CN108774320A - A kind of synthetic method of nickel oxide loaded polyaniline - Google Patents

A kind of synthetic method of nickel oxide loaded polyaniline Download PDF

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Publication number
CN108774320A
CN108774320A CN201810749571.3A CN201810749571A CN108774320A CN 108774320 A CN108774320 A CN 108774320A CN 201810749571 A CN201810749571 A CN 201810749571A CN 108774320 A CN108774320 A CN 108774320A
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China
Prior art keywords
nickel
nickel oxide
oxide loaded
synthetic method
polyaniline
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CN201810749571.3A
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Chinese (zh)
Inventor
汪元元
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New Mstar Technology Ltd In Hefei
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New Mstar Technology Ltd In Hefei
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Priority to CN201810749571.3A priority Critical patent/CN108774320A/en
Publication of CN108774320A publication Critical patent/CN108774320A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/02Polyamines
    • C08G73/026Wholly aromatic polyamines
    • C08G73/0266Polyanilines or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2293Oxides; Hydroxides of metals of nickel

Abstract

The present invention provides a kind of synthetic method of nickel oxide loaded polyaniline, which is characterized in that includes the following steps:In aqueous solution, template is added in nickel salt and aniline monomer dissolving;Aqueous sodium hypochlorite solution or hydrogen peroxide are added dropwise thereto, and is persistently stirred to react 8~24 hours, temperature is room temperature~60 DEG C.The black precipitate obtained after reaction obtains nickel oxide loaded polyaniline powder after washed drying.Present invention process is simple, using common raw material, synthesizes nickel oxide loaded polyaniline structure pattern control at normal temperatures and stablizes, can be used for Electro-Discolor Coating.

Description

A kind of synthetic method of nickel oxide loaded polyaniline
Technical field
The invention belongs to material chemistry technical fields, are related to a kind of synthetic method of nickel oxide loaded polyaniline.
Background technology
Nickel oxide is a kind of important anode electrochromic material, is had on change colour efficiency, switch life, production cost Significant advantage, polyaniline can embody abundant color transfiguration attribute in electrochromic process, and color change interval is enumerated except red Three primary colors other than color.Nickel oxide nanoparticle modification can be generated into collaboration discoloration effect on polyaniline.The prior art synthesizes Oxide nano particles modified polymer material is realized usually using two-step method:I.e. first synthesis oxide nano particle, then will Oxide nano particles are dispersed in in-situ polymerization in polymer monomer.The simultaneously synthesizing nickel oxide of one-step method and polyaniline simultaneously will oxidations Technique of the nano nickel particles modification on polyaniline is rarely reported.
Invention content
The purpose of the present invention is to provide a kind of synthetic methods of nickel oxide loaded polyaniline, which is characterized in that including with Lower step:In aqueous solution, template is added in nickel salt and aniline monomer dissolving;Aqueous sodium hypochlorite solution or dioxygen are added dropwise thereto Water, and be persistently stirred to react 8~24 hours, temperature is room temperature~60 DEG C.The black precipitate obtained after reaction, after washed drying Obtain powder.
The nickel salt includes one kind or combinations thereof in nickel chloride, nickel nitrate, nickel acetate, dense in end reaction solution Degree is 0.01~0.05mol/L;A concentration of 0.04~0.2mol/L of the aniline monomer in end reaction solution;Template is ten One kind or combinations thereof in sodium dialkyl sulfate, neopelex, dodecyl sulphur potassium, Potassium dodecylbenzenesulfonate, A concentration of 0.005mol/L~0.01mol/L in end reaction solution.
The washing is alternately washed with deionized water and ethyl alcohol, is used centrifuge to precipitate or filter each time after washing and is set Standby to be filtered, filtration product is disperseed in deionized water or ethyl alcohol again, and repeated filtration is 7 until filtrate pH value, last It is secondary to be washed with convenient and dry with ethyl alcohol;The drying is dried in 50~80 DEG C of vacuum drying ovens, and vacuum drying condition is true Reciprocal of duty cycle < 133Pa.
Present invention process is simple, using common raw material, synthesizes nickel oxide loaded polyaniline structure pattern control at normal temperatures Stablize, can be used for Electro-Discolor Coating.
Present disclosure and feature have revealed that as above, however the present invention that describes of front only briefly or pertains only to this The specific part of invention, feature of the invention may be more than what content disclosed herein was related to.Therefore, protection model of the invention The revealed content of embodiment should be not limited to by enclosing, and should be included in the combination of all the elements embodied in different piece, with And various replacements and modification without departing substantially from the present invention, and covered by claims of the present invention.
Description of the drawings
Fig. 1 is the SEM photograph that nickel oxide loaded polyaniline is synthesized using (embodiment 1) of the invention.
Specific implementation mode
Embodiment 1
In aqueous solution, 0.005mol/L dodecanes are added in 0.01mol/L nickel chlorides and the dissolving of 0.04mol/L aniline monomers Base sodium sulphate;Aqueous sodium hypochlorite solution is added dropwise thereto, and is persistently stirred to react 8 hours at 60 DEG C.The black obtained after reaction Precipitation, is alternately washed with deionized water and ethyl alcohol, is used centrifuge precipitation or pumping and filtering device to be filtered each time after washing, is filtered Product disperses in deionized water or ethyl alcohol again, and repeated filtration is 7 until filtrate pH value, is washed for the last time with side with ethyl alcohol Just it dries;Nickel oxide loaded polyaniline powder as shown in Figure 1 is obtained after being dried in 60 DEG C of vacuum drying ovens.
Embodiment 2
In aqueous solution, 0.01mol/L dodecyls are added in 0.05mol/L nickel nitrates and the dissolving of 0.2mol/L aniline monomers Benzene sulfonic acid sodium salt;Aqueous sodium hypochlorite solution is added dropwise thereto, and is persistently stirred to react 24 hours in room temperature.The black obtained after reaction Precipitation, is alternately washed with deionized water and ethyl alcohol, is used centrifuge precipitation or pumping and filtering device to be filtered each time after washing, is filtered Product disperses in deionized water or ethyl alcohol again, and repeated filtration is 7 until filtrate pH value, is washed for the last time with side with ethyl alcohol Just it dries;Nickel oxide loaded polyaniline powder is obtained after being dried in 60 DEG C of vacuum drying ovens.
Embodiment 3
In aqueous solution, 0.01mol/L dodecyls are added in 0.02mol/L nickel acetates and the dissolving of 0.1mol/L aniline monomers Sulphur potassium;Hydrogen peroxide is added dropwise thereto, and is persistently stirred to react 10 hours at 50 DEG C.The black precipitate obtained after reaction, spend from Sub- water and ethyl alcohol alternately wash, and use centrifuge precipitation or pumping and filtering device to be filtered each time after washing, filtration product exists again Disperse in deionized water or ethyl alcohol, repeated filtration is 7 until filtrate pH value, is washed for the last time with convenient and dry with ethyl alcohol;? Nickel oxide loaded polyaniline powder is obtained after being dried in 50 DEG C of vacuum drying ovens.
Embodiment 4
In aqueous solution, 0.005mol/L dodecanes are added in 0.04mol/L nickel chlorides and the dissolving of 0.1mol/L aniline monomers Base benzene sulfonic acid potassium;Hydrogen peroxide is added dropwise thereto, and is persistently stirred to react 12 hours at 50 DEG C.The black precipitate obtained after reaction, It is alternately washed with deionized water and ethyl alcohol, uses centrifuge precipitation or pumping and filtering device to be filtered each time after washing, filtration product Again disperse in deionized water or ethyl alcohol, repeated filtration is 7 until filtrate pH value, is washed for the last time with ethyl alcohol dry to facilitate It is dry;Nickel oxide loaded polyaniline powder is obtained after being dried in 80 DEG C of vacuum drying ovens.

