CN101768856B - Super hydrophobic cotton fabric and preparation method thereof - Google Patents
Super hydrophobic cotton fabric and preparation method thereof Download PDFInfo
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- CN101768856B CN101768856B CN2009102545789A CN200910254578A CN101768856B CN 101768856 B CN101768856 B CN 101768856B CN 2009102545789 A CN2009102545789 A CN 2009102545789A CN 200910254578 A CN200910254578 A CN 200910254578A CN 101768856 B CN101768856 B CN 101768856B
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Abstract
The invention belongs to the fabric water-repellent finishing and processing field, in particular relates a super hydrophobic cotton fabric and a preparation method thereof. The preparation method of the super hydrophobic cotton fabric is characterized in that the epoxy-functionalized modification is performed to the cotton fiber of fabric, then aminated nano-SiO2 and epoxy-functionalized nano-SiO2 are used to impregnate the cotton fabric in turn so as to increase the surface roughness of the fabric, finally a low-surface-energy material is adopted to perform hydrophobization treatment to the fabric; the contact angle between the prepared cotton fabric and water drops is more than 150 degrees; the method utilizes the covalent reaction of epoxy groups of cotton fabric, amino groups of nano-SiO2 and epoxy groups of nano-SiO2 to ensure the built rough surface to have good fastness; and the built surface has a large number of Si-OHs and epoxy groups so as to facilitate the chemical combination of the low-surface-energy material and the surface, thus the superhydrophobic property of the prepared fabric has excellent stability.
Description
Technical field
The invention belongs to textiles water repellent finish manufacture field, particularly a kind of preparation method of super-hydrophobic cotton fabric.
Background technology
The super hydrophobic functional textiles not only has important use aspect industrial production, medical treatment, the military use product, and has application widely in daily life.For the automatically cleaning effect Chinese patent CN 1242114C that utilizes super hydrophobic surface discloses nano self-cleaning cashmere or goods and preparation method thereof, Chinese patent CN 1277019C discloses Nanometer self-Cleaning Silk Broadcloth And Products, Chinese patent CN 1824884A discloses the self-cleaning suiting that contains nano-functional material and the method for making of garment products, Chinese patent CN100334291C discloses the preparation method of the feather dress fabric with self-cleaning function, these patent utilization nanoparticles are constructed coarse structure, adopt the Organic fluoride finishing agent that fabric is flooded, coating or spraying, the performance of having given the not only hydrophobic but also oleophobic of fabric.Chinese patent CN 101397754A discloses a kind of preparation method of floride-free super-hydrophobic cotton fabric, and this method adopts silicon dioxide gel to pad COTTON FABRIC, handles obtaining super-hydrophobic cotton fabric again through non-fluothane hydrocarbon.
The preparation of super hydrophobic surface will be constructed micro-nano coarse structure surface on the one hand, another side need reduce the surface energy of rough surface, although the method for the super-hydrophobic textiles of a lot of preparations has been arranged, yet, seldom mention the marriage relation between micro-nano coarse structure surface and the substrate in these methods, still less mention the stability of the ultra-hydrophobicity of prepared super-hydrophobic fabric.
Summary of the invention
The objective of the invention is to super-hydrophobic cotton fabric and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is: earlier the cotton fiber on the COTTON FABRIC is carried out the epoxy radicals modification, adopt amination nano silicon and epoxy radicals nano silicon that COTTON FABRIC is padded then successively, adopt the low-surface-energy material that fabric is padded to handle at last and obtain.
The epoxy radicals method of modifying of said cotton fiber is: it is 5% sodium hydroxide solution that the 2g COTTON FABRIC is put into the 100mL mass concentration, constantly stir the epoxychloropropane that adds 5～10mL down, control reaction temperature is 40～60 ℃ of reactions 5～10 hours, takes out the fabric water it is washed till the dry epoxy radicals COTTON FABRIC that gets in neutral back;
Said amination nano silicon and epoxy radicals preparation method of nano silicon dioxide are:
12mL ethyl orthosilicate and 80mL methanol mixed are got mixed solution A, with the 30mL mass concentration is that 25%～28% ammoniacal liquor and 320mL methanol mixed get mixed solution B, under agitation mixed solution A is added drop-wise among the mixed solution B then and reacts 3～10h, obtain the nano silicon methanol solution;
The mixed solution of the 3-aminopropyltriethoxywerene werene of 0.5～2mL and 5mL methyl alcohol is added drop-wise to the nano silicon methanol solution of 200mL, and sustained response 8～24 hours obtains the amination nano silicon;
The 3-glycidol ether propyl trimethoxy silicane of 0.5～2mL and the mixed solution of 5mL methyl alcohol are added drop-wise in the 200mL nano silicon methanol solution, and sustained response 8～24 hours obtains the epoxy radicals nano silicon.
