CN110002426A - A kind of preparation method of porous carbon microspheres - Google Patents

A kind of preparation method of porous carbon microspheres Download PDF

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Publication number
CN110002426A
CN110002426A CN201910333949.6A CN201910333949A CN110002426A CN 110002426 A CN110002426 A CN 110002426A CN 201910333949 A CN201910333949 A CN 201910333949A CN 110002426 A CN110002426 A CN 110002426A
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temperature
carbon microspheres
porous carbon
heating
obtains
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田龙
王丽
褚学英
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Nanyang Normal University
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    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/05Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30

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Abstract

The present invention provides a kind of preparation method of porous carbon microspheres, comprising the following steps: 1) formalin is heated to 40 ~ 50 DEG C, adjusts the pH of formalin 3.5~4.5;2) urea is added in formalin, is reacted under stirring condition, when solution becomes cloudy, stop stirring, time of repose is washed to neutrality after being 12 ~ 72 h, obtains Lauxite;3) Lauxite is dry to constant weight, obtain urea formaldehyde resin microsphere;4) urea formaldehyde resin microsphere is carried out to the pre-oxidation of gradient increased temperature formula in Muffle furnace, obtains pre-oxidation product;5) pre-oxidation product is placed in tube furnace and is continually fed into nitrogen and is carbonized, obtain carbon microspheres;6) carbon microspheres are mixed with NaOH, under the protection of nitrogen, is carbonized, obtains porous carbon microspheres.The present invention prepares the three-dimensional classifying porous carbon microspheres of Lauxite using a kind of simple and environmentally-friendly method, has the advantages that good dispersion, can be used for the positive electrode of lithium-air battery.

Description

A kind of preparation method of porous carbon microspheres
Technical field
The present invention relates to the technical fields of the preparation of nitrogenous Carbon Materials, and in particular to a kind of preparation side of porous carbon microspheres Method.
Background technique
Lithium ion battery since energy density is high, have extended cycle life, self-discharge rate is low etc., widely used by advantages In convenient and fast electronic equipment.However, large scale equipment needed for power battery and long-term energy storage requires lithium ion battery to have high power Stable performance etc. is maintained under rate performance, high temperature for a long time, these are all urgently to be resolved in power lithium-ion battery development process The problem of.Porous carbon microsphere has excellent heat resistance, corrosion resistance, higher bulk density and resistance to pressure etc., in power electric Pond application in its smooth surface and low specific surface area it is possible to prevente effectively from charge and discharge process electrode surface side reaction hair It is raw, to reduce the coulomb loss in first time charging process.Porous carbon microsphere also possesses unique porous network structure simultaneously, Macropore can store electrolyte, to reduce the diffusion length of lithium ion;Part lithium ion is adsorbed on the surface of mesoporous, in order to mention For high capacity and quick energy storage;Aperture is conducive to the insertion of lithium ion, enhancing storage lithium ability.As negative electrode of lithium ion battery material Material can effectively improve the diffusion rate of lithium ion, diffusion impedance be reduced, to improve the high rate performance of battery.
Summary of the invention
Present invention aim to address the deficiencies of existing preparation method, provide a kind of preparation method of porous carbon microspheres, this It is micro- that invention using urea and formaldehyde as raw material, using a kind of simple and environmentally-friendly method prepares the three-dimensional classifying porous charcoal of Lauxite Ball has the advantages that good dispersion, can be used for the positive electrode of lithium-air battery.On the one hand, three-dimensional classifying porous structure has Conducive to the transmission of oxygen, the transmitting of electronics provides place for lithium-air battery Product bulk;On the other hand, nitrogenous Carbon Materials, It can speed up the absorption of oxygen, the transfer of electronics enhances the electrochemical catalysis activity of Carbon Materials.