Claims (4)

1. a kind of synthetic method of nickel oxide loaded polyaniline, which is characterized in that include the following steps:Nickel salt and aniline monomer are molten In aqueous solution, template is added in solution;Aqueous sodium hypochlorite solution or hydrogen peroxide are added dropwise thereto, and is persistently stirred to react 8~24 Hour, temperature is room temperature~60 DEG C.The black precipitate obtained after reaction obtains powder after washed drying.
2. a kind of synthetic method of nickel oxide loaded polyaniline according to claim 1, it is characterised in that:The nickel salt packet Include one kind or combinations thereof in nickel chloride, nickel nitrate, nickel acetate, a concentration of 0.01~0.05mol/L in end reaction solution; A concentration of 0.04~0.2mol/L of the aniline monomer in end reaction solution;Template is lauryl sodium sulfate, dodecane One kind or combinations thereof in base benzene sulfonic acid sodium salt, dodecyl sulphur potassium, Potassium dodecylbenzenesulfonate, the concentration in end reaction solution For 0.005mol/L~0.01mol/L.
3. a kind of synthetic method of nickel oxide loaded polyaniline as described in claim 1, it is characterised in that:The washing is to use Deionized water and ethyl alcohol alternately wash, and use centrifuge precipitation or pumping and filtering device to be filtered each time after washing, filtration product weight Newly disperse in deionized water or ethyl alcohol, repeated filtration is 7 until filtrate pH value, is washed for the last time with ethyl alcohol dry to facilitate It is dry;The drying is dried in 50~80 DEG C of vacuum drying ovens, and vacuum drying condition is vacuum degree < 133Pa.
4. the oxidation prepared by a kind of synthetic method of nickel oxide loaded polyaniline as described in claims 1 to 3 any one Nickel load polyaniline.
CN201810749571.3A 2018-07-02 2018-07-02 A kind of synthetic method of nickel oxide loaded polyaniline Pending CN108774320A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110105549A (en) * 2019-04-23 2019-08-09 上海萃励电子科技有限公司 A kind of MnO2Load the synthetic method of poly- 3- alkylthrophene
CN110148530A (en) * 2019-06-18 2019-08-20 合肥师范学院 Induced by magnetic field nickel chloride/carbon/polyaniline super capacitor electrode material preparation method

Citations (2)

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Publication number Priority date Publication date Assignee Title
CN102522218A (en) * 2011-12-14 2012-06-27 温州大学 Nano nickel oxide/graphene composite electrode material as well as preparation method and application thereof
CN105037719A (en) * 2015-09-02 2015-11-11 江南大学 Soluble polyaniline synthetic method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102522218A (en) * 2011-12-14 2012-06-27 温州大学 Nano nickel oxide/graphene composite electrode material as well as preparation method and application thereof
CN105037719A (en) * 2015-09-02 2015-11-11 江南大学 Soluble polyaniline synthetic method

Non-Patent Citations (2)

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Title
张磊等: ""乳液聚合法制备聚苯胺及其电容性能研究"", 《化工新型材料》 *
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110105549A (en) * 2019-04-23 2019-08-09 上海萃励电子科技有限公司 A kind of MnO2Load the synthetic method of poly- 3- alkylthrophene
CN110148530A (en) * 2019-06-18 2019-08-20 合肥师范学院 Induced by magnetic field nickel chloride/carbon/polyaniline super capacitor electrode material preparation method
CN110148530B (en) * 2019-06-18 2021-05-25 合肥师范学院 Preparation method of magnetic field induced nickel chloride/polyaniline supercapacitor electrode material

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Application publication date: 20181109