The method that said amination nano silicon and epoxy radicals nano silicon pad COTTON FABRIC is:
The epoxy radicals COTTON FABRIC is immersed the ethanolic solution that mass concentration is 0.2～2.0% amination nano silicon, one soaks one rolls, at 60～120 ℃ of baking 0.5～1h, and then fabric is immersed mass concentration is 0.2～2.0% epoxy radicals nano silicon ethanolic solution, one soaks one rolls, at 60～120 ℃ of baking 0.5～1h.
Said employing low-surface-energy material is that carbon number is one or more in 6～18 long-chain (fluoro) alkyl carboxylic acid, long-chain (fluoro) alkyl ammonia, long-chain (fluoro) alkylsiloxane, long-chain (fluoro) alkyl silicon chlorosilane, the chain alkyl mercaptan, it is that drying obtains end product in the solution made of the above-mentioned low-surface-energy material of 0.5-1.5% that fabric is immersed mass concentration.
The super-hydrophobic cotton fabric of making by preparation method of the present invention, with the contact angle of water droplet above 150 °.
The present invention utilizes the epoxide group of cotton fiber, the amino group on the nano silicon and the covalent reaction between the epoxide group on the nano silicon to make constructed rough surface have good fastness, and constructed surface has silicon hydroxyl and epoxide group when big, therefore help low-surface-energy material and surperficial chemical bond, therefore make the ultra-hydrophobicity of prepared fabric have advantages of excellent stability.
The specific embodiment
Embodiment 1: it is 5% sodium hydroxide solution that the 2g COTTON FABRIC is put into the 100mL mass concentration, constantly stir the epoxychloropropane that adds 8mL down, control reaction temperature is 40 ℃ of reactions 10 hours, takes out the fabric water it is washed till the dry epoxy radicals COTTON FABRIC that gets in neutral back;
12mL ethyl orthosilicate and 80mL methanol mixed are got mixed solution A, with the 30mL mass concentration is that 26% ammoniacal liquor and 320mL methanol mixed get mixed solution B, under agitation mixed solution A is added drop-wise among the mixed solution B then and reacts 3h, obtain the nano silicon methanol solution;
The mixed solution of the 3-aminopropyltriethoxywerene werene of 0.5mL and 5mL methyl alcohol is added drop-wise to the nano silicon methanol solution of 200mL, and sustained response 12 hours obtains the amination nano silicon;
The 3-glycidol ether propyl trimethoxy silicane of 1mL and the mixed solution of 5mL methyl alcohol are added drop-wise in the 200mL nano silicon methanol solution, and sustained response 12 hours obtains the epoxy radicals nano silicon;
The epoxy radicals COTTON FABRIC is immersed the ethanolic solution that mass concentration is 1% amination nano silicon, one soaks one rolls, and at 100 ℃ of baking 0.5～1h, and then fabric is immersed mass concentration is 1% epoxy radicals nano silicon ethanolic solution, one soaks one rolls, at 100 ℃ of baking 0.5～1h;
It is 0.5% stearic acid acetone soln 10 minutes that fabric is immersed mass concentration, and padding machine rolls and removes surplus liquid, and 110 ℃ of bakings are 1 hour then; Get super-hydrophobic cotton fabric.With fabric in ethanolic solution ultrasonic 1 hour, still has good ultra-hydrophobicity.
Embodiment 2: it is 5% sodium hydroxide solution that the 2g COTTON FABRIC is put into the 100mL mass concentration, constantly stir the epoxychloropropane that adds 10mL down, control reaction temperature is 60 ℃ of reactions 5 hours, takes out the fabric water it is washed till the dry epoxy radicals COTTON FABRIC that gets in neutral back;
12mL ethyl orthosilicate and 80mL methanol mixed are got mixed solution A, with the 30mL mass concentration is that 28% ammoniacal liquor and 320mL methanol mixed get mixed solution B, under agitation mixed solution A is added drop-wise among the mixed solution B then and reacts 8h, obtain the nano silicon methanol solution;
The mixed solution of the 3-aminopropyltriethoxywerene werene of 1mL and 5mL methyl alcohol is added drop-wise to the nano silicon methanol solution of 200mL, and sustained response 20 hours obtains the amination nano silicon;
The 3-glycidol ether propyl trimethoxy silicane of 2mL and the mixed solution of 5mL methyl alcohol are added drop-wise in the 200mL nano silicon methanol solution, and sustained response 20 hours obtains the epoxy radicals nano silicon;
The epoxy radicals COTTON FABRIC is immersed the ethanolic solution that mass concentration is 0.5% amination nano silicon, one soaks one rolls, and at 60 ℃ of baking 0.5～1h, and then fabric is immersed mass concentration is 0.5% epoxy radicals nano silicon ethanolic solution, one soaks one rolls, at 60 ℃ of baking 0.5～1h;
It is 1% 17 fluoro decyltrichlorosilane toluene solutions 1 hour that fabric is immersed mass concentration, takes out drying at room temperature, super-hydrophobic cotton fabric.With fabric in ethanolic solution ultrasonic 1 hour, still has good ultra-hydrophobicity.