The present invention to solve above-mentioned technical problem the technical solution adopted is that: a kind of preparation method of porous carbon microspheres, packet Include following steps:
1) it calculates according to the mass fraction, the formaldehyde that 50 ~ 60 parts of concentration are 36 ~ 38% is heated to 40 ~ 50 DEG C, adjusted with acid solution molten The pH of liquid is 3.5~4.5;
2) it calculates according to the mass fraction, 10 ~ 14 parts of urea is added in the formalin in step 1), are reacted under stirring condition, when When solution becomes cloudy, stop stirring, time of repose is washed to neutrality after being 12 ~ 72 h, obtains Lauxite;
3) Lauxite for obtaining step 2 dry 24 ~ 48h under conditions of heating temperature is 55 ~ 65 DEG C is obtained to constant weight Urea formaldehyde resin microsphere;
4) urea formaldehyde resin microsphere for obtaining step 3) carries out gradient increased temperature formula pre-oxidation in Muffle furnace, obtains the pre- oxygen of brown color Change product;
5) the pre-oxidation product that step 4) obtains is placed in tube furnace and is continually fed into nitrogen and is carbonized, obtain carbon microspheres;
6) carbon microspheres that step 5) obtains are mixed with NaOH by weight 1:1 ~ 0.85:1, under the protection of nitrogen, with 4 ~ 6 DEG C/heating rate of min is raised to 740 ~ 760 DEG C, soaking time is 2 ~ 4 h;After natural cooling, it is washed to neutrality, is in temperature Dry 24 ~ 48 h, obtain porous carbon microspheres under conditions of 55 ~ 65 DEG C.
Further, the acid solution in step 1) is one of formic acid or hydrochloric acid.
Further, the Lauxite in step 3) surpasses before it is dried under conditions of ultrasonic power is 1000 ~ 1200w 60 ~ 90min of sonication.
Further, the process that gradient increased temperature formula pre-oxidizes in step 4) are as follows: initial Pre oxidation is 100 ~ 110 DEG C, the temperature gradient of heating is 15 ~ 25 DEG C, and oxidization time of the urea formaldehyde resin microsphere under each temperature gradient is 7 ~ 9h, when pre- When oxidizing temperature reaches 200 ~ 220 DEG C, stop heating, pre-oxidation product is obtained when being cooled to room temperature.
Further, the heating rate in step 4) is 2 ~ 3 DEG C/min.
Further, the process being carbonized in step 5) are as follows: risen to from room temperature with the heating rate heating of 8 ~ 12 DEG C/min 180 ~ 220 DEG C, and 2.5 ~ 3.5h is kept the temperature under the conditions of this temperature, then be raised to 290 ~ 310 with the heating rate of 0.5 ~ 1.5 DEG C/min DEG C, 2.5 ~ 3.5 h are kept the temperature, then with 4 ~ 6 DEG C/min, 580 ~ 620 DEG C is warming up to, keeps the temperature 2.5 ~ 3.5 h, naturally cool to room Temperature.
Beneficial effects of the present invention mainly show such as: the present invention is using urea and formaldehyde as raw material, using a kind of simple and environmentally-friendly Method prepare the three-dimensional classifying porous carbon microspheres of Lauxite, have the advantages that good dispersion, can be used for lithium-air battery Positive electrode.On the one hand, three-dimensional classifying porous structure is conducive to the transmission of oxygen, and the transmitting of electronics produces for lithium-air battery Object accumulation provides place;On the other hand, nitrogenous Carbon Materials, can speed up the absorption of oxygen, and the transfer of electronics enhances raw material of wood-charcoal The electrochemical catalysis activity of material.By scanning electron microscopic observation, complete spherical shape is presented in Lauxite precursor, and microsphere diameter is about 6 μm or so, precursor is pre-oxidized later, charing process, sample possesses more flourishing cellular structure, specific surface area Hold with hole is respectively 555m2·g-1With 2.56 cm/g.
Specific embodiment
The present invention is described in detail in conjunction with the embodiments, the present embodiment based on the technical solution of the present invention, gives Detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following embodiments.
Embodiment 1
A kind of preparation method of porous carbon microspheres, comprising the following steps:
1) it calculates according to the mass fraction, the formaldehyde that 50 ~ 60 parts of concentration are 36 ~ 38% is heated to 40 ~ 50 DEG C, adjusted with acid solution molten The pH of liquid is 3.5~4.5;
2) it calculates according to the mass fraction, 10 ~ 14 parts of urea is added in the formalin in step 1), are reacted under stirring condition, when When solution becomes cloudy, stop stirring, time of repose is washed to neutrality after being 12 ~ 72 h, obtains Lauxite;
3) Lauxite for obtaining step 2 dry 24 ~ 48h under conditions of heating temperature is 55 ~ 65 DEG C is obtained to constant weight Urea formaldehyde resin microsphere;
4) urea formaldehyde resin microsphere for obtaining step 3) carries out gradient increased temperature formula pre-oxidation in Muffle furnace, obtains the pre- oxygen of brown color Change product;
5) the pre-oxidation product that step 4) obtains is placed in tube furnace and is continually fed into nitrogen and is carbonized, obtain carbon microspheres;
6) carbon microspheres that step 5) obtains are mixed with NaOH by weight 1:1 ~ 0.85:1, under the protection of nitrogen, with 4 ~ 6 DEG C/heating rate of min is raised to 740 ~ 760 DEG C, soaking time is 2 ~ 4 h;After natural cooling, it is washed to neutrality, is in temperature Dry 24 ~ 48 h, obtain porous carbon microspheres under conditions of 55 ~ 65 DEG C.
