CN110552205A - preparation method of fabric heat-insulating finishing agent and fabric heat-insulating finishing agent - Google Patents
preparation method of fabric heat-insulating finishing agent and fabric heat-insulating finishing agent Download PDFInfo
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- CN110552205A CN110552205A CN201910696515.2A CN201910696515A CN110552205A CN 110552205 A CN110552205 A CN 110552205A CN 201910696515 A CN201910696515 A CN 201910696515A CN 110552205 A CN110552205 A CN 110552205A
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- finishing agent
- antimony oxide
- tin antimony
- stirring
- fabric heat
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- 239000004744 fabric Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 52
- 229920002635 polyurethane Polymers 0.000 claims abstract description 45
- 239000004814 polyurethane Substances 0.000 claims abstract description 45
- 239000002002 slurry Substances 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 33
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 30
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000839 emulsion Substances 0.000 claims abstract description 19
- 238000009413 insulation Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- XXLJGBGJDROPKW-UHFFFAOYSA-N antimony;oxotin Chemical compound [Sb].[Sn]=O XXLJGBGJDROPKW-UHFFFAOYSA-N 0.000 claims abstract description 12
- 150000002009 diols Chemical class 0.000 claims abstract description 11
- 229920000909 polytetrahydrofuran Polymers 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 10
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 9
- 238000013329 compounding Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims abstract description 7
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 7
- 239000005058 Isophorone diisocyanate Substances 0.000 claims abstract description 6
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011159 matrix material Substances 0.000 claims abstract description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 3
- -1 silane modified tin antimony oxide Chemical class 0.000 claims description 30
- 229910000077 silane Inorganic materials 0.000 claims description 24
- 239000004753 textile Substances 0.000 claims description 13
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 7
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 7
- 239000012752 auxiliary agent Substances 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 229920005989 resin Polymers 0.000 abstract description 7
- 239000011347 resin Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 3
- SKRWFPLZQAAQSU-UHFFFAOYSA-N stibanylidynetin;hydrate Chemical compound O.[Sn].[Sb] SKRWFPLZQAAQSU-UHFFFAOYSA-N 0.000 description 20
- 238000002834 transmittance Methods 0.000 description 11
- 238000000576 coating method Methods 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000004417 polycarbonate Substances 0.000 description 2
- 229920000515 polycarbonate Polymers 0.000 description 2
- 229920005862 polyol Polymers 0.000 description 2
- 150000003077 polyols Chemical class 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 125000000467 secondary amino group Chemical class [H]N([*:1])[*:2] 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
- D06N3/146—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes characterised by the macromolecular diols used
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/06—Properties of the materials having thermal properties
- D06N2209/065—Insulating
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
the invention provides a preparation method of a fabric heat-insulating finishing agent, which comprises the following steps: dissolving polytetrahydrofuran diol in acetone, adding isophorone diisocyanate and a catalyst, reacting at 70-80 ℃ to generate a polyurethane prepolymer, adding N-methyl pyrrolidone and 2, 2-dimethylolpropionic acid to react, adding 1, 4-butanediol to react, cooling to room temperature, adding triethylamine to react, dropwise adding water, stirring at high speed, and removing acetone by a rotary evaporation method to obtain an aqueous polyurethane emulsion; secondly, adding absolute ethyl alcohol after ball milling and dispersing tin antimony oxide, performing magnetic stirring, performing ultrasonic dispersion, adding a silane coupling agent Kh-570, and stirring in a water bath at 60 ℃ to obtain modified tin antimony oxide slurry; and thirdly, compounding the products obtained in the first step and the second step, adding a film forming aid, and magnetically stirring to prepare the fabric heat-insulating finishing agent. The material has good heat insulation performance by doping nano modified ATO, and has the advantages of high bonding strength, good stability, low VOC and the like by using the water-based polyurethane as a resin matrix.
Description
Technical Field
the invention relates to a preparation method of a fabric heat-insulating finishing agent and the fabric heat-insulating finishing agent, belonging to the technical field of fabric heat-insulating finishing agents.
