CN113638240A - Method for implanting nano-silver into fabric - Google Patents
Method for implanting nano-silver into fabric Download PDFInfo
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- CN113638240A CN113638240A CN202110810603.8A CN202110810603A CN113638240A CN 113638240 A CN113638240 A CN 113638240A CN 202110810603 A CN202110810603 A CN 202110810603A CN 113638240 A CN113638240 A CN 113638240A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/128—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with silicon polymers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0061—Organic fillers or organic fibrous fillers, e.g. ground leather waste, wood bark, cork powder, vegetable flour; Other organic compounding ingredients; Post-treatment with organic compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2209/00—Properties of the materials
- D06N2209/04—Properties of the materials having electrical or magnetic properties
- D06N2209/041—Conductive
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Abstract
The invention relates to the technical field of fabric manufacturing, in particular to a method for implanting nano-silver into a fabric. The method comprises the following steps: (1) solution preparation, (2) colloid preparation, (3) catalyst forming, (4) carbon nano tube in-situ loading, (5) nano silver replacement, and (6) nano silver implanted fabric. The invention reasonably prepares the catalyst with higher activity by using ferric nitrate, aluminum nitrate and nickel nitrate, provides a solid reaction foundation for the in-situ synthesis of the carbon nano tube, so that the prepared carbon nano tube has better coating property on silver, and has obvious effect on improving the conductivity and stability of the fabric.
Description
Technical Field
The invention relates to the technical field of fabric manufacturing, in particular to a method for implanting nano-silver into a fabric.
Background
For improving the conductivity of the fabric, the current common methods include a dipping method, a padding method, a printing method, a coating method and the like. Although the printing method can meet the requirements of the circuit pattern, the addition of the adhesive in the printed conductive paste greatly reduces the conductivity of the fabric, and the problem of rapid conductivity loss caused by high-strength use cannot be overcome, so that the doping of a conductive substance and the design of a base material are the fundamental method for solving the conductivity of the fabric, and accordingly, a method for designing the nano silver implanted fabric by using the high-conductivity silver is necessary.
Disclosure of Invention
Based on the problems, the invention provides a method for implanting nano-silver into a fabric, which is used for improving the conductivity of the fabric and avoiding the too fast conductivity loss of the fabric in long-term use. The specific technical scheme is as follows:
a method for implanting nano-silver into a fabric comprises the following steps:
(1) solution preparation
Mixing ferric nitrate, aluminum nitrate and nickel nitrate with water, heating to boil, stirring at a speed of 20-30r/min for 10-15min, cooling to room temperature, placing the solution in a freezing chamber for 10-20h, taking out the frozen matter, and processing into ice particles at 3-5 ℃ by an ice crusher;
(2) colloid preparation
Preparing a potassium hydroxide solution at the temperature of 3-5 ℃, placing the solution in an ultrasonic environment, adding sodium chloride ice beads, shaking for 20-30s, and adding the ice particles prepared in the previous step for 3-8 times, wherein the adding amount of each time is 8-10% of the mass of the potassium hydroxide solution; after the ice particles are added, raising the temperature to 20-50 ℃, and continuing to use ultrasonic waves for 10-15 min; filtering the mixed solution, and washing the obtained precipitate with 13-15% ethanol solution for 3-5 times;
(3) catalyst formation
Placing the substance obtained in the last step into a roasting dish, pumping the air pressure to 0.1-0.3 standard atmospheric pressure, heating to 50-60 ℃, and introducing nitrogen to increase the air pressure to 1-1.5 standard atmospheric pressure; pumping the air pressure to 0.03-0.05 standard atmospheric pressure, raising the temperature to 300-400 ℃, and roasting for 6-8 h; raising the temperature to 500-550 ℃, introducing hydrogen, and reacting for 3-5h to obtain the catalyst;
the flow rate of the hydrogen is 120-150 ml/min;
(4) in-situ loading of carbon nanotubes
Putting the catalyst into a porcelain ark to be uniformly spread, putting the porcelain ark into a constant-temperature area of a tubular furnace, heating the porcelain ark to 200-fold-with-air temperature of 300 ℃ under the protection of nitrogen, introducing hydrogen at 220ml/min of 200-fold-with-air temperature, reacting for 1-2h, stopping the reaction of the hydrogen, heating the porcelain ark to 600-fold-with-air temperature of 650 ℃, introducing nitrogen and methane, reacting for 3-4h, and stopping the injection of methane; introducing nitrogen, and cooling to normal temperature to obtain carbon nanotube loaded metal particles;
the flow rate of the nitrogen is 300-350ml/min, and the flow rate of the methane is 80-90 ml/min;
(5) nano silver substitution
Preparing 1-2mol/L silver nitrate solution, reducing the temperature of the solution to 10-20 ℃, adding sodium dodecyl benzene sulfonate, stirring for 2-3min, adding the carbon nano tube loaded metal particles prepared in the previous step under the ultrasonic oscillation with the power of 200-300W, stirring for 40-50min, filtering, washing the obtained precipitate with pure water for 3-5 times, and drying at the temperature of 180-200 ℃;
the dosage of the sodium dodecyl benzene sulfonate is 0.8 to 1 percent of the mass of the silver nitrate solution; the mass ratio of the carbon nano tube loaded metal particles to the silver nitrate solution is 1: 80-90;
(6) nano-silver implant fabric
And mixing the product obtained in the last step with liquid organic silicon resin according to the mass ratio of 1:120-138, coating the mixture on the surface of the fabric, and drying to obtain the fabric.
