CN116254705A - Organosilicon emulsion type coating agent for fabrics and preparation method thereof - Google Patents
Organosilicon emulsion type coating agent for fabrics and preparation method thereof Download PDFInfo
- Publication number
- CN116254705A CN116254705A CN202310123922.0A CN202310123922A CN116254705A CN 116254705 A CN116254705 A CN 116254705A CN 202310123922 A CN202310123922 A CN 202310123922A CN 116254705 A CN116254705 A CN 116254705A
- Authority
- CN
- China
- Prior art keywords
- silicone oil
- coating agent
- heating
- type coating
- emulsion type
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000004744 fabric Substances 0.000 title claims abstract description 67
- 239000011248 coating agent Substances 0.000 title claims abstract description 35
- 239000000839 emulsion Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920002545 silicone oil Polymers 0.000 claims abstract description 56
- 238000003756 stirring Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000004945 emulsification Methods 0.000 claims abstract description 6
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 230000007935 neutral effect Effects 0.000 claims abstract description 6
- 238000010008 shearing Methods 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 22
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 13
- 239000003607 modifier Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 claims description 5
- PDAWHBQDMPNZQI-UHFFFAOYSA-N 1-bromobut-3-en-2-ol Chemical compound BrCC(O)C=C PDAWHBQDMPNZQI-UHFFFAOYSA-N 0.000 claims description 4
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 claims description 4
- WDJHALXBUFZDSR-UHFFFAOYSA-N acetoacetic acid Chemical compound CC(=O)CC(O)=O WDJHALXBUFZDSR-UHFFFAOYSA-N 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012043 crude product Substances 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims 6
- 210000002268 wool Anatomy 0.000 abstract description 15
- 239000000835 fiber Substances 0.000 abstract description 12
- 102000004169 proteins and genes Human genes 0.000 abstract description 7
- 108090000623 proteins and genes Proteins 0.000 abstract description 7
- 238000005406 washing Methods 0.000 abstract description 7
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- 150000003254 radicals Chemical class 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 241001465754 Metazoa Species 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- 102000011782 Keratins Human genes 0.000 description 2
- 108010076876 Keratins Proteins 0.000 description 2
- 241000283973 Oryctolagus cuniculus Species 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000006459 hydrosilylation reaction Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 1
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000085 cashmere Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 210000004209 hair Anatomy 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Images
Classifications
-
- 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
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/388—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing nitrogen
-
- 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
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/001—Treatment with visible light, infrared or ultraviolet, X-rays
-
- 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
- D06M15/6433—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing carboxylic 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
- D06M2101/12—Keratin fibres or silk
-
- 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
Abstract
The invention discloses an organosilicon emulsion type coating agent for fabrics and a preparation method thereof, and the specific method is as follows: weighing 10-15g of prepared modified silicone oil, adding 3-5g of emulsifier AEO-3, uniformly mixing, adding into a high-speed shearing machine at a rotating speed of 800-1000r/min, adding acetic acid while stirring to adjust the pH of the solution to be neutral, continuously stirring and slowly dropwise adding 5-6ml of deionized water dropwise for emulsification for 25-30min, adding the rest 10-15ml of deionized water after the whole system is phase-inverted, and continuously stirring for 10-15min uniformly to obtain the organosilicon emulsion coating agent; when the organosilicon emulsion type coating agent is used for finishing the wool fabric, modified silicone oil is introduced onto wool protein fibers in a bonding mode under the irradiation of ultraviolet, so that the washing fastness of the fabric is improved, and the antistatic performance of the fabric is greatly prolonged in a bonding mode.
Description
Technical Field
The invention relates to the technical field of fabrics, in particular to an organosilicon emulsion type coating agent for fabrics and a preparation method thereof.
