Patent
US 10,625,214TITANIUM DIOXIDE/SULFONATED GRAPHENE OXIDE/AG NANOPARTICLE COMPOSITE MEMBRANE AND PREPARATION AND APPLICATION THEREOF
Jianmei LU
US
Copyright © 2026 Matter42. All rights reserved.
Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows scanning electron microscopy (SEM) picture of silver nanoparticles and sulfonated graphene oxide composites;
Figure 2 shows scanning electron microscopy (SE M) picture of titanium dioxide nan oro ds arrays;
Figure 3 sh ow s the cr o ss sectional SEM figure of the TSA membrane;
Figure 4 shows the wettability of TSA membrane;
Figure 5 shows the separation step of oil-water emulsion;
Figure 6 sh ow s the separati o n efficiency of TSA membrane;
Figure 7 shows the degradation of the TSA membrane.
Figure 8 shows the measurement o f the separation efficiency o f the same T SA film after 10 cycles of separation.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane, comprising the following steps: (1) mixing graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide uniformly in the water, and then adding concentrated nitric acid to obtain sulfonated graphene oxide; (2) mixing the aqueous solution of said sulfonated graphene oxide with the aqueous solution of silver nitrate, stirring in the dark, then adding ascorbic acid, and continuing to stir to obtain a silver nanoparticle/sulfonated graphene oxide composite material; (3) preparing titanium dioxide nanoclusters on a metal mesh by using tetra-n-butyl titanate, glycerol, and ethanol as raw materials to obtain a metal mesh with titanium dioxide nanoclusters; then the metal mesh with titanium dioxide nanoclusters is put in a mixed solution of titanium trichloride, saturated aqueous solution of sodium chloride and urea, said metal mesh is removed after the reaction to obtain titanium dioxide nanorod arrays; (4) dispersing said silver nanoparticle/sulfonated graphene oxide composite material in water, and then deposited on said titanium dioxide nanorods arrays by vacuum deposition, and vacuum dried to obtain titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane.
The preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1, wherein in step (1), the mass ratio of graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide is 0.2: 3: 1.6; after mixing said graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide uniformly in water, ultrasonic stirring for 3 hours at room temperature, and then adding concentrated nitric acid; after the reaction is completed, the product is centrifuged, washed and dried to obtain sulfonated graphene oxide.
The preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1, wherein in step (2), the mass ratio of sulfonated graphene oxide, silver nitrate and ascorbic acid is 1: 6.8: 8.8; said stirring is carried out in the dark for 3 hours at 25 0 C; the time of continued stirring is 1 hour.
The preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1, wherein in step (3), the volume ratio of tetra-n-butyl titanate, glycerin, and ethanol is 1: 5: 15; the temperature of the preparation of titanium dioxide nanoclusters on the metal mesh is 180 0 C, the time is 24 hours; the mass ratio of urea, titanium trichloride, sodium chloride is 1: 2: 36.6; the temperature of the reaction is 160 0 C, and the time is 2 hours.
A titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane prepared by the preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1.
A preparation method of a silver nanoparticle/sulfonated graphene oxide composite material, comprising the following steps: (1) mixing graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide uniformly in the water, and then adding concentrated nitric acid to obtain sulfonated graphene oxide; (2) mixing the aqueous solution of said sulfonated graphene oxide with the aqueous solution of silver nitrate, stirri ng in the dark, then adding ascorbic acid, and continuing to stir to obtain a silver nanoparticle/sulfonated graphene oxide composite material.
The preparation method of a silver nanoparticle/sulfonated graphene oxide composite material according to claim 5, wherein in step (1), the mass ratio of graphene oxide, sodium ch l oroethanesulfonate, and sodium hydroxide is 0.2: 3: 1.6; after mixing said graphene oxide, sodium ch l oroethanesulfonate, and sodium hydroxide uniformly in water, ultrasonic stirring for 3 hours at room temperature, and then adding concentrated nitric acid; after the reaction is completed, the product is centrifuged, washed and dried to obtain sulfonated graphene oxide; in step (2), the mass ratio of sulfonated graphene oxide, silver nitrate and ascorbic acid is 1: 6.8: 8.8; said stirring is carried out in the dark for 3 hours at 25 0 C; the time of continued stirring is I hour.
