CN104876208A - Preparation method for nickel-containing phenolic resin based carbon ball - Google Patents
Preparation method for nickel-containing phenolic resin based carbon ball Download PDFInfo
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- CN104876208A CN104876208A CN201510337420.3A CN201510337420A CN104876208A CN 104876208 A CN104876208 A CN 104876208A CN 201510337420 A CN201510337420 A CN 201510337420A CN 104876208 A CN104876208 A CN 104876208A
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- Y—GENERAL 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
The invention relates to a preparation method for a nickel-containing phenolic resin based carbon ball. The preparation method for the nickel-containing phenolic resin based carbon ball is aimed to solve the problems that an existing phenolic carbon ball preparation method is complex in technology, high in cost and difficult to control the diameter of the phenolic carbon ball. The preparation method for the nickel-containing phenolic resin based carbon ball includes that placing a nickel-containing phenolic resin based micro-ball in a tube furnace under 700 to 1000 degrees centigrade, and filling nitrogen to carbonize for 2 to 6 hours to obtain the nickel-containing phenolic resin based carbon ball. The preparation method for the nickel-containing phenolic resin based carbon ball is used for preparing anode material of a supercapacitor.
Description
Technical field
The present invention relates to a kind of preparation method of nickeliferous phenolic aldehyde base carbon ball.
Background technology
Ultracapacitor is a kind of novel energy storage device between traditional capacitor and chemical power source, that a kind of novel energy stores and transfer equipment, because of its have capacity large, have extended cycle life, can the advantage such as fast charging and discharging, cause the extensive concern of researchist.Two classes can be divided into: double layer capacitor and Faraday pseudo-capacitance device according to the difference of energy storage mechnism.The performance of electrode materials to electrochemical capacitor has tremendous influence, selects suitable electrode materials, and electrical condenser can be made to have higher operating voltage and higher energy density.It has the duration of charging short, have extended cycle life, the advantage such as power characteristic is good, temperature range is wide, economic environmental protection.Extensive concern is received in a lot of field.And electrode materials is the core component of ultracapacitor, it is problem most crucial in ultracapacitor research.Electrode materials comprises hole carbon material and matrix material, conducting polymer materials and metal oxide electrode material.
The existing method preparing resol carbon ball is dissolved in alcoholic solution by linear phenolic resin, by the tensio-active agent furnishing aqueous solution, resol alcoholic solution is joined in the aqueous solution containing surfactant, constant temperature 30 ~ 180min at the uniform velocity agitation condition is heated to 110 ~ 130 DEG C, obtained phenolic resin microspheres, then adopt the charing of phenolic resin microspheres tube furnace, obtain resol carbon ball.The method complex process, cost are high and phenolic aldehyde carbon ball sphere diameter is wayward.
Summary of the invention
The present invention will solve the high and uppity problem of phenolic aldehyde carbon ball sphere diameter of existing phenolic aldehyde carbon ball preparation method complex process, cost, and provides a kind of preparation method of nickeliferous phenolic aldehyde base carbon ball.
A kind of preparation method of nickeliferous phenolic aldehyde base carbon ball carries out according to the following steps:
Nickeliferous phenolic aldehyde base microballoon is put into the tube furnace that temperature is 700 DEG C ~ 1000 DEG C, and then logical nitrogen carbonizes wherein, and carbonization time is 2h ~ 6h, obtains nickeliferous phenolic aldehyde base carbon ball.
The invention has the beneficial effects as follows:
The present invention by 10 μm ~ 100 μm nickeliferous phenolic aldehyde base microballoons, the phenolic aldehyde sphere of this loaded metal, long period of soaking inside alkali lye, metal difficult drop-off, stable performance.The nickeliferous phenolic aldehyde base carbon ball obtained is for the preparation of electrode materials, and the electrode materials electrode ratio capacitance value of preparation is high, is applicable to the working electrode doing ultracapacitor.
Embodiment
Embodiment one: the preparation method of a kind of nickeliferous phenolic aldehyde base carbon ball of present embodiment carries out according to the following steps:
Nickeliferous phenolic aldehyde base microballoon is put into the tube furnace that temperature is 700 DEG C ~ 1000 DEG C, and then logical nitrogen carbonizes wherein, and carbonization time is 2h ~ 6h, obtains nickeliferous phenolic aldehyde base carbon ball.
