CN108867032B - Preparation method of fluorine-free super-hydrophobic cotton fabric - Google Patents
Preparation method of fluorine-free super-hydrophobic cotton fabric Download PDFInfo
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- CN108867032B CN108867032B CN201810615450.XA CN201810615450A CN108867032B CN 108867032 B CN108867032 B CN 108867032B CN 201810615450 A CN201810615450 A CN 201810615450A CN 108867032 B CN108867032 B CN 108867032B
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- 239000004744 fabric Substances 0.000 title claims abstract description 135
- 229920000742 Cotton Polymers 0.000 title claims abstract description 132
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 98
- 239000000839 emulsion Substances 0.000 claims abstract description 87
- 239000001993 wax Substances 0.000 claims abstract description 72
- 239000002131 composite material Substances 0.000 claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 26
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims abstract description 26
- CSNNHWWHGAXBCP-UHFFFAOYSA-L magnesium sulphate Substances [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 26
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 26
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 24
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 24
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 24
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000004203 carnauba wax Substances 0.000 claims abstract description 16
- 239000012188 paraffin wax Substances 0.000 claims abstract description 16
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 15
- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 claims abstract description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 24
- 238000002791 soaking Methods 0.000 claims description 23
- 239000000126 substance Substances 0.000 claims description 11
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 2
- 230000002209 hydrophobic effect Effects 0.000 abstract description 25
- 230000003068 static effect Effects 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 description 35
- 239000007788 liquid Substances 0.000 description 27
- 238000001914 filtration Methods 0.000 description 20
- 238000002844 melting Methods 0.000 description 20
- 230000008018 melting Effects 0.000 description 20
- 239000003795 chemical substances by application Substances 0.000 description 15
- 238000012360 testing method Methods 0.000 description 11
- 229910000831 Steel Inorganic materials 0.000 description 10
- 239000003995 emulsifying agent Substances 0.000 description 10
- 239000003921 oil Substances 0.000 description 10
- 239000010959 steel Substances 0.000 description 10
- 239000011345 viscous material Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000004753 textile Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 3
- 230000001143 conditioned effect Effects 0.000 description 3
- 230000003750 conditioning effect Effects 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013869 carnauba wax Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000000675 fabric finishing Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000009962 finishing (textile) Methods 0.000 description 1
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000006467 substitution reaction Methods 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
- D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 of the Periodic Table
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
-
- 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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
-
- 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
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/327—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof
- D06M15/333—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated alcohols or esters thereof of vinyl acetate; Polyvinylalcohol
-
- 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
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- 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
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Colloid Chemistry (AREA)
Abstract
The invention discloses a preparation method of a fluorine-free super-hydrophobic cotton fabric, which comprises the following steps of: mixing and heating 10-15 parts by mass of a mixture of paraffin and palm wax and 1-5 parts by mass of a surfactant; adding 0.1 to 1 percent of MgSO40.5 to 1 percent of polyvinyl alcohol, water and homogenizing; modified SiO2Preparing sol: stirring and mixing 1-5 parts of ammonia water and 40-80 parts of ethanol in parts by volume; adding 2-6 parts of tetraethyl orthosilicate and 0.5-1% MgSO4Stirring and mixing with 0.5-1% polyvinyl alcohol, adding 2-8 parts of hexadecyl trimethoxy silane, and stirring and mixing. The invention adopts modified SiO2The sol and the composite wax emulsion finish cotton fabric has a static water contact angle as high as 164.7 degrees, still has high hydrophobic performance after being washed for 50 times, and the wax emulsion and the modified SiO2The grain sizes are all small, and the double-dispersion type characteristic is almost presented.
Description
Technical Field
The invention belongs to the technical field of textile hydrophobic finishing agents, and particularly relates to a preparation method of a fluorine-free super-hydrophobic cotton fabric.
Background
The super-hydrophobic textile has been widely noticed in the industry because of its excellent self-cleaning, anti-ice, anti-pollution and waterproof properties. The method has two paths for performing super-hydrophobic finishing on the textile, wherein the first is to prepare hydrophobic fibers and then prepare the hydrophobic textile, but the production cost is high and the method cannot be adopted generally; and secondly, the hydrophobic finishing agent is used for carrying out hydrophobic finishing on the textile, and is the most important in industrial production and academic research in the industry at present. Therefore, when the textile is subjected to hydrophobic finishing, a hydrophobic finishing agent is inevitably used. The development of the fabric hydrophobic finishing agent dates back hundreds of years, people firstly use oily substances for hydrophobic finishing, and then use metal soaps, aromatic polycarboxylic acids and the like for hydrophobic finishing, but the fabrics finished by the small molecular compounds are easy to discolor and have a non-lasting hydrophobic effect, so that the fabrics are gradually replaced by novel hydrophobic finishing agents. At present, in the market of fabric finishing agents, the hydrophobic finishing agents mainly comprise fluorine-containing hydrophobic agents, organosilicon hydrophobic agents, fluorine-silicon mixed hydrophobic agents, polyurethane hydrophobic agents, acrylate hydrophobic agents and the like.