A preparation method of titanium dioxide nanorod arrays, comprising the following steps: preparing titanium dioxide nanoclusters on a metal mesh by using tetra-n-butyl titanate, glycerol, and ethanol as raw materials to obtain a metal mesh with titanium dioxide nanoclusters; then the metal mesh with titanium dioxide nanoclusters is put in a mixed solution of titanium trichloride, saturated aqueous solution of sodium chloride and urea, said metal mesh is removed after the reaction to obtain titanium dioxide nanorod arrays.
The preparation method of titanium dioxide nanorod arrays according to claim 7, wherein the volume ratio of tetra-n-butyl titanate, glycerin, and ethanol is 1: 5: 15; the temperature of the preparation of titanium dioxide nanoclusters on the metal mesh is 180 0 C, the time is 24 hours; the mass ratio of urea, titanium trichloride, sodium chloride is 1: 2 36.6; the temperature of the reaction is 160 0 C, and the time is 2 hours.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Graphene oxide (200 mg), sodium chloroethanesulfonate (3 g), sodium hydroxide (1.6 g) mixed in 500 mL deionized water with ultrasonic stirring for 3 hours at room temperature. Then 2 mL concentrated nitric acid added while stirring. Product centrifuged, washed three times, dried under dynamic vacuum at 60°C to obtain sulfonated graphene oxide.
4 materials1 process step
Sulfonated graphene oxide (20 mg) dispersed ultrasonically in 20 mL deionized water. Silver nitrate (136 mg) dissolved in 4 mL deionized water. Mixed in 50 mL round bottom flask, stirred for 3 hours at 25°C in dark. Then 2 mL (176 mg) ascorbic acid added quickly and stirred for 1 hour. Product centrifuged, washed, stored in deionized water.
7 materials2 process steps
Washed copper mesh placed in reaction vessel with 2.5 mL tetra-n-butyl titanate, 12.5 mL glycerol, 37.5 mL ethanol. Reacted at 180°C for 24 hours to form TiO₂ nanoclusters on copper mesh. Then 4.05 mL titanium trichloride, 37.5 mL saturated NaCl solution, and 0.3 mg urea mixed and added to reaction vessel with the TiO₂-coated copper mesh. Reacted at 160°C for 2 hours. Upon cooling, copper mesh removed, product washed and dried to obtain TiO₂ nanorod array.
3 materials1 process step
10 mg sulfonated graphene oxide and silver nanoparticle composite material uniformly dispersed in 200 mL deionized water and deposited on titanium dioxide nanorod array by vacuum deposition. Product dried in vacuum to obtain final composite product.
Layer stacks claimed or described, ordered top of device to substrate.
titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane (TSA membrane)
Materials described outside the worked examples.
concentrated nitric acid
HNO₃
copper mesh
Measurements and analyses referenced in the patent, with their drawing references.
Figure 1 shows scanning electron microscopy (SEM) picture of silver nanoparticles and sulfonated graphene oxide composites;
Figure 2 shows scanning electron microscopy (SE M) picture of titanium dioxide nan oro ds arrays;
Figure 3 sh ow s the cr o ss sectional SEM figure of the TSA membrane;
durability. The contact angle of oil droplets in water is more than 1 50. It can also have g oo d and stable separat io n eff ici ency after repeated use of 1 0 tim es. The membrane c an play an effect i ve application in sew age and wastew ate r treatment. 4. T
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
contact angle of oil droplets in water | >150 degrees | titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane |
separation efficiency after repeated use | good and stable | titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane |
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Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows scanning electron microscopy (SEM) picture of silver nanoparticles and sulfonated graphene oxide composites;
Figure 2 shows scanning electron microscopy (SE M) picture of titanium dioxide nan oro ds arrays;
Figure 3 sh ow s the cr o ss sectional SEM figure of the TSA membrane;
Figure 4 shows the wettability of TSA membrane;
Figure 5 shows the separation step of oil-water emulsion;
Figure 6 sh ow s the separati o n efficiency of TSA membrane;
Figure 7 shows the degradation of the TSA membrane.
