Preparation Method and Application of a Tungsten Oxide-Graphene Composite Material

Abstract

The present invention relates to the technical field of tungsten oxide-graphene composite materials, and more specifically to a preparation method and application of tungsten oxide-graphene composite materials; a preparation method of tungsten oxide-graphene composite materials, the method comprising the following steps: Step 1: Prepare an aqueous solution of graphene oxide by adding water to graphene oxide; Step 2: Add a tungsten solution dissolved in ethanol to the aqueous solution of graphene oxide for mixing to obtain a mixed solution; Step 3: Add acetone while stirring the mixed solution and generate a mixture under microwave conditions; Step 4: Wash and dry the mixture; Step 5: Heat the mixture, cool it and then grind it to obtain a tungsten oxide-graphene composite material; the efficiency of preparing the tungsten oxide-graphene composite material can be improved.

Description

Technical Field

[0001] The present invention relates to the technical field of tungsten oxide-graphene composites, and more specifically to a preparation method and application of tungsten oxide-graphene composites. Background Art

[0002] The document with the publication number CN106872063B discloses a preparation method of tungsten oxide-graphene composites. The purpose of this invention is to improve the temperature-sensitive characteristics of graphene materials by preparing tungsten oxide-graphene composites. Method: First, oxidize graphite into graphite oxide powder; second, ultrasonically disperse the graphite oxide powder in n-propanol, then add tungsten hexachloride and carry out a hydrothermal reaction; third, adjust the pH value to 9-10, then add 50% hydrazine hydrate aqueous solution and react in an oil bath. After the reaction, centrifuge and wash, and then dry to obtain black powder, that is, tubular tungsten oxide-graphene composites; however, the efficiency of preparing tungsten oxide-graphene composites by this method is low. Summary of the Invention

[0003] To overcome the deficiencies of the prior art, the present invention provides a preparation method of tungsten oxide-graphene composites, which can improve the efficiency of preparing tungsten oxide-graphene composites.

[0004] The technical solution adopted by the present invention to solve its technical problems is:

[0005] A preparation method of tungsten oxide-graphene composites, the method comprising the following steps:

[0006] Step 1: Add water to graphene oxide to make a graphene oxide aqueous solution;

[0007] Step 2: Add the tungsten solution dissolved in ethanol to the graphene oxide aqueous solution for mixing to obtain a mixed solution;

[0008] Step 3: While stirring the mixed solution, add acetone and generate a mixture under microwave conditions;

[0009] Step 4: Wash and dry the mixture;

[0010] Step 5: Heat the mixture, cool it, and then grind it to obtain tungsten oxide-graphene composites.

[0011] Further, the said step 4 is realized by a washing device. The washing device includes a sleeve with a plurality of fan sleeves, a sleeve arranged on the sleeve, and a motor with a bolt fixed on the output shaft.

[0012] Further, the said device further includes an inner rod sliding in the sleeve, and a plurality of fan blades arranged on the inner rod. The plurality of fan blades can respectively slide into the corresponding plurality of fan sleeves. A plurality of sliding holes for the plurality of fan blades to slide are arranged on the sleeve. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] The present invention will be further described in detail below with reference to the accompanying drawings and specific implementation methods.

[0014] Figure 1 Flowchart of the preparation method of the tungsten oxide-graphene composite material of the present invention;

[0015] Figure 2 Schematic diagram of the structure of the washing device of the present invention;

[0016] Figure 3 is a cross-sectional view of the washing device of the present invention;

[0017] Figure 4 It is a schematic diagram of the structure of a part of the washing device in the present invention;

[0018] Figure 5 Schematic diagram of the structure of the sleeve and fan sleeve in the present invention;

[0019] Figure 6 Schematic diagram of the structure of the inner rod and fan blades in the present invention;

[0020] Figure 7 Schematic diagram of the structure of the motor and the latch in the present invention;

[0021] Figure 8 Schematic diagram of the structure of the sieve hole and the inner cavity in the present invention;

[0022] Figure 9 Schematic diagram of the structure of the bottom plate and outer wall of the present invention;

[0023] Figure 10 Schematic diagram of the structure of the leakage hole in the present invention;

[0024] Figure 11 It is a structural schematic diagram of the block and the funnel in the present invention. DETAILED DESCRIPTION

[0025] See Figure 1 According to the figure, an exemplary working process for preparing a tungsten oxide-graphene composite material is:

[0026] First, graphene oxide is added to water to prepare a graphene oxide aqueous solution; then a tungsten solution dissolved in ethanol is added to the graphene oxide aqueous solution and mixed to obtain a mixed solution; then acetone is added while the mixed solution is stirred and a mixture is generated under microwave conditions; the mixture is then washed, filtered after washing to retain a clean mixture and dried; finally, the mixture is heated, cooled, and then ground to obtain a tungsten oxide-graphene composite material.