The prior textile hydrophobic finishing agent has the defects of poor hydrophobic mechanical stability effect, poor chemical stability and the like, so how to prepare the super-hydrophobic finishing agent with excellent super-hydrophobic effect, good mechanical stability and acid and alkali corrosion resistance is a technical problem to be solved in the prior art.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above-mentioned technical drawbacks.
Therefore, the invention overcomes the defects in the prior art and provides a preparation method of the fluorine-free super-hydrophobic cotton fabric.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of a fluorine-free super-hydrophobic cotton fabric comprises the following steps of: mixing and heating 10-15 parts by mass of a mixture of paraffin and palm wax and 1-5 parts by mass of a surfactant; adding 0.1 to 1 percent of MgSO40.5 to 1 percent of polyvinyl alcohol, water and homogenizing; modified SiO2Preparing sol: stirring and mixing 1-5 parts of ammonia water and 40-80 parts of ethanol in parts by volume; adding 2-6 parts of tetraethyl orthosilicate and 0.5-1% MgSO4Stirring and mixing with 0.5-1% polyvinyl alcohol, adding 2-8 parts of hexadecyl trimethoxy silane, and stirring and mixing.
As an optimal scheme of the preparation method of the fluorine-free super-hydrophobic cotton fabric, the method comprises the following steps: a mixture of the paraffin wax and the carnauba wax, wherein the paraffin wax: 1, palm wax: 9-6: 4.
as an optimal scheme of the preparation method of the fluorine-free super-hydrophobic cotton fabric, the method comprises the following steps: the surfactant comprises fatty alcohol-polyoxyethylene ether, stearic acid and span 60, and the fatty alcohol-polyoxyethylene ether is calculated by mass ratio: stearic acid: span 60 ═ 2:1: 16.
as an optimal scheme of the preparation method of the fluorine-free super-hydrophobic cotton fabric, the method comprises the following steps: and preparing the composite wax emulsion, wherein the heating is carried out at the temperature of 110-120 ℃ for 10-15 min.
As an optimal scheme of the preparation method of the fluorine-free super-hydrophobic cotton fabric, the method comprises the following steps: and preparing the composite wax emulsion, wherein the temperature of the water is 95-98 ℃, and the homogenizing comprises stirring at the rotating speed of 18-21 k rpm for 3-5 min.
As an optimal scheme of the preparation method of the fluorine-free super-hydrophobic cotton fabric, the method comprises the following steps: the modified SiO2And preparing the sol, wherein 1-5 parts of ammonia water and 40-80 parts of ethanol are stirred and mixed, the stirring speed is 100-200 rpm, and the stirring time is 30-50 min.
As an optimal scheme of the preparation method of the fluorine-free super-hydrophobic cotton fabric, the method comprises the following steps: adding 2-6 parts of tetraethyl orthosilicate and 0.5-1% MgSO4And 0.5-1% polyvinyl alcohol are stirred and mixed, the stirring speed is 500-1000 rpm, and the stirring time is 1-3 h.
As an optimal scheme of the preparation method of the fluorine-free super-hydrophobic cotton fabric, the method comprises the following steps: and 2-8 parts of hexadecyl trimethoxy silane is added, stirred and mixed, the stirring speed is 500-1000 rpm, and the stirring time is 1-3 hours.
As an optimal scheme of the preparation method of the fluorine-free super-hydrophobic cotton fabric, the method comprises the following steps: further comprising impregnating a fabric with the modified SiO2Baking the sol, and then soaking the sol in the composite wax emulsion.
As an optimal scheme of the preparation method of the fluorine-free super-hydrophobic cotton fabric, the method comprises the following steps: soaking cotton fabric in the modified SiO2In sol for 20min, pre-baking at 80 ℃ for 5min, baking in an oven at 135 ℃ for 5min, cooling, and soaking in the composite wax emulsion to obtain the fluorine-free super-hydrophobic cotton fabric
The invention has the beneficial effects that: the invention adopts modified SiO2The sol finished cotton fabric and the composite wax emulsion have synergistic effect, so that the cotton fabric has excellent super-hydrophobic performance. Preparing SiO by using tetraethyl orthosilicate (TEOS) as a silicon source, ammonia water as a catalyst and absolute ethyl alcohol as a solvent2Sol, and then SiO by taking hexadecyl trimethoxy silane (HDTMS) as a silane coupling agent2Modification of so that SiO2The sol changes from hydrophilic to hydrophobic. Adopts composite wax emulsion and modified SiO2The sol finished cotton fabric has a static water contact angle as high as 164.7 degrees, still has high hydrophobic performance after being washed for 50 times, and wax emulsion and modified SiO2The grain sizes are all small, and the double-dispersion type characteristic is almost presented.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1:
first, 15g of composite wax (M) is compoundedParaffin wax:MPalm wax2:8) and 0.75g of complex emulsifier (M)O-25:MSA:MSpan-602:1:16) is placed in a beaker and put into an oil bath pan at the temperature of 110 ℃ for heating and melting;
completely melting after 13min, and adding 1% MgSO41% polyvinyl alcohol and 100mL of hot water (96 ℃), stirring for 3min at the rotating speed of 20k rpm by using a homogenizer, and stopping stirring to obtain a milky white liquid;
thirdly, filtering the obtained emulsion through a 180-mesh steel wire mesh screen, and filtering a little residue to obtain uniform and stable milky white liquid.
