CN104058401A - Preparation method of porous carbon microspheres - Google Patents
Preparation method of porous carbon microspheres Download PDFInfo
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- CN104058401A CN104058401A CN201410328871.6A CN201410328871A CN104058401A CN 104058401 A CN104058401 A CN 104058401A CN 201410328871 A CN201410328871 A CN 201410328871A CN 104058401 A CN104058401 A CN 104058401A
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Abstract
The invention relates to a preparation method of porous carbon microspheres and belongs to the field of nano material synthesis. The preparation method of the porous carbon microspheres mainly comprises the steps of uniformly mixing m-benzenediol and formaldehyde, then adding deionized water and stirring to form a uniform carbon source precursor solution; adding polymeric microspheres which are of a hollow structure into the carbon source precursor solution obtained in the step one, thus obtaining a phenolic resin-polymer core-shell structure; adding acetic acid to the phenolic resin-polymer core-shell structure product and heating for curing at the temperature of 40-80 DEG C, thus obtaining cured phenolic resin-polymer core-shell structure microspheres; removing polymers out of the cured phenolic resin-polymer core-shell structure microspheres by using an organic solvent like tetrahydrofuran, thus obtaining resin microspheres; drying the core-shell structure microspheres at the temperature of 60-80 DEG C and carbonizing in a high temperature furnace, thus obtaining the porous carbon microspheres are obtained. The preparation method of the porous carbon microspheres has the advantages that the adopted raw materials are common chemical raw materials, and cost is low; a technology is simple; large-scale industrial production is facilitated.
Description
Technical field
The invention belongs to the synthetic field of nano material, be specifically related to a kind of preparation method of carbosphere.
Background technology
Porous carbon microsphere is widely used owing to having high-specific surface area, and particularly porous resin and carbosphere, have its large specific surface area, large pore volume, good unreactiveness and etc. performance in support of the catalyst, sorbent material, pharmaceutical carrier, the fields such as mould material are widely used.
The method of preparing porous carbon microsphere has a variety of: 1 hard template method 2 soft template method 3 liquid phase synthesizing method 4 vapor-phase thermal cracking method 5 hydrothermal methods etc., every kind of method has its relative merits.For example: although soft template method is simple, the microspheres quality of preparation is not as hard template method; Hydrothermal method large-scale production is more difficult.So, efficient, low cost, the method for preparing to environmental friendliness high quality porous microsphere is the final pursuit of ownership system Preparation Method.
Therefore, single dispersed carbon microsphere preparation technology that employing can industrialization, is conducive to the further investigation of porous mono-dispersion microsphere and applies.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of carbosphere.Utilize the industrialized polymer microballoon with hollow structure as template, efficiently prepare carbosphere.
The present invention is achieved by the following technical solutions:
Step 1: take Resorcinol and formaldehyde mixes, then add deionized water and stirring, form uniform carbon source precursor aqueous solution, standby; Wherein, the mol ratio of described Resorcinol and formaldehyde is 1:2, and the massfraction of resorcinol-formaldehyde in carbon precursor aqueous solution is 15wt%～60wt%.
Step 2: the polymer microballoon of hollow structure is joined to step 1 and obtain in carbon source precursor aqueous solution, sealing room temperature is placed and it reacted in 24-72 hour, and then eccentric cleaning, obtains resol-polymer core-shell structure.Wherein, polymer microballoon and carbon source precursor aqueous solution mass ratio are 1:3-5.
Step 3: step 2 product adds acetic acid at 40-80 degree Celsius and is heating and curing, the resol-polymer core-shell structure microballoon after being solidified.
Step 4: prepare carbosphere: the product 60-80 that step 3 makes ℃ dry; then carbonization in High Temperature Furnaces Heating Apparatus; speed with 0.1L/ minute passes into argon shield; speed with 5K/ minute is warming up to 100-120 ℃; dry and within 1 hour, remove steam; then with the speed of 5K/ minute, be warming up to 420 ℃, be incubated after 3-5 hour and with the speed of 5K/ minute, be warming up to 800-1000 ℃ of carbonization 2-4 hour and then pass into carbonic acid gas and activate 1-2 hour, obtain porous carbon microsphere.
In above-mentioned preparation method's step 1, different precursor aqueous solution concentration can regulate and control the pore structure of carbosphere.
Feature of the present invention is as follows:
(1) provide a kind of novel method of preparing carbosphere, different from conventional preparation method, the present invention adopts hollow polymer microsphere as template, and this method is convenient effectively.
(2) carbosphere that prepared by the present invention, particle diameter is even, pattern homogeneous.
(3) carbosphere that prepared by the present invention, the aperture of the carbon of core is adjustable.
(4) the present invention's equipment used is simple; Raw material used is conventional industrial chemicals, and cost is low; Technique is simple; The industrial production that is conducive to mass-producing.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of carbosphere.