Further, in the step (1), the mass ratio of the ferric nitrate to the aluminum nitrate to the nickel nitrate is 1:18-23: 3-8.
Further, in the step (1), the temperature of the freezing chamber is minus 20-30 ℃.
Further, in the step (1), the fineness of the ice particles is 0.5-1 mm.
Further, in the step (2), the concentration of the potassium hydroxide solution is 0.1-0.3 mol/L.
Further, in the step (2), the power of the ultrasonic wave is 800-.
Further, in the step (2), the preparation method of the sodium chloride iceball comprises the following steps: preparing saturated solution of sodium chloride at 20-25 deg.C, pouring the solution into a mold, and freezing and molding at-40 deg.C to-50 deg.C.
Further, in the step (2), the sodium chloride iceball is in an ellipsoid shape.
Further, in the step (2), the long diameter of the sodium chloride iceball is 3-5 mm.
Further, in the step (2), the amount of the sodium chloride iceballs is 15-20% of the mass of the potassium hydroxide solution.
Compared with the prior art, the invention has the beneficial effects that:
the invention reasonably prepares the catalyst with higher activity by using ferric nitrate, aluminum nitrate and nickel nitrate, provides a solid reaction foundation for the in-situ synthesis of the carbon nano tube, so that the prepared carbon nano tube has better coating property on silver, and has obvious effect on improving the conductivity and stability of the fabric.
According to the invention, sodium chloride iceballs are used in the preparation of the catalyst, and the heat generated by the reaction is absorbed through the heat absorption effect of the iceballs, so that the reaction rate is reduced. Meanwhile, by introducing sodium chloride, the ion complexity in a reaction system is increased, the contact probability of reactive ions is reduced, and the reaction is further controlled, so that the reactive ions can continuously react in the whole precipitation reaction, the copolymerization of precipitates is reduced, the metal ions are coated when the carbon nano tube is synthesized in situ, the efficiency of subsequent silver displacement reaction is obviously improved, and the conductive effect of the fabric is further improved.
According to the invention, sodium dodecyl benzene sulfonate is added during silver replacement reaction of metal in the carbon nano tube, so that the surface activity of the solution is improved, the deposition rate of particles in a reaction system is reduced, and high-efficiency mixing can be performed, but ions in the reaction system are increased, the progress of the replacement reaction is slowed down, so that the replacement of silver ions can be efficiently completed by metal particles coated by the carbon nano tube, and the copolymerization is reduced, so that the silver ions are uniformly distributed in the fabric under the protection of the carbon nano tube, and a remarkable effect is brought to long-acting stability improvement.
