CN104310396A - Preparation method of activated carbon with capability of efficiently adsorbing CO2 - Google Patents

Preparation method of activated carbon with capability of efficiently adsorbing CO2 Download PDF

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CN104310396A
CN104310396A CN201410560606.0A CN201410560606A CN104310396A CN 104310396 A CN104310396 A CN 104310396A CN 201410560606 A CN201410560606 A CN 201410560606A CN 104310396 A CN104310396 A CN 104310396A
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CN104310396B (en
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李开喜
万柳
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Shanxi Institute of Coal Chemistry of CAS
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Shanxi Institute of Coal Chemistry of CAS
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Abstract

The invention provides a preparation method of activated carbon with capability of efficiently adsorbing CO2. The preparation method comprises the following steps: adding p-aminophenol after reaction of melamine and formaldehyde, carrying out reflux reaction for 4-8h, cooling until room temperature, then adding a methanol solution of F127 or P123, respectively segmenting at temperatures of 100-120 DEG C, 130-160 DEG C, 170-190 DEG C, 210-230 DEG C and 240-260 DEG C, respectively curing to obtain nitrogen-containing prepolymer, then carbonizing, mixing a carbonized material and KOH, activating for 0.5-2.0h, repeatedly washing by deionized water until neutrality finally, and drying to obtain the product. The activated carbon has the advantages of high specific surface area, high nitrogen content and high CO2 adsorption performance.