Further, the acid solution in step 1) is one of formic acid or hydrochloric acid.
Further, the Lauxite in step 3) surpasses before it is dried under conditions of ultrasonic power is 1000 ~ 1200w 60 ~ 90min of sonication.
Further, the process that gradient increased temperature formula pre-oxidizes in step 4) are as follows: initial Pre oxidation is 100 ~ 110 DEG C, the temperature gradient of heating is 15 ~ 25 DEG C, and oxidization time of the urea formaldehyde resin microsphere under each temperature gradient is 7 ~ 9h, when pre- When oxidizing temperature reaches 200 ~ 220 DEG C, stop heating, pre-oxidation product is obtained when being cooled to room temperature.
Further, the heating rate in step 4) is 2 ~ 3 DEG C/min.
Further, the process being carbonized in step 5) are as follows: risen to from room temperature with the heating rate heating of 8 ~ 12 DEG C/min 180 ~ 220 DEG C, and 2.5 ~ 3.5h is kept the temperature under the conditions of this temperature, then be raised to 290 ~ 310 with the heating rate of 0.5 ~ 1.5 DEG C/min DEG C, 2.5 ~ 3.5 h are kept the temperature, then with 4 ~ 6 DEG C/min, 580 ~ 620 DEG C is warming up to, keeps the temperature 2.5 ~ 3.5 h, naturally cool to room Temperature.
Embodiment 2
A kind of preparation method of porous carbon microspheres, comprising the following steps:
1) it calculates according to the mass fraction, the formaldehyde that 55 parts of concentration are 37% is heated to 45 DEG C, is existed with the pH that acid solution adjusts solution 4, acid solution is one of formic acid or hydrochloric acid;
2) it calculates according to the mass fraction, 12 parts of urea is added in the formalin in step 1), is reacted under stirring condition, works as solution When becoming cloudy, stop stirring, time of repose is washed to neutrality after being 12 ~ 72 h, obtains Lauxite;By Lauxite in ultrasonic function Under conditions of rate is 1000 ~ 1200w, it is ultrasonically treated 60 ~ 90min.
3) Lauxite for obtaining step 2 under conditions of heating temperature is 55 ~ 65 DEG C dry 24 ~ 48h to constant weight, Obtain urea formaldehyde resin microsphere;
4) urea formaldehyde resin microsphere for obtaining step 3) carries out gradient increased temperature formula pre-oxidation, initial pre-oxidation temperature in Muffle furnace Degree is 90 ~ 110 DEG C, and the temperature gradient of heating is 20 DEG C, and heating rate is 2.5 DEG C/min, and urea formaldehyde resin microsphere is in each temperature Oxidization time under gradient is 8h, when Pre oxidation reaches 200 DEG C, stops heating, obtains when being cooled to room temperature pale brown Color pre-oxidizes product;
5) the pre-oxidation product that step 4) obtains is placed in tube furnace and is continually fed into nitrogen and is carbonized, from room temperature with 10 DEG C/heating of the heating rate of min rises to 200 DEG C, and keeps the temperature 3h, then under the conditions of this temperature with the heating rate of 1 DEG C/min 300 DEG C are raised to, 3 h are kept the temperature, then with 5 DEG C/min, 600 DEG C is warming up to, keeps the temperature 3 h, it is micro- to obtain charcoal for cooled to room temperature Ball.
6) carbon microspheres that step 5) obtains are mixed with NaOH by weight 1:1, under the protection of nitrogen, with 5 DEG C/min Heating rate be raised to 750 DEG C, soaking time is 3 h;After natural cooling, it is washed to neutrality, under conditions of temperature is 60 DEG C Dry 24 h obtain three-dimensional classifying porous carbon microspheres, the positive electrode as lithium-air battery.
