CN107804871A - A kind of preparation method of the compound bismuthic acid zinc nanometer rods of polyaniline - Google Patents
A kind of preparation method of the compound bismuthic acid zinc nanometer rods of polyaniline Download PDFInfo
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- CN107804871A CN107804871A CN201711070604.3A CN201711070604A CN107804871A CN 107804871 A CN107804871 A CN 107804871A CN 201711070604 A CN201711070604 A CN 201711070604A CN 107804871 A CN107804871 A CN 107804871A
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- polyaniline
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Abstract
The invention discloses a kind of preparation method of the compound bismuthic acid zinc nanometer rods of polyaniline, belong to functional material preparing technical field.The preparation method is using sodium bismuthate, zinc acetate and polyaniline as raw material, and argon gas comprises the concrete steps that as carrier gas：Sodium bismuthate is well mixed with zinc acetate first, then the mixed-powder of sodium bismuthate and zinc acetate is placed in the high-temperature region of alundum tube reaction vessel, polyaniline is placed in the low-temperature space of alundum tube reaction vessel, and sealed reaction vessel, by high-temperature region be heated to 1200~1400 DEG C, low-temperature space be heated to 200~300 DEG C, 12~24h is incubated, argon gas flow velocity is 100~200cm3/min.The preparation process that the present invention uses is simple, easily controllable, and the compound bismuthic acid zinc nanometer rods of gained polyaniline have a good application prospect in fields such as electronic device, optics, electrochemical device and lithium ion batteries.
Description
Technical field
The invention belongs to functional material preparing technical field, and in particular to a kind of system of the compound bismuthic acid zinc nanometer rods of polyaniline
Preparation Method.
Background technology
Bismuthic acid zinc nanometer rods have good electricity, optics and chemical property, compound with the polymer phase such as polyaniline, can
Hope and improve its electricity, optics and chemical property, led in electronic device, optics, electrochemical device and lithium ion battery etc.
Domain has a good application prospect, and causes the extensive concern of people.Polymer composite montmorillonoid and layered hydroxide, polymerization
The compound carbon black of thing, polymer composite graphite, polymer composite carbon nanometer tube, polymer compound carbon nanofiber are common polymerizations
Thing composite (Shen Guangxia, Zhuan Yanyan, Lin Chang are good for the progress chemical progress of carbon nano tube-polymer composites,
2014,16(1):21-25.), its preparation method mainly gathers including liquid phase composite method, the co-melting composite algorithm of solid phase, in-situ chemical
(the progress of the western graphenes/polymer composites of Fan Wei, Zhang Chao, Liu Tian is compound for legal and in-situ electrochemical polymerization method
Material journal, 2013,30 (1) 14-21.).However, current polymer complex method still suffers from, preparation process is more complicated, is difficult to
The problems such as preparing the composite of homogeneous performance.
The content of the invention
For overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of compound bismuthic acid zinc nanometer rods of polyaniline
Preparation method.
The preparation method is as follows：
Using sodium bismuthate, zinc acetate and polyaniline as raw material, argon gas first mixes sodium bismuthate with zinc acetate as carrier gas
Uniformly, then the mixed-powder of sodium bismuthate and zinc acetate is placed in the high-temperature region of alundum tube reaction vessel, polyaniline is placed in corundum
The low-temperature space of tube reaction container, and sealed reaction vessel, by high-temperature region be heated to 1200~1400 DEG C, low-temperature space be heated to 200
~300 DEG C, 12~24h is incubated, argon gas flow velocity is 100~200cm3/ min, so as to be obtained in corundum pipe end water cooling end surfaces
Polyaniline compound bismuthic acid zinc nanometer rods.
The mol ratio of the sodium bismuthate and zinc acetate is 38:1.
The weight of the polyaniline accounts for sodium bismuthate, the 15~30% of zinc acetate weight.
