CN101721972A - Method for preparing spherical activated carbon with large CO2absorption capacity - Google Patents
Method for preparing spherical activated carbon with large CO2absorption capacity Download PDFInfo
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- CN101721972A CN101721972A CN200910200119A CN200910200119A CN101721972A CN 101721972 A CN101721972 A CN 101721972A CN 200910200119 A CN200910200119 A CN 200910200119A CN 200910200119 A CN200910200119 A CN 200910200119A CN 101721972 A CN101721972 A CN 101721972A
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Abstract
The invention relates to a method for preparing a spherical activated carbon with large CO2absorption capacity. The method comprises the following steps: filling ethanol solution of phenolic resin, a curing agent and a dispersing agent in an autoclave which is filled with solvent; mixing the mixture to obtain phenolic resin spheres; placing the phenolic resin spheres in a microwave device to solidify the spheres by microwaves; and finally placing the solidified product into a carbonizing furnace to perform high-temperature carbonization and activating treatment to obtain the phenolic resin-based spherical activated carbon. Compared with the prior art, the spherical activated carbon obtained by the invention has the advantages of relatively narrow particle size distribution, substantially controllable particle size range, relatively high stacking density, 55 percent reduction of production energy consumption, and 43.6 percent increase of CO2absorption capacity.
Description
Technical field
The present invention relates to a kind of preparation method of spherical activated charcoal, especially relate to a kind of CO
2Preparation method with spherical activated charcoal of big adsorption capacity.
Background technology
Spherical activated charcoal (SAC) is a kind of novel high-performance active carbon, an important branch as active carbon, have the advantage of common active carbon and the special shape of Yin Qi concurrently and have some special advantages: smooth surface, good sphericity, packed density height, wearability are good, even particle distribution, flow resistance are little, be not easy bits, mechanical strength height, the fast and good serial advantages such as physiological compatibility of adsorption desorption speed in the use, be widely used aspect senior environmental protection, chemical industry and the physiological medical science, and more and more be subjected to researcher's attention.
To CO
2Absorption research in find, influence spherical activated charcoal to CO
2The principal element of adsorption capacity is the aperture and the distribution thereof of active carbon, and the pore-size distribution of active carbon depends on raw material precursor and preparation process to a great extent.In body series, with the raw material of phenolic resins, utilize suspension method as the preparation spherical activated charcoal, phenolic resins is by solidifying to form the bead with initial space.And the pore-size distribution of final products spherical activated charcoal is subject to the initial space that forms in the balling-up process to a great extent.Therefore, the curing mechanism of research phenolic resin ball and then influences solidification process to a certain extent, and the spherical activated charcoal of the pore-size distribution that obtains expecting is had very big meaning.
Summary of the invention
Purpose of the present invention be exactly provide in order to overcome the defective that above-mentioned prior art exists that a kind of energy consumption is lower, particle diameter is controlled, bulk density is bigger to CO
2Preparation method with spherical activated charcoal of big adsorption capacity.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of to CO
2Have the preparation method of the spherical activated charcoal of big adsorption capacity, it is characterized in that, this method may further comprise the steps:
(1) suspension method prepares alkyd resin based ball: phenolic resins ethanolic solution, curing agent and dispersant are placed the autoclave that solvent is housed, open agitating device, the control stir speed (S.S.) is 250-850rpm, heating rate is 0.1-2 ℃/min, stirring reaction to temperature reaches 110-150 ℃, the autoclave internal pressure is 0.2-0.4MPa, promptly obtains phenolic resin ball;
(2) microwave curing: the phenolic resin ball that obtains is placed microwave device, the control microwave power is 40-80W, radiation 10-30min, again microwave power is adjusted to 240-400W, radiation 10-30min, at last microwave power is adjusted to 640-800W, radiation 15-30min, the phenolic resin ball that obtains solidifying;
(3) high-temperature process: the phenolic resin ball that solidifies is placed retort, in retort, feed inert gas, the control heating rate is 1-2 ℃/min, the retort temperature is risen to 800-1000 ℃, insulation 0.5-1h feeds active gases then in retort, activation 0.5-5h, temperature with retort naturally cools to 20-25 ℃ at last, promptly obtains product.