Embodiment 3
A kind of preparation method of porous carbon microspheres, comprising the following steps:
1) it calculates according to the mass fraction, the formaldehyde that 50 parts of concentration are 36% is heated to 40 DEG C, is existed with the pH that acid solution adjusts solution 3.5, acid solution is one of formic acid or hydrochloric acid;
2) it calculates according to the mass fraction, 10 parts of urea is added in the formalin in step 1), is reacted under stirring condition, works as solution When becoming cloudy, stop stirring, time of repose is washed to neutrality after being 12 ~ 72 h, obtains Lauxite;By Lauxite in ultrasonic function Under conditions of rate is 1000 ~ 1200w, it is ultrasonically treated 60 ~ 90min.
3) Lauxite for obtaining step 2 under conditions of heating temperature is 55 ~ 65 DEG C dry 24 ~ 48h to constant weight, Obtain urea formaldehyde resin microsphere;
4) urea formaldehyde resin microsphere for obtaining step 3) carries out gradient increased temperature formula pre-oxidation, initial pre-oxidation temperature in Muffle furnace Degree is 90 DEG C, and the temperature gradient of heating is 15 DEG C, and heating rate is 2 ~ 3 DEG C/min, and urea formaldehyde resin microsphere is in each temperature gradient Under oxidization time be 8h, when Pre oxidation reaches 200 DEG C, stop heating, it is pre- to obtain brown color when being cooled to room temperature Oxidation product;
5) the pre-oxidation product that step 4) obtains is placed in tube furnace and is continually fed into nitrogen and is carbonized, from room temperature with 8 DEG C/ The heating rate heating of min rises to 180 DEG C, and keeps the temperature 2h, then under the conditions of this temperature with the heating rate liter of 0.5 DEG C/min To 290 DEG C, 2.5 h are kept the temperature, then with 4 DEG C/min, 580 DEG C is warming up to, keeps the temperature 2.5 h, cooled to room temperature obtains charcoal Microballoon.
6) carbon microspheres that step 5) obtains are mixed with NaOH by weight 0.85:1, under the protection of nitrogen, with 4 DEG C/ The heating rate of min is raised to 740 DEG C, and soaking time is 2 h;After natural cooling, it is washed to neutrality, is 55 ~ 65 DEG C in temperature Under the conditions of dry 24 ~ 48 h, obtain porous carbon microspheres.
Embodiment 4
A kind of preparation method of porous carbon microspheres, comprising the following steps:
1) it calculates according to the mass fraction, the formaldehyde that 60 parts of concentration are 38% is heated to 40 DEG C, is existed with the pH that acid solution adjusts solution 4.5, acid solution is one of formic acid or hydrochloric acid;
2) it calculates according to the mass fraction, 14 parts of urea is added in the formalin in step 1), is reacted under stirring condition, works as solution When becoming cloudy, stop stirring, time of repose is washed to neutrality after being 12 ~ 72 h, obtains Lauxite;By Lauxite in ultrasonic function Under conditions of rate is 1000 ~ 1200w, it is ultrasonically treated 60 ~ 90min.
3) Lauxite for obtaining step 2 under conditions of heating temperature is 55 ~ 65 DEG C dry 24 ~ 48h to constant weight, Obtain urea formaldehyde resin microsphere;
4) urea formaldehyde resin microsphere for obtaining step 3) carries out gradient increased temperature formula pre-oxidation, initial pre-oxidation temperature in Muffle furnace Degree is 110 DEG C, and the temperature gradient of heating is 25 DEG C, and heating rate is 3 DEG C/min, and urea formaldehyde resin microsphere is under each temperature gradient Oxidization time be 8h, when Pre oxidation reaches 220 DEG C, stop heating, brown color pre- oxygen is obtained when being cooled to room temperature Change product;
5) the pre-oxidation product that step 4) obtains is placed in tube furnace and is continually fed into nitrogen and is carbonized, from room temperature with 12 DEG C/heating of the heating rate of min rises to 220 DEG C, and keeps the temperature 3.5h, then under the conditions of this temperature with the heating of 1.5 DEG C/min Rate is raised to 310 DEG C, keeps the temperature 3.5 h, then with 6 DEG C/min, is warming up to 620 DEG C, keeps the temperature 3.5 h, cooled to room temperature, Obtain carbon microspheres.
6) carbon microspheres that step 5) obtains are mixed with NaOH by weight 1:1.2, under the protection of nitrogen, with 6 DEG C/ The heating rate of min is raised to 760 DEG C, and soaking time is 4 h;After natural cooling, it is washed to neutrality, is 55 ~ 65 DEG C in temperature Under the conditions of dry 24 ~ 48 h, obtain porous carbon microspheres.