The principles of science of the present invention is as follows：
The above-mentioned preparation process of present invention use, sodium bismuthate and zinc acetate mixed-powder are in high-temperature region in 1200~1400 DEG C of quilts
Gaseous state is heated into, sodium bismuthate and zinc acetate are decomposed into bismuth oxide, zinc oxide, sodium oxide molybdena, water and carbon dioxide at high temperature, oxidation
Bismuth and zinc oxide react to form gaseous bismuthic acid zinc at high temperature, and gaseous bismuthic acid zinc is 100~200cm in flow velocity3/ min's
Carrier gas argon gas transports the lower water cooling end surfaces reached positioned at alundum tube reaction vessel end and deposited, and forms bismuthic acid zinc nanocrystalline
Core, bismuthic acid zinc nanocrystalline core absorb atmosphere in bismuthic acid zinc, result in growth of the bismuthic acid zinc in one-dimensional square, with insulation when
Between increase to 12~24h, form the bismuthic acid zinc nanometer rods with certain length in water cooling end surfaces.200~300 DEG C of low-temperature spaces
Polyaniline in flow velocity be 100~200cm3/ min carrier gas argon gas transports the lower water reached positioned at alundum tube reaction vessel end
Cold end surface deposits, and is attached to the surface of bismuthic acid zinc nanometer rods, so as to ultimately form the compound bismuthic acid zinc nanometer of polyaniline
Rod.
Compared with prior art, the present invention has following technique effect：
1st, the preparation method for the compound bismuthic acid zinc nanometer rods of polymer that the present invention uses, preparation process are simple, easily controllable；
2nd, the present invention is using nontoxic sodium bismuthate, zinc acetate and polyaniline, and raw material and preparation process are to environment without dirt
Dye, meets environmental requirement；
3rd, the compound bismuthic acid zinc nanometer rods of polyaniline of the present invention can be used as electricity, optics and electrode material, electronic device,
The fields such as optics, electrochemical device and lithium ion battery have a good application prospect.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the compound bismuthic acid zinc nanometer rods of polyaniline prepared by embodiment 1；
According to JCPDS PDF cards, the gained compound bismuthic acid zinc nanometer rods of polyaniline can be retrieved by a cube ZnBi38O58
(JCPDS cards, card number：42~0183) crystalline phase is formed.
Fig. 2 is transmission electron microscope (TEM) image of the compound bismuthic acid zinc nanometer rods of polyaniline prepared by embodiment 1；
As can be seen from the figure product by the compound bismuthic acid zinc nanometer rods of polyaniline and is attached to the random of nanorod surfaces
Nano particle is formed, and a diameter of 20~100nm of nanometer rods, length are 1~2 μm.
Fig. 3 is the high resolution transmission electron microscopy of the compound bismuthic acid zinc nanometer rods of polyaniline prepared by embodiment 1
(HRTEM) image；
As can be seen from the figure the compound bismuthic acid zinc nanorod inner of polyaniline is clear and uniform lattice fringe, between lattice
Away from for 0.72nm, corresponding to a cube ZnBi38O58{ 110 } crystal face, the random pattern of surface attachment amorphous polyaniline (white
Shown in arrow), show the compound bismuthic acid zinc nanometer rods of polyaniline by the poly- of the internal good random pattern of mono-crystalline structures and surface
Aniline particle is formed.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment, but the present invention is not limited to following embodiments.
Embodiment 1
Sodium bismuthate is well mixed with zinc acetate first, wherein the mol ratio of sodium bismuthate and zinc acetate is 38:1, then will
The mixed-powder of sodium bismuthate and zinc acetate is placed in the high-temperature region of alundum tube reaction vessel, and polyaniline is placed in alundum tube reaction vessel
Low-temperature space, the weight of polyaniline accounts for sodium bismuthate, the 30% of zinc acetate weight, and seals alundum tube, and high-temperature region is heated into temperature
1400 DEG C, low-temperature space be heated to 300 DEG C, be incubated 24h, argon gas flow velocity is 200cm3/ min, so as at corundum pipe end water cooling end
Surface has obtained a diameter of 20~100nm of nanometer rods, length is 1~2 μm, the polyphenyl of the random polyaniline particles of surface attachment
The compound bismuthic acid zinc nanometer rods of amine.