Detailed Description
Example 1
A method for implanting nano-silver into a fabric comprises the following steps:
(1) solution preparation
Mixing ferric nitrate, aluminum nitrate and nickel nitrate with water, heating to boil, stirring at a speed of 20r/min for 10min, reducing the temperature to room temperature, placing the solution in a freezing chamber for 10h, taking out the frozen matter, and processing into ice particles by an ice crusher at the temperature of 3 ℃;
the mass ratio of the ferric nitrate to the aluminum nitrate to the nickel nitrate is 1:18: 3; the temperature of the freezing chamber is minus 20 ℃; the fineness of the ice particles is 0.5 mm;
(2) colloid preparation
Preparing a potassium hydroxide solution at the temperature of 3 ℃, placing the solution in an ultrasonic environment, adding sodium chloride ice beads, shaking for 20s, adding the ice particles prepared in the previous step for 3 times, wherein the adding amount of each time is 8 percent of the mass of the potassium hydroxide solution; after the ice particles are added, raising the temperature to 20 ℃, and continuing to use ultrasonic waves for 10 min; filtering the mixed solution, and washing the obtained precipitate with 13% ethanol solution for 3 times;
the concentration of the potassium hydroxide solution is 0.1 mol/L; the power of the ultrasonic wave is 800W; the preparation method of the sodium chloride iceball comprises the following steps: preparing saturated solution of sodium chloride at 20 ℃, pouring the solution into a mould, and freezing and molding at-40 ℃; the sodium chloride ice beads are in an ellipsoid shape; the long diameter of the sodium chloride ice beads is 3 mm; the amount of the sodium chloride iceballs is 15 percent of the mass of the potassium hydroxide solution;
(3) catalyst formation
Placing the substance prepared in the last step into a roasting dish, pumping the air pressure to 0.1 standard atmospheric pressure, heating to 50 ℃, and introducing nitrogen to increase the air pressure to 1 standard atmospheric pressure; pumping the air pressure to 0.03 standard atmospheric pressure, raising the temperature to 300 ℃, and roasting for 6 hours; raising the temperature to 500 ℃, introducing hydrogen, and reacting for 3 hours to obtain the catalyst;
the flow rate of the hydrogen is 120 ml/min;
(4) in-situ loading of carbon nanotubes
Putting the catalyst into a porcelain ark, uniformly spreading the porcelain ark, putting the porcelain ark into a constant-temperature area of a tube furnace, heating the porcelain ark to 200 ℃ under the protection of nitrogen, introducing hydrogen at a rate of 200ml/min, reacting for 1h, stopping the hydrogen, heating the porcelain ark to 600 ℃, introducing nitrogen and methane, reacting for 3h, and stopping the injection of methane; introducing nitrogen, and cooling to normal temperature to obtain carbon nanotube loaded metal particles;
the flow rate of the nitrogen is 300ml/min, and the flow rate of the methane is 80 ml/min;
(5) nano silver substitution
Preparing 1mol/L silver nitrate solution, reducing the temperature of the solution to 10 ℃, adding sodium dodecyl benzene sulfonate, stirring for 2min, adding the carbon nano tube loaded metal particles prepared in the previous step under the ultrasonic oscillation with the power of 200W, stirring for 40min, filtering, washing the obtained precipitate with pure water for 3 times, and drying at 180 ℃;
the amount of the sodium dodecyl benzene sulfonate is 0.8 percent of the mass of the silver nitrate solution; the mass ratio of the carbon nano tube loaded metal particles to the silver nitrate solution is 1: 80;
(6) nano-silver implant fabric
And (3) mixing the product obtained in the last step with liquid organic silicon resin according to the mass ratio of 1:120, coating the mixture on the surface of the fabric, and drying to obtain the fabric.