Embodiment two: present embodiment and embodiment one unlike: the preparation method of described nickeliferous phenolic aldehyde base microballoon carries out according to the following steps: 1., Resorcinol, formaldehyde and nickel salt are put into distilled water mix, obtain mixed solution A, then stirring reaction 10min ~ 60min under temperature is 20 DEG C ~ 60 DEG C and rotating speed is the condition of 200r/min, obtains mixing solutions B; The mol ratio of described Resorcinol and formaldehyde is 1:(2 ~ 2.5); Described nickel salt is a kind of or wherein several mixture in nickel acetate, nickel formate, single nickel salt and nickelous chloride; The mol ratio of described nickel salt and Resorcinol is 1:(0.1 ~ 1200); The massfraction of described mixed solution A is 10% ~ 60%; 2. the mixing solutions B, to step 1. obtained adds tensio-active agent and hexanaphthene, and stir under temperature is 40 DEG C ~ 80 DEG C and rotating speed is the condition of 10r/min ~ 900r/min, churning time is 1 ~ 5h, obtains mixed solution C; Described tensio-active agent is SPan system tensio-active agent; The mixing solutions B that 1. described step obtains and the volume ratio of hexanaphthene are 1:(10 ~ 15); The volume ratio of described hexanaphthene and tensio-active agent is 1:(0.001 ~ 0.2); 3. the static 6h ~ 12h of mixed solution C, by step 2. obtained, after pouring out supernatant liquid, adopts methyl alcohol to wash surplus materials, then centrifugal 10min ~ 20min, then to put into temperature be that the drying baker of 80 DEG C dries 12h, obtains nickeliferous phenolic aldehyde base microballoon.Other are identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: nickeliferous phenolic aldehyde base microballoon is put into the tube furnace that temperature is 800 DEG C.Other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: nickeliferous phenolic aldehyde base microballoon is put into the tube furnace that temperature is 900 DEG C.Other are identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: carbonization time is 4h.Other are identical with one of embodiment one to four.
Following examples are adopted to verify beneficial effect of the present invention:
Embodiment one: a kind of method utilizing nickeliferous phenolic aldehyde base carbon ball to prepare carbon material electrode is carried out according to the following steps:
One, nickeliferous phenolic aldehyde base microballoon is put into the tube furnace that temperature is 800 DEG C, then logical nitrogen carbonizes wherein, and carbonization time is 3h, obtains nickeliferous phenolic aldehyde base carbon ball; The preparation method of described nickeliferous phenolic aldehyde base microballoon carries out according to the following steps:
1., Resorcinol, formaldehyde and nickel salt are put into distilled water mix, obtain mixed solution A; Then mixed solution A is put into three strength bottles, temperature be 20 DEG C ~ 60 DEG C, rotating speed stirs under being the condition of 200r/min, churning time is 25min, obtains mixing solutions B; The mol ratio of described Resorcinol and formaldehyde is 1:2; Described nickel salt is the mixture of nickel acetate and single nickel salt 1:1 mixing in molar ratio; The mol ratio of described nickel salt and Resorcinol is 1:100; The massfraction of described mixed solution A is 20%; 2. the mixing solutions B, to step 1. obtained adds tensio-active agent and hexanaphthene, and stir under temperature is 75 DEG C and rotating speed is the condition of 120r/min, churning time is 3h, obtains mixed solution C; Described tensio-active agent is SPan85 tensio-active agent; The mixing solutions B that 1. described step obtains and the volume ratio of hexanaphthene are 1:15; The volume ratio of described hexanaphthene and tensio-active agent is 1:0.001; 3. the static 6h of mixed solution C, by step 2. obtained, after pouring out supernatant liquid, adopts methyl alcohol to wash surplus materials, then centrifugal 10min ~ 20min, then to put into temperature be that the drying baker of 80 DEG C dries 12h, obtains nickeliferous phenolic aldehyde base microballoon.