Description

A kind of efficient adsorption CO 2the preparation method of gac
Technical field
The present invention relates to a kind of preparation method of gac, relate in particular to a kind of efficient adsorption CO 2the preparation method of gac.
Background technology
Along with going from bad to worse of the environmental problems such as global warming, conventional fossil fuel burning produces a large amount of greenhouse gases CO 2catch the concern being subject to people with Plugging Technology Applied gradually.Except the methods such as traditional liquefied ammonia absorption process, membrane sepn, low-temperature distillation, active carbon adsorption relies on the advantage such as its cheap cost, high-adsorption-capacity, high Selective adsorption, excellent cyclic regeneration stability in use, is current CO 2one of technology most with prospects in the numerous technology of gas entrapment.Although common commercial gac has higher specific surface area, flourishing microvoid structure and large pore volume, be directly used in CO 2still there is more problem in catching of gas, as lower in loading capacity, poor selectivity, adsorption rate are slow, cyclic regeneration life cycle is long.By modes such as modification or graftings at gac table phase or the body alkaline nitrogen-containing functional group of middle introducing mutually, effectively can improve gac to the loading capacity of acid CO2 gas and adsorption selectivity, thus receive and pay close attention to widely.
Number of patent application is that " having nitrogenous Carbon Materials and the application thereof of good carbon dioxide adsorption separation performance " patent of 201210562808.X is by being polymerized a kind of nitrogenous compound at activated carbon surface, obtain the porous carbon material with different nitrogen contents again through calcining, can be used for CO in multiple gases 2fractionation by adsorption.Patent does not provide corresponding CO 2separation factor, what was certain was that owing to being polymerized polymer at activated carbon surface, its specific surface area will significantly decline, although can improve CO 2separation factor, but its absorption is significantly declined;
Number of patent application be 201210167846.5 " one catches CO in flue gas 2sorbent material and preparation method thereof " patent have employed porous carbon material dipping equally containing nitrogen compound, carries out drying acquisition afterwards to CO in hydrogen atmosphere 2the trapping agent that loading capacity reaches, the specific surface area of its Carbon Materials used is greater than 800m 2/ g, but do not provide its CO 2catch quantity;
Number of patent application be 201110329392.2 " for catching CO 2the preparation method of spheric active carbon " provide a kind of low cost, high nitrogenous for catching CO 2the preparation method of spheric active carbon.Its nitrogen content is between 1.8-5.4wt%, and CO2 quantity of the catch is between 7.4-14.8wt%;
Number of patent application be 201110329424.9 " a kind of resin carbon specific surface area that improves is beneficial to CO 2the method of catching " in, although the specific surface area of resin carbon is the highest reach 1510m 2/ g, but to CO 2quantity of the catch be only 11.8wt%.
Although above-mentioned patent adopts nitrogenous reagent process finished product gac, or directly adopt polymer with nitrogen to carry out carbonizing, activate and synthesize nitrogenous porous carbon material, but shortcoming that ubiquity Carbon Materials specific surface area is little, nitrogen content is low and yield is lower etc., is difficult to meet efficient capture CO 2requirement.
Summary of the invention
The object of this invention is to provide a kind of high-specific surface area, high nitrogen-containing and high CO 2the preparation method of the gac of absorption property.
Preparation method of the present invention comprises the steps:
(1) synthesis of nitrogenous prepolymer: trimeric cyanamide and formaldehyde add p-aminophenol after stirring reaction 30-90min at 60-90 DEG C, back flow reaction 4-8h at 60-120 DEG C afterwards, cool to room temperature, then the methanol solution of F127 or P123 is added, after stirred at ambient temperature 3-6h, pouring in open container methyl alcohol under room temperature into volatilizees after 8-12h naturally, with the temperature rise rate of 0.5-2 DEG C/min respectively at 100-120,130-160,170-190,210-230 and 240-260 DEG C segmentation solidify 3-6h respectively, obtain nitrogenous prepolymer;
P-aminophenol as above: trimeric cyanamide: formaldehyde mole ratio is 1:(0.5-2): (3-12); The mole number ratio of trimeric cyanamide: F127 or P123 is 1:(0.005-0.02); The methyl alcohol of 20-200ml is added in every mole of amino-phenol;
(2) charing of nitrogenous prepolymer: by nitrogenous prepolymer under nitrogen protection with the ramp of 0.5-2 DEG C/min to 500-700 DEG C, and carbonize 2-4h at this temperature, obtain carbonized material;