Background
The heat insulation coating fabric is a fabric which coats a coating with a heat insulation function on the surface of the fabric, has a barrier effect or a high reflectance ratio on solar radiation, so that the temperature rise of the surface of the coating is inhibited, the internal temperature of a fabric covering is reduced, and the functions of energy saving and heat insulation are achieved.
at present, domestic research on the field of textile fabrics for thermal insulation coatings is still in a primary stage, and functional particles are easy to agglomerate in organic matters and generate sedimentation, so that the effect of the coatings is influenced. In addition, most of the resins used in the existing heat insulation coating are oil-soluble resins such as acrylic resin, epoxy resin, alkyd resin and the like, which is not beneficial to environmental protection.
the nanometer ATO (antimony tin oxide) powder has ideal selectivity to the solar spectrum, high transmittance in a visible light region and good shielding performance to infrared light, and the nanometer ATO powder is dispersed and then added into resin to obtain the nanometer transparent heat-insulating coating.
Waterborne polyurethane has the advantages of safety, environmental protection, difficult combustion, excellent elasticity, flexibility, adhesion and the like, and is often used for replacing solvent-based polyurethane.
disclosure of Invention
the invention aims to manufacture a fabric heat-insulating finishing agent, the material uses silane coupling agent (KH-570) modified Antimony Tin Oxide (ATO) as functional particles, and uses water-based polyurethane as a resin matrix, and the fabric heat-insulating finishing agent has the advantages of safety, environmental protection, excellent mechanical properties, high stability and the like.
In order to achieve the above technical object, the present invention adopts the following technical solutions.
The invention provides a preparation method of a fabric heat-insulating finishing agent, which comprises the following steps:
step one, preparing waterborne polyurethane
pumping polytetrahydrofuran diol, dissolving the polytetrahydrofuran diol in acetone, adding isophorone diisocyanate and a catalyst, and reacting at 70-80 ℃ to generate a polyurethane prepolymer;
And then adding N-methyl pyrrolidone and 2, 2-dimethylolpropionic acid for reaction, adding 1, 4-butanediol, cooling to room temperature after reacting for 2 hours, adding triethylamine for reaction, then dripping water, stirring at high speed, and removing acetone by a rotary evaporation method to obtain the aqueous polyurethane emulsion.
step two, preparing modified ATO
And (3) after ball milling and dispersion of Antimony Tin Oxide (ATO), adding absolute ethyl alcohol, performing magnetic stirring, performing ultrasonic dispersion, adding a silane coupling agent Kh-570, and stirring in a water bath at 60 ℃ to obtain silane modified ATO slurry.
Step three, preparing the fabric heat-insulating finishing agent
Compounding the silane modified ATO slurry with the waterborne polyurethane emulsion, adding the film forming aid, and magnetically stirring to prepare the fabric heat-insulating finishing agent.
In particular to a preparation method of the fabric heat-insulating finishing agent,
In the first step, the catalyst is dibutyltin dilaurate;
in the second step, the particle size of the ATO is 20-80 nm;
In the third step, the volume percentage content of the ATO slurry is 10-50 percent;
in the third step, the film-forming assistant is twelve alcohol esters.
The preparation method of the fabric heat-insulating finishing agent comprises the following steps:
Step one, preparing waterborne polyurethane
Pumping water at 150 ℃ from 2 to 5g of polytetrahydrofuran diol 100-;
And then adding 3-7mL of LN-methyl pyrrolidone and 0.100-0.500g of 2, 2-dimethylolpropionic acid to react for 1-3h, adding 0.100-0.200g of 1, 4-butanediol to react for 1-3h, cooling to room temperature, adding 2-5 drops of triethylamine to react for 2-3 min, dropwise adding 10-20mL of water, and simultaneously stirring at high speed to obtain the waterborne polyurethane.
step two, preparing modified ATO
After ATO ball milling dispersion, weighing 1-3g, adding 40mL of absolute ethyl alcohol, magnetically stirring for 10min, then placing into an ultrasonic dispersion instrument for dispersion for 1-2h, adding 1-2mL of silane coupling agent Kh-570, and stirring for 2-3h in water bath at 60 ℃ to obtain silane modified ATO slurry.