Background
The fabric coating agent is an agent which can be coated on the surface of a fabric, has stronger adhesive force and can improve part of the performance of the fabric. By using a fabric coating agent, a common fabric can be changed into a coated fabric with multifunction, the fabric itself is used as a framework to provide basic mechanical strength, and the coating provides unique properties such as water resistance, fire resistance, air permeability, flame retardance, chemical resistance or electromagnetic shielding.
The woolen knitwear mainly uses animal wool fibers such as wool, cashmere, rabbit hair and the like as main raw materials to spin into yarns and then weaves into fabrics, such as rabbit sweaters, snow blue sweaters, sheep jerseys, acrylic jerseys and the like, which are all large families of 'woolen sweaters', are used for comfort and softness of clothing fabrics, but the animal wool fiber fabrics generally have the problems of static electricity, pilling and the like in wearing, and the comfort and convenience are reduced. Therefore, animal wool fiber fabrics factories adopt fabric coating agents for finishing, but the hand feeling is poor after finishing, the washing fastness is poor, and the problem of static electricity is caused after a certain washing times, so that the development of the animal wool fiber fabrics with lasting antistatic property is very important, and the hand feeling of the fabrics is not affected.
Disclosure of Invention
The invention aims to provide an organosilicon emulsion type coating agent for fabrics and a preparation method thereof.
The aim of the invention can be achieved by the following technical scheme:
the organosilicon emulsion type coating agent for the fabric comprises modified silicone oil, wherein the modified silicone oil has the following structural formula:
wherein m=60-80.
Further, the preparation method of the modified silicone oil comprises the following steps:
20-25g of glycidyl ether silicone oil, 6-8g of modifier and 0.3-0.5g of catalyst SnC l are added into a three-neck flask with a stirrer, a thermometer and a nitrogen through pipe 4 Continuously introducing nitrogen in the adding process, adding no solvent, heating to 95-100 ℃ while stirring, and reacting for 4-5h at a constant temperature to obtain the yellow transparent modified silicone oil.
Further, the preparation of the glycidyl ether silicone oil comprises the following steps:
50-60g of hydrogen silicone oil and 2 are weighed.Adding 5-3g allyl glycidyl ether into a reaction bottle, adding 5-10g isopropanol solvent, heating and stirring, heating to 65-70deg.C, adding 0.15-0.18g catalyst H 2 PtCl 6 ·H 2 And O, continuously heating to 80-85 ℃, keeping the temperature for reaction for 4-5h, stopping heating after the reaction is finished, and naturally cooling to room temperature to obtain colorless transparent liquid, namely the glycidyl ether silicone oil.
Further, the molecular weight of the hydrogen-containing silicone oil is m=6000.
Further, the preparation of the modifier
17-18g of 2,2' - (2-hydroxyethyl) azadiyl) diacetic acid and 16-18g of 1-bromobut-3-en-2-ol are weighed into a three-necked flask provided with a thermometer, a condenser and a dropping funnel, 50ml of KI-DMF solution with the mass fraction of 15-20% is filled in the dropping funnel, 800-1000ml of solvent DMF is added into the three-necked flask, heating and stirring are started, when the temperature is raised to 100-105 ℃, the dropping funnel is opened, after the dripping of 15-20mi is completed, the heating is continued to 120-125 ℃, the heat preservation reaction is carried out for 10-15h, heating is stopped after the reaction is completed, DMF is removed by reduced pressure distillation, and anhydrous diethyl ether is adopted for recrystallization of the crude product, and the modifier is obtained.
The preparation method of the organosilicon emulsion type coating agent for the fabric comprises the following specific steps: weighing 10-15g of prepared modified silicone oil, adding 3-5g of emulsifier AEO-3, uniformly mixing, adding into a high-speed shearing machine, regulating the pH of the solution to be neutral by adding acetic acid while stirring, continuously stirring, slowly dropwise adding 5-6ml of deionized water dropwise for emulsification for 25-30min, adding the rest 10-15ml of deionized water after the whole system is phase-inverted, and continuously stirring for 10-15min uniformly to obtain the organosilicon emulsion coating agent.