(3) activation of nitrogenous prepolymer: by the carbonized material obtained and KOH 1:(1-4 in mass ratio) mix after, with the ramp of 2-5 DEG C/min to 500-700 DEG C, and activate 0.5-2.0h at this temperature, finally by deionized water repetitive scrubbing to neutral, after drying, obtain product.
Tool of the present invention has the following advantages:
1, the compound that have employed nitrogen content high due to this patent is polymerized, therefore also containing high nitrogen content in gained prepolymer; Equally, owing to adopting lower charing and activation temperature, also ensure that the nitrogen content in the finished product.
2, this patent have employed the method for chemical activation, and the specific surface area of products obtained therefrom is apparently higher than the performance of conventional physical activation products obtained therefrom.
3, the CO2 absorption property of this patent products obtained therefrom is up to 19.8%.
Embodiment
Embodiment 1
0.5 mol trimeric cyanamide and 3.0 mol formaldehyde add 1.0 mol p-aminophenol after stirring reaction 90 min at 60 DEG C, back flow reaction 4h at 100 DEG C afterwards, cool to room temperature, then methanol solution 20 ml of 0.010 mol F127 is added, after stirred at ambient temperature 5h, pouring in open container methyl alcohol under room temperature into volatilizees after 8h naturally, be placed in baking oven with the temperature rise rate of 0.5 DEG C/min respectively at 100,130,170,210 and 240 DEG C segmentation solidify 6h respectively, obtain nitrogenous prepolymer; Nitrogenous prepolymer is carbonized 4h with at the ramp to 500 of 0.5 DEG C/min DEG C under nitrogen protection, obtains carbonized material; After by the carbonized material that obtains, 1:3 mixes in mass ratio with KOH, with the ramp to 500 of 2 DEG C/min DEG C activation 2.0h.Finally by deionized water repetitive scrubbing to neutral, after drying, obtain product.
The specific surface area of products obtained therefrom is 1520 m 2/ g, nitrogen content are 8.6 wt%, CO 2under 25 DEG C of normal pressures, adsorptive capacity reaches 15.4 wt%.
Embodiment 2
1.0 mol trimeric cyanamides and 5.0 mol formaldehyde add 1.0 mol p-aminophenol after stirring reaction 80 min at 70 DEG C, back flow reaction 5h at 120 DEG C afterwards, cool to room temperature, then methanol solution 80 ml of 0.005 mol F127 is added, after stirred at ambient temperature 3h, pouring in open container methyl alcohol under room temperature into volatilizees after 10h naturally, to be placed in baking oven with the temperature rise rate of 1.0 DEG C/min stage curing 4h at 110,140,180,220 and 250 DEG C respectively, to obtain nitrogenous prepolymer; Nitrogenous prepolymer is carbonized 4h with at the ramp to 600 of 0.5 DEG C/min DEG C under nitrogen protection, obtains carbonized material; After by the carbonized material that obtains, 1:1 mixes in mass ratio with KOH, with the ramp to 700 of 5 DEG C/min DEG C activation 0.5h.Finally by deionized water repetitive scrubbing to neutral, after drying, obtain product.
The specific surface area of products obtained therefrom is 1550 m 2/ g, nitrogen content are 6.7 wt%, CO 2under 25 DEG C of normal pressures, adsorptive capacity reaches 15.1 wt%.
Embodiment 3
2.0 mol trimeric cyanamides and 12.0 mol formaldehyde add 1.0 mol p-aminophenol after stirring reaction 30 min at 80 DEG C, back flow reaction 6h at 60 DEG C afterwards, cool to room temperature, then methanol solution 160 ml of 0.020 mol F127 is added, after stirred at ambient temperature 4h, pouring in open container methyl alcohol under room temperature into volatilizees after 8h naturally, to be placed in baking oven with the temperature rise rate of 2.0 DEG C/min stage curing 2h at 100,150,190,230 and 260 DEG C respectively, to obtain nitrogenous prepolymer; Nitrogenous prepolymer is carbonized 3h with at the ramp to 700 of 0.5 DEG C/min DEG C under nitrogen protection, obtains carbonized material; After by the carbonized material that obtains, 1:2 mixes in mass ratio with KOH, with the ramp to 600 of 3 DEG C/min DEG C activation 1.0h.Finally by deionized water repetitive scrubbing to neutral, after drying, obtain product.
The specific surface area of products obtained therefrom is 1600 m 2/ g, nitrogen content are 7.8 wt%, CO 2under 25 DEG C of normal pressures, adsorptive capacity reaches 18.1 wt%.
Embodiment 4
1.5 mol trimeric cyanamides and 8.0 mol formaldehyde add 2.0 mol p-aminophenol after stirring reaction 70 min at 90 DEG C, back flow reaction 8h at 100 DEG C afterwards, cool to room temperature, then methanol solution 200 ml of 0.020 mol F127 is added, after stirred at ambient temperature 6h, pouring in open container methyl alcohol under room temperature into volatilizees after 8h naturally, to be placed in baking oven with the temperature rise rate of 1.5 DEG C/min stage curing 4h at 120,140,170,210 and 240 DEG C respectively, to obtain nitrogenous prepolymer; Nitrogenous prepolymer is carbonized 4h with at the ramp to 500 of 0.5 DEG C/min DEG C under nitrogen protection, obtains carbonized material; After by the carbonized material that obtains, 1:4 mixes in mass ratio with KOH, with the ramp to 500 of 4 DEG C/min DEG C activation 1.0h.Finally by deionized water repetitive scrubbing to neutral, after drying, obtain product.