step three, preparing the fabric heat-insulating finishing agent
Compounding 10mL of silane modified ATO slurry with 10mL of aqueous polyurethane emulsion, wherein the volume percentage of the slurry is 50%, adding 0.5-1.0g of film-forming auxiliary agent alcohol ester twelve, and magnetically stirring for 2-3h to prepare the fabric heat-insulating finishing agent.
the preparation method of the fabric heat-insulating finishing agent comprises the following steps:
step one, preparing waterborne polyurethane
3g of polytetrahydrofuran diol is pumped at 130 ℃ and then dissolved in 20mL of acetone, 2g of isophorone diisocyanate and 3 drops of catalyst dibutyltin dilaurate are added, and the mixture reacts for 2 hours at 70-80 ℃ to generate a polyurethane prepolymer;
And then adding 5mL of LN-methyl pyrrolidone and 0.275g of 2, 2-dimethylolpropionic acid to react for 2 hours, adding 0.144g of 1, 4-butanediol, cooling to room temperature after reacting for 2 hours, adding 3 drops of triethylamine to react for 2-3 minutes, dropwise adding 15mL of water, stirring at high speed, and removing acetone by a rotary evaporation method to obtain the waterborne polyurethane.
Step two, preparing modified ATO
After ATO ball milling dispersion, weighing 2g, adding 40mL of absolute ethyl alcohol, magnetically stirring for 10min, then placing into an ultrasonic disperser for dispersion for 1-2h, adding 1mL of silane coupling agent Kh-570, and stirring for 2-3h in water bath at 60 ℃ to obtain silane modified ATO slurry.
Step three, preparing the fabric heat-insulating finishing agent
taking 10mL of silane modified ATO slurry and 10mL of aqueous polyurethane emulsion to compound, wherein the volume percentage of the slurry is 50%, adding 0.5g of film-forming auxiliary agent alcohol ester twelve, and magnetically stirring for 2-3h to prepare the fabric heat-insulating finishing agent.
The invention also provides a fabric heat-insulating finishing agent which takes the waterborne polyurethane as a matrix and takes silane modified ATO as functional particles.
Specifically, the fabric heat-insulating finishing agent is prepared by the method.
By adopting the technical scheme, the invention has the following technical effects: synthesizing an environment-friendly fabric heat-insulating finishing agent which takes modified nano ATO as functional particles and aqueous polyurethane as matrix resin.
the material has good heat insulation performance by doping modified nano ATO, and has the advantages of high bonding strength, good stability, low VOC and the like by using the water-based polyurethane as a resin matrix.
Can be applied to the fields of coatings, adhesives, elastomers, flexible and rigid foams, printing ink and the like.
Drawings
FIG. 1 is an infrared spectrum of the aqueous polyurethane emulsion obtained in the first step of example 1;
FIG. 2 is a graph of the UV transmittance of samples of the thermal insulating fabric finishes of examples 1 to 5;
FIG. 3 is a graph of the transmittance in the visible region of samples of the textile thermal-insulating finishes of examples 1 to 5;
Fig. 4 is a graph of the transmittance in the infrared region of samples of the textile thermal insulating finishes of examples 1 to 5.
Detailed Description
The following describes the technical solutions of the present invention in detail with reference to the detailed description and the accompanying drawings, so that those skilled in the art can better understand the present invention and can implement the present invention.
The preparation method of the fabric heat-insulating finishing agent comprises the following steps:
Step one, preparing waterborne polyurethane
Pumping water at 150 ℃ from 2 to 5g of polytetrahydrofuran diol 100-;
And then adding 3-7mL of LN-methyl pyrrolidone and 0.100-0.500g of 2, 2-dimethylolpropionic acid to react for 1-3h, adding 0.100-0.200g of 1, 4-butanediol to react for 1-3h, cooling to room temperature, adding 2-5 drops of triethylamine to react for 2-3 min, dropwise adding 10-20mL of water, and simultaneously stirring at high speed to obtain the waterborne polyurethane.
