CN110098069A - A kind of RuO2Load the synthetic method of poly-1-aminoanthraquinone - Google Patents

A kind of RuO2Load the synthetic method of poly-1-aminoanthraquinone Download PDF

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Publication number
CN110098069A
CN110098069A CN201910379128.6A CN201910379128A CN110098069A CN 110098069 A CN110098069 A CN 110098069A CN 201910379128 A CN201910379128 A CN 201910379128A CN 110098069 A CN110098069 A CN 110098069A
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China
Prior art keywords
poly
aminoanthraquinone
ruo
load
synthetic method
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CN201910379128.6A
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Chinese (zh)
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陆嘉君
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Shanghai Li Li Electronic Technology Co Ltd
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Shanghai Li Li Electronic Technology Co Ltd
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Priority to CN201910379128.6A priority Critical patent/CN110098069A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/46Metal oxides
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/48Conductive polymers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)

Abstract

The present invention provides a kind of RuO2Load the synthetic method of poly-1-aminoanthraquinone, which comprises the following steps: 1- amino anthraquinones monomer is dissolved in deionized water, KI and RuI is added3, ultrasonic agitation dissolution;It is slowly added in hypochloric acid water solution, is persistently stirred in adition process, room temperature~40 DEG C are precipitated after standing reaction 8~12 hours, dry to obtain RuO through filtration washing2Load the poly-1-aminoanthraquinone powder of I2 doping.Present invention process polyvinyl chloride is easy, and situ study synthesizes RuO under room temperature2Uniform load poly-1-aminoanthraquinone, and I simultaneously2Doping to poly-1-aminoanthraquinone, can be used for super capacitance electrode material.

Description

A kind of RuO2Load the synthetic method of poly-1-aminoanthraquinone
Technical field
The invention belongs to material chemistry technical fields, are related to a kind of RuO2Load the synthetic method of poly-1-aminoanthraquinone.
Background technique
Poly-1-aminoanthraquinone is a kind of conjugated polymer with function groups, has trapezoidal conjugate ring, amino, benzoquinonyl Equal functional groups, have good electro-chemical activity.Electrically conductive polyaniline skeleton and quinone redox in poly-1-aminoanthraquinone molecule Active group makes its theoretical fake capacitance with higher, can be used for electrochemical capacitance electrode material.Intrinsic poly-1-aminoanthraquinone conductance Rate is very low, can promote conductivity by I2 doping.Ruthenium-oxide (RuO2) there is very high theoretical fake capacitance (> 1300F/ G), electrochemical reversibility is good, good cycle, is most potential oxide super capacitance material.But pure RuO2Price is high It is expensive, synergistic effect can be played with the compound composition compound super capacitance electrode material of poly-1-aminoanthraquinone.RuO2Load poly- 1- amino The synthesis of anthraquinone there is no report.
Summary of the invention
The purpose of the present invention is to provide a kind of RuO2Load the synthetic method of poly-1-aminoanthraquinone, which is characterized in that packet It includes following steps: 1- amino anthraquinones monomer is dissolved in deionized water, KI and RuI is added3, ultrasonic agitation dissolution;It is slowly added to It in hypochloric acid water solution, is persistently stirred in adition process, room temperature~40 DEG C are precipitated after standing reaction 8~12 hours, are passed through Filter washing dries to obtain RuO2Load the poly-1-aminoanthraquinone powder of I2 doping.
Concentration of the 1- amino anthraquinones monomer in reaction solution is 0.02~0.1mol/L.
Concentration of the potassium iodide in end reaction solution is 10~20gL-1, RuI3It is dense in end reaction solution Degree is 1~5gL-1
Hypochlorous acid concentration in reaction solution is 1~2mol/L.
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 dispersed in deionized water or ethyl alcohol again, and repeated filtration is 7 until filtrate pH value, last It is secondary to use ethanol washing with convenient and dry;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 polyvinyl chloride is easy, and situ study synthesizes RuO under room temperature2Uniform load poly-1-aminoanthraquinone, And I simultaneously2Doping to poly-1-aminoanthraquinone, can be used for super capacitance electrode material.
The contents of the present invention 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 include the combination of all the elements embodied in different piece, with And it is various without departing substantially from replacement and modification of the invention, and covered by claims of the present invention.
Detailed description of the invention
Fig. 1 is to synthesize RuO using (embodiment 1) of the invention2Load sweeping for the poly-1-aminoanthraquinone micromorphology of I2 doping Retouch electromicroscopic photograph.
Specific embodiment
Embodiment 1
The 1- amino anthraquinones monomer of 0.04mol/L is dissolved in 50mL deionized water, 20gL is added-1KI and 2gL-1RuI3, Ultrasonic agitation dissolution;It is slowly added in 50mL 2mol/L hypochloric acid water solution, is persistently stirred in adition process, is stored at room temperature anti- It is precipitated after answering 12 hours, dries to obtain flaky RuO as shown in Figure 1 through filtration washing2Load the poly- 1- ammonia of I2 doping Base anthraquinone powder.Using the powder of preparation use PVDF as adhesive coated on a pet film, then uniformly coating one layer of PVA/H3PO4It is solidifying Glue electrolyte is cut into the identical 2 5cm × 8cm sheet materials of size, respectively as positive and negative electrode, to the electrolysis above two electrodes When matter is in leather hard, 2 electrodes faces are sticked together, drying obtains all solid state symmetric form supercapacitor, specific volume Amount is 493Fg-1
Embodiment 2
The 1- amino anthraquinones monomer of 0.2mol/L is dissolved in 50mL deionized water, 30gL is added-1KI and 6gL-1RuI3, surpass Sound stirring and dissolving;It is slowly added in 50mL 4mol/L hypochloric acid water solution, is persistently stirred in adition process, 40 DEG C of standing reactions 8 It is precipitated after hour, dries to obtain RuO through filtration washing2Load the poly-1-aminoanthraquinone powder of I2 doping.By the powder of preparation Body use PVDF as adhesive coated on a pet film, then uniformly coating one layer of PVA/H3PO4It is identical to be cut into size for gel electrolyte 2 5cm × 8cm sheet materials, respectively as positive and negative electrode, when the electrolyte above two electrodes is in leather hard, by 2 Electrodes face sticks together, and drying obtains all solid state symmetric form supercapacitor, specific capacity 480Fg-1
Embodiment 3
The 1- amino anthraquinones monomer of 0.1mol/L is dissolved in 50mL deionized water, 40gL is added-1KI and 10gL-1RuI3, Ultrasonic agitation dissolution;It is slowly added in 50mL 3mol/L hypochloric acid water solution, is persistently stirred in adition process, is stored at room temperature anti- It is precipitated after answering 8 hours, dries to obtain RuO through filtration washing2Load the poly-1-aminoanthraquinone powder of I2 doping.By preparation Powder use PVDF as adhesive coated on a pet film, then uniformly coating one layer of PVA/H3PO4Gel electrolyte is cut into size phase 2 same 5cm × 8cm sheet materials, respectively as positive and negative electrode, when the electrolyte above two electrodes is in leather hard, by 2 A electrodes face sticks together, and drying obtains all solid state symmetric form supercapacitor, specific capacity 440Fg-1

