaining an intermediate product 1.
(2) Under the nitrogen atmosphere, 26.2g of intermediate 1 and 32g of 1, 3-propane sulfonate lactone are added into a methanol solvent, stirred and mixed uniformly, heated to 65 ℃ for reaction for 36h, 53g of sodium carbonate is added into the mixture, the stirring reaction is continued for 3h, and after the reaction is finished, the mixture is filtered, distilled under reduced pressure and recrystallized to obtain intermediate 2.
(3) Under the nitrogen atmosphere, 28.5g of intermediate 2, 17.1g of chloropropyl methyl diethoxy silane and 20g of sodium iodide are added into an ethanol solvent, stirred and dispersed, heated to 75 ℃, stirred and reacted for 32 hours, and after the reaction is finished, suction filtration is carried out, and the filtrate is distilled under reduced pressure to obtain the quaternary ammonium salt modified siloxane.
(4) Under the nitrogen atmosphere, 100g of octamethyl cyclotetrasiloxane and 0.05g of tetramethylammonium hydroxide are added into a flask, the mixture is stirred and heated to 70 ℃, then 5g of N-beta- (aminoethyl) -gamma-aminopropyl methyldimethoxy silane and 5g of quaternary ammonium salt modified siloxane are added into the flask, the mixture is heated to 105 ℃, the reaction is carried out for 4 hours, the temperature is continuously increased to 135 ℃, the reaction is carried out for 2 hours, and after the reaction is finished, the quaternary ammonium salt modified polysiloxane is obtained through reduced pressure distillation.
(5) 50G of quaternary ammonium salt modified polysiloxane is added into deionized water, 10g of emulsifier AEO-3 is added into the deionized water and mixed uniformly, 2.5g of ethylene glycol monobutyl ether is added into the mixture, 3g/L of acetic acid aqueous solution is used for regulating the pH value to 7, and the mixture is stirred and mixed uniformly to obtain the quaternary ammonium salt modified polysiloxane finishing liquid.
(6) Adding deionized water into quaternary ammonium salt modified polysiloxane finishing liquid at room temperature to prepare a solution with the concentration of 20g/L, soaking the polyester fabric in the solution for 50s, carrying out one-step padding on a vertical padder, controlling the padding residual rate to be 75%, drying at 100 ℃, setting at 150 ℃ for 2min to obtain finished polyester fabric, placing the polyester fabric into the deionized water, adding disperse yellow 54 and disperse leveling agent 2119 into the deionized water, controlling the concentration of the disperse yellow 54 to be 4g/L, controlling the concentration of the disperse leveling agent 2119 to be 2g/L, controlling the bath ratio to be 1:10, heating to 130 ℃ at the rate of 2 ℃ per min, preserving heat for 1h, cooling to 90 ℃ at the rate of 2 ℃ per min after finishing, preserving heat for 15min, taking out, and drying to obtain the comfortable skin-friendly fabric.
Example 2
(1) Adding 15g of 3-aminoethyl-4-aminobutyric acid into an ethanol solvent, stirring and mixing uniformly, adding 30g of bromoacetic acid into the mixture, heating to 80 ℃, reacting for 24 hours, distilling under reduced pressure, washing with diethyl ether, and recrystallizing to obtain an intermediate product 1.
(2) 26.2G of intermediate 1 and 36.5g of 1, 3-propane sulfonate lactone are added into a methanol solvent under the nitrogen atmosphere, stirred and mixed uniformly, heated to 60 ℃ for reaction for 30h, 53g of sodium carbonate is added into the mixture, the stirring reaction is continued for 2h, and after the reaction is finished, the mixture is filtered, distilled under reduced pressure and recrystallized to obtain intermediate 2.
(3) Under the nitrogen atmosphere, 28.5g of intermediate 2, 18g of chloropropyl methyl diethoxy silane and 16g of sodium iodide are added into an ethanol solvent, stirred and dispersed, heated to 75 ℃, stirred and reacted for 36 hours, and after the reaction is finished, suction filtration is carried out, and filtrate is distilled under reduced pressure to obtain the quaternary ammonium salt modified siloxane.