The weight ratio of phenolic resins ethanolic solution, curing agent, dispersant and solvent in the described step (1) is 1: (0.06-0.2): (0.0001-0.06): (3-6).
The concentration expressed in percentage by weight of the phenolic resins ethanolic solution in the described step (1) is 50-70%.
Curing agent in the described step (1) comprises di-2-ethylhexylphosphine oxide hexamethylene alkanamine, diethyl amino propylamine, hexamethylenetetramine or trimethylhexamethylenediamine.
Dispersant in the described step (1) comprises polyvinyl alcohol.
Solvent in the described step (1) comprises deionized water, acetone or alcohol.
Inert gas in the described step (3) comprises high pure nitrogen.
Active gases in the described step (3) comprises air, oxygen, steam or nitrogen.
Compared with prior art, the present invention has the following advantages:
(1) spherical activated charcoal that obtains, particle diameter narrow distribution, particle size range are controlled substantially;
(2) adopt microwave curing, reduce 80% than traditional approach hardening time, and energy consumption reduces 55%;
(3) there is not the thermograde in the heat cure in this spherical activated charcoal because microwave curing belongs to " in the molecule " heating, and then has avoided the inhomogeneous and incomplete of curing, so bulk density is far longer than other spherical activated charcoals.
(4) the made spherical activated charcoal of this law because quick, the unique mode of heating of microwave has considerable influence to cured resin structure and performance, produces specific pore structure, to CO
2Adsorption capacity 2.24mmol/g, and in the contrast test without the spherical activated charcoal of microwave radiation to CO
2Adsorption capacity be 1.56mmol/g, improved 43.6%.
The specific embodiment
The present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
(1) suspension method prepares phenolic resin base globe activated char: with concentration expressed in percentage by weight is that 50% phenolic resins ethanolic solution, curing agent di-2-ethylhexylphosphine oxide hexamethylene alkanamine and polyethylene of dispersing agent alcohol place the autoclave that deionized water is housed, wherein the weight ratio of phenolic resins ethanolic solution, di-2-ethylhexylphosphine oxide hexamethylene alkanamine, polyvinyl alcohol and deionized water is 1: 0.06: 0.0001: 3, open agitating device, the control stir speed (S.S.) is 250rpm, heating rate is 2 ℃/min, stirring reaction to temperature reaches 150 ℃, the autoclave internal pressure is 0.2MPa, obtains phenolic resin ball;
(2) microwave curing: the phenolic resin ball that obtains is placed microwave device, and the control microwave power is 40W, radiation 10min, again microwave power is adjusted to 240W, radiation 30min is adjusted to 640W with microwave power at last, radiation 30min, the phenolic resin ball that obtains solidifying;
(3) high-temperature process: the phenolic resin ball that solidifies is placed retort, in retort, feed high pure nitrogen, the control heating rate is 1 ℃/min, the retort temperature is risen to 800 ℃, under this temperature, be incubated 0.5h, in retort, feed water vapour then, activation 5h, temperature with retort naturally cools to 20 ℃ at last, promptly obtains spherical activated charcoal.