Fourthly, taking 2mL of ammonia water into another beaker, adding 50mL of absolute ethyl alcohol, and stirring for 40min under a magnetic stirrer at the stirring speed of 200 rpm;
fifthly, adding 3mL of TEOS and 1% of MgSO4And 1% polyvinyl alcohol, the reaction temperature is 40 ℃, a magnetic stirrer is used for stirring for 2 hours, and the stirring speed is 800 rpm;
sixthly, adding 2mL of hexadecyl trimethoxy silane, and continuously stirring for 2.5h at the stirring speed of 1000 rpm;
the stirring is stopped, the beaker is slightly shaken to observe that milky white liquid contains a small amount of white viscous substances, and the surface of the emulsion has a very small amount of oily substances, which indicates that the super-hydrophobic modified SiO is successfully prepared2And (3) sol.
And (3) testing and results:
taking modified SiO produced by stephania2And (3) soaking 3 pieces of cotton cloth in 30mL of sol in a beaker for 20min, taking out, placing in an oven, pre-baking for 5min at 80 ℃, baking for 5min at 135 ℃ in the oven, and finally placing the cotton cloth in a room to cool to room temperature. And (4) putting 30mL of the composite wax emulsion prepared in the step (three) into another beaker, soaking the cotton cloth finished by the composite wax emulsion into the beaker, and finishing the cotton cloth in the same way according to the method. Dropping water drops on the cotton cloth cooled to room temperature, wherein the water drops are spherical, the cotton cloth is slightly inclined, and the water drops can freely roll so that the cotton cloth shows excellent super-hydrophobic performance.
And measuring the contact angle of 1 piece of the cotton cloth obtained by baking to be as high as 164.7 degrees under a DSA100 contact angle measuring instrument.
The particle diameter of the composite wax emulsion is 50nm measured by a zeta potential and particle diameter instrument, and the modified SiO2The particle size was 54 nm.
Example 2:
first, 15g of composite wax (M) is compoundedParaffin wax:MPalm wax3:7) and 0.75g of complex emulsifier (M)O-25:MSA:MSpan-602:1:16) is placed in a beaker and put into an oil bath pan at the temperature of 110 ℃ for heating and melting;
completely melting after 14min, and adding 1% MgSO41% polyvinyl alcohol and 100mL of hot water (95 ℃), stirring for 3min at the rotating speed of 20k rpm by using a homogenizer, and stopping stirring to obtain a milky white liquid;
thirdly, filtering the obtained emulsion through a 180-mesh steel wire mesh screen, and filtering a little residue to obtain uniform and stable milky white liquid.
Fourthly, taking 2mL of ammonia water into another beaker, adding 50mL of absolute ethyl alcohol, and stirring for 40min under a magnetic stirrer at the stirring speed of 200 rpm;
fifthly, adding 3mL of TEOS and 1% of MgSO4And 1% polyvinyl alcohol, the reaction temperature is 40 ℃, a magnetic stirrer is used for stirring for 2 hours, and the stirring speed is 807 rpm;
sixthly, adding 2mL of hexadecyl trimethoxy silane, and continuing to stir for 2.5h at a stirring speed of 1030 rpm;
the stirring is stopped, the beaker is slightly shaken to observe that milky white liquid contains a small amount of white viscous substances, and the surface of the emulsion has a very small amount of oily substances, which indicates that the super-hydrophobic modified SiO is successfully prepared2And (3) sol.
And (3) testing and results:
taking modified SiO produced by stephania2And (3) soaking 3 pieces of cotton cloth in 30mL of sol in a beaker for 20min, taking out, placing in an oven, pre-baking for 5min at 80 ℃, baking for 5min at 135 ℃ in the oven, and finally placing the cotton cloth in a room to cool to room temperature. And (4) putting 30mL of the composite wax emulsion prepared in the step (three) into another beaker, soaking the cotton cloth finished by the composite wax emulsion into the beaker, and finishing the cotton cloth in the same way according to the method. Dropping water drops on the cotton cloth cooled to room temperature, wherein the water drops are spherical, the cotton cloth is slightly inclined, and the water drops can freely roll so that the cotton cloth shows excellent super-hydrophobic performance.
And measuring the contact angle of 1 other piece of cotton cloth obtained by baking to be up to 158 degrees under a DSA100 contact angle measuring instrument.
The particle diameter of the composite wax emulsion is 86nm measured by a zeta potential and particle diameter instrument, and the modified SiO2The particle size was 54 nm.
