CN111218816A - Preparation method of modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric - Google Patents
Preparation method of modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric Download PDFInfo
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- CN111218816A CN111218816A CN202010145959.XA CN202010145959A CN111218816A CN 111218816 A CN111218816 A CN 111218816A CN 202010145959 A CN202010145959 A CN 202010145959A CN 111218816 A CN111218816 A CN 111218816A
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- 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
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- 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
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- 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
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- 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
- D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments
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- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a preparation method of a modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric, wherein the surface of the cellulose fabric is covered with functional nano-silica. The preparation method comprises the following steps: adding polyamino compound and double bond ester group or anhydride into silicon alkoxide serving as a precursor and absolute ethyl alcohol serving as a solvent to prepare silicon dioxide sol, and putting the silicon dioxide sol into a rotary evaporator for polymerization to obtain amino-coated nano silicon dioxide particles; the amino nano-silica reacts with long-chain fatty acid in methanol solution for grafting to obtain amphiphilic nano-silica powder; and soaking the cellulose fabric in an amphiphilic silica solution by adopting a soaking method, and drying to obtain the silica-loaded uvioresistant super-hydrophobic cellulose fabric.
Description
Technical Field
The invention relates to the technical field of functional nano materials and textile materials, in particular to a preparation method of a modified nano silicon dioxide ultraviolet-proof super-hydrophobic cellulose fabric.
Background
Cellulose fiber is a widely used textile material, has good hygroscopicity and air permeability, and is mainly applied to the fields of clothing, household textiles, medical materials and the like. In recent years, functional finishing of cellulose fibersHave been the subject of numerous studies. The nano material can endow a plurality of new functions, such as antibacterial deodorization, ultraviolet protection performance, super hydrophobicity, self-cleaning, photocatalytic degradation and the like. Nano SiO2The composite fiber has the advantages of small particle size, large specific surface area, large surface polarity, easy agglomeration and insufficient fiber affinity. Through physical adsorption, nano SiO2The fabric is difficult to fix on the surface of the fabric and easy to fall off, and after mechanical abrasion and low-surface-energy substance loss, the hydrophobicity of the fabric is greatly reduced, which limits the application of fabric hydrophobicity.
Chengyang et al (printing and dyeing 2018No.18, 6-9) introduce modified nano-silica superhydrophobic finishing of cotton fabrics: tetraethyl orthosilicate (TEOS) is used as a silicon source, KH540 is used as a modifier, the cotton fabric treated by the nano silica sol is obtained, and the fabric is modified by a hydrophobic agent Polydimethylsiloxane (PDMS) to obtain the super cotton fabric. The fabric prepared by the method has single function, the price of the super-hydrophobic agent dimethyl siloxane (PDMS) is high, and the binding force of the fabric is poor. Patent CN105400239B discloses a method for preparing super-hydrophobic modified silica, silica base material powder, organosilane coupled as modifier. The super-hydrophobic silicon dioxide prepared by the method has no hydrophilic group and cannot be applied to textile finishing.
Disclosure of Invention
The invention aims to provide a preparation method of a modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric comprises the following steps:
A. preparing amino nano silicon dioxide;
B. putting the nanometer silicon dioxide precursor into a rotary evaporator, continuously reacting for 4h at 150-180 ℃ under 0.09Mpa, stopping the reaction to prepare polyamino loaded nanometer silicon dioxide powder, taking out and drying for 30min-2h in a drying oven at 100-120 ℃;
C. the amino nano silicon dioxide reacts with long-chain fatty acid in methanol solution for grafting, the mass of the silicon dioxide and the long-chain fatty acid is 10:1-20:1, the reaction temperature is 40-60 ℃, and the reaction time is 30-90min, so that amphiphilic nano silicon dioxide powder is obtained;
D. the cellulose fabric is soaked in the amphiphilic silica solution by adopting a soaking method to prepare the silica-loaded uvioresistant super-hydrophobic cellulose fabric.
Preferably, in the step A, titanium alkoxide is used as a precursor, absolute ethyl alcohol is used as a solvent, equimolar polyamino compound and double bond ester group or acid anhydride are added, the mass ratio of the monomer to the titanium alkoxide is 3:1-1:1, 3-5ml of ammonia water is continuously added, and the mixture is stirred by magnetic force at 400rpm and reacts for 4-8 hours to obtain the nano silicon dioxide precursor.