(4) Under the nitrogen atmosphere, 100g of octamethyl cyclotetrasiloxane and 0.05g of tetramethylammonium hydroxide are added into a flask, the mixture is stirred and heated to 70 ℃, 6g of N-beta- (aminoethyl) -gamma-aminopropyl methyldimethoxy silane and 10g of quaternary ammonium salt modified siloxane are added into the flask, the mixture is heated to 105 ℃, the reaction is carried out for 4 hours, the temperature is continuously increased to 135 ℃, the reaction is carried out for 2 hours, and after the reaction is finished, the quaternary ammonium salt modified polysiloxane is obtained through reduced pressure distillation.
(5) 50G of quaternary ammonium salt modified polysiloxane is added into deionized water, 15g of emulsifier AEO-9 is added into the deionized water and mixed uniformly, 3g of ethylene glycol monobutyl ether is added into the mixture, 3g/L of acetic acid aqueous solution is used for regulating the pH value to 6, and the mixture is stirred and mixed uniformly to obtain the quaternary ammonium salt modified polysiloxane finishing liquid.
(6) Adding deionized water into quaternary ammonium salt modified polysiloxane finishing liquid at room temperature to prepare a solution with the concentration of 22g/L, soaking the polyester fabric in the solution for 60s, carrying out one-step padding on a vertical padder, controlling the padding residual rate to be 70%, drying at 100 ℃, setting at 150 ℃ for 2min to obtain finished polyester fabric, placing the polyester fabric into deionized water, adding disperse yellow 54 and disperse leveling agent 2119 into the deionized water, controlling the concentration of the disperse yellow 54 to be 4g/L, controlling the concentration of the disperse leveling agent 2119 to be 2g/L, controlling the bath ratio to be 1:10, heating to 130 ℃ at the rate of 2 ℃ per min, preserving heat for 1h, cooling to 90 ℃ at the rate of 2 ℃ per min after finishing, preserving heat for 10-20min, taking out and drying to obtain the comfortable skin-friendly fabric.
Example 3
(1) 15G of 3-aminoethyl-4-aminobutyric acid is added into ethanol solvent, stirred and mixed uniformly, 33g of bromoacetic acid is added into the mixture, the temperature is raised to 60 ℃, the reaction is carried out for 36 hours, and after the reaction is completed, the mixture is distilled under reduced pressure, washed by diethyl ether and recrystallized, thus obtaining an intermediate product 1.
(2) 26.2G of intermediate 1 and 36.5g of 1, 3-propane sulfonate lactone are added into a methanol solvent under the nitrogen atmosphere, stirred and mixed uniformly, heated to 60 ℃ for reaction for 48 hours, 53g of sodium carbonate is added into the mixture, the stirring reaction is continued for 1 hour, and after the reaction is finished, the mixture is filtered, distilled under reduced pressure and recrystallized to obtain intermediate 2.
(3) Under the nitrogen atmosphere, 28.5g of intermediate 2, 28.5g of chloropropyl methyl diethoxy silane and 22.8g of sodium iodide are added into an ethanol solvent, stirred and dispersed, heated to 70 ℃, stirred and reacted for 36 hours, and after the reaction is finished, suction filtration is carried out, and the filtrate is distilled under reduced pressure to obtain the quaternary ammonium salt modified siloxane.
(4) Under the nitrogen atmosphere, 100g of octamethyl cyclotetrasiloxane and 0.1g of tetramethylammonium hydroxide are added into a flask, the mixture is stirred and heated to 75 ℃, then 8g of N-beta- (aminoethyl) -gamma-aminopropyl methyldimethoxy silane and 15g of quaternary ammonium salt modified siloxane are added into the flask, the mixture is heated to 100 ℃, the reaction is carried out for 3 hours, the temperature is continuously increased to 140 ℃, the reaction is carried out for 2 hours, and after the reaction is finished, the quaternary ammonium salt modified polysiloxane is obtained through reduced pressure distillation.