Example 3:
first, 15g of composite wax (M) is compoundedParaffin wax:MPalm wax2:8) and 0.75g of complex emulsifier (M)O-25:MSA:MSpan-602:1:16) is placed in a beaker and put into an oil bath pan at the temperature of 110 ℃ for heating and melting;
completely melting after 13min, and adding 1% MgSO41% polyvinyl alcohol and 100mL of hot water (96 ℃), stirring for 3min at the rotating speed of 20k rpm by using a homogenizer, and stopping stirring to obtain a milky white liquid;
thirdly, filtering the obtained emulsion through a 180-mesh steel wire mesh screen, and filtering a little residue to obtain uniform and stable milky white liquid.
Fourthly, taking 2mL of ammonia water into another beaker, adding 50mL of absolute ethyl alcohol, and stirring for 40min under a magnetic stirrer at the stirring speed of 200 rpm;
fifthly, adding 3mL of TEOS and 1% of MgSO4And 1% polyvinyl alcohol, the reaction temperature is 42 ℃, a magnetic stirrer is used for stirring for 2 hours, and the stirring speed is 810 rpm;
sixthly, adding 3mL of hexadecyl trimethoxy silane, and continuously stirring for 2.5h at the stirring speed of 1020 rpm;
the stirring is stopped, the beaker is slightly shaken to observe that milky white liquid contains a small amount of white viscous substances, and the surface of the emulsion has a very small amount of oily substances, which indicates that the super-hydrophobic modified SiO is successfully prepared2And (3) sol.
And (3) testing and results:
taking modified SiO produced by stephania2And (3) soaking 3 pieces of cotton cloth in 30mL of sol in a beaker for 20min, taking out, placing in an oven, pre-baking for 5min at 80 ℃, baking for 5min at 135 ℃ in the oven, and finally placing the cotton cloth in a room to cool to room temperature. And (4) putting 30mL of the composite wax emulsion prepared in the step (three) into another beaker, soaking the cotton cloth finished by the composite wax emulsion into the beaker, and finishing the cotton cloth in the same way according to the method. Dropping water drop on cotton cloth cooled to room temperature, the water drop is spherical, slightly inclining the cotton cloth, and the waterThe beads can roll freely so that the cotton cloth shows excellent superhydrophobic performance.
And measuring the contact angle of 1 other piece of cotton cloth obtained by baking under a DSA100 contact angle measuring instrument to be up to 161 degrees.
The particle diameter of the composite wax emulsion is 50nm measured by a zeta potential and particle diameter instrument, and the modified SiO2The particle size was 67 nm.
Example 4:
first, 14.7g of composite wax (M) is compoundedParaffin wax:MPalm wax2:8) and 0.73g of complex emulsifier (M)O-25:MSA:MSpan-602:1:16) is placed in a beaker and put into an oil bath pan at the temperature of 110 ℃ for heating and melting;
completely melting after 12min, and adding 1% MgSO41% polyvinyl alcohol and 100mL of hot water (96 ℃), stirring for 3min at the rotating speed of 20k rpm by using a homogenizer, and stopping stirring to obtain a milky white liquid;
thirdly, filtering the obtained emulsion through a 180-mesh steel wire mesh screen, and filtering a little residue to obtain uniform and stable milky white liquid.
Taking 2mL of ammonia water into another beaker, adding 50mL of absolute ethyl alcohol, and stirring for 40min under a magnetic stirrer at the stirring speed of 210 rpm;
fifthly, adding 3mL of TEOS and 1% of MgSO4And 1% polyvinyl alcohol, the reaction temperature is 42 ℃, a magnetic stirrer is used for stirring for 2 hours, and the stirring speed is 820 rpm;
sixthly, adding 4mL of hexadecyl trimethoxy silane, and continuously stirring for 2.5h at the stirring speed of 1010 rpm;
the stirring is stopped, the beaker is slightly shaken to observe that milky white liquid contains a small amount of white viscous substances, and the surface of the emulsion has a very small amount of oily substances, which indicates that the super-hydrophobic modified SiO is successfully prepared2And (3) sol.
And (3) testing and results:
taking modified SiO produced by stephania2And (3) soaking 3 pieces of cotton cloth in 30mL of sol in a beaker for 20min, taking out, placing in an oven, pre-baking for 5min at 80 ℃, baking for 5min at 135 ℃ in the oven, and finally placing the cotton cloth in a room to cool to room temperature. Prepared from the step three30mL of the composite wax emulsion is put in another beaker, and the cotton cloth finished by the composite wax emulsion is soaked in the composite wax emulsion and is finished by the same method. Dropping water drops on the cotton cloth cooled to room temperature, wherein the water drops are spherical, the cotton cloth is slightly inclined, and the water drops can freely roll so that the cotton cloth shows excellent super-hydrophobic performance.
And measuring the contact angle of 1 piece of the cotton cloth obtained by baking under a DSA100 contact angle measuring instrument to be as high as 159 degrees.
The particle diameter of the composite wax emulsion is 50nm measured by a zeta potential and particle diameter instrument, and the modified SiO2The particle size was 97 nm.