Embodiment 3: it is 5% sodium hydroxide solution that the 2g COTTON FABRIC is put into the 100mL mass concentration, constantly stir the epoxychloropropane that adds 6mL down, control reaction temperature is 50 ℃ of reactions 7.5 hours, takes out the fabric water it is washed till the dry epoxy radicals COTTON FABRIC that gets in neutral back;
12mL ethyl orthosilicate and 80mL methanol mixed are got mixed solution A, with the 30mL mass concentration is that 27% ammoniacal liquor and 320mL methanol mixed get mixed solution B, under agitation mixed solution A is added drop-wise among the mixed solution B then and reacts 5h, obtain the nano silicon methanol solution;
The mixed solution of the 3-aminopropyltriethoxywerene werene of 2mL and 5mL methyl alcohol is added drop-wise to the nano silicon methanol solution of 200mL, and sustained response 8 hours obtains the amination nano silicon;
The 3-glycidol ether propyl trimethoxy silicane of 0.8mL and the mixed solution of 5mL methyl alcohol are added drop-wise in the 200mL nano silicon methanol solution, and sustained response 8 hours obtains the epoxy radicals nano silicon;
The epoxy radicals COTTON FABRIC is immersed the ethanolic solution that mass concentration is 0.2% amination nano silicon, one soaks one rolls, and at 80 ℃ of baking 0.5～1h, and then fabric is immersed mass concentration is 0.2% epoxy radicals nano silicon ethanolic solution, one soaks one rolls, at 80 ℃ of baking 0.5～1h;
It is 1.5% stearic acid acetone soln 10 minutes that fabric is immersed mass concentration, and padding machine rolls and removes surplus liquid, and 110 ℃ of bakings are 1 hour then, super-hydrophobic cotton fabric.With fabric in ethanolic solution ultrasonic 1 hour, still has good ultra-hydrophobicity.
Embodiment 4: it is 5% sodium hydroxide solution that the 2g COTTON FABRIC is put into the 100mL mass concentration, constantly stir the epoxychloropropane that adds 9mL down, control reaction temperature is 45 ℃ of reactions 8 hours, takes out the fabric water it is washed till the dry epoxy radicals COTTON FABRIC that gets in neutral back;
12mL ethyl orthosilicate and 80mL methanol mixed are got mixed solution A, with the 30mL mass concentration is that 25% ammoniacal liquor and 320mL methanol mixed get mixed solution B, under agitation mixed solution A is added drop-wise among the mixed solution B then and reacts 10h, obtain the nano silicon methanol solution;
The mixed solution of the 3-aminopropyltriethoxywerene werene of 1.5mL and 5mL methyl alcohol is added drop-wise to the nano silicon methanol solution of 200mL, and sustained response 16 hours obtains the amination nano silicon;
The 3-glycidol ether propyl trimethoxy silicane of 0.8mL and the mixed solution of 5mL methyl alcohol are added drop-wise in the 200mL nano silicon methanol solution, and sustained response 16 hours obtains the epoxy radicals nano silicon;
The epoxy radicals COTTON FABRIC is immersed the ethanolic solution that mass concentration is 1.5% amination nano silicon, one soaks one rolls, at 120 ℃ of baking 0.5～1h, and then fabric is immersed mass concentration is 1.5% epoxy radicals nano silicon ethanolic solution, one soaks one rolls, at 120 ℃ of baking 0.5～1h;
It is 0.8% 17 fluoro decyl trimethoxy silane toluene solutions 1 hour that fabric is immersed mass concentration, takes out drying at room temperature, super-hydrophobic cotton fabric.With fabric in ethanolic solution ultrasonic 1 hour, still has good ultra-hydrophobicity.