Preferably, the cellulose fabric comprises one or more of cotton fabric, linen fabric, viscose, tencel and other main components.
Preferably, the titanium alkoxide is one of n-butyl titanate, ethyl butyl titanate, methyl orthosilicate and propyl orthosilicate.
Preferably, the double-bonded ester group and the acid anhydride comprise one or more of succinic anhydride, phthalic anhydride, cyclobutyric anhydride, methyl acrylate, hexyl acrylate or methyl methacrylate, and the multi-amino monomer is one or more of polyethylene polyamine, including divinyl triamine, trivinyl tetramine or tetravinyl pentamine.
Preferably, the long chain fatty acid is: one or more of lauric acid, palmitic acid and stearic acid.
Preferably, when the preparation in the step D is carried out, the bath ratio is 1:30-1:50, the concentration of the silicon dioxide powder is 2-8g/L, the dipping temperature is 60-80 ℃, the dipping time is 40-80min, the silicon dioxide-loaded uvioresistant superhydrophobic cellulose fabric is obtained after the steps of dipping twice, rolling twice, pre-baking at 80 ℃ for 5min and baking at 120 ℃ for 3min and drying.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention has simple experimental operation, mild reaction, no fluorine and siloxane hydrophobic agent, little influence on the original performance of the fabric, low cost and easy industrial production.
(2) The silicon dioxide particles prepared by the invention are coated by amino compounds, so that the problem that nano zinc oxide is easy to agglomerate is solved.
(3) According to the invention, part of amino groups on the surface of the silicon dioxide is subjected to hydrophobic treatment by long-chain fatty acids for the first time, so that the amphiphilic nano silicon dioxide is obtained. In the process of loading cellulose fibers, the hydrophilic end is loaded on the cotton fabric, and the hydrophobic end points to air to endow the fabric with hydrophobicity.
(4) The invention adopts the hydrophobic chain segment to carry out low surface energy finishing on the fabric, can increase the combining fastness of the nano particles and the fabric, and the prepared fabric is super-hydrophobic and washable. Due to the function of amino, the cellulose fabric can be endowed with excellent ultraviolet resistance.
Drawings
FIG. 1 is a SEM image of the surface of a prepared fabric according to one embodiment of the invention;
FIG. 2 is an SEM image of the surface of a fabric prepared according to a second embodiment of the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
the invention provides a technical scheme that: the preparation method of the modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric comprises a cellulose fabric matrix, wherein the cellulose fabric matrix is internally provided with dispersed modified nano-silica particles, and the size of nano-zinc oxide powder is 50-400 nm.
In this embodiment, the preparation method of the modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric comprises the following steps:
A. fully stirring and mixing 45g of absolute ethyl alcohol and 1.5g of TEOS, respectively adding 0.01mol of diethylenetriamine and methyl acrylate, dropwise adding ammonia water, and reacting for 4 hours under magnetic stirring at 400rpm to obtain a nano silicon dioxide precursor;
B. putting the nano silicon dioxide precursor into a rotary evaporator, continuously reacting for 4 hours at 160 ℃ under reduced pressure of 0.09Mpa, stopping the reaction to prepare polyamino loaded nano silicon dioxide powder, taking out the powder and drying the powder in an oven at 120 ℃ for 30 min;
C. dissolving 1.5g of silicon dioxide powder and 0.15g of lauric acid in 20ml of methanol solution, reacting at 40 ℃ for 30min, and evaporating out the solvent methanol by a rotary evaporator to obtain amphiphilic nano silicon dioxide powder;
D. putting 2g of cotton fabric into 100ml of solution, adding 0.2g of silicon dioxide powder to ensure that the concentration is 2g/L, the impregnation temperature is 60 ℃, the impregnation time is 40min, pre-drying for 5min at 80 ℃ and baking for 3min at 120 ℃ to obtain silicon dioxide loaded uvioresistant super-hydrophobic cellulose fabric through two-time soaking and two-time rolling with the rolling residue rate between 60 and 70 percent;
the properties were tested as shown in table 1 and figure 1: compared with the common fabric, the modified nano-silica loaded fabric obviously improves the super-hydrophobic and ultraviolet-resistant performances of the fiber, and the prepared fiber has better fastness.