Embodiment 5
A kind of preparation method of porous carbon microspheres, comprising the following steps:
1) it calculates according to the mass fraction, the formaldehyde that 70 parts of concentration are 35 ~ 36% is heated to 40 DEG C, the pH of solution is adjusted with acid solution 3.5, acid solution is one of formic acid or hydrochloric acid;
2) it calculates, 12 parts of urea is added in the formalin in step 1), in order to preferably be crosslinked, in formaldehyde according to the mass fraction The hydrochloric acid solution of different solubility is added in solution, solidifies 36 h, washes into neutrality, obtains Lauxite;By Lauxite in ultrasound Under conditions of power is 1000 ~ 1200w, it is ultrasonically treated 60 ~ 90min.
3) Lauxite for obtaining step 2 under conditions of heating temperature is 55 ~ 65 DEG C dry 24 ~ 48h to constant weight, Obtain urea formaldehyde resin microsphere;
4) urea formaldehyde resin microsphere for obtaining step 3) carries out gradient increased temperature formula pre-oxidation, initial pre-oxidation temperature in Muffle furnace Degree is 100 ~ 110 DEG C, and the temperature gradient of heating is 15 ~ 25 DEG C, and heating rate is 2 ~ 3 DEG C/min, and urea formaldehyde resin microsphere is each Oxidization time under temperature gradient is 7 ~ 9h, when Pre oxidation reaches 200 ~ 220 DEG C, stops heating, is cooled to room temperature When obtain brown color pre-oxidation product;
5) the pre-oxidation product that step 4) obtains is placed in tube furnace and is continually fed into nitrogen and is carbonized, from room temperature with 8 ~ 12 DEG C/heating of the heating rate of min rises to 180 ~ 220 DEG C, and keeps the temperature 2.5 ~ 3.5h, then under the conditions of this temperature with 0.5 ~ 1.5 DEG C/heating rate of min is raised to 290 ~ 310 DEG C, 2.5 ~ 3.5 h, which are kept the temperature, then with 4 ~ 6 DEG C/min is warming up to 580 ~ 620 DEG C, 2.5 ~ 3.5 h are kept the temperature, cooled to room temperature obtains carbon microspheres.
6) carbon microspheres that step 5) obtains are mixed with NaOH by weight 1:2, under the protection of nitrogen, with 4 ~ 6 DEG C/ The heating rate of min is raised to 740 ~ 760 DEG C, and soaking time is 2 ~ 4 h;After natural cooling, be washed to neutrality, temperature be 55 ~ Dry 24 ~ 48 h, obtain porous carbon microspheres under conditions of 65 DEG C.
The present invention prepares the classification of Lauxite three-dimensional using urea and formaldehyde as raw material, using a kind of simple and environmentally-friendly method Porous carbon microspheres have the advantages that good dispersion, can be used for the positive electrode of lithium-air battery.On the one hand, three-dimensional classifying porous Structure be conducive to the transmission of oxygen, the transmitting of electronics provides place for lithium-air battery Product bulk;On the other hand, nitrogenous Carbon Materials, can speed up the absorption of oxygen, the transfer of electronics enhances the electrochemical catalysis activity of Carbon Materials.Pass through scanning Electronic Speculum observation, Lauxite precursor are presented complete spherical shape, about 6 μm of microsphere diameter or so, carry out later to precursor pre- Oxidation, charing process, sample possess more flourishing cellular structure, and it is respectively 555m that specific surface area and hole, which hold,2·g-1With 2.56 cm/g。
Technical solution cited by the present invention and embodiment and non-limiting, with technical solution cited by the present invention and Embodiment is equivalent or effect same approach is all in the range of the present invention is protected.It should also be noted that, herein, I, the relational terms such as II, III are only used to distinguish one entity or operation from another entity or operation, and Without necessarily requiring or implying that between these entities or operation, there are any actual relationship or orders.Moreover, term "include", "comprise" or any other variant thereof is intended to cover non-exclusive inclusion, so that including a series of elements Process, method, article or equipment not only include those elements, but also including other elements that are not explicitly listed, or Person is to further include for elements inherent to such a process, method, article, or device.In the absence of more restrictions, by The element that sentence "including a ..." limits, it is not excluded that in the process, method, article or apparatus that includes the element There is also other identical elements.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other The difference of embodiment, the same or similar parts in each embodiment may refer to each other.