Embodiment 2
(1) suspension method prepares phenolic resin base globe activated char: with concentration expressed in percentage by weight is that inferior diethyl amino propylamine of 60% phenolic resins ethanolic solution, curing agent and polyethylene of dispersing agent alcohol place the autoclave that ethanol is housed, wherein the weight ratio of phenolic resins ethanolic solution, inferior diethyl amino propylamine, polyvinyl alcohol and ethanol is 1: 0.12: 0.01: 5, open agitating device, the control stir speed (S.S.) is 550rpm, heating rate is 1 ℃/min, stirring reaction to temperature reaches 130 ℃, the autoclave internal pressure is 0.3MPa, obtains phenolic resin ball;
(2) microwave curing: the phenolic resin ball that obtains is placed microwave device, and the control microwave power is 50W, radiation 6min, again microwave power is adjusted to 350W, radiation 20min is adjusted to 750W with microwave power at last, radiation 25min, the phenolic resin ball that obtains solidifying;
(3) high-temperature process: the phenolic resin ball that solidifies is placed retort, in retort, feed high pure nitrogen, the control heating rate is 2 ℃/min, the retort temperature is risen to 300 ℃, regulating heating rate again is 1 ℃/min, the retort temperature is risen to 600 ℃, regulating heating rate then is 2 ℃/min, the retort temperature is risen to 800 ℃ and be incubated 0.5h under this temperature, and the control and regulation heating rate is 2 ℃/min, and the retort temperature is risen to 900 ℃ and be incubated 0.5h under this temperature, in retort, feed water vapour then, activation 0.5-1.5h, the temperature with retort naturally cools to 20 ℃ of room temperatures at last, promptly obtains phenolic resin base globe activated char.This spherical activated charcoal is carried out CO
2The adsorption capacity test, the result shows: this spherical activated charcoal is to CO
2Adsorption capacity 2.24mmol/g, improved 43.6% than adsorption capacity without the spherical activated charcoal of microwave radiation.
Embodiment 3
(1) suspension method prepares phenolic resin base globe activated char: with concentration expressed in percentage by weight is that 60% phenolic resins ethanolic solution, curing agent hexamethylenetetramine and polyethylene of dispersing agent alcohol place the autoclave that deionized water is housed, wherein the weight ratio of phenolic resins ethanolic solution, hexamethylenetetramine, polyvinyl alcohol and deionized water is 1: 0.15: 0.03: 5, open agitating device, the control stir speed (S.S.) is 600rpm, heating rate is 1 ℃/min, stirring reaction to temperature reaches 110 ℃, the autoclave internal pressure is 0.4MPa, obtains phenolic resin ball;
(2) microwave curing: the phenolic resin ball that obtains is placed microwave device, and the control microwave power is 80W, radiation 3min, again microwave power is adjusted to 400W, radiation 10min is adjusted to 800W with microwave power at last, radiation 15min, the phenolic resin ball that obtains solidifying;
(3) high-temperature process: the phenolic resin ball that solidifies is placed retort, in retort, feed high pure nitrogen, the control heating rate is 1 ℃/min, the retort temperature is risen to 1000 ℃, under this temperature, be incubated 5h, in retort, feed water vapour then, activation 0.5h, temperature with retort naturally cools to 25 ℃ at last, promptly obtains spherical activated charcoal.
Embodiment 4
(1) suspension method prepares phenolic resin base globe activated char: with concentration expressed in percentage by weight is that 70% phenolic resins ethanolic solution, curing agent trimethylhexamethylenediamine and polyethylene of dispersing agent alcohol place the autoclave that acetone is housed, wherein the weight ratio of phenolic resins ethanolic solution, trimethylhexamethylenediamine, polyvinyl alcohol and acetone is 1: 0.2: 0.06: 6, open agitating device, the control stir speed (S.S.) is 850rpm, heating rate is 1 ℃/min, stirring reaction to temperature reaches 150 ℃, the autoclave internal pressure is 0.4MPa, obtains phenolic resin ball;
(2) microwave curing: the phenolic resin ball that obtains is placed microwave device, and the control microwave power is 80W, radiation 3min, again microwave power is adjusted to 300W, radiation 15min is adjusted to 700W with microwave power at last, radiation 20min, the phenolic resin ball that obtains solidifying;
(3) high-temperature process: the phenolic resin ball that solidifies is placed retort, in retort, feed high pure nitrogen, the control heating rate is 2 ℃/min, the retort temperature is risen to 900 ℃, under this temperature, be incubated 3h, in retort, feed water vapour then, activation 2h, temperature with retort naturally cools to 25 ℃ at last, promptly obtains spherical activated charcoal.