Figure 8 shows the measurement o f the separation efficiency o f the same T SA film after 10 cycles of separation.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane, comprising the following steps: (1) mixing graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide uniformly in the water, and then adding concentrated nitric acid to obtain sulfonated graphene oxide; (2) mixing the aqueous solution of said sulfonated graphene oxide with the aqueous solution of silver nitrate, stirring in the dark, then adding ascorbic acid, and continuing to stir to obtain a silver nanoparticle/sulfonated graphene oxide composite material; (3) preparing titanium dioxide nanoclusters on a metal mesh by using tetra-n-butyl titanate, glycerol, and ethanol as raw materials to obtain a metal mesh with titanium dioxide nanoclusters; then the metal mesh with titanium dioxide nanoclusters is put in a mixed solution of titanium trichloride, saturated aqueous solution of sodium chloride and urea, said metal mesh is removed after the reaction to obtain titanium dioxide nanorod arrays; (4) dispersing said silver nanoparticle/sulfonated graphene oxide composite material in water, and then deposited on said titanium dioxide nanorods arrays by vacuum deposition, and vacuum dried to obtain titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane.
The preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1, wherein in step (1), the mass ratio of graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide is 0.2: 3: 1.6; after mixing said graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide uniformly in water, ultrasonic stirring for 3 hours at room temperature, and then adding concentrated nitric acid; after the reaction is completed, the product is centrifuged, washed and dried to obtain sulfonated graphene oxide.
The preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1, wherein in step (2), the mass ratio of sulfonated graphene oxide, silver nitrate and ascorbic acid is 1: 6.8: 8.8; said stirring is carried out in the dark for 3 hours at 25 0 C; the time of continued stirring is 1 hour.
The preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1, wherein in step (3), the volume ratio of tetra-n-butyl titanate, glycerin, and ethanol is 1: 5: 15; the temperature of the preparation of titanium dioxide nanoclusters on the metal mesh is 180 0 C, the time is 24 hours; the mass ratio of urea, titanium trichloride, sodium chloride is 1: 2: 36.6; the temperature of the reaction is 160 0 C, and the time is 2 hours.
A titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane prepared by the preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1.
A preparation method of a silver nanoparticle/sulfonated graphene oxide composite material, comprising the following steps: (1) mixing graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide uniformly in the water, and then adding concentrated nitric acid to obtain sulfonated graphene oxide; (2) mixing the aqueous solution of said sulfonated graphene oxide with the aqueous solution of silver nitrate, stirri ng in the dark, then adding ascorbic acid, and continuing to stir to obtain a silver nanoparticle/sulfonated graphene oxide composite material.
The preparation method of a silver nanoparticle/sulfonated graphene oxide composite material according to claim 5, wherein in step (1), the mass ratio of graphene oxide, sodium ch l oroethanesulfonate, and sodium hydroxide is 0.2: 3: 1.6; after mixing said graphene oxide, sodium ch l oroethanesulfonate, and sodium hydroxide uniformly in water, ultrasonic stirring for 3 hours at room temperature, and then adding concentrated nitric acid; after the reaction is completed, the product is centrifuged, washed and dried to obtain sulfonated graphene oxide; in step (2), the mass ratio of sulfonated graphene oxide, silver nitrate and ascorbic acid is 1: 6.8: 8.8; said stirring is carried out in the dark for 3 hours at 25 0 C; the time of continued stirring is I hour.
A preparation method of titanium dioxide nanorod arrays, comprising the following steps: preparing titanium dioxide nanoclusters on a metal mesh by using tetra-n-butyl titanate, glycerol, and ethanol as raw materials to obtain a metal mesh with titanium dioxide nanoclusters; then the metal mesh with titanium dioxide nanoclusters is put in a mixed solution of titanium trichloride, saturated aqueous solution of sodium chloride and urea, said metal mesh is removed after the reaction to obtain titanium dioxide nanorod arrays.
The preparation method of titanium dioxide nanorod arrays according to claim 7, wherein the volume ratio of tetra-n-butyl titanate, glycerin, and ethanol is 1: 5: 15; the temperature of the preparation of titanium dioxide nanoclusters on the metal mesh is 180 0 C, the time is 24 hours; the mass ratio of urea, titanium trichloride, sodium chloride is 1: 2 36.6; the temperature of the reaction is 160 0 C, and the time is 2 hours.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Graphene oxide (200 mg), sodium chloroethanesulfonate (3 g), sodium hydroxide (1.6 g) mixed in 500 mL deionized water with ultrasonic stirring for 3 hours at room temperature. Then 2 mL concentrated nitric acid added while stirring. Product centrifuged, washed three times, dried under dynamic vacuum at 60°C to obtain sulfonated graphene oxide.