TABLE 1 contact Angle and UPF value of the fabrics before and after finishing
Example two:
the preparation method of the modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric comprises a cellulose matrix, wherein modified nano-silica particles are dispersed in the cellulose matrix. The size of the nano zinc oxide powder is 50-400 nm.
In this embodiment, the preparation method of the modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric comprises the following steps:
A. fully stirring and mixing 45g of absolute ethyl alcohol and 2g of tetraethoxysilane, respectively adding 0.01mol of tetraethylenepentamine and methyl acrylate, dropwise adding ammonia water, and reacting for 4 hours under magnetic stirring at 400rpm to obtain a nano silicon dioxide precursor;
B. putting the nano silicon dioxide precursor into a rotary evaporator, continuously reacting for 4 hours at 160 ℃ under reduced pressure of 0.09Mpa, stopping the reaction to prepare polyamino loaded nano silicon dioxide powder, taking out the powder and drying the powder in an oven at 120 ℃ for 30 min;
C. dissolving 1g of silicon dioxide powder and 0.1g of stearic acid in 20ml of methanol solution, reacting at the temperature of 60 ℃ for 30min, and evaporating the solvent methanol by a rotary evaporator to obtain amphiphilic nano silicon dioxide powder;
D. putting 2g of viscose fabric into 100ml of solution, adding 0.2g of silicon dioxide powder to ensure that the concentration is 2g/L, the dipping temperature is 60 ℃, the dipping time is 40min, carrying out two-dipping and two-rolling with the rolling residue rate of 60-70 percent, pre-drying at 80 ℃ for 5min, and baking at 120 ℃ for 3min to obtain the silicon dioxide loaded uvioresistant super-hydrophobic cellulose fabric.
The performance of the test is shown in table 2 and fig. 2: compared with the common fabric, the modified nano-silica loaded fabric obviously improves the super-hydrophobic and ultraviolet-resistant performances of the fiber, and the prepared fiber has better fastness.
TABLE 2 contact Angle and UPF value of the fabric before and after finishing
In conclusion, the beneficial effects of the invention are as follows:
the invention has simple experimental operation, mild reaction, no fluorine and siloxane hydrophobic agent, little influence on the original performance of the fabric, low cost and easy industrial production; the silicon dioxide particles prepared by the invention are coated by amino compounds, so that the problem that nano zinc oxide is easy to agglomerate is solved; according to the invention, part of amino groups on the surface of the silicon dioxide is subjected to hydrophobic treatment by long-chain fatty acids for the first time, so that the amphiphilic nano silicon dioxide is obtained. In the process of loading cellulose fibers, the hydrophilic end is loaded on the cotton fabric, and the hydrophobic end points to the air to endow the fabric with hydrophobicity; the invention adopts the hydrophobic chain segment to carry out low surface energy finishing on the fabric, can increase the combining fastness of the nano particles and the fabric, and the prepared fabric is super-hydrophobic and washable. Due to the function of amino, the cellulose fabric can be endowed with excellent ultraviolet resistance.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A preparation method of a modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric is provided, the ultraviolet-proof super-hydrophobic cellulose fabric fiber comprises a cellulose fabric matrix, and modified nano-silica particles are dispersed in the cellulose fabric matrix, and the preparation method is characterized by comprising the following steps:
A. preparing amino nano silicon dioxide;
B. putting the nanometer silicon dioxide precursor into a rotary evaporator, continuously reacting for 4h at 150-180 ℃ under 0.09Mpa, stopping the reaction to prepare polyamino loaded nanometer silicon dioxide powder, taking out and drying for 30min-2h in a drying oven at 100-120 ℃;
C. the amino nano silicon dioxide reacts with long-chain fatty acid in methanol solution for grafting, the mass of the silicon dioxide and the long-chain fatty acid is 10:1-20:1, the reaction temperature is 40-60 ℃, and the reaction time is 30-90min, so that amphiphilic nano silicon dioxide powder is obtained;
D. the cellulose fabric is soaked in the amphiphilic silica solution by adopting a soaking method to prepare the silica-loaded uvioresistant super-hydrophobic cellulose fabric.