Proof test: nickeliferous phenolic aldehyde base carbon ball embodiment one obtained is placed in mortar, add after distilled water is ground to pasty state and add tetrafluoroethylene, obtain mashed prod, then mashed prod is coated in foam nickel sheet on the surface, be be placed in air dry oven under the condition of 60 DEG C to dry 4h in temperature, obtain pre-prepared electrode materials; The nickeliferous phenolic aldehyde base carbon ball that described step one obtains and the mass ratio of tetrafluoroethylene are 1:(0.1 ~ 0.01); Coating thickness is 0.2mm; Then pre-prepared electrode materials is pressed into the thin slice that thickness is 1.1mm on twin-roll machine, is carbon material electrode.
The carbon material electrode prepared by employing nickeliferous phenolic aldehyde base microballoon of the present invention, as electrode for super capacitor materials'use, has the highest ratio capacitance value and reaches 455.46F/g, be suitable as the positive electrode material of ultracapacitor.
Claims (5)
1. a preparation method for nickeliferous phenolic aldehyde base carbon ball, is characterized in that the preparation method of nickeliferous phenolic aldehyde base carbon ball carries out according to the following steps:
Nickeliferous phenolic aldehyde base microballoon is put into the tube furnace that temperature is 700 DEG C ~ 1000 DEG C, and then logical nitrogen carbonizes wherein, and carbonization time is 2h ~ 6h, obtains nickeliferous phenolic aldehyde base carbon ball.
2. the preparation method of a kind of nickeliferous phenolic aldehyde base carbon ball according to claim 1, it is characterized in that the preparation method of described nickeliferous phenolic aldehyde base microballoon carries out according to the following steps: 1., Resorcinol, formaldehyde and nickel salt are put into distilled water mix, obtain mixed solution A, then stirring reaction 10min ~ 60min under temperature is 20 DEG C ~ 60 DEG C and rotating speed is the condition of 200r/min, obtains mixing solutions B; The mol ratio of described Resorcinol and formaldehyde is 1:(2 ~ 2.5); Described nickel salt is a kind of or wherein several mixture in nickel acetate, nickel formate, single nickel salt and nickelous chloride; The mol ratio of described nickel salt and Resorcinol is 1:(0.1 ~ 1200); The massfraction of described mixed solution A is 10% ~ 60%; 2. the mixing solutions B, to step 1. obtained adds tensio-active agent and hexanaphthene, and stir under temperature is 40 DEG C ~ 80 DEG C and rotating speed is the condition of 10r/min ~ 900r/min, churning time is 1 ~ 5h, obtains mixed solution C; Described tensio-active agent is SPan system tensio-active agent; The mixing solutions B that 1. described step obtains and the volume ratio of hexanaphthene are 1:(10 ~ 15); The volume ratio of described hexanaphthene and tensio-active agent is 1:(0.001 ~ 0.2); 3. the static 6h ~ 12h of mixed solution C, by step 2. obtained, after pouring out supernatant liquid, adopts methyl alcohol to wash surplus materials, then centrifugal 10min ~ 20min, then to put into temperature be that the drying baker of 80 DEG C dries 12h, obtains nickeliferous phenolic aldehyde base microballoon.
3. the preparation method of a kind of nickeliferous phenolic aldehyde base carbon ball according to claim 1, is characterized in that nickeliferous phenolic aldehyde base microballoon to put into the tube furnace that temperature is 800 DEG C.
4. the preparation method of a kind of nickeliferous phenolic aldehyde base carbon ball according to claim 1, is characterized in that nickeliferous phenolic aldehyde base microballoon to put into the tube furnace that temperature is 900 DEG C.
5. the preparation method of a kind of nickeliferous phenolic aldehyde base carbon ball according to claim 1, is characterized in that carbonization time is 4h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111994895A (en) * | 2020-09-08 | 2020-11-27 | 沙县宏盛塑料有限公司 | Phenolic resin carbon microsphere and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102709017A (en) * | 2012-06-11 | 2012-10-03 | 合肥工业大学 | Preparation method of carbon-aerogel-based spherical anticorrosion magnetic material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102709017A (en) * | 2012-06-11 | 2012-10-03 | 合肥工业大学 | Preparation method of carbon-aerogel-based spherical anticorrosion magnetic material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111994895A (en) * | 2020-09-08 | 2020-11-27 | 沙县宏盛塑料有限公司 | Phenolic resin carbon microsphere and preparation method and application thereof |
| CN111994895B (en) * | 2020-09-08 | 2022-03-08 | 沙县宏盛塑料有限公司 | Phenolic resin carbon microsphere and preparation method and application thereof |
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