[0027] See Figures 2 to 7, an exemplary working process for washing the mixture can be obtained according to what is shown in the figure:

[0028] The mixture washing is realized by a washing device. The washing device includes a sleeve 01 and a motor 10 with a pin 11 fixed on the output shaft. A plurality of fan sleeves 07 are arranged on the sleeve 01, and a sleeve 05 is arranged on the sleeve 01. The pin 11 can be inserted into the sleeve 05. When washing the mixture, first put the mixture into the washing container, then insert the sleeve 01 into the container, insert the pin 11 into the sleeve 05 and fix the motor 10 on the axis of the container, and then power on the motor 10 to make the output shaft of the motor 10 drive the pin 11 to rotate around the axis of the container, so that the pin 11 drives the sleeve 01 to rotate on the axis of the container. Use the plurality of fan sleeves 07 on the sleeve 01 to stir the clear water and the mixture in the container, so that each part of the mixture can be fully contacted with the clear water, and the clear water can wash off the excess and unreacted raw materials on the mixture.

[0029] See Figures 2 to 7 , an exemplary working process for quickly erecting the sleeve 01 can be obtained according to what is shown in the figure:

[0030] The device further includes a lid 09 for fixing the motor 10. To facilitate the quick erection of the sleeve 01, only need to fix the lid 09 on the washing container, cover the upper opening of the washing container with the lid 09, and at the same time make the sleeve 01 located on the axis of the washing container.

[0031] See Figures 2 to 7 , an exemplary working process for changing the stirring range and intensity can be obtained according to what is shown in the figure:

[0032] The device further includes an inner rod 02 slidingly contacting in the sleeve 01 and a plurality of fan blades 08 fixedly connected to the inner rod 02. The plurality of fan blades 08 can respectively slide into the corresponding plurality of fan sleeves 07 when the inner rod 02 slides up and down along the sleeve 01. A plurality of sliding holes 06 for the plurality of fan blades 08 to slide are arranged on the sleeve 01. When the inner rod 02 slides up and down in the sleeve 01, it can be realized that the inner rod 02 drives the plurality of fan blades 08 to slide in the plurality of sliding holes 06, so as to realize the vertical expansion and contraction of the plurality of fan blades 08 in the plurality of fan sleeves 07 respectively;

[0033] When the inner rod 02 descends, the inner rod 02 drives multiple fan blades 08 to respectively extend downward from multiple fan sleeves 07, so that the area formed by the fan blades 08 and the fan sleeves 07 for agitating the clear water and the mixture increases, facilitating the improvement of the washing of the mixture. At the same time, the centrifugal force generated when the fan blades 08 and the fan sleeves 07 jointly drive the clear water and the mixture to be agitated can be increased, which is beneficial to the separation of the mixture after washing;

[0034] See Figures 2 to 7 , an exemplary working process for sealing the sleeve 01 can be obtained according to the illustration in the figure:

[0035] The fan blade 08 contacts the outer wall surface of the sleeve 01. When the fan blade 08 is located in the fan sleeve 07, it covers the corresponding sliding hole 06, and the fan blade 08 is in surface contact with the fan sleeve 07; when the fan blade 08 slides up and down, the fan blade 08 always maintains a surface contact state with the outer wall of the sleeve 01, thereby realizing that the fan blade 08 always blocks the corresponding sliding hole 06 on the sleeve 01, preventing the clear water and the mixture from entering the sleeve 01 through the sliding hole 06.

[0036] See Figures 2 to 7 , an exemplary working process for adjusting the stirring range formed by the fan blade 08 and the fan sleeve 07 can be obtained according to the illustration in the figure:

[0037] The inner rod 02 is provided with a thread 03, and the nut 04 rotates on the sleeve 01, and the thread 03 is threadedly connected to the nut 04; when adjusting the telescopic movement of the fan blade 08 in the fan sleeve 07, only by rotating the nut 04 can the nut 04 drive the inner rod 02 to move up and down in the sleeve 01, thereby realizing the stirring range of the fan blade 08 and the fan sleeve 07 in the vertical range, changing the efficiency and ability of agitating the mixture and the clear water, and further improving the efficiency and ability of washing the mixture.

[0038] See Figures 2 to 9 , an exemplary working process for filtering the sewage generated from the washed mixture can be obtained according to the illustration in the figure:

[0039] The device further includes an inner wall 12 provided with multiple sieve holes 13, a bottom plate 15 fixed to the inner wall 12, and an outer wall 16 fixed to the inner wall 12; the mixture and the clear water are added into the inner wall 12, and then when the sleeve 01 drives the fan blade 08 and the fan sleeve 07 to agitate the clear water and the mixture, by using the centrifugal force generated by the agitation on the mixture and the clear water, the clear water and the mixture are made to adhere to the inner wall 12. At the same time, when a swirling flow is formed, the generated sewage is thrown out through the multiple sieve holes 13. When the sewage touches the outer wall 16, it is blocked and finally collected and flows out concentratedly from the opening at the lower end of the outer wall 16 for easy collection; the mixture after being centrifuged remains in the inner wall 12.

[0040] Refer to Figures 2 to 9 , an exemplary working process of the concentrated mixture can be obtained according to what is shown in the figure:

[0041] A plurality of inner cavities 14 are circumferentially arranged on the inner wall 12, and the plurality of inner cavities 14 and the inner wall 12 are both connected by inclined surfaces; when the swirling flow formed by clear water and the mixture passes through the plurality of inner cavities 14, the mixture can slide along the inclined surface into the plurality of inner cavities 14, and continuously concentrate in the plurality of inner cavities 14. At the same time, the sewage is thrown out through the plurality of sieve holes 13. It can be seen from the figure that the plurality of sieve holes 13 are also communicated with the plurality of inner cavities 14. When the mixture continuously concentrates and accumulates in the plurality of inner cavities 14, the extrusion between the mixtures can squeeze the sewage out of the inner cavities 14, so that the mixture is concentrated in the plurality of inner cavities 14 after centrifugal filtration, which is convenient for centralized collection, and at the same time avoids the mixture from colliding and tumbling with each other during continuous centrifugation and causing fragmentation.

[0042] Refer to Figures 2 to 11 , an exemplary working process of taking out the mixture can be obtained according to what is shown in the figure:

[0043] The device further includes a plurality of leakage holes 17 arranged on the bottom plate 15, a funnel 19 provided with a plug 18 capable of blocking the leakage holes 17, and a base 20 fixed on the outer wall 16 and driving the funnel 19 to lift through a cylinder; after the sewage is filtered out, the cylinder is used to drive the funnel 19 to descend, so that the funnel 19 drives the plurality of plugs 18 thereon to slide out downward from the plurality of leakage holes 17 respectively. The plurality of leakage holes 17 are respectively located directly below the plurality of inner cavities 14. When the plurality of plugs 18 completely leave the plurality of leakage holes 17, the mixture concentrated in the plurality of inner cavities 14 will slide down from the plurality of leakage holes 17 into the funnel 19. Only by placing a collection container below the funnel 19 can the washed mixture be centrally collected.

[0044] The tungsten oxide-graphene composite material prepared by the above tungsten oxide-graphene composite material method can achieve good sensitivity in gas detection, and can improve the gas detection effect and accuracy.

Claims

1. A preparation method of tungsten oxide-graphene composite material, characterized in that, The method includes the following steps: Step 1: Add water to graphene oxide to make an aqueous solution of graphene oxide; Step 2: Add a tungsten solution dissolved in ethanol to the aqueous solution of graphene oxide for mixing to obtain a mixture; Step 3: Add acetone while stirring the mixture and generate a mixture under microwave conditions; Step 4: Wash and dry the mixture; Step 5: Heat the mixture, cool it, and then grind it to obtain a tungsten oxide-graphene composite material; The said Step 4 is realized by a washing device. The washing device includes a sleeve (01) provided with a plurality of fan sleeves (07), a sleeve (05) arranged on the sleeve (01), and a motor (10) with a pin (11) fixedly connected to the output shaft; The device further includes a cover (09) for fixing the motor (10); The device further includes an inner rod (02) sliding in the sleeve (01), and a plurality of fan blades (08) arranged on the inner rod (02). The plurality of fan blades (08) can respectively slide into the corresponding plurality of fan sleeves (07). A plurality of sliding holes (06) for the plurality of fan blades (08) to slide are arranged on the sleeve (01); The fan blades (08) are in contact with the outer wall surface of the sleeve (01). When the fan blades (08) are located in the fan sleeves (07), they cover the corresponding sliding holes (06), and the fan blades (08) are in surface contact with the fan sleeves (07); Threads (03) are arranged on the inner rod (02), and a nut (04) rotates on the sleeve (01). The threads (03) are threadedly connected to the nut (04); The device further includes an inner wall (12) provided with a plurality of sieve holes (13), a bottom plate (15) fixed on the inner wall (12), and an outer wall (16) fixed on the inner wall (12); A plurality of inner cavities (14) are circumferentially arranged on the inner wall (12). The plurality of inner cavities (14) and the inner wall (12) are both connected by inclined surfaces; When the swirling flow formed by the clear water and the mixture passes through the plurality of inner cavities (14), the mixture can slide along the inclined surface into the plurality of inner cavities (14), and continuously concentrate in the plurality of inner cavities (14). At the same time, the sewage is thrown out through the plurality of sieve holes (13). When the mixture continuously concentrates and accumulates in the plurality of inner cavities (14), the extrusion between the mixtures can squeeze the sewage out of the inner cavities (14), so that the mixture is concentrated in the plurality of inner cavities (14) after centrifugal filtration; The device further includes a plurality of leakage holes (17) arranged on the bottom plate (15), a funnel (19) provided with a plug (18) capable of blocking the leakage holes (17), and a base (20) fixed on the outer wall (16) and driving the funnel (19) to lift through a cylinder.

2. Application of the tungsten oxide-graphene composite material prepared by the method for preparing tungsten oxide-graphene composite material according to claim 1 in gas detection.

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