CN101181986A - Micron porous carbon microsphere and preparation method thereof - Google Patents
Micron porous carbon microsphere and preparation method thereof Download PDFInfo
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- CN101181986A CN101181986A CNA2007100505491A CN200710050549A CN101181986A CN 101181986 A CN101181986 A CN 101181986A CN A2007100505491 A CNA2007100505491 A CN A2007100505491A CN 200710050549 A CN200710050549 A CN 200710050549A CN 101181986 A CN101181986 A CN 101181986A
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Abstract
The invention discloses a micron porous carbon microsphere and a preparation method thereof. The steps of the preparation method of the micron porous carbon microsphere are as follows: 1) coating agent and porous starch are adopted and then put into water so as to be mixed evenly, and the mixture obtained is dried, thus gaining dried mixture; 2) the dried mixture is put in an environment which is protected by inert gas and then is heated to 300-1000 DEG C, having insulation for 1-36 hours; after being cooled, carbonized product obtained is washed and dried before gaining the micron porous carbon microsphere. The preparation method of the invention has high yield, low cost and simple technique, and the monodisperse micron porous carbon microsphere prepared has wide application and can be used as catalyst carrier, lithium-ion cell electrode materials, absorbent, drug-releasing materials, etc.
Description
(1) technical field:
The present invention relates to carbon materials, particularly micron porous carbon microsphere; The invention still further relates to the preparation method of this micron porous carbon microsphere.
(2) background technology:
Since finding soccerballene and CNT (carbon nano-tube), worldwide just carried out comprehensive research to carbon materials.The different-shape carbon material has the potential using value in many aspects, and as support of the catalyst, lithium ion battery electrode material, sorbent material, medicinal slow release agent etc., the carbon material that therefore has unique texture has caused widely to be paid close attention to.According to the difference of employed method and use carbon matrix precursor, many different-shape carbon materials such as onion type carbon, pyramidal structure carbon, the little tree of carbon, the little volume of carbon etc. successfully are synthesized.The discovery of spherical carbon material is in the sixties in 20th century, and people find that in the forming process of research coke the pitch compounds intermediate phase can take place changes in heat treatment process, generate mesophase ball.1973, Honda and Yamada separated mesophase ball from the pitch parent, and the micron-size spherical material separated be referred to as carbonaceous mesophase spherules (mesocarbon microbeads, MCMB).In recent years, size spherical carbon material different with structure from the nano level to the micron order successfully prepares by diverse ways, as application number be: 02118730.4, name is called the Chinese invention patent of " manufacture method of hollow nano carbon microsphere ", it discloses a kind of manufacture method of hollow nano carbon microsphere, this method comprises the following steps: that (a) provides one to contain the electric arc reaction chamber of graphite anode and graphite cathode, and feeds a rare gas element in the electric arc reaction chamber; (b) apply a voltage between above-mentioned negative electrode and the anode with a pulsed current, thereby produce the arc-over reaction; (c) collect the product that is deposited on graphite cathode, comprise the principal product and the CNT (carbon nano-tube) of hollow nano carbon microsphere; (d) separation and purification goes out the hollow nano carbon microsphere from settling.But use the method for preparing nano carbon microsphere, its output is not high, preparation technology is comparatively complicated, and production cost is also higher relatively.
(3) summary of the invention:
The present invention will disclose the micron porous carbon microsphere that preparation technology is simple, low-cost, utilize porous-starch to prepare for presoma, and the present invention will disclose the preparation method of this micron porous carbon microsphere.
The preparation method of micron porous carbon microsphere of the present invention, its step is as follows:
1) gets coating and porous-starch, add entry and mix, the mixture of gained is carried out drying, obtain dried mixture; For guaranteeing that coating can coat porous-starch completely effectively, in general, the proportioning of coating and porous-starch is counted by weight, coating: porous-starch 〉=get final product at 1: 20; But coating: the proportional quantity of porous-starch is best≤be advisable at 2: 1, i.e. coating: the weight proportion of porous-starch is preferably 1: 20～and 2: 1; Described coating is generally the solubility stannate, or the solubility pink salt, or soluble silicate, or can play other materials of coating effect equally, for example can be sodium stannate, or tin chloride, or tin protochloride, or water glass etc.; And the add-on of water generally is advisable coating and porous-starch can be mixed;
2) place the environment of inert atmosphere to be heated to 300～1000 ℃ in dried mixture, and be incubated 1～36 hour, cooling then, the carbonizing production of gained washs, drying, promptly obtains micron porous carbon microsphere; In general, the temperature rise rate in the heat-processed is 0.2～20 ℃/min, and general water gets final product the carbonizing production washing to neutral.