Claims (6)

1. a kind of preparation method of porous carbon microspheres, it is characterised in that: the following steps are included:
1) it calculates according to the mass fraction, the formaldehyde that 50 ~ 60 parts of concentration are 36 ~ 38% is heated to 40 ~ 50 DEG C, adjusted with acid solution molten The pH of liquid is 3.5~4.5;
2) it calculates according to the mass fraction, 10 ~ 14 parts of urea is added in the formalin in step 1), are reacted under stirring condition, when When solution becomes cloudy, stop stirring, time of repose is washed to neutrality after being 12 ~ 72 h, obtains Lauxite;
3) Lauxite for obtaining step 2 dry 24 ~ 48h under conditions of heating temperature is 55 ~ 65 DEG C is obtained to constant weight Urea formaldehyde resin microsphere;
4) urea formaldehyde resin microsphere for obtaining step 3) carries out gradient increased temperature formula pre-oxidation in Muffle furnace, obtains the pre- oxygen of brown color Change product;
5) the pre-oxidation product that step 4) obtains is placed in tube furnace and is continually fed into nitrogen and is carbonized, obtain carbon microspheres;
6) carbon microspheres that step 5) obtains are mixed with NaOH by weight 1:1 ~ 0.85:1, under the protection of nitrogen, with 4 ~ 6 DEG C/heating rate of min is raised to 740 ~ 760 DEG C, soaking time is 2 ~ 4 h;After natural cooling, it is washed to neutrality, is in temperature Dry 24 ~ 48 h, obtain porous carbon microspheres under conditions of 55 ~ 65 DEG C.
2. a kind of preparation method of porous carbon microspheres according to claim 1, it is characterised in that: the acid solution in step 1) For one of formic acid or hydrochloric acid.
3. a kind of preparation method of porous carbon microspheres according to claim 1, it is characterised in that: the ureaformaldehyde tree in step 3) Rouge under conditions of ultrasonic power is 1000 ~ 1200w, is ultrasonically treated 60 ~ 90min before it is dried.
4. a kind of preparation method of porous carbon microspheres according to claim 1, it is characterised in that: gradient increased temperature in step 4) The process of formula pre-oxidation are as follows: initial Pre oxidation is 100 ~ 110 DEG C, and the temperature gradient of heating is 15 ~ 25 DEG C, Lauxite Oxidization time of the microballoon under each temperature gradient is 7 ~ 9h, when Pre oxidation reaches 200 ~ 220 DEG C, stops heating, to Pre-oxidation product is obtained when being cooled to room temperature.
5. a kind of preparation method of porous carbon microspheres according to claim 4, it is characterised in that: the heating speed in step 4) Rate is 2 ~ 3 DEG C/min.
6. a kind of preparation method of porous carbon microspheres according to claim 1, it is characterised in that: the mistake being carbonized in step 5) Journey are as follows: rise to 180 ~ 220 DEG C from room temperature with the heating of the heating rate of 8 ~ 12 DEG C/min, and under the conditions of this temperature heat preservation 2.5 ~ 3.5h, then be raised to 290 ~ 310 DEG C with the heating rate of 0.5 ~ 1.5 DEG C/min, keeps the temperature 2.5 ~ 3.5 h, then with 4 ~ 6 DEG C/min, 580 ~ 620 DEG C are warming up to, 2.5 ~ 3.5 h, cooled to room temperature are kept the temperature.
CN201910333949.6A 2019-04-24 2019-04-24 A kind of preparation method of porous carbon microspheres Pending CN110002426A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111408348A (en) * 2020-04-28 2020-07-14 南阳师范学院 Preparation method of straw-based porous biochar nanospheres

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106654278A (en) * 2016-11-29 2017-05-10 南方科技大学 Novel carbon sphere and preparation method and application thereof
CN108584952A (en) * 2018-08-01 2018-09-28 国家能源投资集团有限责任公司 Spherical porous charcoal and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106654278A (en) * 2016-11-29 2017-05-10 南方科技大学 Novel carbon sphere and preparation method and application thereof
CN108584952A (en) * 2018-08-01 2018-09-28 国家能源投资集团有限责任公司 Spherical porous charcoal and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111408348A (en) * 2020-04-28 2020-07-14 南阳师范学院 Preparation method of straw-based porous biochar nanospheres

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