The invention has the beneficial effects that:
(1) The organosilicon emulsion type coating agent for the fabrics is white, uniform and fine in emulsion, and the finished wool fabrics have smooth hand feeling and silk feeling;
(2) The main components of the organosilicon emulsion type coating agent are modified silicone oil, firstly, hydrogen-containing silicone oil and allyl glycidyl ether are used as raw materials, glycidyl ether silicone oil containing double-end epoxy groups is prepared through hydrosilylation reaction, then 2,2' - (2-hydroxyethyl) aza-diyl) diacetic acid and 1-bromobut-3-en-2-ol are used as raw materials to prepare a double-bond-containing modifier, finally, the glycidyl ether silicone oil and the modifier are subjected to ring-opening reaction to prepare modified silicone oil, the organosilicon on the modified silicone oil reduces the friction coefficient of the surface of the fiber, and in addition, the modified silicone oil contains a plurality of hydrophilic groups which act on water molecules in the fabric and can absorb air, so that the hydrophilicity and antistatic performance of the fabric are improved;
(3) When the organosilicon emulsion type coating agent is used for finishing the wool fabric, groups on keratin of the wool protein fiber are broken into free radicals under the irradiation of ultraviolet, then under the action of an initiator, the free radicals are polymerized with double bonds on the wool protein fiber containing the free radicals and the modified silicone oil, the modified silicone oil is introduced onto the wool protein fiber in a bonding mode, the washing fastness of the fabric is improved, and the antistatic performance of the fabric is greatly prolonged in a bonding mode.
Of course, it is not necessary for any one product to practice the invention to achieve all of the advantages set forth above at the same time.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of the preparation of a modified silicone oil;
FIG. 2 shows the infrared spectra of hydrogen-containing silicone oil (a), glycidyl ether silicone oil (b), modifier (c), and modified silicone oil (d).
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
As shown in fig. 1, the preparation method of the modified silicone oil comprises the following steps:
step one, preparation of glycidyl ether silicone oil
50g of hydrogen-containing silicone oil (molecular weight M=6000) and 2.6g of allyl glycidyl ether are weighed into a reaction flask, 10g of isopropanol solvent is then added, heating and stirring are started, after the temperature is raised to 70 ℃, 0.15g of catalyst H is added 2 PtCl 6 ·H 2 O, continuously heating to 85 ℃, preserving heat and reacting for 4 hours, stopping heating after the reaction is finished, and naturally cooling to room temperature to obtain colorless transparent liquid, namely glycidol ether silicone oil;
step two, preparation of modifier
18g of 2,2' - (2-hydroxyethyl) azadiyl) diacetic acid and 18g of 1-bromobut-3-en-2-ol are weighed into a three-necked flask provided with a thermometer, a condenser and a dropping funnel, 50ml of KI-DMF solution with the mass fraction of 20% is filled in the dropping funnel, 1000ml of solvent DMF is added into the three-necked flask, heating and stirring are started, when the temperature is raised to 100 ℃, the dropping funnel is opened, the dropping funnel is stopped after the completion of the dropping, the heating is continued to 120 ℃, the heat preservation reaction is carried out for 15 hours, DMF is removed by reduced pressure distillation, and the crude product is recrystallized by anhydrous diethyl ether, thus obtaining the modifier;
step three, preparation of modified silicone oil
20g of glycidyl ether silicone oil, 6.5g of modifier and 0.5g of catalyst SnC l are put into a three-necked flask equipped with a stirrer, a thermometer and a nitrogen tube 4 And continuously introducing nitrogen in the adding process, adding no solvent, heating to 100 ℃ while stirring, and reacting for 4 hours while preserving heat to obtain the yellow transparent modified silicone oil.