4 materials1 process step
Sulfonated graphene oxide (20 mg) dispersed ultrasonically in 20 mL deionized water. Silver nitrate (136 mg) dissolved in 4 mL deionized water. Mixed in 50 mL round bottom flask, stirred for 3 hours at 25°C in dark. Then 2 mL (176 mg) ascorbic acid added quickly and stirred for 1 hour. Product centrifuged, washed, stored in deionized water.
7 materials2 process steps
Washed copper mesh placed in reaction vessel with 2.5 mL tetra-n-butyl titanate, 12.5 mL glycerol, 37.5 mL ethanol. Reacted at 180°C for 24 hours to form TiO₂ nanoclusters on copper mesh. Then 4.05 mL titanium trichloride, 37.5 mL saturated NaCl solution, and 0.3 mg urea mixed and added to reaction vessel with the TiO₂-coated copper mesh. Reacted at 160°C for 2 hours. Upon cooling, copper mesh removed, product washed and dried to obtain TiO₂ nanorod array.
3 materials1 process step
10 mg sulfonated graphene oxide and silver nanoparticle composite material uniformly dispersed in 200 mL deionized water and deposited on titanium dioxide nanorod array by vacuum deposition. Product dried in vacuum to obtain final composite product.
Layer stacks claimed or described, ordered top of device to substrate.
titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane (TSA membrane)
Materials described outside the worked examples.
concentrated nitric acid
HNO₃
copper mesh
Measurements and analyses referenced in the patent, with their drawing references.
Figure 1 shows scanning electron microscopy (SEM) picture of silver nanoparticles and sulfonated graphene oxide composites;
Figure 2 shows scanning electron microscopy (SE M) picture of titanium dioxide nan oro ds arrays;
Figure 3 sh ow s the cr o ss sectional SEM figure of the TSA membrane;
durability. The contact angle of oil droplets in water is more than 1 50. It can also have g oo d and stable separat io n eff ici ency after repeated use of 1 0 tim es. The membrane c an play an effect i ve application in sew age and wastew ate r treatment. 4. T
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
contact angle of oil droplets in water | >150 degrees | titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane |
separation efficiency after repeated use | good and stable | titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane |
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Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows scanning electron microscopy (SEM) picture of silver nanoparticles and sulfonated graphene oxide composites;
Figure 2 shows scanning electron microscopy (SE M) picture of titanium dioxide nan oro ds arrays;
Figure 3 sh ow s the cr o ss sectional SEM figure of the TSA membrane;
Figure 4 shows the wettability of TSA membrane;
Figure 5 shows the separation step of oil-water emulsion;
Figure 6 sh ow s the separati o n efficiency of TSA membrane;
Figure 7 shows the degradation of the TSA membrane.
Figure 8 shows the measurement o f the separation efficiency o f the same T SA film after 10 cycles of separation.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane, comprising the following steps: (1) mixing graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide uniformly in the water, and then adding concentrated nitric acid to obtain sulfonated graphene oxide; (2) mixing the aqueous solution of said sulfonated graphene oxide with the aqueous solution of silver nitrate, stirring in the dark, then adding ascorbic acid, and continuing to stir to obtain a silver nanoparticle/sulfonated graphene oxide composite material; (3) preparing titanium dioxide nanoclusters on a metal mesh by using tetra-n-butyl titanate, glycerol, and ethanol as raw materials to obtain a metal mesh with titanium dioxide nanoclusters; then the metal mesh with titanium dioxide nanoclusters is put in a mixed solution of titanium trichloride, saturated aqueous solution of sodium chloride and urea, said metal mesh is removed after the reaction to obtain titanium dioxide nanorod arrays; (4) dispersing said silver nanoparticle/sulfonated graphene oxide composite material in water, and then deposited on said titanium dioxide nanorods arrays by vacuum deposition, and vacuum dried to obtain titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane.
The preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1, wherein in step (1), the mass ratio of graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide is 0.2: 3: 1.6; after mixing said graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide uniformly in water, ultrasonic stirring for 3 hours at room temperature, and then adding concentrated nitric acid; after the reaction is completed, the product is centrifuged, washed and dried to obtain sulfonated graphene oxide.
The preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1, wherein in step (2), the mass ratio of sulfonated graphene oxide, silver nitrate and ascorbic acid is 1: 6.8: 8.8; said stirring is carried out in the dark for 3 hours at 25 0 C; the time of continued stirring is 1 hour.
The preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1, wherein in step (3), the volume ratio of tetra-n-butyl titanate, glycerin, and ethanol is 1: 5: 15; the temperature of the preparation of titanium dioxide nanoclusters on the metal mesh is 180 0 C, the time is 24 hours; the mass ratio of urea, titanium trichloride, sodium chloride is 1: 2: 36.6; the temperature of the reaction is 160 0 C, and the time is 2 hours.
A titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane prepared by the preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1.
A preparation method of a silver nanoparticle/sulfonated graphene oxide composite material, comprising the following steps: (1) mixing graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide uniformly in the water, and then adding concentrated nitric acid to obtain sulfonated graphene oxide; (2) mixing the aqueous solution of said sulfonated graphene oxide with the aqueous solution of silver nitrate, stirri ng in the dark, then adding ascorbic acid, and continuing to stir to obtain a silver nanoparticle/sulfonated graphene oxide composite material.
The preparation method of a silver nanoparticle/sulfonated graphene oxide composite material according to claim 5, wherein in step (1), the mass ratio of graphene oxide, sodium ch l oroethanesulfonate, and sodium hydroxide is 0.2: 3: 1.6; after mixing said graphene oxide, sodium ch l oroethanesulfonate, and sodium hydroxide uniformly in water, ultrasonic stirring for 3 hours at room temperature, and then adding concentrated nitric acid; after the reaction is completed, the product is centrifuged, washed and dried to obtain sulfonated graphene oxide; in step (2), the mass ratio of sulfonated graphene oxide, silver nitrate and ascorbic acid is 1: 6.8: 8.8; said stirring is carried out in the dark for 3 hours at 25 0 C; the time of continued stirring is I hour.
A preparation method of titanium dioxide nanorod arrays, comprising the following steps: preparing titanium dioxide nanoclusters on a metal mesh by using tetra-n-butyl titanate, glycerol, and ethanol as raw materials to obtain a metal mesh with titanium dioxide nanoclusters; then the metal mesh with titanium dioxide nanoclusters is put in a mixed solution of titanium trichloride, saturated aqueous solution of sodium chloride and urea, said metal mesh is removed after the reaction to obtain titanium dioxide nanorod arrays.
The preparation method of titanium dioxide nanorod arrays according to claim 7, wherein the volume ratio of tetra-n-butyl titanate, glycerin, and ethanol is 1: 5: 15; the temperature of the preparation of titanium dioxide nanoclusters on the metal mesh is 180 0 C, the time is 24 hours; the mass ratio of urea, titanium trichloride, sodium chloride is 1: 2 36.6; the temperature of the reaction is 160 0 C, and the time is 2 hours.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Graphene oxide (200 mg), sodium chloroethanesulfonate (3 g), sodium hydroxide (1.6 g) mixed in 500 mL deionized water with ultrasonic stirring for 3 hours at room temperature. Then 2 mL concentrated nitric acid added while stirring. Product centrifuged, washed three times, dried under dynamic vacuum at 60°C to obtain sulfonated graphene oxide.
4 materials1 process step
Sulfonated graphene oxide (20 mg) dispersed ultrasonically in 20 mL deionized water. Silver nitrate (136 mg) dissolved in 4 mL deionized water. Mixed in 50 mL round bottom flask, stirred for 3 hours at 25°C in dark. Then 2 mL (176 mg) ascorbic acid added quickly and stirred for 1 hour. Product centrifuged, washed, stored in deionized water.
7 materials2 process steps
Washed copper mesh placed in reaction vessel with 2.5 mL tetra-n-butyl titanate, 12.5 mL glycerol, 37.5 mL ethanol. Reacted at 180°C for 24 hours to form TiO₂ nanoclusters on copper mesh. Then 4.05 mL titanium trichloride, 37.5 mL saturated NaCl solution, and 0.3 mg urea mixed and added to reaction vessel with the TiO₂-coated copper mesh. Reacted at 160°C for 2 hours. Upon cooling, copper mesh removed, product washed and dried to obtain TiO₂ nanorod array.
3 materials1 process step
10 mg sulfonated graphene oxide and silver nanoparticle composite material uniformly dispersed in 200 mL deionized water and deposited on titanium dioxide nanorod array by vacuum deposition. Product dried in vacuum to obtain final composite product.
Layer stacks claimed or described, ordered top of device to substrate.
titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane (TSA membrane)
Materials described outside the worked examples.
concentrated nitric acid
HNO₃
copper mesh
Measurements and analyses referenced in the patent, with their drawing references.