Fig. 2 is the stereoscan photograph of carbosphere.
Fig. 3 is the stereoscan photograph of carbosphere.
Specific embodiments
Below in conjunction with accompanying drawing and example, enforcement of the present invention is further described, but enforcement of the present invention is not limited to this.
Embodiment 1:
Prepare carbosphere.Take 3.88g Resorcinol, 5.2ml formaldehyde, mix and blend 1 hour, adds 30ml deionized water, and mix and blend forms uniform carbon precursor aqueous solution for 2 hours, measures 15ml polymer hollow particles, is uniformly mixed under room temperature and places 24 hours.Eccentric cleaning, adds 80 ℃ of 1ml acetic acid to solidify 24 hours.
60 ℃ dry, and powder is put into high-temperature atmosphere furnace, with the speed of 0.1L/ minute, passes into argon gas, with the speed of 5K/ minute, is warming up to 100 ℃, is incubated 2 hours.With the speed of 5K/ minute, be warming up to 420 ℃ of insulations 3 hours again, and then the speed of 5K/ minute is warming up to 800 ℃ of insulations 4 hours, changes logical carbon dioxide activation 2 hours, obtain carbosphere.
Embodiment 2:
Prepare carbosphere.Take 3.88g Resorcinol, 5.2ml formaldehyde, mix and blend 1 hour, adds 30ml deionized water, and mix and blend forms uniform carbon precursor aqueous solution for 2 hours, measures 15ml polymer hollow particles, is uniformly mixed under room temperature and places 48 hours.Eccentric cleaning, adds 40 ℃ of 1ml acetic acid to solidify 24 hours.
60 ℃ dry, and powder is put into high-temperature atmosphere furnace, with the speed of 0.1L/ minute, passes into argon gas, with the speed of 5K/ minute, is warming up to 100 ℃, is incubated 2 hours.With the speed of 5K/ minute, be warming up to 420 ℃ of insulations 3 hours again, and then the speed of 5K/ minute is warming up to 900 ℃ of insulations 3 hours, changes logical carbon dioxide activation 1 hour, obtain carbosphere.
Embodiment 3:
Prepare carbosphere.Take 3.88g Resorcinol, 5.2ml formaldehyde, mix and blend 1 hour, adds 30ml deionized water, and mix and blend forms uniform carbon precursor aqueous solution for 2 hours, measures 15ml polymer hollow particles, is uniformly mixed under room temperature and places 24 hours.Eccentric cleaning, adds 60 ℃ of 1ml acetic acid to solidify 24 hours.
60 ℃ dry, and powder is put into high-temperature atmosphere furnace, with the speed of 0.1L/ minute, passes into argon gas, with the speed of 5K/ minute, is warming up to 100 ℃, is incubated 2 hours.With the speed of 5K/ minute, be warming up to 420 ℃ of insulations 3 hours again, and then the speed of 5K/ minute is warming up to 1000 ℃ of insulations 3 hours, changes logical carbon dioxide activation 1 hour, obtain carbosphere.
Embodiment 4:
Prepare carbosphere.Take 3.88g Resorcinol, 5.2ml formaldehyde, mix and blend 1 hour, adds 60ml deionized water, and mix and blend forms uniform carbon precursor aqueous solution for 2 hours, measures 15ml polymer hollow particles, is uniformly mixed under room temperature and places 72 hours.Eccentric cleaning, adds 80 ℃ of 1ml acetic acid to solidify 24 hours.
60 ℃ dry, and powder is put into high-temperature atmosphere furnace, with the speed of 0.1L/ minute, passes into argon gas, with the speed of 5K/ minute, is warming up to 100 ℃, is incubated 2 hours.With the speed of 5K/ minute, be warming up to 420 ℃ of insulations 3 hours again, and then the speed of 5K/ minute is warming up to 900 ℃ of insulations 2 hours, changes logical carbon dioxide activation 2 hours, obtain carbosphere.
Embodiment 5:
Prepare carbosphere.Take 3.88g Resorcinol, 5.2ml formaldehyde, mix and blend 1 hour, adds 30ml deionized water, and mix and blend forms uniform carbon precursor aqueous solution for 2 hours, measures 15ml polymer hollow particles, is uniformly mixed under room temperature and places 24 hours.Eccentric cleaning, adds 80 ℃ of 1ml acetic acid to solidify 24 hours.
60 ℃ dry, and powder is put into high-temperature atmosphere furnace, with the speed of 0.1L/ minute, passes into argon gas, with the speed of 5K/ minute, is warming up to 100 ℃, is incubated 2 hours.With the speed of 5K/ minute, be warming up to 420 ℃ of insulations 3 hours again, and then the speed of 5K/ minute is warming up to 900 ℃ of insulations 2 hours, changes logical carbon dioxide activation 2 hours, obtain carbosphere.