(5) 50G of quaternary ammonium salt modified polysiloxane is added into deionized water, 20g of emulsifier AEO-3 is added into the deionized water and mixed uniformly, 3g of ethylene glycol monobutyl ether is added into the mixture, 3g/L of acetic acid aqueous solution is used for regulating the pH value to 7, and the mixture is stirred and mixed uniformly to obtain the quaternary ammonium salt modified polysiloxane finishing liquid.
(6) Adding deionized water into quaternary ammonium salt modified polysiloxane finishing liquid at room temperature to prepare a solution with the concentration of 25g/L, soaking the polyester fabric in the solution for 50s, carrying out one-step padding on a vertical padder, controlling the padding residual rate to be 60%, drying at 100 ℃, setting at 150 ℃ for 2min to obtain finished polyester fabric, placing the polyester fabric into the deionized water, adding disperse yellow 54 and disperse leveling agent 2119 into the deionized water, controlling the concentration of the disperse yellow 54 to be 4g/L, controlling the concentration of the disperse leveling agent 2119 to be 3g/L, controlling the bath ratio to be 1:10, heating to 130 ℃ at the rate of 2 ℃ per min, preserving heat for 1h, cooling to 90 ℃ at the rate of 2 ℃ per min after finishing, preserving heat for 20min, taking out, and drying to obtain the comfortable skin-friendly fabric.
Example 4
(1) 15G of 3-aminoethyl-4-aminobutyric acid is added into ethanol solvent, stirred and mixed uniformly, 30g of bromoacetic acid is added into the mixture, the temperature is raised to 75 ℃, the reaction is carried out for 36 hours, and after the reaction is completed, the mixture is distilled under reduced pressure, washed by diethyl ether and recrystallized, thus obtaining an intermediate product 1.
(2) Under the nitrogen atmosphere, 26.2g of intermediate 1 and 28g of 1, 3-propane sulfonate lactone are added into a methanol solvent, stirred and mixed uniformly, heated to 65 ℃ and reacted for 24 hours, 53g of sodium carbonate is added into the mixture, the stirring and the reaction are continued for 3 hours, and after the reaction is finished, the mixture is filtered, distilled under reduced pressure and recrystallized to obtain intermediate 2.
(3) Under the nitrogen atmosphere, 28.5g of intermediate 2, 20g of chloropropyl methyl diethoxy silane and 18g of sodium iodide are added into an ethanol solvent, stirred and dispersed, heated to 80 ℃, stirred and reacted for 24 hours, and after the reaction is finished, suction filtration is carried out, and filtrate is distilled under reduced pressure to obtain the quaternary ammonium salt modified siloxane.
(4) Under the nitrogen atmosphere, 100g of octamethyl cyclotetrasiloxane and 0.1g of tetramethylammonium hydroxide are added into a flask, the mixture is stirred and heated to 65 ℃, 9g of N-beta- (aminoethyl) -gamma-aminopropyl methyldimethoxy silane and 20g of quaternary ammonium salt modified siloxane are added into the flask, the mixture is heated to 110 ℃, the reaction is carried out for 5 hours, the temperature is continuously increased to 130 ℃, the reaction is carried out for 2 hours, and after the reaction is finished, the quaternary ammonium salt modified polysiloxane is obtained through reduced pressure distillation.
(5) 50G of quaternary ammonium salt modified polysiloxane is added into deionized water, 10g of emulsifier AEO-9 is added into the deionized water and mixed uniformly, 2g of ethylene glycol monobutyl ether is added into the mixture, 3g/L of acetic acid aqueous solution is used for regulating the pH value to 7, and the mixture is stirred and mixed uniformly to obtain the quaternary ammonium salt modified polysiloxane finishing liquid.
