Graphene Oxide In-situ Growth Method to Prepare Hollow Structure Nano Tungsten Oxide Wire Preparation Method

Abstract

The present invention discloses a method for preparing hollow structure tungsten oxide nano-wires through a graphene oxide in-situ growth method. The method comprises: 1) weighing a certain amount of graphene oxide and a tungsten-containing precursor compound; 2) dispersing in a certain amount of deionized water, and carrying out ultrasonic dispersing; 3) dissolving the weighed tungsten-containing precursor compound in the graphene oxide aqueous solution prepared in the step 2) to obtain graphene oxide and tungsten-containing precursor compound powder, placing into an oven, carrying out thermal insulation for a certain time at a certain temperature to obtain dried mixed powder; and 4) placing the dried graphene oxide and tungsten-containing precursor compound powder obtained in the step 3) in an alumina crucible, and naturally cooling to a room temperature in a H2 atmosphere so as to obtain the hollow structure tungsten oxide nano-wires. Compared to the conventional preparation method using the high-pressure reactor with the polytetrafluoroethylene inner lining, the preparation method of the present invention has advantages of lower energy consumption, lower cost, less investment in industrial production, low product cost, and convenient achievement of the mass production.

Description

technical field

[0001] The invention belongs to the field of nanometer materials, in particular to a preparation method for preparing hollow structure nano tungsten oxide wires by in-situ growth method of graphene oxide. Background technique

[0002] With the rapid development of my country's industry in recent years, the discharge of industrial waste gas has made safety issues increasingly prominent, and the threat of PM2.5 to people's health has also been paid more and more attention. Therefore, the requirements for reliable gas detection are getting higher and higher. The sensitivity of nanosensors to detect pollutant gases also puts forward higher requirements. Compared with traditional oxide materials, the specific surface area of ​​tungsten oxide nanowires is larger, and it is effective for NO and NO 2 The gas detection has good selectivity and sensitivity. Its sensitive mechanism belongs to the surface resistance control type. The detection of nitrogen dioxide gas is...

Examples

Embodiment 1

[0027] The invention provides a method for preparing hollow structure nano-tungsten oxide wires by in-situ growth method of graphene oxide, which comprises the steps of: adding a certain amount of graphite powder to the mixture of concentrated H2SO4 (12mL), K2S2O8 (2.5g) and P2O5 (2.5g) ) in a solution composed of 80°C for 4.5 hours. After cooling to room temperature, 0.5 L of deionized water was added. and dry at room temperature. Add this pre-oxidized graphite powder to 150mL of concentrated H2SO4, keep the environment at 0°C with an ice-water bath, gradually add 15g KMnO4, and keep the temperature not exceeding 20°C, and stir at 35°C for 2 hours after the addition. Then 250 mL of deionized water was added and stirred for 2 hours. Then add 0.7 L of deionized water, then add 30 mL of 30% H2O2, dry at room temperature, and then dialyze in a dialysis bag for 1 week to remove heteroions. Finally, it was vacuum filtered and dried at room temperature to obtain graphene oxide. ...

Embodiment 2

[0033] On the basis of the above examples, the steps of this example are as follows: add a certain amount of graphite powder to a solution composed of concentrated H2SO4 (12mL), K2S2O8 (2.5g) and P2O5 (2.5g), and react at 80°C for 4.5 Hour. After cooling to room temperature, 0.5 L of deionized water was added. and dry at room temperature. Add this pre-oxidized graphite powder to 150mL of concentrated H2SO4, keep the environment at 0°C with an ice-water bath, gradually add 15g KMnO4, and keep the temperature not exceeding 20°C, and stir at 35°C for 2 hours after the addition. Then 250 mL of deionized water was added and stirred for 2 hours. Then add 0.7 L of deionized water, then add 30 mL of 30% H2O2, dry at room temperature, and then dialyze in a dialysis bag for 1 week to remove heteroions. Finally, it was vacuum filtered and dried at room temperature to obtain graphene oxide.

[0034] Weigh 2g of graphene oxide, add 1000g of absolute ethanol, stir and mix evenly, add 60...