Claims (1)
1. a preparation method for porous carbon microsphere, is characterized in that:
Step 1, take Resorcinol and formaldehyde mixes, then add deionized water and stirring, form uniform carbon source precursor aqueous solution, standby; The mol ratio of described Resorcinol and formaldehyde is 1:2, and the massfraction of resorcinol-formaldehyde in carbon precursor aqueous solution is 15wt%～60wt%;
Step 2, the polymer microballoon of hollow structure is joined to step 1 obtain in carbon source precursor aqueous solution, sealing room temperature is placed and it was reacted in 24-72 hour, and then eccentric cleaning, obtains resol-polymer core-shell structure; Wherein, polymer microballoon and carbon source precursor aqueous solution mass ratio are 1:3-5;
Step 3: resol-polymer core-shell structure is added to acetic acid at 40-80 ℃ and be heating and curing, the resol-polymer core-shell structure microballoon after being solidified;
Step 4: prepare carbosphere: the resol-polymer core-shell structure microballoon after solidifying is dry at 60-80 ℃; then carbonization in High Temperature Furnaces Heating Apparatus; speed with 0.1L/ minute passes into argon shield; speed with 5K/ minute is warming up to 100-120 ℃; dry and within 1 hour, remove steam; then with the speed of 5K/ minute, be warming up to 420 ℃; be incubated after 3-5 hour and with the speed of 5K/ minute, be warming up to 800-1000 ℃ of carbonization 2-4 hour and then pass into carbonic acid gas and activate 1-2 hour, obtain porous carbon microsphere.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016150406A1 (en) * | 2015-03-26 | 2016-09-29 | 中国科学院化学研究所 | Single-layer and multi-layer hollow carbon nanosphere, and preparation and application thereof |
| CN106824132A (en) * | 2017-03-03 | 2017-06-13 | 南京理工大学 | A kind of water process chromium sorbing material and preparation method thereof |
| CN112158822A (en) * | 2020-09-09 | 2021-01-01 | 中国科学院山西煤炭化学研究所 | Preparation method of porous carbon microspheres |
| CN112547008A (en) * | 2020-11-13 | 2021-03-26 | 广东宜纳新材料科技有限公司 | Carbon microsphere for adsorbing dioxin |
| CN114685282A (en) * | 2022-05-10 | 2022-07-01 | 安徽东至广信农化有限公司 | Production process for hydrogenation reduction of o-phenylenediamine |
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| CN102718205A (en) * | 2012-06-27 | 2012-10-10 | 北京科技大学 | Method for preparing three-dimensional hierarchical porous carbon |
| CN102716702A (en) * | 2012-06-27 | 2012-10-10 | 北京科技大学 | Preparation method of layered porous carbon particles in yolk-shell structure |
| CN103880006A (en) * | 2014-03-13 | 2014-06-25 | 常州中科海纳碳素科技有限公司 | Method for preparing large particle size phenolic resin spherical activated carbon |
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- 2014-07-11 CN CN201410328871.6A patent/CN104058401A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718205A (en) * | 2012-06-27 | 2012-10-10 | 北京科技大学 | Method for preparing three-dimensional hierarchical porous carbon |
| CN102716702A (en) * | 2012-06-27 | 2012-10-10 | 北京科技大学 | Preparation method of layered porous carbon particles in yolk-shell structure |
| CN103880006A (en) * | 2014-03-13 | 2014-06-25 | 常州中科海纳碳素科技有限公司 | Method for preparing large particle size phenolic resin spherical activated carbon |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016150406A1 (en) * | 2015-03-26 | 2016-09-29 | 中国科学院化学研究所 | Single-layer and multi-layer hollow carbon nanosphere, and preparation and application thereof |
| CN106824132A (en) * | 2017-03-03 | 2017-06-13 | 南京理工大学 | A kind of water process chromium sorbing material and preparation method thereof |
| CN106824132B (en) * | 2017-03-03 | 2019-05-07 | 南京理工大学 | A kind of water process chromium adsorbent material and preparation method thereof |
| CN112158822A (en) * | 2020-09-09 | 2021-01-01 | 中国科学院山西煤炭化学研究所 | Preparation method of porous carbon microspheres |
| CN112547008A (en) * | 2020-11-13 | 2021-03-26 | 广东宜纳新材料科技有限公司 | Carbon microsphere for adsorbing dioxin |
| CN114685282A (en) * | 2022-05-10 | 2022-07-01 | 安徽东至广信农化有限公司 | Production process for hydrogenation reduction of o-phenylenediamine |
| WO2023216458A1 (en) * | 2022-05-10 | 2023-11-16 | 杨镭 | Production process for hydrogenation of o-phenylenediamine |
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