Example 5:
first, 14.7g of composite wax (M) is compoundedParaffin wax:MPalm wax2:8) and 0.73g of complex emulsifier (M)O-25:MSA:MSpan-602:1:16) is placed in a beaker and put into an oil bath pan at the temperature of 110 ℃ for heating and melting;
completely melting after 12min, and adding 1% MgSO41% polyvinyl alcohol and 100mL of hot water (96 ℃), stirring for 3min at the rotating speed of 20k rpm by using a homogenizer, and stopping stirring to obtain a milky white liquid;
thirdly, filtering the obtained emulsion through a 180-mesh steel wire mesh screen, and filtering a little residue to obtain uniform and stable milky white liquid.
Taking 2mL of ammonia water into another beaker, adding 50mL of absolute ethyl alcohol, and stirring for 41min under a magnetic stirrer at a stirring speed of 205 rpm;
fifthly, adding 4mL of TEOS and 1% of MgSO4And 1% polyvinyl alcohol, the reaction temperature is 42 ℃, a magnetic stirrer is used for stirring for 2 hours, and the stirring speed is 830 rpm;
sixthly, adding 2mL of hexadecyl trimethoxy silane, and continuously stirring for 2.5h at the stirring speed of 1020 rpm;
the stirring is stopped, the beaker is slightly shaken to observe that milky white liquid contains a small amount of white viscous substances, and the surface of the emulsion has a very small amount of oily substances, which indicates that the super-hydrophobic modified SiO is successfully prepared2And (3) sol.
And (3) testing and results:
taking modified SiO produced by stephania2And (3) soaking 3 pieces of cotton cloth in 30mL of sol in a beaker for 20min, taking out, placing in an oven, pre-baking for 5min at 80 ℃, baking for 5min at 135 ℃ in the oven, and finally placing the cotton cloth in a room to cool to room temperature. And (4) putting 30mL of the composite wax emulsion prepared in the step (three) into another beaker, soaking the cotton cloth finished by the composite wax emulsion into the beaker, and finishing the cotton cloth in the same way according to the method. Dropping water drops on the cotton cloth cooled to room temperature, wherein the water drops are spherical, the cotton cloth is slightly inclined, and the water drops can freely roll so that the cotton cloth shows excellent super-hydrophobic performance.
And measuring the contact angle of 1 other piece of cotton cloth obtained by baking to be up to 160 degrees under a DSA100 contact angle measuring instrument.
The particle diameter of the composite wax emulsion is 50nm measured by a zeta potential and particle diameter instrument, and the modified SiO2The particle size was 74 nm.
Example 6:
first, 14.8g of composite wax (M) is compoundedParaffin wax:MPalm wax2:8) and 0.76g of complex emulsifier (M)O-25:MSA:MSpan-602:1:16) is placed in a beaker and put into an oil bath pan at the temperature of 110 ℃ for heating and melting;
completely melting after 12min, and adding 1% MgSO41% polyvinyl alcohol and 100mL hot water (97 ℃), stirring for 3min at the rotating speed of 20.1k rpm by a homogenizer, and stopping stirring to obtain a milky white liquid;
thirdly, filtering the obtained emulsion through a 180-mesh steel wire mesh screen, and filtering a little residue to obtain uniform and stable milky white liquid.
Taking 3mL of ammonia water into another beaker, adding 50mL of absolute ethyl alcohol, and stirring for 40min under a magnetic stirrer at the stirring speed of 210 rpm;
fifthly, adding 3mL of TEOS and 1% of MgSO4And 1% polyvinyl alcohol, the reaction temperature is 42 ℃, a magnetic stirrer is used for stirring for 2 hours, and the stirring speed is 825 rpm;
sixthly, adding 2mL of hexadecyl trimethoxy silane, and continuing to stir for 2.5h at the stirring speed of 1019 rpm;
the stirring was stopped and observed with gentle shaking of the beakerThe milky white liquid contains a small amount of white viscous substances, and the surface of the emulsion contains a very small amount of oily substances, which indicates that the super-hydrophobic modified SiO is successfully prepared2And (3) sol.
And (3) testing and results:
taking modified SiO produced by stephania2And (3) soaking 3 pieces of cotton cloth in 30mL of sol in a beaker for 20min, taking out, placing in an oven, pre-baking for 5min at 80 ℃, baking for 5min at 135 ℃ in the oven, and finally placing the cotton cloth in a room to cool to room temperature. And (4) putting 30mL of the composite wax emulsion prepared in the step (three) into another beaker, soaking the cotton cloth finished by the composite wax emulsion into the beaker, and finishing the cotton cloth in the same way according to the method. Dropping water drops on the cotton cloth cooled to room temperature, wherein the water drops are spherical, the cotton cloth is slightly inclined, and the water drops can freely roll so that the cotton cloth shows excellent super-hydrophobic performance.
And measuring the contact angle of 1 other piece of cotton cloth obtained by baking to be as high as 164 degrees under a DSA100 contact angle measuring instrument.
The particle diameter of the composite wax emulsion is 50nm measured by a zeta potential and particle diameter instrument, and the modified SiO2The particle size was 75 nm.