Figure 1 shows scanning electron microscopy (SEM) picture of silver nanoparticles and sulfonated graphene oxide composites;
Figure 2 shows scanning electron microscopy (SE M) picture of titanium dioxide nan oro ds arrays;
Figure 3 sh ow s the cr o ss sectional SEM figure of the TSA membrane;
durability. The contact angle of oil droplets in water is more than 1 50. It can also have g oo d and stable separat io n eff ici ency after repeated use of 1 0 tim es. The membrane c an play an effect i ve application in sew age and wastew ate r treatment. 4. T
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
contact angle of oil droplets in water | >150 degrees | titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane |
separation efficiency after repeated use | good and stable | titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane |
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Method of Manufacturing Graphene Using Photoreduction
METHOD FOR MAKING GRAPHENE/CARBON NANOTUBE COMPOSITE STRUCTURE
A METHOD FOR DIRECTLY GROWING ULTRATHIN POROUS GRAPHENE SEPARATION MEMBRANE
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Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 shows scanning electron microscopy (SEM) picture of silver nanoparticles and sulfonated graphene oxide composites;
Figure 2 shows scanning electron microscopy (SE M) picture of titanium dioxide nan oro ds arrays;
Figure 3 sh ow s the cr o ss sectional SEM figure of the TSA membrane;
Figure 4 shows the wettability of TSA membrane;
Figure 5 shows the separation step of oil-water emulsion;
Figure 6 sh ow s the separati o n efficiency of TSA membrane;
Figure 7 shows the degradation of the TSA membrane.
Figure 8 shows the measurement o f the separation efficiency o f the same T SA film after 10 cycles of separation.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
A preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane, comprising the following steps: (1) mixing graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide uniformly in the water, and then adding concentrated nitric acid to obtain sulfonated graphene oxide; (2) mixing the aqueous solution of said sulfonated graphene oxide with the aqueous solution of silver nitrate, stirring in the dark, then adding ascorbic acid, and continuing to stir to obtain a silver nanoparticle/sulfonated graphene oxide composite material; (3) preparing titanium dioxide nanoclusters on a metal mesh by using tetra-n-butyl titanate, glycerol, and ethanol as raw materials to obtain a metal mesh with titanium dioxide nanoclusters; then the metal mesh with titanium dioxide nanoclusters is put in a mixed solution of titanium trichloride, saturated aqueous solution of sodium chloride and urea, said metal mesh is removed after the reaction to obtain titanium dioxide nanorod arrays; (4) dispersing said silver nanoparticle/sulfonated graphene oxide composite material in water, and then deposited on said titanium dioxide nanorods arrays by vacuum deposition, and vacuum dried to obtain titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane.
The preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1, wherein in step (1), the mass ratio of graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide is 0.2: 3: 1.6; after mixing said graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide uniformly in water, ultrasonic stirring for 3 hours at room temperature, and then adding concentrated nitric acid; after the reaction is completed, the product is centrifuged, washed and dried to obtain sulfonated graphene oxide.
The preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1, wherein in step (2), the mass ratio of sulfonated graphene oxide, silver nitrate and ascorbic acid is 1: 6.8: 8.8; said stirring is carried out in the dark for 3 hours at 25 0 C; the time of continued stirring is 1 hour.
The preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1, wherein in step (3), the volume ratio of tetra-n-butyl titanate, glycerin, and ethanol is 1: 5: 15; the temperature of the preparation of titanium dioxide nanoclusters on the metal mesh is 180 0 C, the time is 24 hours; the mass ratio of urea, titanium trichloride, sodium chloride is 1: 2: 36.6; the temperature of the reaction is 160 0 C, and the time is 2 hours.
A titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane prepared by the preparation method of titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane according to claim 1.
A preparation method of a silver nanoparticle/sulfonated graphene oxide composite material, comprising the following steps: (1) mixing graphene oxide, sodium chloroethanesulfonate, and sodium hydroxide uniformly in the water, and then adding concentrated nitric acid to obtain sulfonated graphene oxide; (2) mixing the aqueous solution of said sulfonated graphene oxide with the aqueous solution of silver nitrate, stirri ng in the dark, then adding ascorbic acid, and continuing to stir to obtain a silver nanoparticle/sulfonated graphene oxide composite material.