2. The preparation method of the modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric according to claim 1, characterized in that: and in the step A, adding equimolar polyamino compound and double bond ester group or acid anhydride by taking titanium alkoxide as a precursor and absolute ethyl alcohol as a solvent, wherein the mass ratio of the monomer to the titanium alkoxide is 3:1-1:1, continuously adding 3-5ml of ammonia water, and reacting for 4-8 hours under magnetic stirring at 400rpm to obtain the nano silicon dioxide precursor.
3. The preparation method of the modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric according to claim 1, characterized in that: the cellulose fabric comprises one or more of cotton fabric, linen fabric, viscose, tencel and the like as main components.
4. The preparation method of the modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric according to claim 1, characterized in that: the titanium alkoxide is one of tetrabutyl titanate, methyl orthosilicate and propyl orthosilicate.
5. The preparation method of the modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric according to claim 1, characterized in that: preferably, the double-bond ester group and the anhydride comprise one or more of succinic anhydride, phthalic anhydride, cyclobutyric anhydride, methyl acrylate, hexyl acrylate or methyl methacrylate, and the multi-amino monomer is one or more of polyethylene polyamine, including divinyl triamine, triethylene tetramine or tetraethylene pentamine.
6. The preparation method of the modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric according to claim 1, characterized in that: the long-chain fatty acid is: one or more of lauric acid, palmitic acid and stearic acid.
7. The preparation method of the modified nano-silica ultraviolet-proof super-hydrophobic cellulose fabric according to claim 1, characterized in that: and D, when the preparation in the step D is carried out, the bath ratio is 1:30-1:50, the concentration of silicon dioxide powder is 2-8g/L, the dipping temperature is 60-80 ℃, the dipping time is 40-80min, the silicon dioxide-loaded uvioresistant superhydrophobic cellulose fabric is obtained after the steps of two dipping and two rolling, pre-baking at 80 ℃ for 5min and baking at 120 ℃ for 3min and drying.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113308872A (en) * | 2021-06-07 | 2021-08-27 | 苏州大学 | Functional textile material, preparation method thereof and application thereof in environmental water replenishing or evaporation prevention |
| CN114394601A (en) * | 2021-12-09 | 2022-04-26 | 盐城工学院 | Preparation method and application of silica with raspberry structure |
| CN115109550A (en) * | 2022-08-29 | 2022-09-27 | 中国林业科学研究院木材工业研究所 | Antibacterial and antiviral polymer resin composition and adhesive film paper using same |
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| EP3380078A1 (en) * | 2015-11-23 | 2018-10-03 | Association for the Advancement of Tissue Engineering and Cell based Technologies & Therapies (A4TEC) - Associação | Composition comprising polyeletrolyte complexes, methods and uses thereof |
| CN110747534A (en) * | 2019-11-18 | 2020-02-04 | 东北师范大学 | Antibacterial polysaccharide fiber material and preparation method thereof |
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| CN102345229B (en) * | 2011-08-10 | 2013-04-03 | 东华大学 | Arranging method of nanometer magnesium oxide anti-ultraviolet hydrophobic cellulose fabric |
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Patent Citations (3)
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| JP2002339155A (en) * | 2001-05-18 | 2002-11-27 | Ueda Seni Kagaku Shinkokai | Method for polyamino acid conjugate fiber production by aqueous solution interfacial spinning process and apparatus for continuous spinning |
| EP3380078A1 (en) * | 2015-11-23 | 2018-10-03 | Association for the Advancement of Tissue Engineering and Cell based Technologies & Therapies (A4TEC) - Associação | Composition comprising polyeletrolyte complexes, methods and uses thereof |
| CN110747534A (en) * | 2019-11-18 | 2020-02-04 | 东北师范大学 | Antibacterial polysaccharide fiber material and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113308872A (en) * | 2021-06-07 | 2021-08-27 | 苏州大学 | Functional textile material, preparation method thereof and application thereof in environmental water replenishing or evaporation prevention |
| CN114394601A (en) * | 2021-12-09 | 2022-04-26 | 盐城工学院 | Preparation method and application of silica with raspberry structure |
| CN115109550A (en) * | 2022-08-29 | 2022-09-27 | 中国林业科学研究院木材工业研究所 | Antibacterial and antiviral polymer resin composition and adhesive film paper using same |
| CN115109550B (en) * | 2022-08-29 | 2022-10-28 | 中国林业科学研究院木材工业研究所 | Antibacterial and antiviral polymer resin composition and adhesive film paper using same |
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