The specific surface area of products obtained therefrom is 1635 m 2/ g, nitrogen content are 8.2 wt%, CO 2under 25 DEG C of normal pressures, adsorptive capacity reaches 19.8 wt%.
Embodiment 5
0.5 mol trimeric cyanamide and 12.0 mol formaldehyde add 1.0 mol p-aminophenol after stirring reaction 80 min at 70 DEG C, back flow reaction 4h at 60 DEG C afterwards, cool to room temperature, then methanol solution 140 ml of 0.016 mol P123 is added, after stirred at ambient temperature 5h, pouring in open container methyl alcohol under room temperature into volatilizees after 8h naturally, to be placed in baking oven with the temperature rise rate of 0.5 DEG C/min stage curing 6h at 110,130,170,220 and 250 DEG C respectively, to obtain nitrogenous prepolymer; Nitrogenous prepolymer is carbonized 4h with at the ramp to 700 of 0.5 DEG C/min DEG C under nitrogen protection, obtains carbonized material; After by the carbonized material that obtains, 1:3 mixes in mass ratio with KOH, with the ramp to 700 of 3 DEG C/min DEG C activation 1.5h.Finally by deionized water repetitive scrubbing to neutral, after drying, obtain product.
The specific surface area of products obtained therefrom is 1842 m 2/ g, nitrogen content are 5.8 wt%, CO 2under 25 DEG C of normal pressures, adsorptive capacity reaches 15.6 wt%.
Embodiment 6
1.5 mol trimeric cyanamides and 9.0 mol formaldehyde add 1.0 mol p-aminophenol after stirring reaction 30 min at 90 DEG C, back flow reaction 4h at 110 DEG C afterwards, cool to room temperature, then methanol solution 90 ml of 0.020 mol P123 is added, after stirred at ambient temperature 3h, pouring in open container methyl alcohol under room temperature into volatilizees after 8h naturally, to be placed in baking oven with the temperature rise rate of 1.5 DEG C/min stage curing 5h at 120,150,180,210 and 240 DEG C respectively, to obtain nitrogenous prepolymer; Nitrogenous prepolymer is carbonized 3h with at the ramp to 600 of 1.0 DEG C/min DEG C under nitrogen protection, obtains carbonized material; After by the carbonized material that obtains, 1:2 mixes in mass ratio with KOH, with the ramp to 600 of 2 DEG C/min DEG C activation 0.5h.Finally by deionized water repetitive scrubbing to neutral, after drying, obtain product.
The specific surface area of products obtained therefrom is 1930 m 2/ g, nitrogen content are 7.7 wt%, CO 2under 25 DEG C of normal pressures, adsorptive capacity reaches 17.7 wt%.
Embodiment 7
2.0 mol trimeric cyanamides and 3.0 mol formaldehyde add 1.0 mol p-aminophenol after stirring reaction 60 min at 70 DEG C, back flow reaction 8h at 80 DEG C afterwards, cool to room temperature, then methanol solution 120 ml of 0.018 mol P123 is added, after stirred at ambient temperature 3h, pouring in open container methyl alcohol under room temperature into volatilizees after 12h naturally, to be placed in baking oven with the temperature rise rate of 2.0 DEG C/min stage curing 3h at 100,140,180,230 and 250 DEG C respectively, to obtain nitrogenous prepolymer; Nitrogenous prepolymer is carbonized 2h with at the ramp to 700 of 2 DEG C/min DEG C under nitrogen protection, obtains carbonized material; After by the carbonized material that obtains, 1:1 mixes in mass ratio with KOH, with the ramp to 500 of 4 DEG C/min DEG C activation 2.0h.Finally by deionized water repetitive scrubbing to neutral, after drying, obtain product.
The specific surface area of products obtained therefrom is 2090 m 2/ g, nitrogen content are 8.2 wt%, CO 2under 25 DEG C of normal pressures, adsorptive capacity reaches 18.9 wt%.
Embodiment 8
1.0 mol trimeric cyanamides and 6.0 mol formaldehyde add 1.0 mol p-aminophenol after stirring reaction 90 min at 70 DEG C, back flow reaction 5h at 120 DEG C afterwards, cool to room temperature, then the methanol solution 100ml of 0.018 mol P123 is added, after stirred at ambient temperature 6h, pouring in open container methyl alcohol under room temperature into volatilizees after 10h naturally, to be placed in baking oven with the temperature rise rate of 1.0 DEG C/min stage curing 3h at 110,160,190,230 and 260 DEG C respectively, to obtain nitrogenous prepolymer; Nitrogenous prepolymer is carbonized 2h with at the ramp to 500 of 2 DEG C/min DEG C under nitrogen protection, obtains carbonized material; After by the carbonized material that obtains, 1:1 mixes in mass ratio with KOH, with the ramp to 700 of 5 DEG C/min DEG C activation 0.5h.Finally by deionized water repetitive scrubbing to neutral, after drying, obtain product.
The specific surface area of products obtained therefrom is 2180 m 2/ g, nitrogen content are 6.0 wt%, CO 2under 25 DEG C of normal pressures, adsorptive capacity reaches 19.2 wt%.