Embodiment 2
Sodium bismuthate is well mixed with zinc acetate first, wherein the mol ratio of sodium bismuthate and zinc acetate is 38:1, then will
The mixed-powder of sodium bismuthate and zinc acetate is placed in the high-temperature region of alundum tube reaction vessel, and polyaniline is placed in alundum tube reaction vessel
Low-temperature space, the weight of polyaniline accounts for sodium bismuthate, the 15% of zinc acetate weight, and seals alundum tube, and high-temperature region is heated into temperature
1200 DEG C, low-temperature space be heated to 200 DEG C, be incubated 12h, argon gas flow velocity is 100cm3/ min, so as at corundum pipe end water cooling end
Surface has obtained a diameter of 20~100nm of nanometer rods, length is 1~2 μm, the polyphenyl of the random polyaniline particles of surface attachment
The compound bismuthic acid zinc nanometer rods of amine.
Embodiment 3
Sodium bismuthate is well mixed with zinc acetate first, wherein the mol ratio of sodium bismuthate and zinc acetate is 38:1, then will
The mixed-powder of sodium bismuthate and zinc acetate is placed in the high-temperature region of alundum tube reaction vessel, and polyaniline is placed in alundum tube reaction vessel
Low-temperature space, the weight of polyaniline accounts for sodium bismuthate, the 16% of zinc acetate weight, and seals alundum tube, and high-temperature region is heated into temperature
1220 DEG C, low-temperature space be heated to 210 DEG C, be incubated 13h, argon gas flow velocity is 120cm3/ min, so as at corundum pipe end water cooling end
Surface has obtained a diameter of 20~100nm of nanometer rods, length is 1~2 μm, the polyphenyl of the random polyaniline particles of surface attachment
The compound bismuthic acid zinc nanometer rods of amine.
Embodiment 4
Sodium bismuthate is well mixed with zinc acetate first, wherein the mol ratio of sodium bismuthate and zinc acetate is 38:1, then will
The mixed-powder of sodium bismuthate and zinc acetate is placed in the high-temperature region of alundum tube reaction vessel, and polyaniline is placed in alundum tube reaction vessel
Low-temperature space, the weight of polyaniline accounts for sodium bismuthate, the 18% of zinc acetate weight, and seals alundum tube, and high-temperature region is heated into temperature
1250 DEG C, low-temperature space be heated to 230 DEG C, be incubated 15h, argon gas flow velocity is 140cm3/ min, so as at corundum pipe end water cooling end
Surface has obtained a diameter of 20~100nm of nanometer rods, length is 1~2 μm, the polyphenyl of the random polyaniline particles of surface attachment
The compound bismuthic acid zinc nanometer rods of amine.
Embodiment 5
Sodium bismuthate is well mixed with zinc acetate first, wherein the mol ratio of sodium bismuthate and zinc acetate is 38:1, then will
The mixed-powder of sodium bismuthate and zinc acetate is placed in the high-temperature region of alundum tube reaction vessel, and polyaniline is placed in alundum tube reaction vessel
Low-temperature space, the weight of polyaniline accounts for sodium bismuthate, the 21% of zinc acetate weight, and seals alundum tube, and high-temperature region is heated into temperature
1280 DEG C, low-temperature space be heated to 250 DEG C, be incubated 17h, argon gas flow velocity is 150cm3/ min, so as at corundum pipe end water cooling end
Surface has obtained a diameter of 20~100nm of nanometer rods, length is 1~2 μm, the polyphenyl of the random polyaniline particles of surface attachment
The compound bismuthic acid zinc nanometer rods of amine.
Embodiment 6
Sodium bismuthate is well mixed with zinc acetate first, wherein the mol ratio of sodium bismuthate and zinc acetate is 38:1, then will
The mixed-powder of sodium bismuthate and zinc acetate is placed in the high-temperature region of alundum tube reaction vessel, and polyaniline is placed in alundum tube reaction vessel
Low-temperature space, the weight of polyaniline accounts for sodium bismuthate, the 24% of zinc acetate weight, and seals alundum tube, and high-temperature region is heated into temperature
1310 DEG C, low-temperature space be heated to 260 DEG C, be incubated 19h, argon gas flow velocity is 170cm3/ min, so as at corundum pipe end water cooling end
Surface has obtained a diameter of 20~100nm of nanometer rods, length is 1~2 μm, the polyphenyl of the random polyaniline particles of surface attachment
The compound bismuthic acid zinc nanometer rods of amine.