As shown in FIG. 2, the infrared spectrum of hydrogen-containing silicone oil (a), glycidyl ether silicone oil (b), modifier (c) and modified silicone oil (d) is 2921cm -1 、2965cm -1 at-CH 2 -and-CH 3 The stretching vibration peak of (C) is 1002cm in the range of hydrogen-containing silicone oil (a), glycidyl ether silicone oil (b) and modified silicone oil (d) -1 -1135cm -1 The broad peak at the position is a telescopic vibration peak of S i-O-S i, and as can be seen from the figures (a) and (b), the S i-H bond on the hydrogen-containing silicone oil disappears in (b), which indicates that the hydrogen-containing silicone oil and the allyl glycidyl ether react to react fully through hydrosilylation; 1715cm in FIGS. (c) and (d) -1 Is provided with a-COOH ester group stretching vibration peak at 1545cm -1 Where is N + Is 3380cm -1 The stretching vibration peaks of-OH and-COOH are shown.
Example 2
The invention relates to an organosilicon emulsion type coating agent for fabrics, which is prepared by the following steps: weighing 10g of prepared modified silicone oil, adding 3g of emulsifier AEO-3, uniformly mixing, adding into a high-speed shearing machine at a rotating speed of 800 r/min, adding acetic acid while stirring to adjust the pH of the solution to be neutral, continuously stirring and slowly dropwise adding 5ml of deionized water for emulsification for 30min, adding the rest 10ml of deionized water after the whole system is phase-inverted, and continuously stirring for 10 min uniformly to obtain the organosilicon emulsion coating agent, wherein the prepared emulsion is white, uniform and fine.
Example 3
The invention relates to an organosilicon emulsion type coating agent for fabrics, which is prepared by the following steps: weighing 12g of prepared modified silicone oil, adding 4g of emulsifier AEO-3, uniformly mixing, adding into a high-speed shearing machine at a rotating speed of 1000r/min, adding acetic acid while stirring to adjust the pH of the solution to be neutral, continuously stirring and slowly dropwise adding 6ml of deionized water for emulsification for 30min, adding the rest 10ml of deionized water after the whole system is phase-inverted, and continuously stirring for 15min uniformly to obtain the organosilicon emulsion coating agent, wherein the prepared emulsion is white, uniform and fine.
Example 4
The invention relates to an organosilicon emulsion type coating agent for fabrics, which is prepared by the following steps: 15g of prepared modified silicone oil is weighed, 5g of emulsifier AEO-3 is added, the mixture is uniformly mixed, the mixture is added into a high-speed shearing machine, the rotating speed is 1000r/min, acetic acid is added while stirring to adjust the pH value of the solution to be neutral, then 5ml of deionized water is continuously stirred and slowly and dropwise added for emulsification for 30min, after the whole system is phase-inverted, the rest 12ml of deionized water is added, and the mixture is continuously stirred for 10 min uniformly, so that the prepared emulsion is white, uniform and fine.
Application of organosilicon emulsion type coating agent:
cutting the woolen sweater fabric into the size of 3cm x 3cm, cleaning the woolen sweater fabric in the soaked water, and radiating the woolen sweater fabric by an ultraviolet lamp after airing, turning over every 5min and radiating for 30min for later use;
adding sodium persulfate serving as an initiator (the addition amount is 5 percent of that of the organosilicon emulsion type coating agent) into the organosilicon emulsion type coating agent, and uniformly stirring and mixing for later use;
immersing the sweater fabric subjected to ultraviolet irradiation in a container containing sodium persulfate-organosilicon emulsion type coating agents (examples 2, 3 and 4 correspond to application examples 1, 2 and 3 respectively), placing the container in a water bath kettle with the water bath temperature of 45 ℃, continuously irradiating with an ultraviolet lamp for 20min, taking out, performing two-padding with a padder with the padding allowance of 75%, then drying the fabric in a drying oven with the temperature of 105 ℃ for 5min, curing the fabric at the high temperature of 150 ℃ for 100s, and finally drying the treated fabric at room temperature for 24h, thereby performing performance test on the fabric.
