CN106000412B - A kind of preparation method of sodium tantalate based composites - Google Patents
A kind of preparation method of sodium tantalate based composites Download PDFInfo
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- CN106000412B CN106000412B CN201610452719.8A CN201610452719A CN106000412B CN 106000412 B CN106000412 B CN 106000412B CN 201610452719 A CN201610452719 A CN 201610452719A CN 106000412 B CN106000412 B CN 106000412B
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 109
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 109
- 239000011734 sodium Substances 0.000 title claims abstract description 109
- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 59
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 26
- 239000000725 suspension Substances 0.000 claims abstract description 26
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 25
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000013459 approach Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 20
- 238000007146 photocatalysis Methods 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 238000005215 recombination Methods 0.000 abstract 1
- 230000006798 recombination Effects 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 22
- 239000003643 water by type Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 20
- 239000002904 solvent Substances 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 12
- 239000007795 chemical reaction product Substances 0.000 description 11
- 235000019441 ethanol Nutrition 0.000 description 11
- 238000013019 agitation Methods 0.000 description 10
- 238000002604 ultrasonography Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 150000001875 compounds Chemical class 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- LRPWSMQGXLANTG-UHFFFAOYSA-M iodogallium Chemical compound I[Ga] LRPWSMQGXLANTG-UHFFFAOYSA-M 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8476—Tantalum
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/009—Preparation by separation, e.g. by filtration, decantation, screening
Abstract
The present invention provides a kind of preparation methods of sodium tantalate based composites, include the following steps：One, tantalum pentoxide powder is added in sodium hydrate aqueous solution and is stirred by ultrasonic uniformly, then carried out hydro-thermal reaction, sodium tantalate powder is obtained after dry；Two, sodium tantalate powder and graphene oxide are added in deionized water, suspension is obtained after ultrasonic disperse is uniform；Three, rotary evaporation drying process is carried out, sodium tantalate based composites are obtained.Recombination process of the present invention is simple, and composite effect is good, and the photocatalysis performance of made sodium tantalate based composites is obviously improved, and the usage amount of graphene can be greatly reduced, to reduce composite cost.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of preparation method of sodium tantalate based composites.
Background technology
Environmental pollution and energy shortage problem have become the current two big bottlenecks for restricting human social development, using partly leading
Body photocatalysis technology realizes that the Efficient Conversion of solar energy utilizes the effective way for being this two hang-up of solution.People have been directed to half
Conductor photocatalysis has carried out numerous studies, and has developed a variety of catalysis materials, have research point out to have special layer structure or
The tantalate photocatalyst of column structure has excellent photocatalytic activity and good chemical stability, in photocatalytic cleavage
There is some superiority, therefore before photocatalysis field has wide application in deionization aquatic products hydrogen and degradable organic pollutant
Scape.Wherein, sodium tantalate is the tantalic acid salt material with most strong photocatalytic activity, and sodium tantalate has perovskite structure, by TaO6
Octahedron is constituted, and conduction band is mainly made of Ta 5d tracks, under ultraviolet light, even if the case where no co-catalyst loads
Very high photocatalytic cleavage deionized water activity can also be shown down.The activity of photochemical catalyst is heavily dependent on light and urges
Change the separative efficiency of the photo-generate electron-hole pair generated in the process, and sodium tantalate conduction band is limited to the capture ability of light induced electron,
It is easy to happen the compound again of photo-generate electron-hole, therefore how by promoting electron-hole separative efficiency to further increase tantalum
The photocatalysis efficiency of sour sodium is the technical barrier for needing to solve at present.
Graphene oxide has excellent electronic transport performance and surface chemistry as a kind of novel two-dimentional carbon-based material
Performance can effectively carry out the transmission of electronics, hole, and in addition the bigger serface of graphene oxide is conducive to photocatalytic process
The absorption of middle organic pollution, so that point of its composite material adsorption efficiency in the photocatalytic process, photo-generated carrier
It is greatly improved from efficiency and photocatalysis efficiency.Therefore, the effective compound of graphene oxide and sodium tantalate material is realized,
The transmission for contributing to photo-generate electron-hole in sodium tantalate is the effective means for promoting sodium tantalate catalytic performance.
Invention content
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, providing, a kind of sodium tantalate base is multiple
The preparation method of condensation material.This method by the way that sodium tantalate powder and graphene oxide are sufficiently mixed in deionized water solution,
Again solvent is dried to obtain by way of rotary evaporation, the composite effect of sodium tantalate powder and graphene oxide can be made more
It is good, to improve the photocatalysis performance of sodium tantalate based composites.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of preparation of sodium tantalate based composites
Method, which is characterized in that this approach includes the following steps：
It is stirred by ultrasonic uniformly, then in temperature Step 1: tantalum pentoxide powder is added in sodium hydrate aqueous solution
Hydro-thermal reaction 2h~20h under conditions of being 120 DEG C~180 DEG C obtains sodium tantalate powder after dry；
Step 2: sodium tantalate powder described in step 1 and graphene oxide are added in deionized water, ultrasonic disperse is equal
Suspension is obtained after even；
Step 3: carrying out rotary evaporation drying process to suspension described in step 2, sodium tantalate based composites are obtained.
A kind of preparation method of above-mentioned sodium tantalate based composites, which is characterized in that sodium hydroxide described in step 1
A concentration of 0.2mol/L~0.6mol/L of aqueous solution.
A kind of preparation method of above-mentioned sodium tantalate based composites, which is characterized in that five oxidation two described in step 1
The molar ratio of tantalum powder body and sodium hydroxide in sodium hydrate aqueous solution is 1: (8~24).
A kind of preparation method of above-mentioned sodium tantalate based composites, which is characterized in that tantalic acid sodium powder described in step 2
The mass ratio of body and graphene oxide is 1: (0.03~0.08).
A kind of preparation method of above-mentioned sodium tantalate based composites, which is characterized in that tantalic acid sodium powder described in step 2
Body and the mass ratio of deionized water are (0.001~0.1): 1.
A kind of preparation method of above-mentioned sodium tantalate based composites, which is characterized in that rotary evaporation described in step 3
Temperature be 50 DEG C~70 DEG C.
Graphene oxide of the present invention is all made of conventional Hummer methods and prepares, because of preparation method maturation, the present invention
In be not described in detail.
Compared with the prior art, the present invention has the following advantages：
1, the present invention uses rotary evaporation as drying process, compared to the method that conventional heating dries solvent, not only
The photocatalysis performance of composite material can be effectively improved, moreover it is possible to reduce the dosage of graphene oxide.
2, rotary evaporation of the present invention carries out under negative pressure.The operating method of rotary evaporation is to evaporitic environment
Negative pressure is carried out at a lower temperature to be evaporated solution to reduce the boiling point of solvent.It is molten in evaporation process
Liquid is also always maintained at rotation disturbance state, is more advantageous to the mixing of suspension, it is made to be not easy to precipitate.
Invention is further described in detail with reference to the accompanying drawings and examples.
Description of the drawings
Fig. 1 is the XRD diagram of 1 sodium tantalate powder of comparative example of the present invention.
Fig. 2 is the SEM photograph of 1 sodium tantalate powder of comparative example of the present invention.
Fig. 3 is the UV-Vis absorption spectrums of 1 sodium tantalate powder of comparative example of the present invention.
Fig. 4 is 1 sodium tantalate powder of 1-3 of the embodiment of the present invention and comparative example 2-4 sodium tantalates based composites and comparative example
Carry out the comparison of test results figure of photocatalytic degradation of dye experiment.
Specific implementation mode
Embodiment 1
The preparation method of the present embodiment sodium tantalate based composites includes the following steps：
Step 1: 0.64g sodium hydroxides are dissolved in 40mL deionized waters, 0.441g tantalum pentoxides, ultrasound is added
20min is mixed, then continues at and carries out hydro-thermal reaction in water heating kettle, hydrothermal temperature is 140 DEG C, and the hydro-thermal time is 12h.Hydro-thermal reaction
Reaction product is cleaned with deionized water and ethyl alcohol afterwards, sodium tantalate powder is obtained after dry；
Step 2: taking 0.5g sodium tantalates powder and mass fraction for the graphene oxide of sodium tantalate powder 3% respectively, it is added
In 50mL deionized waters, ultrasonic agitation is sufficiently mixed uniformly to the two, obtains suspension；
Step 3: suspension described in step 2 is transferred in rotary evaporator, in the case where temperature is 60 DEG C of condition of negative pressure
Solvent is volatilized completely dry, obtains sodium tantalate based composites.
Embodiment 2
The preparation method of the present embodiment sodium tantalate based composites includes the following steps：
Step 1: 0.64g sodium hydroxides are dissolved in 40mL deionized waters, 0.441g tantalum pentoxides, ultrasound is added
20min is mixed, then continues at and carries out hydro-thermal reaction in water heating kettle, hydrothermal temperature is 140 DEG C, and the hydro-thermal time is 12h.Hydro-thermal reaction
Reaction product is cleaned with deionized water and ethyl alcohol afterwards, sodium tantalate powder is obtained after dry；
Step 2: taking 0.5g sodium tantalates powder and mass fraction for the graphene oxide of sodium tantalate powder 5% respectively, it is added
In 50mL deionized waters, ultrasonic agitation is sufficiently mixed uniformly to the two, obtains suspension；
Step 3: suspension described in step 2 is transferred in rotary evaporator, in the case where temperature is 60 DEG C of condition of negative pressure
Solvent is volatilized completely dry, obtains sodium tantalate based composites.
Embodiment 3
The preparation method of the present embodiment sodium tantalate based composites includes the following steps：
Step 1: 0.64g sodium hydroxides are dissolved in 40mL deionized waters, 0.441g tantalum pentoxides, ultrasound is added
20min is mixed, then continues at and carries out hydro-thermal reaction in water heating kettle, hydrothermal temperature is 140 DEG C, and the hydro-thermal time is 12h.Hydro-thermal reaction
Reaction product is cleaned with deionized water and ethyl alcohol afterwards, sodium tantalate powder is obtained after dry；
Step 2: taking 0.5g sodium tantalates powder and mass fraction for the graphene oxide of sodium tantalate powder 8% respectively, it is added
In 50mL deionized waters, ultrasonic agitation is sufficiently mixed uniformly to the two, obtains suspension；
Step 3: suspension described in step 2 is transferred in rotary evaporator, in the case where temperature is 60 DEG C of condition of negative pressure
Solvent is volatilized completely dry, obtains sodium tantalate based composites.
Embodiment 4
The preparation method of the present embodiment sodium tantalate based composites includes the following steps：
Step 1: 0.8g sodium hydroxides are dissolved in 40mL deionized waters, 0.441g tantalum pentoxides are added, ultrasound is mixed
20min is closed, then continues at and carries out hydro-thermal reaction in water heating kettle, hydrothermal temperature is 120 DEG C, and the hydro-thermal time is 20h.After hydro-thermal reaction
Reaction product is cleaned with deionized water and ethyl alcohol, sodium tantalate powder is obtained after dry；
Step 2: taking 1g sodium tantalates powder and mass fraction for the graphene oxide of sodium tantalate powder 3% respectively, it is added
In 50mL deionized waters, ultrasonic agitation is sufficiently mixed uniformly to the two, obtains suspension；
Step 3: suspension described in step 2 is transferred in rotary evaporator, in the case where temperature is 70 DEG C of condition of negative pressure
Solvent is volatilized completely dry, obtains sodium tantalate based composites.
Embodiment 5
The preparation method of the present embodiment sodium tantalate based composites includes the following steps：
Step 1: 0.4g sodium hydroxides are dissolved in 40mL deionized waters, 0.441g tantalum pentoxides are added, ultrasound is mixed
20min is closed, then continues at and carries out hydro-thermal reaction in water heating kettle, hydrothermal temperature is 180 DEG C, and the hydro-thermal time is 4h.After hydro-thermal reaction
Reaction product is cleaned with deionized water and ethyl alcohol, sodium tantalate powder is obtained after dry；
Step 2: taking 0.2g sodium tantalates powder and mass fraction for the graphene oxide of sodium tantalate powder 8% respectively, it is added
In 50mL deionized waters, ultrasonic agitation is sufficiently mixed uniformly to the two, obtains suspension；
Step 3: suspension described in step 2 is transferred in rotary evaporator, in the case where temperature is 60 DEG C of condition of negative pressure
Solvent is volatilized completely dry, obtains sodium tantalate based composites.
Embodiment 6
The preparation method of the present embodiment sodium tantalate based composites includes the following steps：
Step 1: 0.32g sodium hydroxides are dissolved in 40mL deionized waters, 0.441g tantalum pentoxides, ultrasound is added
20min is mixed, then continues at and carries out hydro-thermal reaction in water heating kettle, hydrothermal temperature is 180 DEG C, and the hydro-thermal time is 2h.Hydro-thermal reaction
Reaction product is cleaned with deionized water and ethyl alcohol afterwards, sodium tantalate powder is obtained after dry；
Step 2: 0.05g sodium tantalates powder and mass fraction is taken to add for the graphene oxide of sodium tantalate powder 8% respectively
Enter in 50mL deionized waters, ultrasonic agitation is sufficiently mixed uniformly to the two, obtains suspension；
Step 3: suspension described in step 2 is transferred in rotary evaporator, in the case where temperature is 60 DEG C of condition of negative pressure
Solvent is volatilized completely dry, obtains sodium tantalate based composites.
Embodiment 7
The preparation method of the present embodiment sodium tantalate based composites includes the following steps：
Step 1: 0.96g sodium hydroxides are dissolved in 40mL deionized waters, 0.441g tantalum pentoxides, ultrasound is added
20min is mixed, then continues at and carries out hydro-thermal reaction in water heating kettle, hydrothermal temperature is 120 DEG C, and the hydro-thermal time is 8h.Hydro-thermal reaction
Reaction product is cleaned with deionized water and ethyl alcohol afterwards, sodium tantalate powder is obtained after dry；
Step 2: taking 5g sodium tantalates powder and mass fraction for the graphene oxide of sodium tantalate powder 8% respectively, it is added
In 50mL deionized waters, ultrasonic agitation is sufficiently mixed uniformly to the two, obtains suspension；
Step 3: suspension described in step 2 is transferred in rotary evaporator, in the case where temperature is 50 DEG C of condition of negative pressure
Solvent is volatilized completely dry, obtains sodium tantalate based composites.
Comparative example 1
Material prepared by this comparative example is sodium tantalate powder, and preparation method is：
0.64g sodium hydroxides are dissolved in 40mL deionized waters, 0.441g tantalum pentoxides, ultrasonic mixing is added
20min is then continued at and is carried out hydro-thermal reaction in water heating kettle, and hydrothermal temperature is 140 DEG C, and the hydro-thermal time is 12h.It is used after hydro-thermal reaction
Deionized water and ethyl alcohol clean reaction product, and sodium tantalate powder is obtained after dry.
Fig. 1 show the XRD diagram of sodium tantalate powder, and the powder obtained as seen from Figure 1 is sodium tantalate pure phase；Fig. 2 institutes
The SEM figures of sodium tantalate powder are shown as, the powder obtained as seen from Figure 2 has cube appearance, and grain size is submicron order,
Fig. 3 show the UV-Vis absorption spectrums of sodium tantalate powder, and the energy gap of sodium tantalate powder is about as seen from Figure 3
3.6eV。
Comparative example 2
The preparation method of this comparative example sodium tantalate based composites includes the following steps：
Step 1: 0.64g sodium hydroxides are dissolved in 40mL deionized waters, 0.441g tantalum pentoxides, ultrasound is added
20min is mixed, then continues at and carries out hydro-thermal reaction in water heating kettle, hydrothermal temperature is 140 DEG C, and the hydro-thermal time is 12h.Hydro-thermal reaction
Reaction product is cleaned with deionized water and ethyl alcohol afterwards, sodium tantalate powder is obtained after dry；
Step 2: taking 0.5g sodium tantalates powder and mass fraction for the graphene oxide of sodium tantalate powder 3% respectively, it is added
In 50mL deionized waters, ultrasonic agitation makes the two be sufficiently mixed uniformly, obtains suspension；
Step 3: solvent to be volatilized to dry for 95 DEG C suspension described in step 2 completely under normal pressure, sodium tantalate base is obtained
Composite material.
Comparative example 3
The preparation method of this comparative example sodium tantalate based composites includes the following steps：
Step 1: 0.64g sodium hydroxides are dissolved in 40mL deionized waters, 0.441g tantalum pentoxides, ultrasound is added
20min is mixed, then continues at and carries out hydro-thermal reaction in water heating kettle, hydrothermal temperature is 140 DEG C, and the hydro-thermal time is 12h.Hydro-thermal reaction
Reaction product is cleaned with deionized water and ethyl alcohol afterwards, sodium tantalate powder is obtained after dry；
Step 2: taking 0.5g sodium tantalates powder and mass fraction for the graphene oxide of sodium tantalate powder 5% respectively, it is added
In 50mL deionized waters, ultrasonic agitation makes the two be sufficiently mixed uniformly, obtains suspension；
Step 3: it is dry that lower 95 DEG C of suspension normal pressure described in step 2 is volatilized solvent completely, it is multiple to obtain sodium tantalate base
Condensation material.
Comparative example 4
The preparation method of this comparative example sodium tantalate based composites includes the following steps：
Step 1: 0.64g sodium hydroxides are dissolved in 40mL deionized waters, 0.441g tantalum pentoxides, ultrasound is added
20min is mixed, then continues at and carries out hydro-thermal reaction in water heating kettle, hydrothermal temperature is 140 DEG C, and the hydro-thermal time is 12h.Hydro-thermal reaction
Reaction product is cleaned with deionized water and ethyl alcohol afterwards, sodium tantalate powder is obtained after dry；
Step 2: taking 0.5g sodium tantalates powder and mass fraction for the graphene oxide of sodium tantalate powder 8% respectively, it is added
In 50mL deionized waters, ultrasonic agitation makes the two be sufficiently mixed uniformly, obtains suspension；
Step 3: it is dry that lower 95 DEG C of suspension normal pressure described in step 2 is volatilized solvent completely, it is multiple to obtain sodium tantalate base
Condensation material.
The application of sodium tantalate based composites of the present invention is as follows：
Photocatalytic degradation of dye：Using under full spectrum (400W Iodine gallium lights) illumination condition, sodium tantalate based composites are to first
The degradation rate of base orange (MO) assesses its photocatalytic activity.
The sodium tantalate based composites (embodiment 1-3, comparative example 2-4) or sodium tantalate powder (comparative example 1) of 100mg are added
Enter in 100mL methyl oranges deionized water solution (10mg/L), 30min is stirred to reach adsorption equilibrium in dark place in a reservoir.Then,
Photocatalysis performance test is carried out under light illumination, is taken out 5mL solution examples after illumination 1h, after the solution taken is centrifuged, is taken upper layer
Clear liquid measures absorption spectrum using spectrophotometer (Hitachi U-3010), and according to the characteristic absorption at methyl orange 464nm
The relative concentration of methyl orange in solution is calculated in peak intensity.
Photocatalysis effect is as shown in Figure 4.When carrying out photocatalysis using individual sodium tantalate it can be seen from Fig. 4, illumination
It is 43% (comparative example 1) that 1h, which waits remaining MO ratios, obtained composite material is dried for lower 95 DEG C using normal pressure, in different composite ratio
It is 30% (comparative example 2), 24% (comparative example 3), 27% (comparative example 4), it can be seen that tantalic acid that the lower 1h of example, which waits remaining MO ratios,
Its photocatalysis performance can be improved after sodium and graphene oxide are compound, and preferably compositely proportional is 5% mass in comparative example 3
The graphene oxide compound quantity of score (compared with sodium tantalate).
And the composite material of 60 DEG C of drying of rotary evaporation under negative pressure is used, 1h waits remaining MO ratios under different composite ratio
Example is 15% (embodiment 1), 17% (embodiment 2), 20% (embodiment 3), and the photocatalysis performance under all compositely proportionals is bright
Aobvious lower 95 DEG C of the corresponding normal pressure that is better than dries obtained composite material, and preferably compositely proportional is 3% mass in embodiment 1
The graphene oxide compound quantity of score (compared with sodium tantalate), the point also illustrate answering using 60 DEG C of drying of rotary evaporation under negative pressure
The more excellent compositely proportional of condensation material, which will be less than lower 95 DEG C of normal pressure, dries obtained composite material, this is beneficial to reduce graphite oxide
The usage amount of alkene, to reduce the cost of composite material.
The above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention.It is every according to invention skill
Art essence still falls within technical solution of the present invention to any simple modification, change and equivalence change made by above example
Protection domain in.
Claims (4)
1. a kind of preparation method of sodium tantalate based composites, which is characterized in that this approach includes the following steps：
It is stirred by ultrasonic uniformly Step 1: tantalum pentoxide powder is added in sodium hydrate aqueous solution, is then 120 in temperature
DEG C~180 DEG C under conditions of hydro-thermal reaction 2h~20h, obtain sodium tantalate powder after dry；
Step 2: sodium tantalate powder described in step 1 and graphene oxide are added in deionized water, after ultrasonic disperse is uniform
Obtain suspension；The mass ratio of the sodium tantalate powder and graphene oxide is 1: (0.03~0.08)；
Step 3: carrying out rotary evaporation drying process to suspension described in step 2, sodium tantalate based composites are obtained；It is described
Rotary evaporation carries out under negative pressure, and the temperature of the rotary evaporation is 50 DEG C~70 DEG C.
2. a kind of preparation method of sodium tantalate based composites according to claim 1, which is characterized in that institute in step 1
State a concentration of 0.2mol/L~0.6mol/L of sodium hydrate aqueous solution.
3. a kind of preparation method of sodium tantalate based composites according to claim 1, which is characterized in that institute in step 1
The molar ratio for stating tantalum pentoxide powder and sodium hydroxide in sodium hydrate aqueous solution is 1: (8~24).
4. a kind of preparation method of sodium tantalate based composites according to claim 1, which is characterized in that institute in step 2
The mass ratio for stating sodium tantalate powder and deionized water is (0.001~0.1): 1.
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