Example 7:
first, 14.6g of composite wax (M) is compoundedParaffin wax:MPalm wax2:8) and 0.75g of complex emulsifier (M)O-25:MSA:MSpan-602:1:16) is placed in a beaker and put into an oil bath pan at the temperature of 110 ℃ for heating and melting;
completely melting after 12min, and adding 1% MgSO40.5 percent of polyvinyl alcohol and 100mL of hot water (95 ℃), stirring for 3min at the rotating speed of 20.1k rpm by a homogenizer, and stopping stirring to obtain milky white liquid;
thirdly, filtering the obtained emulsion through a 180-mesh steel wire mesh screen, and filtering a little residue to obtain uniform and stable milky white liquid.
Taking 2mL of ammonia water into another beaker, adding 50mL of absolute ethyl alcohol, and stirring for 40min under a magnetic stirrer at the stirring speed of 210 rpm;
fifthly, adding 3mL of TEOS and 1% of MgSO4And 1% polyvinyl alcohol at 42 deg.C, magnetically stirringStirring for 2 hours by using a stirrer, wherein the stirring speed is 820 rpm;
sixthly, adding 2mL of hexadecyl trimethoxy silane, and continuously stirring for 2.5h at the stirring speed of 1010 rpm;
the stirring is stopped, the beaker is slightly shaken to observe that milky white liquid contains a small amount of white viscous substances, and the surface of the emulsion has a very small amount of oily substances, which indicates that the super-hydrophobic modified SiO is successfully prepared2And (3) sol.
And (3) testing and results:
taking modified SiO produced by stephania2And (3) soaking 3 pieces of cotton cloth in 30mL of sol in a beaker for 20min, taking out, placing in an oven, pre-baking for 5min at 80 ℃, baking for 5min at 135 ℃ in the oven, and finally placing the cotton cloth in a room to cool to room temperature. And (4) putting 30mL of the composite wax emulsion prepared in the step (three) into another beaker, soaking the cotton cloth finished by the composite wax emulsion into the beaker, and finishing the cotton cloth in the same way according to the method. Dropping water drops on the cotton cloth cooled to room temperature, wherein the water drops are spherical, the cotton cloth is slightly inclined, and the water drops can freely roll so that the cotton cloth shows excellent super-hydrophobic performance.
And measuring the contact angle of 1 other piece of cotton cloth obtained by baking to be up to 158 degrees under a DSA100 contact angle measuring instrument.
The particle diameter of the composite wax emulsion is 50nm measured by a zeta potential and particle diameter instrument, and the modified SiO2The particle size was 95 nm.
Example 8:
first, 14.7g of composite wax (M) is compoundedParaffin wax:MPalm wax2:8) and 0.73g of complex emulsifier (M)O-25:MSA:MSpan-602:1:16) is placed in a beaker and put into an oil bath pan at the temperature of 110 ℃ for heating and melting;
completely melting after 12min, and adding 1% MgSO41% polyvinyl alcohol and 100mL of hot water (96 ℃), stirring for 3min at the rotating speed of 20k rpm by using a homogenizer, and stopping stirring to obtain a milky white liquid;
thirdly, filtering the obtained emulsion through a 180-mesh steel wire mesh screen, and filtering a little residue to obtain uniform and stable milky white liquid.
Taking 2mL of ammonia water into another beaker, adding 50mL of absolute ethyl alcohol, and stirring for 40min under a magnetic stirrer at the stirring speed of 210 rpm;
fifthly, 3mL of TEOS and 0.5% MgSO4And 0.5 percent of polyvinyl alcohol, the reaction temperature is 42 ℃, a magnetic stirrer is used for stirring for 2 hours, and the stirring speed is 820 rpm;
sixthly, adding 2mL of hexadecyl trimethoxy silane, and continuously stirring for 2.5h at the stirring speed of 1010 rpm;
the stirring is stopped, the beaker is slightly shaken to observe that milky white liquid contains a small amount of white viscous substances, and the surface of the emulsion has a very small amount of oily substances, which indicates that the super-hydrophobic modified SiO is successfully prepared2And (3) sol.
And (3) testing and results:
taking modified SiO produced by stephania2And (3) soaking 3 pieces of cotton cloth in 30mL of sol in a beaker for 20min, taking out, placing in an oven, pre-baking for 5min at 80 ℃, baking for 5min at 135 ℃ in the oven, and finally placing the cotton cloth in a room to cool to room temperature. And (4) putting 30mL of the composite wax emulsion prepared in the step (three) into another beaker, soaking the cotton cloth finished by the composite wax emulsion into the beaker, and finishing the cotton cloth in the same way according to the method. Dropping water drops on the cotton cloth cooled to room temperature, wherein the water drops are spherical, the cotton cloth is slightly inclined, and the water drops can freely roll so that the cotton cloth shows excellent super-hydrophobic performance.
And measuring the contact angle of 1 piece of the cotton cloth obtained by baking under a DSA100 contact angle measuring instrument to be as high as 159 degrees.