Comparative application example
Cutting the sweater fabric into the size of 3cm x 3cm, cleaning in the soaking water, and airing for later use; the method comprises the steps of immersing a sweater fabric in a container containing an organosilicon emulsion type coating agent (examples 2, 3 and 4 correspond to comparative application examples 1, 2 and 3 respectively), placing the container in a water bath at a water bath temperature of 45 ℃ and a padding ratio of 75% by using a padder for two padding, drying the fabric in a drying oven at 105 ℃ for 5min, curing the fabric at 150 ℃ for 100s at high temperature, drying the treated fabric at room temperature for 24h, and testing the performance of the fabric.
Performance test of finished fabrics
Hydrophilic property test
The detection is carried out by referring to an AATCC79-2000 drip method, and the time is counted until the light reflection phenomenon of the water drops disappears (the drip amount is 5 ul) per second; the results are shown in the following table:
as is clear from the above table, the fabrics obtained by the finishing methods of the application examples and the comparative application examples have good hydrophilicity, probably because the modified silicone oil contains a large amount of hydrophilic groups such as-OH, -COOH, -N at the main chain end + Thereby greatly providing the hydrophilicity of the fabric.
Hand feel and softness test
Softness was tested with an RH-R/100 computer softness tester, the results of which are shown in the following table:
antistatic and wash fastness test
Detecting the surface resistance of the fabric according to GB/T12703-91 textile static test method;
the cleaning method comprises the following steps: putting a fabric sample into water containing a proper amount of laundry detergent, manually washing 3mi n, then manually washing 2mi n with clear water for 2 times, naturally airing, and counting once; the fabrics after 50 washes were tested for antistatic properties and the results are shown in the following table:
when the surface resistance of the fabric is less than 10 11 When the fabric is used, the fabric is considered to have good antistatic performance; as can be seen from the above table, the electrical resistance of the unfinished fabric is poor, and the new fabric finished by the methods of the application example and the comparative application example has good antistatic performance, but the surface resistance of the comparative application example is greater than 10 as the number of times of washing is increased 11 The antistatic performance is not possessed, because in the application example, under the irradiation of ultraviolet, the radical on keratin of the wool protein fiber is broken into free radical, then under the action of an initiator, the double bond on the wool protein fiber containing the free radical and the modified silicone oil is polymerized by the free radical, so that the modified silicone oil is introduced onto the wool protein fiber in a bonding mode, and the antistatic performance of the fabric is greatly prolonged in the bonding mode.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (6)
1. A silicone emulsion type coating agent for fabrics is characterized in that: the coating agent contains modified silicone oil, and the structural formula of the modified silicone oil is as follows:
wherein m=60-80.
2. A silicone emulsion type coating agent for fabrics according to claim 1, characterized in that: the preparation method of the modified silicone oil comprises the following steps:
20-25g of glycidyl ether silicone oil, 6-8g of modifier and 0.3-0.5g of catalyst SnCl are added into a three-neck flask with a stirrer, a thermometer and a nitrogen through pipe 4 Continuously introducing nitrogen in the adding process, adding no solvent, heating to 95-100 ℃ while stirring, and reacting for 4-5h at a constant temperature to obtain the yellow transparent modified silicone oil.
3. A silicone emulsion type coating agent for fabrics according to claim 2, characterized in that: the preparation of the glycidyl ether silicone oil comprises the following steps:
weighing 50-60g hydrogen-containing silicone oil and 2.5-3g allyl glycidyl ether, adding 5-10g isopropanol solvent, heating and stirring, heating to 65-70deg.C, and adding 0.15-0.18g catalyst H 2 PtCl 6 ·H 2 And O, continuously heating to 80-85 ℃, keeping the temperature for reaction for 4-5h, stopping heating after the reaction is finished, and naturally cooling to room temperature to obtain colorless transparent liquid, namely the glycidyl ether silicone oil.