Preparation method of the present invention is to be presoma with the porous-starch, utilizes the method that coats charing, coats layer protective layer at the porous-starch particle surface, prepares monodispersed micrometer level porous carbosphere under the pyritous condition.Use the method for the invention is prepared, and the productive rate height, cost is low, technology is simple, and the monodispersed micrometer level porous carbosphere of gained is of many uses, can be used as uses such as support of the catalyst, lithium ion battery electrode material, sorbent material, medicinal slow release agent.
(4) description of drawings:
Fig. 1 is the scanning electron microscope shape appearance figure of porous carbon microsphere of the present invention.
(5) embodiment:
Embodiment 1:
1) takes by weighing 5g sodium stannate and 10g porous-starch, add 200g distilled water and also mix, the mixture of gained is carried out lyophilize, obtain dried mixture;
2) get the High Temperature Furnaces Heating Apparatus that dried mixture is put into argon shield; temperature rise rate with 20 ℃/min; be heated to 300 ℃ from room temperature; and this temperature insulation 3 hours; naturally cool to room temperature then; the carbonizing production of gained is washed with distilled water to neutrality, promptly gets micron porous carbon microsphere, and the structure of the micron porous carbon microsphere of gained as shown in Figure 1.
Embodiment 2:
1) take by weighing 3g water glass and 10g porous-starch, add 200g distilled water they are mixed, the mixture of gained carries out lyophilize, obtains dried mixture;
2) get the High Temperature Furnaces Heating Apparatus that dried mixture is put into argon shield; temperature rise rate with 10 ℃/min; be heated to 600 ℃ from room temperature; and this temperature insulation 2 hours; naturally cooling then; the carbonizing production of gained is washed with distilled water to neutrality successively earlier, uses hydrofluoric acid (mass concentration is 40%) washing to remove silicon compound, to be washed with distilled water to neutrality then again, and drying promptly gets micron porous carbon microsphere.
Embodiment 3:
1) take by weighing 6g tin protochloride and 10g porous-starch, add 200g distilled water they are mixed, the mixture of gained carries out lyophilize, obtains dried mixture;
2) get the High Temperature Furnaces Heating Apparatus that dried mixture is put into argon shield,, be heated to 800 ℃ from room temperature with the temperature rise rate of 2 ℃/min; and, naturally cooling to room temperature then this temperature insulation 1 hour, the carbonizing production of gained is washed with distilled water to neutrality; drying promptly gets micron porous carbon microsphere.
Embodiment 4:
1) take by weighing 4g tin chloride and 10g porous-starch, add 200g distilled water they are mixed, the mixture of gained carries out lyophilize, obtains dried mixture;
2) get the High Temperature Furnaces Heating Apparatus that dried mixture is put into argon shield,, be heated to 300 ℃ from room temperature with the temperature rise rate of 5 ℃/min; and, naturally cooling to room temperature then this temperature insulation 6 hours, the carbonizing production of gained is washed with distilled water to neutrality; drying promptly gets micron porous carbon microsphere.
Claims (7)
1. the preparation method of micron porous carbon microsphere, its step is as follows:
1) get coating and porous-starch, add entry and mix, the mixture of gained carries out drying, obtains dried mixture;
2) place the environment of inert atmosphere to be heated to 300～1000 ℃ in dried mixture, and be incubated 1～36 hour, cooling then, the carbonizing production of gained washs, drying, obtains micron porous carbon microsphere.
2. the preparation method of micron porous carbon microsphere according to claim 1, it is characterized in that: in the step 1), the proportioning of coating and porous-starch is counted by weight, coating: porous-starch 〉=1: 20.
3. the preparation method of micron porous-starch according to claim 2, it is characterized in that: described coating: porous-starch is 1: 20～2: 1.
4. according to the preparation method of any one described micron porous-starch in the claim 1～3, it is characterized in that: step 2) in, the temperature rise rate during heating is 0.2～20 ℃/min.
5. according to the preparation method of any one described micron porous-starch in the claim 1～3, it is characterized in that: described coating is the solubility stannate, or the solubility pink salt, or soluble silicate.
6. the preparation method of micron porous-starch according to claim 5, it is characterized in that: described coating is a sodium stannate, or tin chloride, or tin protochloride, or water glass.
7. the micron porous carbon microsphere of any one described method preparation in the claim 1～6.