Example 2
A method for implanting nano-silver into a fabric comprises the following steps:
(1) solution preparation
Mixing ferric nitrate, aluminum nitrate and nickel nitrate with water, heating to boil, stirring at the speed of 30r/min for 15min, reducing the temperature to room temperature, placing the solution in a freezing chamber for storage for 20h, taking out the frozen matter, and processing into ice particles by an ice crusher at the temperature of 5 ℃;
the mass ratio of the ferric nitrate to the aluminum nitrate to the nickel nitrate is 1:23: 8; the temperature of the freezing chamber is minus 30 ℃; the fineness of the ice particles is 1 mm;
(2) colloid preparation
Preparing a potassium hydroxide solution at 5 ℃, placing the solution in an ultrasonic environment, adding sodium chloride ice beads, shaking for 30s, and adding the ice particles prepared in the previous step for 8 times, wherein the adding amount of each time is 10% of the mass of the potassium hydroxide solution; after the ice particles are added, raising the temperature to 50 ℃, and continuing to use ultrasonic waves for 15 min; filtering the mixed solution, and washing the obtained precipitate with 15% ethanol solution for 5 times;
the concentration of the potassium hydroxide solution is 0.3 mol/L; the power of the ultrasonic wave is 900W; the preparation method of the sodium chloride iceball comprises the following steps: preparing saturated solution of sodium chloride at 25 ℃, pouring the solution into a mould, and freezing and molding at-50 ℃; the sodium chloride ice beads are in an ellipsoid shape; the long diameter of the sodium chloride ice beads is 5 mm; the amount of the sodium chloride iceballs is 20 percent of the mass of the potassium hydroxide solution;
(3) catalyst formation
Placing the substance prepared in the last step into a roasting dish, pumping the air pressure to 0.3 standard atmospheric pressure, heating to 60 ℃, and introducing nitrogen to increase the air pressure to 1.5 standard atmospheric pressure; pumping the air pressure to 0.05 standard atmospheric pressure, raising the temperature to 400 ℃, and roasting for 8 hours; raising the temperature to 550 ℃, introducing hydrogen, and reacting for 5 hours to obtain the catalyst;
the flow rate of the hydrogen is 150 ml/min;
(4) in-situ loading of carbon nanotubes
Putting the catalyst into a porcelain ark, uniformly spreading the porcelain ark, putting the porcelain ark into a constant-temperature area of a tube furnace, heating the porcelain ark to 300 ℃ under the protection of nitrogen, introducing hydrogen at a rate of 220ml/min, reacting for 2 hours, stopping the hydrogen, heating the porcelain ark to 650 ℃, introducing nitrogen and methane, reacting for 4 hours, and stopping the injection of methane; introducing nitrogen, and cooling to normal temperature to obtain carbon nanotube loaded metal particles;
the flow rate of the nitrogen is 350ml/min, and the flow rate of the methane is 90 ml/min;
(5) nano silver substitution
Preparing 2mol/L silver nitrate solution, reducing the temperature of the solution to 20 ℃, adding sodium dodecyl benzene sulfonate, stirring for 3min, adding the carbon nano tube loaded metal particles prepared in the last step under the ultrasonic oscillation with the power of 300W, stirring for 50min, filtering, washing the obtained precipitate with pure water for 5 times, and drying at 200 ℃;
the amount of the sodium dodecyl benzene sulfonate is 1 percent of the mass of the silver nitrate solution; the mass ratio of the carbon nano tube loaded metal particles to the silver nitrate solution is 1: 90;
(6) nano-silver implant fabric
And (3) mixing the product obtained in the last step with liquid organic silicon resin according to the mass ratio of 1:138, coating the mixture on the surface of the fabric, and drying to obtain the fabric.
Example 3
A method for implanting nano-silver into a fabric comprises the following steps:
(1) solution preparation
Mixing ferric nitrate, aluminum nitrate and nickel nitrate with water, heating to boil, stirring at 25r/min for 13min, cooling to room temperature, storing the solution in a freezing chamber for 16h, taking out the frozen matter, and processing into ice particles at 5 ℃ by an ice crusher;
the mass ratio of the ferric nitrate to the aluminum nitrate to the nickel nitrate is 1:18: 8; the temperature of the freezing chamber is minus 30 ℃; the fineness of the ice particles is 0.5 mm;