Claims (8)
1. one kind to CO
2Have the preparation method of the spherical activated charcoal of big adsorption capacity, it is characterized in that, this method may further comprise the steps:
(1) suspension method prepares alkyd resin based ball: phenolic resins ethanolic solution, curing agent and dispersant are placed the autoclave that solvent is housed, open agitating device, the control stir speed (S.S.) is 250-850rpm, heating rate is 0.1-2 ℃/min, stirring reaction to temperature reaches 110-150 ℃, the autoclave internal pressure is 0.2-0.4MPa, promptly obtains phenolic resin ball;
(2) microwave curing: the phenolic resin ball that obtains is placed microwave device, the control microwave power is 40-80W, radiation 10-30min, again microwave power is adjusted to 240-400W, radiation 10-30min, at last microwave power is adjusted to 640-800W, radiation 15-30min, the phenolic resin ball that obtains solidifying;
(3) high-temperature process: the phenolic resin ball that solidifies is placed retort, in retort, feed inert gas, the control heating rate is 1-2 ℃/min, the retort temperature is risen to 800-1000 ℃, insulation 0.5-1h feeds active gases then in retort, activation 0.5-5h, temperature with retort naturally cools to 20-25 ℃ at last, promptly obtains product.
2. according to claim 1 a kind of to CO
2Have the preparation method of the spherical activated charcoal of big adsorption capacity, it is characterized in that, the weight ratio of phenolic resins ethanolic solution, curing agent, dispersant and solvent in the described step (1) is 1: (0.06-0.2): (0.0001-0.06): (3-6).
3. according to claim 1 a kind of to CO
2Have the preparation method of the spherical activated charcoal of big adsorption capacity, it is characterized in that, the concentration expressed in percentage by weight of the phenolic resins ethanolic solution in the described step (1) is 50-70%.
4. according to claim 1 a kind of to CO
2Have the preparation method of the spherical activated charcoal of big adsorption capacity, it is characterized in that, the curing agent in the described step (1) comprises di-2-ethylhexylphosphine oxide hexamethylene alkanamine, diethyl amino propylamine, hexamethylenetetramine or trimethylhexamethylenediamine.
5. according to claim 1 a kind of to CO
2Have the preparation method of the spherical activated charcoal of big adsorption capacity, it is characterized in that, the dispersant in the described step (1) comprises polyvinyl alcohol.
6. according to claim 1 a kind of to CO
2Have the preparation method of the spherical activated charcoal of big adsorption capacity, it is characterized in that, the solvent in the described step (1) comprises deionized water, acetone or alcohol.
7. according to claim 1 a kind of to CO
2Have the preparation method of the spherical activated charcoal of big adsorption capacity, it is characterized in that, the inert gas in the described step (3) comprises high pure nitrogen.
8. according to claim 1 a kind of to CO
2Have the preparation method of the spherical activated charcoal of big adsorption capacity, it is characterized in that, the active gases in the described step (3) comprises air, oxygen, steam or nitrogen.
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| CN2009102001192A CN101721972B (en) | 2009-12-08 | 2009-12-08 | Method for preparing spherical activated carbon with large CO2 absorption capacity |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430396A (en) * | 2011-09-16 | 2012-05-02 | 华东理工大学 | Synthetic method of spherical nitrogen-enriched micro-reticular resin for CO2 adsorption |
| CN102502624A (en) * | 2011-10-22 | 2012-06-20 | 中国科学院山西煤炭化学研究所 | Preparation method for acquiring spherical activated carbon of carbon dioxide |
| CN102500320A (en) * | 2011-10-22 | 2012-06-20 | 中国科学院山西煤炭化学研究所 | Method for improving resin carbon specific surface area so as to facilitate capture of CO2 |
| CN103056964A (en) * | 2013-01-10 | 2013-04-24 | 湖南南方搏云新材料有限责任公司 | Method for curing carbon/carbon composite blanks by industrial microwave oven |