Step two, preparing modified ATO
After ATO ball milling dispersion, weighing 1-3g, adding 40mL of absolute ethyl alcohol, magnetically stirring for 10min, then placing into an ultrasonic dispersion instrument for dispersion for 1-2h, adding 1-2mL of silane coupling agent Kh-570, and stirring for 2-3h in water bath at 60 ℃ to obtain silane modified ATO slurry.
Step three, preparing the fabric heat-insulating finishing agent
taking 2-10mL of silane modified ATO slurry and 10-18mL of aqueous polyurethane emulsion according to the proportion to compound, adding 0.5-1.0g of film-forming auxiliary agent alcohol ester twelve, and magnetically stirring for 2-3h to prepare the fabric heat-insulating finishing agent, wherein the volume percentage content of the obtained slurry is 10-50%.
The above method is described below by specific examples, and it should be noted that, although the following examples are prepared according to the corresponding parameter conditions, the other parameters in the above method are selected for preparation, and the corresponding textile thermal insulation finishing agent can also be prepared.
Example 1
A preparation method of a fabric heat-insulating finishing agent comprises the following steps:
Step one, preparing waterborne polyurethane
3g of polytetrahydrofuran diol is pumped at 130 ℃ and then dissolved in 20mL of acetone, 2g of isophorone diisocyanate and 3 drops of catalyst dibutyltin dilaurate are added, and the mixture reacts for 2 hours at 70-80 ℃ to generate a polyurethane prepolymer;
And then adding 5mL of LN-methyl pyrrolidone and 0.275g of 2, 2-dimethylolpropionic acid to react for 2 hours, adding 0.144g of 1, 4-butanediol, cooling to room temperature after reacting for 2 hours, adding 3 drops of triethylamine to react for 2-3 minutes, dropwise adding 15mL of water, stirring at high speed, and removing acetone by a rotary evaporation method to obtain the waterborne polyurethane.
Step two, preparing modified ATO
After ATO ball milling dispersion, weighing 2g, adding 40mL of absolute ethyl alcohol, magnetically stirring for 10min, then placing into an ultrasonic disperser for dispersion for 1-2h, adding 1mL of silane coupling agent Kh-570, and stirring for 2-3h in water bath at 60 ℃ to obtain silane modified ATO slurry.
Step three, preparing the fabric heat-insulating finishing agent
Taking 10mL of silane modified ATO slurry and 10mL of aqueous polyurethane emulsion to compound, wherein the volume percentage of the slurry is 50%, adding 0.5g of film-forming auxiliary agent alcohol ester twelve, and magnetically stirring for 2-3h to prepare the fabric heat-insulating finishing agent.
example 2
a method of preparing a textile thermal insulation finish, otherwise the same as in example 1, except that:
And step three, compounding 8mL of silane modified ATO slurry with 12mL of aqueous polyurethane emulsion, wherein the volume percentage of the slurry is 40%.
Example 3
A method of preparing a textile thermal insulation finish, otherwise the same as in example 1, except that:
And step three, compounding 6mL of silane modified ATO slurry with 14mL of aqueous polyurethane emulsion, wherein the volume percentage of the slurry is 30%.
Example 4
A method of preparing a textile thermal insulation finish, otherwise the same as in example 1, except that:
And step three, compounding 4mL of silane modified ATO slurry with 16mL of aqueous polyurethane emulsion, wherein the volume percentage of the slurry is 20%.
Example 5
A method of preparing a textile thermal insulation finish, otherwise the same as in example 1, except that:
And step three, compounding 2mL of silane modified ATO slurry with 18mL of aqueous polyurethane emulsion, wherein the volume percentage of the slurry is 10%.
Comparative example 1
A method of preparing a textile thermal insulation finish, otherwise the same as in example 1, except that:
step one, taking oil-soluble polyurethane which is prepared from polycarbonate polyol and toluene diisocyanate and takes acetone as a solvent.