4. A silicone emulsion type coating agent for fabrics according to claim 3, characterized in that: the molecular weight of the hydrogen-containing silicone oil is M=6000.
5. A silicone emulsion type coating agent for fabrics according to claim 2, characterized in that: preparation of the modifier
17-18g of 2,2' - (2-hydroxyethyl) azadiyl) diacetic acid and 16-18g of 1-bromobut-3-en-2-ol are weighed into a three-necked flask provided with a thermometer, a condenser and a dropping funnel, 50ml of KI-DMF solution with the mass fraction of 15-20% is filled in the dropping funnel, 800-1000ml of solvent DMF is added into the three-necked flask, heating and stirring are started, when the temperature is raised to 100-105 ℃, the dropping funnel is opened, after the dripping is completed for 15-20min, the heating is continued to 120-125 ℃, the heat preservation reaction is carried out for 10-15h, the heating is stopped after the reaction is completed, DMF is removed by reduced pressure distillation, and the crude product is recrystallized by anhydrous diethyl ether, thus obtaining the modifier.
6. A process for the preparation of a silicone emulsion coating agent for fabrics according to any one of claims 1 to 5, characterized in that: the specific method comprises the following steps: weighing 10-15g of prepared modified silicone oil, adding 3-5g of emulsifier AEO-3, uniformly mixing, adding into a high-speed shearing machine at a rotating speed of 800-1000r/min, adding acetic acid while stirring to adjust the pH of the solution to be neutral, continuously stirring and slowly dropwise adding 5-6ml of deionized water dropwise for emulsification for 25-30min, adding the rest 10-15ml of deionized water after the whole system is phase-inverted, and continuously stirring for 10-15min uniformly to obtain the organosilicon emulsion coating agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310123922.0A CN116254705B (en) | 2023-02-16 | 2023-02-16 | Finishing method for wool fabric by adopting organosilicon emulsion type coating agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310123922.0A CN116254705B (en) | 2023-02-16 | 2023-02-16 | Finishing method for wool fabric by adopting organosilicon emulsion type coating agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116254705A true CN116254705A (en) | 2023-06-13 |
| CN116254705B CN116254705B (en) | 2023-11-21 |
Family
ID=86683835
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310123922.0A Active CN116254705B (en) | 2023-02-16 | 2023-02-16 | Finishing method for wool fabric by adopting organosilicon emulsion type coating agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116254705B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010111908A1 (en) * | 2009-03-31 | 2010-10-07 | 北京华美精创纳米相材料科技有限责任公司 | Ultra-hydrophilic wool fabric with wash fastness and nano-finishing method for preparing the same |
| KR101423649B1 (en) * | 2013-04-05 | 2014-08-01 | (주)시그마소재 | Textile softener base on self-emulsified type silicone oil |
| CN107034675A (en) * | 2017-04-21 | 2017-08-11 | 常州市蓝勖化工有限公司 | A kind of preparation method of modified organic silicon textile coating agent |
| CN107881787A (en) * | 2017-11-08 | 2018-04-06 | 常州欣彬纺织品有限公司 | A kind of preparation method of high washable antistatic additive |
| CN109942821A (en) * | 2019-03-26 | 2019-06-28 | 吉林乾仁新材料有限公司 | Preparation method of hydroxylamino-modified silicone oil cation emulsion and products thereof and application |
| CN111877020A (en) * | 2020-08-08 | 2020-11-03 | 广东创新精细化工实业有限公司 | Modified silicone oil softening agent and preparation method thereof |
| WO2022001575A1 (en) * | 2020-06-30 | 2022-01-06 | 江苏四新科技应用研究所股份有限公司 | Organosilicone emulsion and preparation method |
-
2023
- 2023-02-16 CN CN202310123922.0A patent/CN116254705B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010111908A1 (en) * | 2009-03-31 | 2010-10-07 | 北京华美精创纳米相材料科技有限责任公司 | Ultra-hydrophilic wool fabric with wash fastness and nano-finishing method for preparing the same |