Claims (6)

1. a kind of RuO2Load the synthetic method of poly-1-aminoanthraquinone, which comprises the following steps: by 1- amino anthraquinones Monomer is dissolved in deionized water, and KI and RuI is added3, ultrasonic agitation dissolution;It is slowly added in hypochloric acid water solution, adition process In persistently stir, room temperature~40 DEG C stand reaction 8~12 hours after precipitated, dry to obtain RuO through filtration washing2Load iodine The poly-1-aminoanthraquinone powder of doping.
2. a kind of RuO according to claim 12Load the synthetic method of poly-1-aminoanthraquinone, it is characterised in that: the 1- ammonia Concentration of the base anthraquinone monomer in reaction solution is 0.02~0.1mol/L.
3. a kind of RuO according to claim 12Load the synthetic method of poly-1-aminoanthraquinone, it is characterised in that: the iodate Concentration of the potassium in end reaction solution is 10~20gL-1, RuI3Concentration in end reaction solution is 1~5gL-1
4. a kind of RuO according to claim 12Load the synthetic method of poly-1-aminoanthraquinone, it is characterised in that: the secondary chlorine Acid concentration in reaction solution is 1~2mol/L.
5. a kind of RuO according to claim 12Load the synthetic method of poly-1-aminoanthraquinone, it is characterised in that: described washes Washing alternately is washed with deionized water and ethyl alcohol, is filtered, is filtered using centrifuge precipitating or pumping and filtering device each time after washing Product disperses in deionized water or ethyl alcohol again, and repeated filtration is 7 until filtrate pH value, for the last time with ethanol washing with side Just it dries;The drying is dried in 50~80 DEG C of vacuum drying ovens, and vacuum drying condition is vacuum degree < 133Pa.
6. a kind of RuO as claimed in any one of claims 1 to 5, wherein2Prepared by the synthetic method for loading poly-1-aminoanthraquinone RuO2Load poly-1-aminoanthraquinone.
CN201910379128.6A 2019-04-23 2019-04-23 A kind of RuO2Load the synthetic method of poly-1-aminoanthraquinone Withdrawn CN110098069A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0426536A1 (en) * 1989-10-31 1991-05-08 Sumitomo Chemical Company, Limited Production of aromatic amines
CN101220149A (en) * 2008-01-23 2008-07-16 同济大学 Method for synthesizing poly-1-aminoanthraquinone in aqueous phase
CN104916455A (en) * 2014-03-12 2015-09-16 中国科学院大连化学物理研究所 Colloidal electrolyte super capacitor adopting reticular diaphragm
CN109456479A (en) * 2018-11-08 2019-03-12 上海萃励电子科技有限公司 A kind of RuO2Load the synthetic method of poly 1,5-naphthalene diamine nanotube

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0426536A1 (en) * 1989-10-31 1991-05-08 Sumitomo Chemical Company, Limited Production of aromatic amines
CN101220149A (en) * 2008-01-23 2008-07-16 同济大学 Method for synthesizing poly-1-aminoanthraquinone in aqueous phase
CN104916455A (en) * 2014-03-12 2015-09-16 中国科学院大连化学物理研究所 Colloidal electrolyte super capacitor adopting reticular diaphragm
CN109456479A (en) * 2018-11-08 2019-03-12 上海萃励电子科技有限公司 A kind of RuO2Load the synthetic method of poly 1,5-naphthalene diamine nanotube

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