Specifically, 4-6g of polycarbonate polyol (PCDL: M ═ 2000) is taken to be dehydrated for 3-5h in vacuum at 130 ℃, and then dissolved in acetone after dehydration, and reacts with 3-5g of Toluene Diisocyanate (TDI) under the catalysis of 3 drops of dibutyltin Dilaurate (DBTL) to obtain a polyurethane prepolymer; and finally, adding 0.2-0.8g of 1, 4-butanediol for chain extension to obtain the oil-soluble polyurethane.
and step three, compounding 8mL of silane modified ATO slurry with 12mL of oil-soluble polyurethane, wherein the volume percentage of the slurry is 40%.
Examples of the experiments
1. Infrared test of the aqueous polyurethane emulsion:
preparing a potassium bromide salt tablet, then dropping the aqueous polyurethane emulsion obtained in the first step of the example 1 on a salt tablet, drying and testing, wherein the testing range is 4000-400 cm -1, referring to fig. 1, fig. 1 is an infrared spectrogram of the aqueous polyurethane emulsion obtained in the first step of the example 1, and it can be seen from the infrared spectrogram that the peak at 3320cm -1 is aliphatic NH secondary amine stretching vibration, and the isocyanate-N ═ C ═ O antisymmetric stretching vibration at 2275-.
2. Characterization of heat-insulating property of the fabric heat-insulating finishing agent:
And (3) respectively adding 1-3mL of absolute ethyl alcohol into the fabric heat-insulating finishing agent obtained in the embodiment 1-5, keeping the speed at 500-1500rad/min for 1-2h, coating the mixture on a glass slide, and drying the glass slide at room temperature to obtain a fabric heat-insulating finishing agent sample. The average transmittance of the obtained fabric heat-insulating finishing agent sample in ultraviolet, visible and infrared light regions is measured by an LS102 type optical transmittance measuring instrument.
fig. 2 is a graph of the transmittance in the ultraviolet region of samples of the textile thermal-insulating finish of examples 1 to 5.
fig. 3 is a graph of the transmittance in the visible region of samples of the textile thermal-insulating finishes of examples 1 to 5.
fig. 4 is a graph of the transmittance in the infrared region of samples of the textile thermal insulating finishes of examples 1 to 5.
as can be seen from the figure, as the volume percentage content of the ATO slurry in the fabric heat-insulating finishing agent is reduced, the transmittance in ultraviolet, visible and infrared regions generally shows an upward trend, wherein the effect in the infrared region is most obvious, and the overall effect is best when the content is 40 percent and the comprehensive physical property and transmittance are both good.
3. adhesive strength and stability of fabric heat-insulating finishing agent
The fabric thermal insulating finishes of examples 1 to 5, and comparative example 1 were left for one week and observed for phenomena. The fabric thermal insulation finishing agents of examples 1 to 5 did not show delamination and precipitation, and the fabric thermal insulation finishing agent of comparative example 1 showed delamination. The fabric heat-insulating finishing agent shows good bonding strength and stability.
in addition, the low VOC fabric heat-insulating finishing agent is prepared by the method, because only acetone is used in the preparation process of the waterborne polyurethane and is removed by rotary evaporation.
The technical solution provided by the present invention is not limited by the above embodiments, and all technical solutions formed by utilizing the structure and the mode of the present invention through conversion and substitution are within the protection scope of the present invention.
Claims (5)
1. A preparation method of a fabric heat-insulating finishing agent is characterized by comprising the following steps:
Step one, preparing waterborne polyurethane
Pumping polytetrahydrofuran diol, dissolving the polytetrahydrofuran diol in acetone, adding isophorone diisocyanate and a catalyst, and reacting at 70-80 ℃ to generate a polyurethane prepolymer;
Then adding N-methyl pyrrolidone and 2, 2-dimethylolpropionic acid for reaction, adding 1, 4-butanediol, continuously reacting, cooling to room temperature, adding triethylamine for reaction, dripping water, simultaneously stirring at high speed, and removing acetone by a rotary evaporation method to obtain a waterborne polyurethane emulsion;
Step two, preparing silane modified tin antimony oxide
After ball milling and dispersing tin antimony oxide, adding absolute ethyl alcohol, performing magnetic stirring, performing ultrasonic dispersion, adding a silane coupling agent Kh-570, and stirring in a water bath at 60 ℃ to obtain modified tin antimony oxide slurry;
Step three, preparing the fabric heat-insulating finishing agent
Compounding the silane modified tin antimony oxide slurry with the waterborne polyurethane emulsion, adding a film forming aid, and magnetically stirring to prepare a fabric heat-insulating finishing agent;
Wherein,
in the first step, the catalyst is dibutyltin dilaurate;
In the second step, the grain size of the tin antimony oxide is 20 nm-80 nm;
In the third step, the volume percentage content of the tin antimony oxide slurry is 10-50%;
In the third step, the film-forming assistant is twelve alcohol esters.