The particle diameter of the composite wax emulsion is 50nm measured by a zeta potential and particle diameter instrument, and the modified SiO2The particle size was 98 nm. Comparative example 1:
first, 16g of composite wax (M) is providedParaffin wax:MPalm wax2:8) and 0.76g of complex emulsifier (M)O-25:MSA:MSpan-602:1:16) is placed in a beaker and put into an oil bath pan at the temperature of 110 ℃ for heating and melting;
completely melting after 13min, and adding 1% MgSO41% polyvinyl alcohol and 100mL hot water (97 ℃), stirring with a homogenizer at 20k rpm for 3min, and stopping stirring to obtain milky white liquidA body;
thirdly, filtering the obtained emulsion through a 180-mesh steel wire mesh screen, and filtering a little residue to obtain uniform and stable milky white liquid.
And (3) testing and results:
and (3) putting 30mL of the composite wax emulsion prepared in the step (three) into a beaker, soaking 3 pieces of cotton cloth in the beaker for 20min, taking out the composite wax emulsion, putting the composite wax emulsion into an oven, pre-drying the composite wax emulsion for 5min at 80 ℃, baking the composite wax emulsion for 5min at 135 ℃ in the oven, and finally cooling the cotton cloth indoors to room temperature. Dropping water drops on the cotton cloth cooled to room temperature, wherein the water drops are spherical, the cotton cloth is slightly inclined, and the water drops can freely roll so that the cotton cloth shows excellent super-hydrophobic performance.
And measuring the contact angle of 1 piece of the cotton cloth obtained by baking to be as high as 150.8 degrees under a DSA100 contact angle measuring instrument.
The particle size of the composite wax emulsion is 50nm measured by a zeta potential and particle size instrument.
Comparative example 2:
first, 16.2g composite wax (M) is appliedParaffin wax:MPalm wax2:8) and 0.81g of complex emulsifier (M)O-25:MSA:MSpan-601:1:7) is placed in a beaker, and is placed in an oil bath pan at the temperature of 110 ℃ for heating and melting;
completely melting after 14min, and adding 1% MgSO41% polyvinyl alcohol and 100mL of hot water (96 ℃), stirring for 3min at the rotating speed of 20.1k rpm by using a homogenizer, and stopping stirring to obtain a milky white liquid;
thirdly, filtering the obtained emulsion through a 180-mesh steel wire mesh screen, and filtering a little residue to obtain uniform and stable milky white liquid.
And (3) testing and results:
and (3) putting 30mL of the composite wax emulsion prepared in the step (three) into a beaker, soaking 3 pieces of cotton cloth in the beaker for 20min, taking out the composite wax emulsion, putting the composite wax emulsion into an oven, pre-drying the composite wax emulsion for 5min at 80 ℃, baking the composite wax emulsion for 5min at 135 ℃ in the oven, and finally cooling the cotton cloth indoors to room temperature. The water drops are dropped on the cotton cloth cooled to the room temperature, the water drops are spherical, the cotton cloth is slightly inclined, the water drops have certain adhesion with the cotton cloth, and the cotton cloth is not easy to roll.
And measuring the contact angle of 1 other piece of cotton cloth obtained by baking to be 148.7 degrees under a DSA100 contact angle measuring instrument.
The particle size of the composite wax emulsion is 124nm measured by a zeta potential and particle size instrument.
TABLE 1 Experimental results of hydrophobic cotton fabric prepared by different component ratios of the composite wax emulsion of the invention
The particle size of the composite wax emulsion can be influenced by the rotating speed of the homogenizer, and the inventor finds that when the rotating speed of the homogenizer is within the range of 0.5K-10K rpm, the particle size of the composite wax emulsion is larger and is within the range of 0.1-1 um; the grain size of the homogenizer is smaller within the range of 10K-20K rpm and is within the range of 50-100 nm; when the rotating speed of the homogenizer is more than 20K rpm, the particle size of the emulsion tends to be stable. When preparing the emulsion, the emulsification temperature was set to 110 ℃.
TABLE 2 modified SiO of the invention2Different components of sol are proportioned and prepared hydrophobic cotton fabric experimental result
Description of the drawings: in Table 2, the modified SiO of each experiment number in Table 2 is used2The sol formula is used for finishing cotton fabrics respectively, and then the cotton fabrics are finished by soaking, rolling, pre-baking and baking according to the formula of the composite wax emulsion with the experiment number 3 in the table 1.
TABLE 3 static contact angle and static water absorption time of the super-hydrophobic cotton fabric prepared by the present invention after soaping
Description of the drawings: table 3 modified SiO prepared with cotton fabric from example No. 2 in table 22After sol conditioning, the composite wax emulsion prepared in example No. 3 of 1 was further conditioned as an experimental object.
TABLE 4 static contact angle and static water absorption time of the super-hydrophobic cotton fabric prepared by the invention after friction treatment
Description of the drawings: table 4 modified SiO prepared from example No. 2 in table 2 as a cotton fabric2After sol conditioning, the composite wax emulsion prepared in example No. 3 of 1 was further conditioned as an experimental object.
Table 5 shows the test results of the water impact resistance of the super-hydrophobic cotton fabric prepared by the invention
Description of the drawings: table 5 modified SiO with cotton fabric prepared from example No. 2 in table 22After sol conditioning, the composite wax emulsion prepared in example No. 3 of 1 was further conditioned as an experimental object.