(2) colloid preparation
Preparing a potassium hydroxide solution at 5 ℃, placing the solution in an ultrasonic environment, adding sodium chloride ice beads, shaking for 20s, and adding the ice particles prepared in the previous step for 8 times, wherein the adding amount of each time is 10% of the mass of the potassium hydroxide solution; after the ice particles are added, raising the temperature to 20 ℃, and continuing to use ultrasonic waves for 10 min; filtering the mixed solution, and washing the obtained precipitate with 15% ethanol solution for 5 times;
the concentration of the potassium hydroxide solution is 0.3 mol/L; the power of the ultrasonic wave is 800W; the preparation method of the sodium chloride iceball comprises the following steps: preparing saturated solution of sodium chloride at 25 ℃, pouring the solution into a mould, and freezing and molding at-40 ℃; the sodium chloride ice beads are in an ellipsoid shape; the long diameter of the sodium chloride ice beads is 5 mm; the amount of the sodium chloride iceballs is 15 percent of the mass of the potassium hydroxide solution;
(3) catalyst formation
Placing the substance prepared in the last step into a roasting dish, pumping the air pressure to 0.3 standard atmospheric pressure, heating to 50 ℃, and introducing nitrogen to increase the air pressure to 1.5 standard atmospheric pressure; pumping the air pressure to 0.03 standard atmospheric pressure, raising the temperature to 400 ℃, and roasting for 6 hours; raising the temperature to 550 ℃, introducing hydrogen, and reacting for 5 hours to obtain the catalyst;
the flow rate of the hydrogen is 120 ml/min;
(4) in-situ loading of carbon nanotubes
Putting the catalyst into a porcelain ark, uniformly spreading the porcelain ark, putting the porcelain ark into a constant-temperature area of a tube furnace, heating the porcelain ark to 300 ℃ under the protection of nitrogen, introducing hydrogen at a rate of 220ml/min, reacting for 1h, stopping the hydrogen, heating the porcelain ark to 650 ℃, introducing nitrogen and methane, reacting for 4h, and stopping the injection of methane; introducing nitrogen, and cooling to normal temperature to obtain carbon nanotube loaded metal particles;
the flow rate of the nitrogen is 350ml/min, and the flow rate of the methane is 80 ml/min;
(5) nano silver substitution
Preparing 2mol/L silver nitrate solution, reducing the temperature of the solution to 10 ℃, adding sodium dodecyl benzene sulfonate, stirring for 3min, adding the carbon nano tube loaded metal particles prepared in the previous step under the ultrasonic oscillation with the power of 200W, stirring for 50min, filtering, washing the obtained precipitate for 3 times by pure water, and drying at 200 ℃;
the amount of the sodium dodecyl benzene sulfonate is 1 percent of the mass of the silver nitrate solution; the mass ratio of the carbon nano tube loaded metal particles to the silver nitrate solution is 1: 80;
(6) nano-silver implant fabric
And (3) mixing the product obtained in the last step with liquid organic silicon resin according to the mass ratio of 1:138, coating the mixture on the surface of the fabric, and drying to obtain the fabric.
To verify the inventive scheme, the following comparative examples were set up:
test examples
Fabrics were produced according to examples 1 to 3 and comparative examples 1 to 3, respectively, using pure cotton fabrics, and the resistivity of each fabric was measured by washing the fabric 10 times, 50 times, and 150 times in clean water. The test results are shown in table 1.
| Resistivity of 10 times omega/cm | Resistivity of 50 times omega/cm | Resistivity of 150 times omega/cm | |
| Example 1 | 35.33 | 36.78 | 38.49 |
| Example 2 | 36.05 | 36.99 | 39.87 |
| Example 3 | 35.81 | 37.41 | 39.03 |
| Comparative example 1 | 55.36 | 68.83 | 86.50 |
| Comparative example 2 | 58.36％ | 72.60 | 91.66 |
| Comparative example 3 | 63.94％ | 75.29 | 98.85 |
As can be seen from the table, examples 1 to 3 using the method of implanting nano-silver into a fabric according to the present invention have good conductive effects, and the conductive ability is still good after a plurality of times of cleaning. Obviously, the scheme of the invention has obvious effect of improving the conductivity of the fabric and extremely high stability.