2. The preparation method of the fabric heat-insulating finishing agent according to claim 1, characterized by comprising the following steps:
step one, preparing waterborne polyurethane
Pumping water at 150 ℃ from 2 to 5g of polytetrahydrofuran diol 100-;
Then adding 3-7mL of LN-methyl pyrrolidone and 0.100-0.500g of 2, 2-dimethylolpropionic acid to react for 1-3h, adding 0.100-0.200g of 1, 4-butanediol to react for 1-3h, cooling to room temperature, adding 2-5 drops of triethylamine to react for 2-3 min, dropwise adding 10-20mL of water, and simultaneously stirring at high speed to obtain waterborne polyurethane;
Step two, preparing silane modified tin antimony oxide
after ball milling and dispersing tin antimony oxide, weighing 1-3g of the tin antimony oxide, adding 40mL of absolute ethyl alcohol, magnetically stirring for 10min, then placing the mixture into an ultrasonic disperser for dispersing for 1-2h, adding 1-2mL of silane coupling agent Kh-570, and stirring for 2-3h in water bath at 60 ℃ to obtain silane modified tin antimony oxide slurry;
Step three, preparing the fabric heat-insulating finishing agent
Taking 10mL of silane modified tin antimony oxide slurry and 10mL of aqueous polyurethane emulsion to compound, wherein the volume percentage of the slurry is 50%, adding 0.5-1.0g of film-forming auxiliary agent alcohol ester twelve, and magnetically stirring for 2-3h to prepare the fabric heat-insulating finishing agent.
3. The preparation method of the fabric heat-insulating finishing agent according to claim 2, characterized by comprising the following steps:
Step one, preparing waterborne polyurethane
3g of polytetrahydrofuran diol is pumped at 130 ℃ and then dissolved in 20mL of acetone, 2g of isophorone diisocyanate and 3 drops of catalyst dibutyltin dilaurate are added, and the mixture reacts for 2 hours at 70-80 ℃ to generate a polyurethane prepolymer;
Then adding 5mL of LN-methyl pyrrolidone and 0.275g of 2, 2-dimethylolpropionic acid to react for 2 hours, adding 0.144g of 1, 4-butanediol, cooling to room temperature after reacting for 2 hours, adding 3 drops of triethylamine to react for 2-3 minutes, dropwise adding 15mL of water, stirring at high speed, and removing acetone by a rotary evaporation method to obtain waterborne polyurethane;
Step two, preparing modified tin antimony oxide
after ball milling and dispersing tin antimony oxide, weighing 2g of the tin antimony oxide, adding 40mL of absolute ethyl alcohol, magnetically stirring for 10min, then placing the mixture into an ultrasonic disperser for dispersing for 1-2h, adding 1mL of silane coupling agent Kh-570, and stirring for 2-3h in water bath at 60 ℃ to obtain silane modified tin antimony oxide slurry;
step three, preparing the fabric heat-insulating finishing agent
Taking 10mL of silane modified tin antimony oxide slurry and 10mL of aqueous polyurethane emulsion to compound, wherein the volume percentage of the slurry is 50%, adding 0.5g of film-forming auxiliary agent alcohol ester twelve, and magnetically stirring for 2-3h to prepare the fabric heat-insulating finishing agent.
4. a fabric heat insulation finishing agent is characterized in that: the fabric heat-insulating finishing agent takes water-based polyurethane as a matrix and takes silane modified tin antimony oxide as functional particles.
5. The plant heat-insulating finishing agent according to claim 4, characterized in that: the textile thermal insulation finishing agent is prepared according to the preparation method of any one of claims 1 to 3.
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