The preparation method of a silver nanoparticle/sulfonated graphene oxide composite material according to claim 5, wherein in step (1), the mass ratio of graphene oxide, sodium ch l oroethanesulfonate, and sodium hydroxide is 0.2: 3: 1.6; after mixing said graphene oxide, sodium ch l oroethanesulfonate, and sodium hydroxide uniformly in water, ultrasonic stirring for 3 hours at room temperature, and then adding concentrated nitric acid; after the reaction is completed, the product is centrifuged, washed and dried to obtain sulfonated graphene oxide; in step (2), the mass ratio of sulfonated graphene oxide, silver nitrate and ascorbic acid is 1: 6.8: 8.8; said stirring is carried out in the dark for 3 hours at 25 0 C; the time of continued stirring is I hour.
A preparation method of titanium dioxide nanorod arrays, comprising the following steps: preparing titanium dioxide nanoclusters on a metal mesh by using tetra-n-butyl titanate, glycerol, and ethanol as raw materials to obtain a metal mesh with titanium dioxide nanoclusters; then the metal mesh with titanium dioxide nanoclusters is put in a mixed solution of titanium trichloride, saturated aqueous solution of sodium chloride and urea, said metal mesh is removed after the reaction to obtain titanium dioxide nanorod arrays.
The preparation method of titanium dioxide nanorod arrays according to claim 7, wherein the volume ratio of tetra-n-butyl titanate, glycerin, and ethanol is 1: 5: 15; the temperature of the preparation of titanium dioxide nanoclusters on the metal mesh is 180 0 C, the time is 24 hours; the mass ratio of urea, titanium trichloride, sodium chloride is 1: 2 36.6; the temperature of the reaction is 160 0 C, and the time is 2 hours.
Embodiments described in the patent, grouped by the materials and process steps they use.
4 materials1 process step
Graphene oxide (200 mg), sodium chloroethanesulfonate (3 g), sodium hydroxide (1.6 g) mixed in 500 mL deionized water with ultrasonic stirring for 3 hours at room temperature. Then 2 mL concentrated nitric acid added while stirring. Product centrifuged, washed three times, dried under dynamic vacuum at 60°C to obtain sulfonated graphene oxide.
4 materials1 process step
Sulfonated graphene oxide (20 mg) dispersed ultrasonically in 20 mL deionized water. Silver nitrate (136 mg) dissolved in 4 mL deionized water. Mixed in 50 mL round bottom flask, stirred for 3 hours at 25°C in dark. Then 2 mL (176 mg) ascorbic acid added quickly and stirred for 1 hour. Product centrifuged, washed, stored in deionized water.
7 materials2 process steps
Washed copper mesh placed in reaction vessel with 2.5 mL tetra-n-butyl titanate, 12.5 mL glycerol, 37.5 mL ethanol. Reacted at 180°C for 24 hours to form TiO₂ nanoclusters on copper mesh. Then 4.05 mL titanium trichloride, 37.5 mL saturated NaCl solution, and 0.3 mg urea mixed and added to reaction vessel with the TiO₂-coated copper mesh. Reacted at 160°C for 2 hours. Upon cooling, copper mesh removed, product washed and dried to obtain TiO₂ nanorod array.
3 materials1 process step
10 mg sulfonated graphene oxide and silver nanoparticle composite material uniformly dispersed in 200 mL deionized water and deposited on titanium dioxide nanorod array by vacuum deposition. Product dried in vacuum to obtain final composite product.
Layer stacks claimed or described, ordered top of device to substrate.
titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane (TSA membrane)
Materials described outside the worked examples.
concentrated nitric acid
HNO₃
copper mesh
Measurements and analyses referenced in the patent, with their drawing references.
Figure 1 shows scanning electron microscopy (SEM) picture of silver nanoparticles and sulfonated graphene oxide composites;
Figure 2 shows scanning electron microscopy (SE M) picture of titanium dioxide nan oro ds arrays;
Figure 3 sh ow s the cr o ss sectional SEM figure of the TSA membrane;
durability. The contact angle of oil droplets in water is more than 1 50. It can also have g oo d and stable separat io n eff ici ency after repeated use of 1 0 tim es. The membrane c an play an effect i ve application in sew age and wastew ate r treatment. 4. T
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
contact angle of oil droplets in water | >150 degrees | titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane |
separation efficiency after repeated use | good and stable | titanium dioxide/sulfonated graphene oxide/silver nanoparticle composite membrane |
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