Claims (10)
1. A method for implanting nano-silver into a fabric is characterized by comprising the following steps:
(1) solution preparation
Mixing ferric nitrate, aluminum nitrate and nickel nitrate with water, heating to boil, stirring at a speed of 20-30r/min for 10-15min, cooling to room temperature, placing the solution in a freezing chamber for 10-20h, taking out the frozen matter, and processing into ice particles at 3-5 ℃ by an ice crusher;
(2) colloid preparation
Preparing a potassium hydroxide solution at the temperature of 3-5 ℃, placing the solution in an ultrasonic environment, adding sodium chloride ice beads, shaking for 20-30s, and adding the ice particles prepared in the previous step for 3-8 times, wherein the adding amount of each time is 8-10% of the mass of the potassium hydroxide solution; after the ice particles are added, raising the temperature to 20-50 ℃, and continuing to use ultrasonic waves for 10-15 min; filtering the mixed solution, and washing the obtained precipitate with 13-15% ethanol solution for 3-5 times;
(3) catalyst formation
Placing the substance obtained in the last step into a roasting dish, pumping the air pressure to 0.1-0.3 standard atmospheric pressure, heating to 50-60 ℃, and introducing nitrogen to increase the air pressure to 1-1.5 standard atmospheric pressure; pumping the air pressure to 0.03-0.05 standard atmospheric pressure, raising the temperature to 300-400 ℃, and roasting for 6-8 h; raising the temperature to 500-550 ℃, introducing hydrogen, and reacting for 3-5h to obtain the catalyst;
the flow rate of the hydrogen is 120-150 ml/min;
(4) in-situ loading of carbon nanotubes
Putting the catalyst into a porcelain ark to be uniformly spread, putting the porcelain ark into a constant-temperature area of a tubular furnace, heating the porcelain ark to 200-fold-with-air temperature of 300 ℃ under the protection of nitrogen, introducing hydrogen at 220ml/min of 200-fold-with-air temperature, reacting for 1-2h, stopping the reaction of the hydrogen, heating the porcelain ark to 600-fold-with-air temperature of 650 ℃, introducing nitrogen and methane, reacting for 3-4h, and stopping the injection of methane; introducing nitrogen, and cooling to normal temperature to obtain carbon nanotube loaded metal particles;
the flow rate of the nitrogen is 300-350ml/min, and the flow rate of the methane is 80-90 ml/min;
(5) nano silver substitution
Preparing 1-2mol/L silver nitrate solution, reducing the temperature of the solution to 10-20 ℃, adding sodium dodecyl benzene sulfonate, stirring for 2-3min, adding the carbon nano tube loaded metal particles prepared in the previous step under the ultrasonic oscillation with the power of 200-300W, stirring for 40-50min, filtering, washing the obtained precipitate with pure water for 3-5 times, and drying at the temperature of 180-200 ℃;
the dosage of the sodium dodecyl benzene sulfonate is 0.8 to 1 percent of the mass of the silver nitrate solution; the mass ratio of the carbon nano tube loaded metal particles to the silver nitrate solution is 1: 80-90;
(6) nano-silver implant fabric
And mixing the product obtained in the last step with liquid organic silicon resin according to the mass ratio of 1:120-138, coating the mixture on the surface of the fabric, and drying to obtain the fabric.
2. The method for implanting nano-silver into a fabric according to claim 1, wherein in the step (1), the mass ratio of the ferric nitrate to the aluminum nitrate to the nickel nitrate is 1:18-23: 3-8.
3. The method for implanting nano-silver into fabric according to claim 1, wherein the temperature of the freezing chamber is-20-30 ℃ below zero in the step (1).
4. The method for implanting nano-silver into a fabric according to claim 1, wherein in the step (1), the fineness of the ice particles is 0.5 to 1 mm.
5. The method for implanting nano-silver into a fabric according to claim 1, wherein the concentration of the potassium hydroxide solution in the step (2) is 0.1 to 0.3 mol/L.
6. The method for implanting nano-silver into fabric according to claim 1, wherein in the step (2), the power of the ultrasonic wave is 800-.
7. The method for implanting nano-silver into the fabric according to claim 1, wherein in the step (2), the sodium chloride iceballs are prepared by the following steps: preparing saturated solution of sodium chloride at 20-25 deg.C, pouring the solution into a mold, and freezing and molding at-40 deg.C to-50 deg.C.
8. The method for implanting nano-silver into a fabric according to claim 1, wherein in the step (2), the sodium chloride iceballs are in an ellipsoidal shape.
9. The method for implanting nano-silver into a fabric according to claim 1, wherein in the step (2), the long diameter of the sodium chloride iceballs is 3-5 mm.
10. The method for implanting nano-silver into a fabric according to claim 1, wherein in the step (2), the sodium chloride iceballs are used in an amount of 15-20% by mass of the potassium hydroxide solution.
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| CN108147391A (en) * | 2017-12-28 | 2018-06-12 | 深圳市百柔新材料技术有限公司 | The preparation method of carrying nano silver carbon nanotube |
| CN108018014A (en) * | 2018-01-12 | 2018-05-11 | 深圳名飞远科技有限公司 | A kind of preparation method of novel nano silver conductive adhesive |
| CN111554942A (en) * | 2020-05-07 | 2020-08-18 | 上海理工大学 | Silver-loaded cellulose/carbon nanotube composite material and preparation method and application thereof |
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