Embodiment 5: it is 5% sodium hydroxide solution that the 2g COTTON FABRIC is put into the 100mL mass concentration, constantly stir the epoxychloropropane that adds 5mL down, control reaction temperature is 55 ℃ of reactions 6 hours, takes out the fabric water it is washed till the dry epoxy radicals COTTON FABRIC that gets in neutral back;
12mL ethyl orthosilicate and 80mL methanol mixed are got mixed solution A, with the 30mL mass concentration is that 28% ammoniacal liquor and 320mL methanol mixed get mixed solution B, under agitation mixed solution A is added drop-wise among the mixed solution B then and reacts 7h, obtain the nano silicon methanol solution;
The mixed solution of the 3-aminopropyltriethoxywerene werene of 0.8mL and 5mL methyl alcohol is added drop-wise to the nano silicon methanol solution of 200mL, and sustained response 24 hours obtains the amination nano silicon;
The 3-glycidol ether propyl trimethoxy silicane of 1.5mL and the mixed solution of 5mL methyl alcohol are added drop-wise in the 200mL nano silicon methanol solution, and sustained response 24 hours obtains the epoxy radicals nano silicon;
The epoxy radicals COTTON FABRIC is immersed the ethanolic solution that mass concentration is 2.0% amination nano silicon, one soaks one rolls, and at 90 ℃ of baking 0.5～1h, and then fabric is immersed mass concentration is 2.0% epoxy radicals nano silicon ethanolic solution, one soaks one rolls, at 90 ℃ of baking 0.5～1h;
It is 1.2% dodecyl trimethoxy silane ethanolic solution 1 hour that fabric is immersed mass concentration, takes out drying at room temperature, super-hydrophobic cotton fabric.With fabric in ethanolic solution ultrasonic 1 hour, still has good ultra-hydrophobicity.
Claims (4)
1. the preparation method of a super-hydrophobic cotton fabric, it is characterized in that: earlier the cotton fiber on the COTTON FABRIC is carried out the epoxy radicals modification, adopt amination nano silicon and epoxy radicals nano silicon that COTTON FABRIC is padded then successively, adopt the low-surface-energy material that fabric is padded to handle at last and obtain;
The epoxy radicals method of modifying of described cotton fiber is: it is 5% sodium hydroxide solution that the 2g COTTON FABRIC is put into the 100mL mass concentration, constantly stir the epoxychloropropane that adds 5～10mL down, control reaction temperature is 40～60 ℃ of reactions 5～10 hours, takes out the fabric water it is washed till the dry epoxy radicals COTTON FABRIC that gets in neutral back;
Described employing low-surface-energy material is in 6～18 long-chain (fluoro) alkyl carboxylic acid, long-chain (fluoro) alkyl ammonia, long-chain (fluoro) alkylsiloxane, long-chain (fluoro) alkyl silicon chlorosilane, the chain alkyl mercaptan one or more for carbon number on the long carbochain, it is in the solution made of the above-mentioned low-surface-energy material of 0.5-1.5% that fabric is immersed mass concentration, takes out drying and obtains end product.
2. the preparation method of super-hydrophobic cotton fabric according to claim 1, it is characterized in that: said amination nano silicon and epoxy radicals preparation method of nano silicon dioxide are:
12mL ethyl orthosilicate and 80mL methanol mixed are got mixed solution A, with the 30mL mass concentration is that 25%～28% ammoniacal liquor and 320mL methanol mixed get mixed solution B, under agitation mixed solution A is added drop-wise among the mixed solution B then and reacts 3～10h, obtain the nano silicon methanol solution;
The mixed solution of the 3-aminopropyltriethoxywerene werene of 0.5～2mL and 5mL methyl alcohol is added drop-wise to the nano silicon methanol solution of 200mL, and sustained response 8～24 hours obtains the amination nano silicon;
The 3-glycidol ether propyl trimethoxy silicane of 0.5～2mL and the mixed solution of 5mL methyl alcohol are added drop-wise in the 200mL nano silicon methanol solution, and sustained response 8～24 hours obtains the epoxy radicals nano silicon.
3. the preparation method of super-hydrophobic cotton fabric according to claim 1 and 2, it is characterized in that: the method that said amination nano silicon and epoxy radicals nano silicon pad COTTON FABRIC is:
The epoxy radicals COTTON FABRIC is immersed the ethanolic solution that mass concentration is 0.2～2.0% amination nano silicon, one soaks one rolls, at 60～120 ℃ of baking 0.5～1h, and then fabric is immersed mass concentration is 0.2～2.0% epoxy radicals nano silicon ethanolic solution, one soaks one rolls, at 60～120 ℃ of baking 0.5～1h.
4. super-hydrophobic cotton fabric of making according to the preparation method of the described super-hydrophobic cotton fabric of claim 1, it is characterized in that: the contact angle of this COTTON FABRIC and water droplet is above 150 °.
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