(6) Adding deionized water into quaternary ammonium salt modified polysiloxane finishing liquid at room temperature to prepare a solution with the concentration of 28g/L, soaking spandex fabric in the solution for 20s, performing one-padding on a vertical padding machine, controlling the padding residual rate to be 70%, drying at 100 ℃, setting at 150 ℃ for 1min to obtain finished spandex fabric, placing the spandex fabric into deionized water, adding disperse yellow 54 and disperse leveling agent 2119 into the deionized water, controlling the concentration of the disperse yellow 54 to be 3g/L, controlling the concentration of the disperse leveling agent 2119 to be 1g/L, controlling the bath ratio to be 1:10, heating to 130 ℃ at the rate of 2 ℃ per min, preserving heat for 1h, cooling to 90 ℃ at the rate of 2 ℃ per min after finishing, preserving heat for 15min, taking out and drying to obtain the comfortable skin-friendly fabric.
Example 5
(1) 15G of 3-aminoethyl-4-aminobutyric acid is added into ethanol solvent, stirred and mixed uniformly, 30g of bromoacetic acid is added into the mixture, the temperature is raised to 70 ℃, the reaction is carried out for 48 hours, and after the reaction is completed, the mixture is distilled under reduced pressure, washed by diethyl ether and recrystallized, thus obtaining an intermediate product 1.
(2) Under the nitrogen atmosphere, 26.2g of intermediate 1 and 21g of 1, 3-propane sulfonate lactone are added into a methanol solvent, stirred and mixed uniformly, heated to 70 ℃, reacted for 48 hours, then 53g of sodium carbonate is added into the mixture, stirred and reacted for 2 hours continuously, and after the reaction is finished, the mixture is filtered, distilled under reduced pressure and recrystallized to obtain intermediate 2.
(3) Under the nitrogen atmosphere, 28.5g of intermediate 2, 17.1g of chloropropyl methyl diethoxy silane and 14.3g of sodium iodide are added into an ethanol solvent, stirred and dispersed, heated to 75 ℃, stirred and reacted for 36 hours, and after the reaction is finished, suction filtration is carried out, and the filtrate is distilled under reduced pressure to obtain the quaternary ammonium salt modified siloxane.
(4) Under the nitrogen atmosphere, 100g of octamethyl cyclotetrasiloxane and 0.05g of tetramethylammonium hydroxide are added into a flask, the mixture is stirred and heated to 70 ℃, 10g of N-beta- (aminoethyl) -gamma-aminopropyl methyldimethoxy silane and 25g of quaternary ammonium salt modified siloxane are added into the flask, the mixture is heated to 105 ℃, the reaction is carried out for 4 hours, the temperature is continuously increased to 135 ℃, the reaction is carried out for 1 hour, and after the reaction is finished, the quaternary ammonium salt modified polysiloxane is obtained through reduced pressure distillation.
(5) 50G of quaternary ammonium salt modified polysiloxane is added into deionized water, 7.5g of emulsifier AEO-3 is added into the deionized water and mixed uniformly, 3.5g of ethylene glycol monobutyl ether is added into the mixture, 3g/L of acetic acid aqueous solution is used for regulating the pH value to 7, and the mixture is stirred and mixed uniformly to obtain the quaternary ammonium salt modified polysiloxane finishing liquid.
(6) Adding deionized water into quaternary ammonium salt modified polysiloxane finishing liquid at room temperature to prepare a solution with the concentration of 30g/L, soaking spandex fabric in the solution for 40s, performing one-padding on a vertical padding machine, controlling the padding residual rate to be 80%, drying at 100 ℃, setting at 150 ℃ for 2min to obtain finished spandex fabric, placing the spandex fabric into deionized water, adding disperse yellow 54 and disperse leveling agent 2119 into the deionized water, controlling the concentration of the disperse yellow 54 to be 5g/L, controlling the concentration of the disperse leveling agent 2119 to be 2g/L, controlling the bath ratio to be 1:10, heating to 130 ℃ at the rate of 2 ℃ per min, preserving heat for 1h, cooling to 90 ℃ at the rate of 2 ℃ per min after finishing, preserving heat for 20min, taking out and drying to obtain the comfortable skin-friendly fabric.