The invention adopts modified SiO in a breakthrough manner2The super-hydrophobic cotton fabric is prepared from the sol and the composite wax emulsion through two steps, and the sol and the composite wax emulsion have synergistic effect, so that the low surface energy advantage of the sol and the composite wax emulsion is fully exerted. The super-hydrophobic cotton fabric prepared by the method has excellent super-hydrophobic performance, the water contact angle is as high as 164 degrees, and the super-hydrophobic performance is far superior to that of the super-hydrophobic cotton fabric prepared by some fluorine-containing finishing agents. The invention relates to modified SiO adopted for preparing super-hydrophobic cotton fabric2The particle sizes of the sol and the composite wax emulsion are relatively small, are respectively 50-100 nm and 50nm, almost show a double-dispersion characteristic, and bulges with different sizes are easily formed on the surface of the cotton fabric, so that an excellent micro-nano coarse structure is formed. Modified SiO prepared by the invention2The particle size of the sol is within the range of 50-100 nm, and the fine and narrow distribution particle size endows the nano SiO2The hydroxyl group of the particle is easy to combine with the hydroxyl group contained in the cotton fiber, thereby endowing the cotton fabric with excellent super-hydrophobicityCan reach the durability. The composite wax emulsion used for preparing the super-hydrophobic cotton fabric has the grain diameter of only 50nm, is easy to adhere to the surface of the cotton fabric under the action of an adhesive and is not easy to fall off, so that the cotton fabric has excellent super-hydrophobic performance and durability.
The super-hydrophobic cotton fabric prepared by the method has good mechanical stability and acid and alkali corrosion resistance, the application range of the cotton fabric is greatly enlarged, and the service life of the cotton fabric is greatly prolonged.
The invention relates to modified SiO adopted for preparing super-hydrophobic cotton fabric2The sol and the composite wax emulsion both have good stability, so that compared with similar products in the market, the emulsion has the advantages that the service life of the emulsion is greatly prolonged, and the industrial large-scale production requirement can be met.
The emulsion used for preparing the super-hydrophobic cotton fabric is added with special adhesive and stabilizer, so that the emulsion has good binding force with the cotton fabric, the super-hydrophobic property of the cotton fabric is greatly improved, and the cotton fabric has excellent stability.
The emulsion used for preparing the super-hydrophobic cotton fabric is environment-friendly, has easily obtained raw materials and low cost, and is suitable for industrial production.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (4)
1. A preparation method of fluorine-free super-hydrophobic cotton fabric is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
preparing the composite wax emulsion: mixing 10-15 parts by mass of a mixture of paraffin and palm wax with 1-5 parts by mass of a surfactant, and heating at 110-120 ℃ for 10-15 min; adding 0.1 to 1 percent of MgSO4Stirring the mixture for 3-5 min at the rotating speed of 18 k-21 krpm by using 0.5-1% of polyvinyl alcohol and water at the temperature of 95-98 ℃ to obtain a composite wax emulsion; wherein the content of the first and second substances,
the mass ratio of the paraffin to the palm wax is 3: 7-6: 4;
the surfactant comprises fatty alcohol-polyoxyethylene ether, stearic acid and span 60, and the fatty alcohol-polyoxyethylene ether is calculated by mass ratio: stearic acid: span 60 ═ 2:1: 16;
modified SiO2Preparing sol: stirring and mixing 1-5 parts of ammonia water and 40-80 parts of ethanol in parts by volume; adding 2-6 parts of tetraethyl orthosilicate and 0.5-1% MgSO4Stirring and mixing with 0.5-1% polyvinyl alcohol, adding 2-8 parts of hexadecyl trimethoxy silane, stirring and mixing to obtain modified SiO2Sol;
soaking cotton fabric in the modified SiO2And (3) dissolving in the sol for 20min, pre-baking at 80 ℃ for 5min, baking in an oven at 135 ℃ for 5min, cooling, and soaking in the composite wax emulsion to obtain the fluorine-free super-hydrophobic cotton fabric.
2. The method for preparing a fluorine-free superhydrophobic cotton fabric of claim 1, wherein: the modified SiO2And preparing the sol, wherein 1-5 parts of ammonia water and 40-80 parts of ethanol are stirred and mixed, the stirring speed is 100-200 rpm, and the stirring time is 30-50 min.
3. The method for preparing a fluorine-free superhydrophobic cotton fabric according to claim 1 or 2, characterized in that: adding 2-6 parts of tetraethyl orthosilicate and 0.5-1% MgSO4And 0.5-1% polyvinyl alcohol are stirred and mixed, the stirring speed is 500-1000 rpm, and the stirring time is 1-3 h.
4. The method for preparing a fluorine-free superhydrophobic cotton fabric according to claim 1 or 2, characterized in that: and 2-8 parts of hexadecyl trimethoxy silane is added, stirred and mixed, the stirring speed is 500-1000 rpm, and the stirring time is 1-3 hours.
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