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Cited By (12)
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| CN102560452A (en) * | 2011-12-08 | 2012-07-11 | 广西师范大学 | Chemical tin plating solution, preparation method for tin plating solution, method for preparing tin/ carbon composite material by using tin plating solution and obtained product |
| CN102583318A (en) * | 2012-02-24 | 2012-07-18 | 大连理工大学 | Method for preparing nitrogen doped grading-hole porous carbon microspheres |
| CN102580637A (en) * | 2012-02-24 | 2012-07-18 | 大连理工大学 | Simple preparation method of graded-hole micronscale magnetic carbon microspheres |
| CN103623779A (en) * | 2013-12-06 | 2014-03-12 | 河北工业大学 | Hydrophilic functional carbon sphere and application thereof for removing heavy metal ions in waste water |
| CN104045074A (en) * | 2014-06-18 | 2014-09-17 | 广西师范大学 | Starch-based hollow porous carbon microsphere and preparation method thereof |
| CN104355887A (en) * | 2014-11-18 | 2015-02-18 | 李�杰 | Preparation method of special carbon-based slow release fertilizer for wheat |
| CN104477879A (en) * | 2014-12-05 | 2015-04-01 | 辽宁石油化工大学 | Preparation method of starch-based carbon material |
| CN108565411A (en) * | 2018-03-20 | 2018-09-21 | 无锡新锂辰能源科技有限公司 | A kind of Sn-C composite electrodes material and its preparation method and application |
| CN111153394A (en) * | 2020-01-16 | 2020-05-15 | 昆明理工大学 | Preparation method of carbon-silicon negative electrode material of lithium ion battery |
| CN111569933A (en) * | 2020-06-22 | 2020-08-25 | 中认英泰检测技术有限公司 | Porous carbon-based metal catalyst, preparation method and application thereof |
| CN112175263A (en) * | 2020-09-22 | 2021-01-05 | 苏州市桔园管业有限公司 | High-toughness flame-retardant heat-insulation pipe |
| CN117567730A (en) * | 2024-01-15 | 2024-02-20 | 江苏国望高科纤维有限公司 | Nano-supported solid-phase titanium-based multielement metal catalyst and preparation method and application thereof |
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2007
- 2007-11-16 CN CNB2007100505491A patent/CN100556801C/en not_active Expired - Fee Related
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560452A (en) * | 2011-12-08 | 2012-07-11 | 广西师范大学 | Chemical tin plating solution, preparation method for tin plating solution, method for preparing tin/ carbon composite material by using tin plating solution and obtained product |
| CN102583318A (en) * | 2012-02-24 | 2012-07-18 | 大连理工大学 | Method for preparing nitrogen doped grading-hole porous carbon microspheres |
| CN102580637A (en) * | 2012-02-24 | 2012-07-18 | 大连理工大学 | Simple preparation method of graded-hole micronscale magnetic carbon microspheres |
| CN103623779A (en) * | 2013-12-06 | 2014-03-12 | 河北工业大学 | Hydrophilic functional carbon sphere and application thereof for removing heavy metal ions in waste water |
| CN104045074B (en) * | 2014-06-18 | 2016-06-15 | 广西师范大学 | A kind of starch base Porous hollow carbosphere and preparation method thereof |
| CN104045074A (en) * | 2014-06-18 | 2014-09-17 | 广西师范大学 | Starch-based hollow porous carbon microsphere and preparation method thereof |
| CN104355887A (en) * | 2014-11-18 | 2015-02-18 | 李�杰 | Preparation method of special carbon-based slow release fertilizer for wheat |
| CN104477879B (en) * | 2014-12-05 | 2016-08-17 | 辽宁石油化工大学 | A kind of preparation method of starch base material with carbon element |
| CN104477879A (en) * | 2014-12-05 | 2015-04-01 | 辽宁石油化工大学 | Preparation method of starch-based carbon material |
| CN108565411A (en) * | 2018-03-20 | 2018-09-21 | 无锡新锂辰能源科技有限公司 | A kind of Sn-C composite electrodes material and its preparation method and application |
| CN111153394A (en) * | 2020-01-16 | 2020-05-15 | 昆明理工大学 | Preparation method of carbon-silicon negative electrode material of lithium ion battery |
| CN111153394B (en) * | 2020-01-16 | 2023-01-20 | 昆明理工大学 | Preparation method of carbon-silicon negative electrode material of lithium ion battery |
| CN111569933A (en) * | 2020-06-22 | 2020-08-25 | 中认英泰检测技术有限公司 | Porous carbon-based metal catalyst, preparation method and application thereof |
| CN111569933B (en) * | 2020-06-22 | 2021-08-03 | 中认英泰检测技术有限公司 | Porous carbon-based metal catalyst, preparation method and application thereof |
| WO2021258425A1 (en) * | 2020-06-22 | 2021-12-30 | 中认英泰检测技术有限公司 | Porous carbon-based metal catalyst and preparation method therefor and application thereof |
| CN112175263A (en) * | 2020-09-22 | 2021-01-05 | 苏州市桔园管业有限公司 | High-toughness flame-retardant heat-insulation pipe |
| CN117567730A (en) * | 2024-01-15 | 2024-02-20 | 江苏国望高科纤维有限公司 | Nano-supported solid-phase titanium-based multielement metal catalyst and preparation method and application thereof |
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| CN100556801C (en) | 2009-11-04 |
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Granted publication date: 20091104 Termination date: 20191116 |