Hydrophilicity test fabric hydrophilicity was tested with reference to AATCC 79-2000. Pouring 20L of water into a washing machine, adding 20g of washing powder and comfortable skin-friendly fabric, rotating and washing for 5 times, 10 minutes each time, washing the fabric with clear water, drying, and testing the hydrophilicity.
Table 1:
comparative example 1 is a fabric finished with a commercial finishing liquid, and the finishing process is the same as example 1.
As shown in the table, the fabric prepared by the invention has better hydrophilic moisture absorption performance, and the better the hydrophilic moisture absorption performance is along with the increase of the using amount of the finishing agent.
And the hand feeling test is that a plurality of hand feeling evaluation experts with abundant experience perform comprehensive evaluation in aspects of softness and smoothness, and the hand feeling of the original cloth is evaluated as 1 minute and the highest hand feeling is 5 minutes.
Table 2:
| Softness/min | Slip/min | |
| Example 1 | 4 | 4 |
| Example 2 | 4 | 4-5 |
| Example 3 | 4-5 | 4-5 |
| Example 4 | 4-5 | 5 |
| Example 5 | 5 | 5 |
| Comparative example 1 | 3 | 4 |
Comparative example 1 is a fabric finished with a commercial finishing liquid, and the finishing process is the same as example 1.
As can be seen from the table, the fabric prepared by the method has better softness and smoothness.
And (3) antibacterial performance test, namely adding finished fabric into a flask containing diluent by adopting an oscillation flask method, adding bacterial liquid, culturing for 1h at 37 ℃, taking out 1mL of test liquid, placing into a solid culture medium, calculating antibacterial rate by adopting a dilution plate counting method, wherein antibacterial rate (%) = (average viable count in the flask before finishing cloth sample dipping and oscillating-average viable count in the flask before finishing cloth sample dipping and oscillating)/average viable count in the flask before finishing cloth sample dipping and oscillating is multiplied by 100%, and the test strains are staphylococcus aureus and escherichia coli.
Table 3:
As shown in the table, the fabric prepared by the invention has better antibacterial performance, and the highest antibacterial rate can reach 99.9%.
Many possible variations and modifications of the disclosed technology can be made by anyone skilled in the art without departing from the scope of the technology, or the technology can be modified to be equivalent. Therefore, any simple modification, equivalent variation and modification of the above embodiments according to the technical substance of the present invention shall still fall within the scope of the technical solution of the present invention.
Claims (10)
1. The preparation process of the comfortable skin-friendly fabric is characterized by comprising the following steps of:
Adding deionized water into quaternary ammonium salt modified polysiloxane finishing liquid at room temperature to prepare a solution with the concentration of 20-30g/L, soaking the fiber fabric in the solution for 20-60s, performing one-dip-rolling on a vertical rolling mill, controlling the rolling residual rate to be 60-80%, drying at 100 ℃, shaping at 150 ℃ for 1-2min to obtain finished fiber fabric, placing the fiber fabric into deionized water, adding disperse yellow 54 and disperse leveling agent 2119 into the fiber fabric, controlling the bath ratio to be 1:10, heating to 130 ℃ at the rate of 2 ℃ per min, preserving heat for 1h, cooling to 90 ℃ at the rate of 2 ℃ per min after finishing, preserving heat for 10-20min, taking out and drying to obtain the comfortable skin-friendly fabric.
2. The process for preparing a comfortable skin-friendly fabric according to claim 1, wherein the concentration of the disperse yellow 54 is 3-5g/L, and the concentration of the disperse leveling agent 2119 is 1-3g/L.