Embodiment 7
Sodium bismuthate is well mixed with zinc acetate first, wherein the mol ratio of sodium bismuthate and zinc acetate is 38:1, then will
The mixed-powder of sodium bismuthate and zinc acetate is placed in the high-temperature region of alundum tube reaction vessel, and polyaniline is placed in alundum tube reaction vessel
Low-temperature space, the weight of polyaniline accounts for sodium bismuthate, the 26% of zinc acetate weight, and seals alundum tube, and high-temperature region is heated into temperature
1350 DEG C, low-temperature space be heated to 280 DEG C, be incubated 21h, argon gas flow velocity is 180cm3/ min, so as at corundum pipe end water cooling end
Surface has obtained a diameter of 20~100nm of nanometer rods, length is 1~2 μm, the polyphenyl of the random polyaniline particles of surface attachment
The compound bismuthic acid zinc nanometer rods of amine.
Embodiment 8
Sodium bismuthate is well mixed with zinc acetate first, wherein the mol ratio of sodium bismuthate and zinc acetate is 38:1, then will
The mixed-powder of sodium bismuthate and zinc acetate is placed in the high-temperature region of alundum tube reaction vessel, and polyaniline is placed in alundum tube reaction vessel
Low-temperature space, the weight of polyaniline accounts for sodium bismuthate, the 29% of zinc acetate weight, and seals alundum tube, and high-temperature region is heated into temperature
1380 DEG C, low-temperature space be heated to 290 DEG C, be incubated 23h, argon gas flow velocity is 190cm3/ min, so as at corundum pipe end water cooling end
Surface has obtained a diameter of 20~100nm of nanometer rods, length is 1~2 μm, the polyphenyl of the random polyaniline particles of surface attachment
The compound bismuthic acid zinc nanometer rods of amine.
Claims (1)
1. a kind of preparation method of the compound bismuthic acid zinc nanometer rods of polyaniline, it is characterised in that the preparation method is as follows：
Using sodium bismuthate, zinc acetate and polyaniline as raw material, argon gas first mixes sodium bismuthate with zinc acetate as carrier gas
It is even, then the mixed-powder of sodium bismuthate and zinc acetate is placed in the high-temperature region of alundum tube reaction vessel, polyaniline is placed in alundum tube
The low-temperature space of reaction vessel, and sealed reaction vessel, by high-temperature region be heated to 1200~1400 DEG C, low-temperature space be heated to 200~
300 DEG C, 12~24h is incubated, argon gas flow velocity is 100~200cm3/ min, so as to be obtained in corundum pipe end water cooling end surfaces
The compound bismuthic acid zinc nanometer rods of polyaniline；
The mol ratio of the sodium bismuthate and zinc acetate is 38:1；
The weight of the polyaniline accounts for sodium bismuthate, the 15~30% of zinc acetate weight.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109603805A (en) * | 2018-12-28 | 2019-04-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of antimony bismuthic acid zinc self-assembled nanometer stick of self supporting structure and products thereof and application |
| CN112456554A (en) * | 2020-11-30 | 2021-03-09 | 安徽工业大学 | Preparation method of polymer composite copper vanadate nanobelt |
| CN113955800A (en) * | 2021-12-03 | 2022-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of self-assembled zinc antimonate nanorod with self-curling structure, product and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109603805A (en) * | 2018-12-28 | 2019-04-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of antimony bismuthic acid zinc self-assembled nanometer stick of self supporting structure and products thereof and application |
| CN109603805B (en) * | 2018-12-28 | 2021-07-20 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of self-supporting zinc antimonate self-assembled nanorod, product and application thereof |
| CN112456554A (en) * | 2020-11-30 | 2021-03-09 | 安徽工业大学 | Preparation method of polymer composite copper vanadate nanobelt |
| CN112456554B (en) * | 2020-11-30 | 2022-06-14 | 安徽工业大学 | Preparation method of polymer composite copper vanadate nanobelt |
| CN113955800A (en) * | 2021-12-03 | 2022-01-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of self-assembled zinc antimonate nanorod with self-curling structure, product and application thereof |
| CN113955800B (en) * | 2021-12-03 | 2024-02-13 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of self-assembled zinc antimonate bismuth nanorod with self-curling structure, product and application thereof |
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