| KR101423649B1 (en) * | 2013-04-05 | 2014-08-01 | (주)시그마소재 | Textile softener base on self-emulsified type silicone oil |
| CN107034675A (en) * | 2017-04-21 | 2017-08-11 | 常州市蓝勖化工有限公司 | A kind of preparation method of modified organic silicon textile coating agent |
| CN107881787A (en) * | 2017-11-08 | 2018-04-06 | 常州欣彬纺织品有限公司 | A kind of preparation method of high washable antistatic additive |
| CN109942821A (en) * | 2019-03-26 | 2019-06-28 | 吉林乾仁新材料有限公司 | Preparation method of hydroxylamino-modified silicone oil cation emulsion and products thereof and application |
| WO2022001575A1 (en) * | 2020-06-30 | 2022-01-06 | 江苏四新科技应用研究所股份有限公司 | Organosilicone emulsion and preparation method |
| CN111877020A (en) * | 2020-08-08 | 2020-11-03 | 广东创新精细化工实业有限公司 | Modified silicone oil softening agent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 杨玉各: "季铵盐改性有机硅柔软剂的合成与应用", 印染助剂, no. 2, pages 32 - 36 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116254705B (en) | 2023-11-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102643435B (en) | Supersoft hydrophilic block silicone oil compound and preparation method thereof | |
| CN101914206B (en) | Quaternized modified amino silicone oil softener and preparation and application thereof | |
| CN101805994B (en) | Organosilicon emulsion used for hand feel finishing of wool and blended yarn thereof and preparation method and application thereof | |
| CN102644200B (en) | Super-soft finishing agent of silicone oil | |
| CN104086779A (en) | Super-soft/smooth block silicon oil and preparation method thereof | |
| CN114941244B (en) | Waterproof finishing method for nylon fabric, waterproof finishing liquid and waterproof component | |
| CN110230216A (en) | A kind of Lyocell fibers fabric of natural dye dying and preparation method thereof | |
| CN109554911A (en) | A kind of dyeing and finishing processing method of 400 fabric of memory T based on bio-based materials | |
| CN102660029B (en) | Cation modified supersoft hydrophilic block silicone oil compound and preparation method and application | |
| CN105755837B (en) | A kind of preparation method of quaternised modified amino-silicone oil softener and application | |
| CN110904687B (en) | Pure cotton satin fabric imitated silk finishing agent and preparation method thereof | |
| CN112661966A (en) | Quaternary ammonium salt modified organic silicon and preparation method and application thereof | |
| CN114561811B (en) | Wear-resistant cloth and preparation method thereof | |
| CN102643436B (en) | Supersoft hydrophilic block silicone oil intermediate compound and preparation method thereof | |
| CN116254705B (en) | Finishing method for wool fabric by adopting organosilicon emulsion type coating agent | |
| CN104233601B (en) | A kind of super soft knitted fabric and its processing method | |
| CN111320757B (en) | Preparation method of high-fastness ultralow-yellowing silicone oil for polyester fabric and polyester fabric | |
| CN106758213B (en) | A kind of cotton fabric hydroscopic fast-drying method for sorting based on alkyl oxy silane | |
| CN102086591B (en) | Organic germanium-containing home textile fabric and preparation method thereof | |
| CN109629097B (en) | Antistatic light luxury worsted woolen fabric | |
| CN113461969B (en) | Organic functional group modified polysiloxane polymerization emulsion and preparation method thereof | |
| CN115262241A (en) | Surface treatment method of textile, special hyperchromic repairing agent and preparation method thereof | |
| JPH04214482A (en) | Deep-colorable polyester fiber cloth and production thereof | |
| CN105601844A (en) | Preparation method and application of novel modified organic silicon softening agent | |
| Islam et al. | Synthesis and Application of Amino-Modified Silicone Oil on Cotton Fabric |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |