CN110560174B - BiOI/C/PANI heterojunction material and preparation method thereof - Google Patents
BiOI/C/PANI heterojunction material and preparation method thereof Download PDFInfo
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- 229920000767 polyaniline Polymers 0.000 title claims abstract description 46
- 239000000463 material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical group [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 27
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 18
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 16
- 239000008103 glucose Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 238000009210 therapy by ultrasound Methods 0.000 claims description 15
- 235000006408 oxalic acid Nutrition 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 9
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical group O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 7
- 238000010335 hydrothermal treatment Methods 0.000 claims description 7
- 229910052740 iodine Inorganic materials 0.000 claims description 7
- 239000011630 iodine Substances 0.000 claims description 7
- 239000002135 nanosheet Substances 0.000 claims description 4
- 229910052797 bismuth Inorganic materials 0.000 claims 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims 6
- 230000000379 polymerizing effect Effects 0.000 claims 2
- 238000010907 mechanical stirring Methods 0.000 claims 1
- 229910000510 noble metal Inorganic materials 0.000 abstract description 4
- 238000011068 loading method Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 5
- 229910021612 Silver iodide Inorganic materials 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 3
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 229940045105 silver iodide Drugs 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000011805 ball Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940073609 bismuth oxychloride Drugs 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
- 238000003889 chemical engineering Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 239000011807 nanoball Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
-
- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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- B01J35/39—
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- B01J35/40—
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- B01J35/51—
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- B01J35/61—
Abstract
The invention discloses a BiOI/C/PANI heterojunction material and a preparation method thereof. Preparing carbon spheres by a one-step hydrothermal method, then loading the BiOI on the carbon spheres by the hydrothermal method, washing and drying. And then preparing the conductive polyaniline by a normal-temperature stirring method, and compounding the conductive polyaniline and the conductive polyaniline to form a heterojunction. The material prepared by the invention has no noble metal, and the preparation method is simple and convenient, has short experimental period and is beneficial to mass production. And the synthesized material is in a nanometer flower spherical shape, the specific surface area is large, and the active sites are exposed more.
Description
Technical Field
The invention relates to a BiOI/C/PANI heterojunction material and a preparation method thereof, belonging to the field of nano-material preparation.
Background
Environmental problems have become one of the focus problems in the world today, and photocatalytic oxidation technology has been receiving much attention in order to effectively degrade industrial waste and improve pollution problems. The photocatalytic semiconductor material plays a crucial role in photocatalytic technology. The current research difficulty is that the photo-generated carriers have short service life and high recombination rate, so that the photocatalytic performance is limited. The current methods for improving the problem mainly comprise nonmetal or metal doping, noble metal deposition, compound semiconductors and the like.
Zhou et al synthesized a composite of silver iodide and bismuth oxychloride to improve the recombination rate of photogenerated carriers by forming heterojunctions [ Zhou C, Lai C, Xu P, et al in Situ growth AgI/Bi12O17Cl2Heterojunction catalysts for visual Light Degradation of sunlight and Mechanism [ J ] ACS sunlight Chemistry & Engineering,2018: assosmeng.7 b04584 ]. Yang et al prepared a composite of bismuth oxyiodide with silver and silver iodide to form a Z-based heterojunction to improve catalytic performance [ Yang Y, Zeng, Zhuotong, Zhang, Chen, et al.construction of iodine variation-rich BiOI/Ag @ AgI Z-scheme heterojunction catalysis for visible-light-drive biochemical degradation [ J ] Chemical Engineering Journal 2018: S1385894718309069 ]. The above methods for improving the photocatalytic performance all involve the participation of noble metals, which limits the batch use of the material.
Disclosure of Invention
The invention aims to provide a BiOI/C/PANI heterojunction material and a preparation method thereof.
The technical solution for realizing the purpose of the invention is as follows: a heterojunction material of BiOI/C/PANI is prepared by loading two-dimensional nanosheets BiOI on carbon spheres, compounding the carbon spheres with strip-shaped polyaniline to form a heterojunction, and mechanically stirring to obtain the heterojunction material;
Wherein, the BiOI is two-dimensional nano-sheet with the width of about 200 nm; the size of the carbon spheres is about 100nm, the polyaniline is strip-shaped, the width is about 50nm, and the mass ratio of C to BiOI to PANI is about 1:9:2, and the mass ratio of C to BiOI to PANI is about 0.5:9: 2.
The preparation method of the BiOI/C/PANI heterojunction material comprises the following steps:
firstly, glucose is dissolved in water and then put in a reaction kettle to be hydrothermally treated for 20 hours at 180 ℃. Then washing and drying the obtained product;
and secondly, putting the carbon spheres obtained in the first step into an ethanol solution, and performing ultrasonic treatment to obtain a homogeneous phase. Dissolving bismuth nitrate pentahydrate in ethylene glycol, dissolving potassium iodide in ethanol, mixing the three dropwise, and heating at 180 deg.C for 6 hr;
thirdly, respectively dissolving aniline, ammonium persulfate and oxalic acid in water, mixing the solution drop by drop, and reacting at normal temperature for 6 hours to obtain dark green polyaniline;
and step four, dissolving the products obtained in the step two and the step three in acetone, performing ultrasonic treatment to form a homogeneous phase, stirring at 45 ℃ until the homogeneous phase is stirred, and collecting a sample to obtain the heterojunction material of the semiconductor BiOI and the PANI by taking the carbon spheres as the template.
Compared with the prior art, the invention has the advantages that: (1) the synthetic material has no noble metal, and the preparation method is simple and convenient, has short experimental period and is beneficial to mass production. (2) The synthesized material is in a nanometer flower ball shape, the specific surface area is large, and the active sites are exposed more.
Drawings
FIG. 1 is a schematic diagram of the preparation method of the BiOI/C/PANI heterojunction material of the invention.
FIG. 2 is a transmission electron micrograph of polyaniline (a) of (b) of the boundary of polyaniline, (C) of a single carbon sphere, (d) of the carbon sphere stack, (e) of BiOI/C of (f) of BiOI/C of another angle, (g) of BiOI/C/PANI of high magnification of transmission electron micrograph, and (h) of BiOI/C/PANI of heterogeneous junction formation, for materials prepared according to comparative example 1, comparative example 2, comparative example 3, and example 2 of the present invention.
FIG. 3 is a scanning electron micrograph of BiOI/C/PANI in example 2 of the present invention.
Fig. 4 is an XRD spectrum of the materials prepared in comparative example 1, comparative example 3 and example 2 of the present invention.
Detailed Description
Firstly, glucose is dissolved in water and then is put in a reaction kettle for hydrothermal treatment for 20 hours at 180 ℃. Then washing and drying the obtained product;
and secondly, putting the carbon spheres obtained in the first step into an ethanol solution, and performing ultrasonic treatment to obtain a homogeneous phase. Dissolving bismuth nitrate pentahydrate in ethylene glycol, dissolving potassium iodide in ethanol, wherein the molar ratio of the bismuth nitrate pentahydrate to the potassium iodide is 1:1, then mixing the bismuth nitrate pentahydrate and the potassium iodide drop by drop, and heating for 6 hours at 180 ℃;
Thirdly, respectively dissolving aniline, oxalic acid and ammonium persulfate in a molar ratio of 1:1:0.3 into water, dropwise mixing, and reacting at normal temperature for 6 hours to obtain dark green polyaniline;
and step four, dissolving the products obtained in the step two and the step three in acetone, performing ultrasonic treatment to form a homogeneous phase, stirring at 45 ℃ until the homogeneous phase is completely stirred, and collecting a sample to obtain the BiOI/C/PANI heterojunction material.
Example 1
In the first step, 16g of glucose is dissolved in 40mL of deionized water, and after the glucose is dissolved, the glucose is placed into a reaction kettle and is subjected to hydrothermal treatment at 180 ℃ for 20 hours. Then washing and drying the obtained product;
and step two, taking 0.01g of the carbon spheres obtained in the step one, putting the carbon spheres into 30mL of ethanol solution, and performing ultrasonic treatment to obtain a homogeneous phase. Dissolving 0.25mmol of bismuth nitrate pentahydrate in 10mL of ethylene glycol and 0.25mmol of potassium iodide in 10mL of ethanol, then mixing the three dropwise, and heating for 6h at 180 ℃;
thirdly, dissolving 1.4mmol of aniline in 0.047mol/L oxalic acid solution (20mL), dissolving 0.53mmol of ammonium persulfate in 0.047mol/L oxalic acid solution (10mL), mixing dropwise, and reacting at normal temperature for 6h to obtain dark green polyaniline;
and step four, respectively dissolving the products obtained in the step two and the step three in 10mL of acetone, performing ultrasonic treatment to form a homogeneous phase, dropwise mixing, stirring at 45 ℃ until the mixture is stirred to be dry, and collecting a sample to obtain the BiOI/C/PANI heterojunction material.
Example 2
In the first step, 16g of glucose is dissolved in 40mL of deionized water, and after the glucose is dissolved, the glucose is placed into a reaction kettle and is subjected to hydrothermal treatment at 180 ℃ for 20 hours. Then washing and drying the obtained product;
and step two, taking 0.005g of the carbon spheres obtained in the step one, putting the carbon spheres into 30mL of ethanol solution, and performing ultrasonic treatment to obtain a homogeneous phase. Dissolving 0.25mmol of bismuth nitrate pentahydrate in 10mL of ethylene glycol and 0.25mmol of potassium iodide in 10mL of ethanol, dropwise mixing the three, and performing hydrothermal treatment at 180 ℃ for 6 hours;
thirdly, dissolving 1.4mmol of aniline in 0.047mol/L oxalic acid solution (20mL), dissolving 0.53mmol of ammonium persulfate in 0.047mol/L oxalic acid solution (10mL), mixing dropwise, and reacting at normal temperature for 6h to obtain dark green polyaniline;
and step four, respectively dissolving the products obtained in the step two and the step three in 10mL of acetone, performing ultrasonic treatment to form a homogeneous phase, dropwise mixing, stirring at 45 ℃ until the mixture is stirred to be dry, and collecting a sample to obtain the BiOI/C/PANI heterojunction material.
Comparative example 1:
in the first step, 1.4mmol of aniline is dissolved in 0.047mol/L oxalic acid solution (20mL), and 0.53mmol of ammonium persulfate is dissolved in 0.047mol/L oxalic acid solution (10 mL);
step two, mixing the two solutions drop by drop, and reacting for 6 hours at normal temperature;
and thirdly, washing and drying the product to obtain dark green polyaniline.
Comparative example 2:
step one, dissolving 16g of glucose in 40mL of deionized water, placing the solution into a reaction kettle, and carrying out hydrothermal treatment at 180 ℃ for 20 hours;
and secondly, washing and drying the obtained product to obtain the carbon spheres.
Comparative example 3:
in the first step, 16g of glucose is dissolved in 40mL of deionized water, and after the glucose is dissolved, the glucose is placed into a reaction kettle and is subjected to hydrothermal treatment at 180 ℃ for 20 hours. Then washing and drying the obtained product;
and step two, taking 0.01g of the carbon spheres obtained in the step one, putting the carbon spheres into 30mL of ethanol solution, and performing ultrasonic treatment to obtain a homogeneous phase. Dissolving 0.25mmol of bismuth nitrate pentahydrate in 10mL of ethylene glycol and 0.25mmol of potassium iodide in 10mL of ethanol, then mixing the three dropwise, and heating for 6h at 180 ℃;
and thirdly, washing and drying the product obtained in the second step to obtain the BiOI/C composite material.
Referring to fig. 2, (a), (b) show that the prepared polyaniline is twisted together in a strip shape of about 50 nm; (c) the (d) shows that the grain diameter of the prepared carbon spheres is relatively uniform and is about 100 nm; (e) (f) showing the prepared BiOI/C material, and the BiOI can be seen to be loaded on the surface of the carbon sphere in a sheet structure; (g) and (h) the prepared novel BiOI/C/PANI material is shown, the lattice line of the BiOI can be clearly seen, and the BiOI, the C and the PANI are closely combined together to form a heterojunction.
With reference to fig. 3, it can be seen that the prepared BiOI/C/PANI composite material is in a shape of nano-ball and has uniform size.
Referring to FIG. 4, the BiOI/C and BiOI/C/PANI materials prepared were in agreement with the standard spectrum of BiOI. The XRD pattern of BiOI/C/PANI was unchanged from that of BiOI, indicating that the loading with PANI did not alter the crystal structure of BiOI. The peak of the carbon spheres was about 21 degrees, weak with respect to the peak of the BiOI, and thus not obvious.
Claims (9)
- The heterojunction material of BiOI/C/PANI is characterized in that two-dimensional nanosheets BiOI are loaded on carbon spheres, the carbon spheres and strip-shaped polyaniline are compounded to form a heterojunction, and the heterojunction material is obtained through mechanical stirring;wherein, the BiOI is two-dimensional nano-sheet with the width of about 200 nm; the size of the carbon spheres is about 100nm, the polyaniline is strip-shaped, the width is about 50nm, and the mass ratio of C to BiOI to PANI is about 1:9: 2;the method comprises the following steps:firstly, dissolving glucose in water, placing the glucose in a reaction kettle, carrying out hydrothermal reaction at 180 ℃, and then washing and drying the obtained product to obtain carbon spheres;secondly, putting the carbon spheres obtained in the first step into an ethanol solution, performing ultrasonic treatment to enable the carbon spheres to be homogeneous, dissolving a bismuth source in ethylene glycol and an iodine source in ethanol, mixing the bismuth source, the ethylene glycol and the iodine source, and performing hydrothermal reaction at 180 ℃;Thirdly, respectively dissolving aniline, ammonium persulfate and oxalic acid in water, then dropwise mixing the solution, and polymerizing at normal temperature to obtain a dark green product;and fourthly, dissolving the products obtained in the second step and the third step in acetone, performing ultrasonic treatment to form a homogeneous phase, and then stirring until the homogeneous phase is stirred to be dry to obtain the BiOI/C/PANI heterojunction material.
- 2. The BiOI/C/PANI heterojunction material of claim 1, wherein the mass ratio is set to C: BiOI: PANI ≈ 0.5:9: 2.
- 3. A method of fabricating a heterojunction material based on the BiOI/C/PANI as claimed in claim 1, comprising the steps of:firstly, dissolving glucose in water, placing the solution in a reaction kettle, carrying out hydrothermal reaction at 180 ℃, and then washing and drying the obtained product to obtain carbon spheres;secondly, putting the carbon spheres obtained in the first step into an ethanol solution, performing ultrasonic treatment to enable the carbon spheres to be homogeneous, dissolving a bismuth source in ethylene glycol and an iodine source in ethanol, mixing the bismuth source, the ethylene glycol and the iodine source, and performing hydrothermal reaction at 180 ℃;thirdly, respectively dissolving aniline, ammonium persulfate and oxalic acid in water, then dropwise mixing the solution, and polymerizing at normal temperature to obtain a dark green product;and fourthly, dissolving the products obtained in the second step and the third step in acetone, performing ultrasonic treatment to form a homogeneous phase, and then stirring until the homogeneous phase is stirred to be dry to obtain the BiOI/C/PANI heterojunction material.
- 4. The process according to claim 3, wherein in the first step the glucose is reacted hydrothermally for 20h at 180 ℃.
- 5. The method of claim 3, wherein in the second step the bismuth source is bismuth nitrate pentahydrate, the iodine source is potassium iodide, and the molar ratio of bismuth source to iodine source is 1: 1.
- 6. the method of claim 3, wherein the specific steps in the second step are ultrasonic treatment of carbon spheres in ethanol for 15-20min to homogeneous phase, dropwise addition of ethylene glycol solution of bismuth nitrate pentahydrate, dropwise addition of ethanol solution of potassium iodide, and hydrothermal treatment at 180 ℃ for 6 h.
- 7. The method of claim 3, wherein in the third step, the molar ratio of aniline, oxalic acid, and ammonium persulfate is 1:1: 0.3.
- 8. The method of claim 3, wherein in the third step, an oxalic acid solution of ammonium persulfate is added dropwise to an oxalic acid solution of aniline, and stirred at normal temperature for 6 hours.
- 9. The method of claim 3, wherein in the fourth step, the solutions obtained in the second and third steps are dissolved in acetone respectively, ultrasonic treatment is carried out for 15-20min until the solution is homogeneous, the acetone solution of polyaniline is added dropwise, and then the solution is stirred in a water bath at 45 ℃ until the solution is stirred to dryness, and the product is collected.
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