3. The process for preparing the comfortable skin-friendly fabric according to claim 1, wherein the fiber fabric is one of polyester fabric and spandex fabric.
4. The process for preparing the comfortable skin-friendly fabric according to claim 1, wherein the process for preparing the quaternary ammonium salt modified polysiloxane finishing liquid is as follows:
(1) Adding 3-aminoethyl-4-aminobutyric acid into an ethanol solvent, stirring and mixing uniformly, adding bromoacetic acid into the mixture, heating to 60-80 ℃, reacting for 24-48 hours, performing reduced pressure distillation, washing with diethyl ether, and recrystallizing to obtain an intermediate product 1;
(2) Adding the intermediate product 1, 3-propane sulfonic acid lactone into a methanol solvent under the nitrogen atmosphere, stirring and mixing uniformly, heating to 60-70 ℃, reacting for 24-48h, adding sodium carbonate into the mixture, continuing stirring and reacting for 1-3h, filtering, distilling under reduced pressure after the reaction is finished, and recrystallizing to obtain an intermediate product 2;
(3) Adding an intermediate product 2, chloropropyl methyl diethoxy silane and sodium iodide into an ethanol solvent under the nitrogen atmosphere, stirring and dispersing, heating to 70-80 ℃, stirring and reacting for 24-36h, filtering after the reaction is finished, and distilling the filtrate under reduced pressure to obtain quaternary ammonium salt modified siloxane;
(4) Under the nitrogen atmosphere, octamethyl cyclotetrasiloxane and tetramethylammonium hydroxide are added into a flask, stirred and heated to 65-75 ℃, then N-beta- (aminoethyl) -gamma-aminopropyl methyldimethoxy silane and quaternary ammonium salt modified siloxane are added into the flask, the temperature is raised to 100-110 ℃, the reaction is carried out for 3-5 hours, the temperature is continuously raised to 130-140 ℃, the reaction is carried out for 1-2 hours, and after the reaction is finished, the reduced pressure distillation is carried out to obtain quaternary ammonium salt modified polysiloxane;
(5) Adding the quaternary ammonium salt modified polysiloxane into deionized water, adding an emulsifier into the deionized water, uniformly mixing, adding ethylene glycol monobutyl ether into the mixture, adjusting the pH to 6-7 by using 3g/L acetic acid aqueous solution, and uniformly stirring and mixing to obtain the quaternary ammonium salt modified polysiloxane finishing liquid.
5. The process for preparing the comfortable skin-friendly fabric according to claim 4, wherein in the step (1), the mass ratio of the 3-aminoethyl-4-aminobutyric acid to the bromoacetic acid is 1:1.8-2.2.
6. The process for preparing a comfortable skin-friendly fabric according to claim 4, wherein in the step (2), the mass ratio of the intermediate product 1 to the 1, 3-propane sultam is 1:0.8-1.4.
7. The process for preparing a comfortable skin-friendly fabric according to claim 4, wherein in the step (3), the mass ratio of the intermediate product 2 to the chloropropyl methyldiethoxysilane to the sodium iodide is 1:0.6-1:0.5-0.8.
8. The process for preparing a comfortable skin-friendly fabric according to claim 4, wherein in the step (4), the mass ratio of octamethyl cyclotetrasiloxane, tetramethylammonium hydroxide, N-beta- (aminoethyl) -gamma-aminopropyl methyldimethoxy silane and quaternary ammonium salt modified siloxane is 100:0.05-0.1:5-10:5-25.
9. The process for preparing a comfortable skin-friendly fabric according to claim 4, wherein in the step (4), the mass ratio of the quaternary ammonium salt modified polysiloxane to the emulsifier to the ethylene glycol monobutyl ether is 100:15-40:4-7.
10. The process for preparing a comfortable skin-friendly fabric as claimed in claim 4, wherein in the step (4), the emulsifier is one of an emulsifier AEO-3 and an emulsifier AEO-9.
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