| CN105772089A (en) * | 2016-04-25 | 2016-07-20 | 张玲 | Preparation method of triethyl citrate catalyst |
| CN107051382A (en) * | 2017-04-21 | 2017-08-18 | 中国科学院城市环境研究所 | A kind of carbon dioxide adsorption porous carbon nanofiber material and preparation method thereof |
| CN107262027A (en) * | 2016-04-05 | 2017-10-20 | 现代自动车株式会社 | Method For Manufacturing Activated Carbon |
| CN107876005A (en) * | 2017-10-31 | 2018-04-06 | 上海绿强新材料有限公司 | A kind of adsorbent for removing chlorinated contaminants and its preparation method and application |
| CN108014777A (en) * | 2016-11-01 | 2018-05-11 | 中国石油化工股份有限公司 | The system supported hydrogenation catalyst of carbon carrier for hydrogenation catalyst and preparation method thereof, palladium and its application |
| WO2019223113A1 (en) * | 2018-05-21 | 2019-11-28 | 成都威能士医疗科技有限公司 | Method of capturing and enriching carbon dioxide from air by using active material or modified active material and application thereof |
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2009
- 2009-12-08 CN CN2009102001192A patent/CN101721972B/en not_active Expired - Fee Related
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102430396B (en) * | 2011-09-16 | 2013-11-13 | 华东理工大学 | Synthetic method of spherical nitrogen-enriched micro-reticular resin for CO2 adsorption |
| CN102430396A (en) * | 2011-09-16 | 2012-05-02 | 华东理工大学 | Synthetic method of spherical nitrogen-enriched micro-reticular resin for CO2 adsorption |
| CN102502624A (en) * | 2011-10-22 | 2012-06-20 | 中国科学院山西煤炭化学研究所 | Preparation method for acquiring spherical activated carbon of carbon dioxide |
| CN102500320A (en) * | 2011-10-22 | 2012-06-20 | 中国科学院山西煤炭化学研究所 | Method for improving resin carbon specific surface area so as to facilitate capture of CO2 |
| CN102502624B (en) * | 2011-10-22 | 2013-04-17 | 中国科学院山西煤炭化学研究所 | Preparation method for acquiring spherical activated carbon of carbon dioxide |
| CN102500320B (en) * | 2011-10-22 | 2013-05-01 | 中国科学院山西煤炭化学研究所 | Method for improving resin carbon specific surface area so as to facilitate capture of CO2 |
| CN103056964A (en) * | 2013-01-10 | 2013-04-24 | 湖南南方搏云新材料有限责任公司 | Method for curing carbon/carbon composite blanks by industrial microwave oven |
| CN103056964B (en) * | 2013-01-10 | 2015-11-18 | 湖南南方搏云新材料有限责任公司 | A kind of method of industrial microwave oven solidification carbon/carbon composite base substrate |
| CN107262027A (en) * | 2016-04-05 | 2017-10-20 | 现代自动车株式会社 | Method For Manufacturing Activated Carbon |
| CN107262027B (en) * | 2016-04-05 | 2021-06-08 | 现代自动车株式会社 | Method for producing activated carbon |
| CN105772089A (en) * | 2016-04-25 | 2016-07-20 | 张玲 | Preparation method of triethyl citrate catalyst |
| CN108014777A (en) * | 2016-11-01 | 2018-05-11 | 中国石油化工股份有限公司 | The system supported hydrogenation catalyst of carbon carrier for hydrogenation catalyst and preparation method thereof, palladium and its application |
| CN108014777B (en) * | 2016-11-01 | 2020-11-10 | 中国石油化工股份有限公司 | Carbon carrier for hydrogenation catalyst, preparation method of carbon carrier, palladium-based supported hydrogenation catalyst and application of palladium-based supported hydrogenation catalyst |
| CN107051382B (en) * | 2017-04-21 | 2020-12-18 | 中国科学院城市环境研究所 | Porous carbon nanofiber material for carbon dioxide adsorption and preparation method thereof |
| CN107051382A (en) * | 2017-04-21 | 2017-08-18 | 中国科学院城市环境研究所 | A kind of carbon dioxide adsorption porous carbon nanofiber material and preparation method thereof |
| CN107876005A (en) * | 2017-10-31 | 2018-04-06 | 上海绿强新材料有限公司 | A kind of adsorbent for removing chlorinated contaminants and its preparation method and application |
| WO2019223113A1 (en) * | 2018-05-21 | 2019-11-28 | 成都威能士医疗科技有限公司 | Method of capturing and enriching carbon dioxide from air by using active material or modified active material and application thereof |
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