Claims (2)

1. an efficient adsorption CO 2the preparation method of gac, it is characterized in that comprising the steps:
(1) synthesis of nitrogenous prepolymer: trimeric cyanamide and formaldehyde add p-aminophenol after stirring reaction 30-90min at 60-90 DEG C, back flow reaction 4-8h at 60-120 DEG C afterwards, cool to room temperature, then the methanol solution of F127 or P123 is added, after stirred at ambient temperature 3-6h, pouring in open container methyl alcohol under room temperature into volatilizees after 8-12h naturally, with the temperature rise rate of 0.5-2 DEG C/min respectively at 100-120,130-160,170-190,210-230 and 240-260 DEG C segmentation solidify 3-6h respectively, obtain nitrogenous prepolymer;
(2) charing of nitrogenous prepolymer: by nitrogenous prepolymer under nitrogen protection with the ramp of 0.5-2 DEG C/min to 500-700 DEG C, and carbonize 2-4h at this temperature, obtain carbonized material;
(3) activation of nitrogenous prepolymer: after 1:1-4 mixes in mass ratio by the carbonized material and the KOH that obtain, with the ramp of 2-5 DEG C/min to 500-700 DEG C, and activate 0.5-2.0h at this temperature, finally by deionized water repetitive scrubbing to neutral, after drying, obtain product.
2. a kind of efficient adsorption CO as claimed in claim 1 2the preparation method of gac, it is characterized in that described p-aminophenol: trimeric cyanamide: formaldehyde mole ratio is 1:0.5-2:3-12; The mole number ratio of trimeric cyanamide: F127 or P123 is 1:0.005-0.02; The methyl alcohol of 20-200ml is added in every mole of amino-phenol.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105664850A (en) * 2016-01-26 2016-06-15 中国科学院上海高等研究院 Preparation method and application of high-performance carbon-based carbon dioxide adsorbing material
CN108529588A (en) * 2018-03-06 2018-09-14 河南工程学院 The preparation method of ordered mesoporous carbon
CN109748279A (en) * 2019-02-21 2019-05-14 南京大学 One kind is based on poromeric micro-pore carbon material of benzoxazine and its preparation method and application

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58213613A (en) * 1982-06-03 1983-12-12 Sumitomo Bakelite Co Ltd Preparation of spherical active carbon
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
CN102553641A (en) * 2010-12-08 2012-07-11 中国中化股份有限公司 Preparation method for nitrogen-containing activated carbon catalyst

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58213613A (en) * 1982-06-03 1983-12-12 Sumitomo Bakelite Co Ltd Preparation of spherical active carbon
CN102553641A (en) * 2010-12-08 2012-07-11 中国中化股份有限公司 Preparation method for nitrogen-containing activated carbon catalyst
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

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105664850A (en) * 2016-01-26 2016-06-15 中国科学院上海高等研究院 Preparation method and application of high-performance carbon-based carbon dioxide adsorbing material
CN105664850B (en) * 2016-01-26 2018-06-26 中国科学院上海高等研究院 A kind of preparation method and applications of high performance carbon base carbon dioxide sorbing material
CN108529588A (en) * 2018-03-06 2018-09-14 河南工程学院 The preparation method of ordered mesoporous carbon
CN109748279A (en) * 2019-02-21 2019-05-14 南京大学 One kind is based on poromeric micro-pore carbon material of benzoxazine and its preparation method and application

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