Embodiment 3

[0036] On the basis of the above examples, the steps of this example are as follows: add a certain amount of graphite powder to a solution composed of concentrated H2SO4 (12mL), K2S2O8 (2.5g) and P2O5 (2.5g), and react at 80°C for 4.5 Hour. After cooling to room temperature, 0.5 L of deionized water was added. and dry at room temperature. Add this pre-oxidized graphite powder to 150mL of concentrated H2SO4, keep the environment at 0°C with an ice-water bath, gradually add 15g KMnO4, and keep the temperature not exceeding 20°C, and stir at 35°C for 2 hours after the addition. Then 250 mL of deionized water was added and stirred for 2 hours. Then add 0.7 L of deionized water, then add 30 mL of 30% H2O2, dry at room temperature, and then dialyze in a dialysis bag for 1 week to remove heteroions. Finally, it was vacuum filtered and dried at room temperature to obtain graphene oxide.

[0037] Weigh 3g of graphene oxide, add 1000g of absolute ethanol, stir and mix evenly, add 70...

technical field

[0001] The invention belongs to the field of nanometer materials, in particular to a preparation method for preparing hollow structure nano tungsten oxide wires by in-situ growth method of graphene oxide. Background technique

[0002] With the rapid development of my country's industry in recent years, the discharge of industrial waste gas has made safety issues increasingly prominent, and the threat of PM2.5 to people's health has also been paid more and more attention. Therefore, the requirements for reliable gas detection are getting higher and higher. The sensitivity of nanosensors to detect pollutant gases also puts forward higher requirements. Compared with traditional oxide materials, the specific surface area of ​​tungsten oxide nanowires is larger, and it is effective for NO and NO 2 The gas detection has good selectivity and sensitivity. Its sensitive mechanism belongs to the surface resistance control type. The detection of nitrogen dioxide gas is...

Examples

Embodiment 1

[0027] The invention provides a method for preparing hollow structure nano-tungsten oxide wires by in-situ growth method of graphene oxide, which comprises the steps of: adding a certain amount of graphite powder to the mixture of concentrated H2SO4 (12mL), K2S2O8 (2.5g) and P2O5 (2.5g) ) in a solution composed of 80°C for 4.5 hours. After cooling to room temperature, 0.5 L of deionized water was added. and dry at room temperature. Add this pre-oxidized graphite powder to 150mL of concentrated H2SO4, keep the environment at 0°C with an ice-water bath, gradually add 15g KMnO4, and keep the temperature not exceeding 20°C, and stir at 35°C for 2 hours after the addition. Then 250 mL of deionized water was added and stirred for 2 hours. Then add 0.7 L of deionized water, then add 30 mL of 30% H2O2, dry at room temperature, and then dialyze in a dialysis bag for 1 week to remove heteroions. Finally, it was vacuum filtered and dried at room temperature to obtain graphene oxide. ...

Embodiment 2

[0033] On the basis of the above examples, the steps of this example are as follows: add a certain amount of graphite powder to a solution composed of concentrated H2SO4 (12mL), K2S2O8 (2.5g) and P2O5 (2.5g), and react at 80°C for 4.5 Hour. After cooling to room temperature, 0.5 L of deionized water was added. and dry at room temperature. Add this pre-oxidized graphite powder to 150mL of concentrated H2SO4, keep the environment at 0°C with an ice-water bath, gradually add 15g KMnO4, and keep the temperature not exceeding 20°C, and stir at 35°C for 2 hours after the addition. Then 250 mL of deionized water was added and stirred for 2 hours. Then add 0.7 L of deionized water, then add 30 mL of 30% H2O2, dry at room temperature, and then dialyze in a dialysis bag for 1 week to remove heteroions. Finally, it was vacuum filtered and dried at room temperature to obtain graphene oxide.

[0034] Weigh 2g of graphene oxide, add 1000g of absolute ethanol, stir and mix evenly, add 60...

Embodiment 3

[0036] On the basis of the above examples, the steps of this example are as follows: add a certain amount of graphite powder to a solution composed of concentrated H2SO4 (12mL), K2S2O8 (2.5g) and P2O5 (2.5g), and react at 80°C for 4.5 Hour. After cooling to room temperature, 0.5 L of deionized water was added. and dry at room temperature. Add this pre-oxidized graphite powder to 150mL of concentrated H2SO4, keep the environment at 0°C with an ice-water bath, gradually add 15g KMnO4, and keep the temperature not exceeding 20°C, and stir at 35°C for 2 hours after the addition. Then 250 mL of deionized water was added and stirred for 2 hours. Then add 0.7 L of deionized water, then add 30 mL of 30% H2O2, dry at room temperature, and then dialyze in a dialysis bag for 1 week to remove heteroions. Finally, it was vacuum filtered and dried at room temperature to obtain graphene oxide.

[0037] Weigh 3g of graphene oxide, add 1000g of absolute ethanol, stir and mix evenly, add 70...

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