CN107857264A - Weaken the preparation method of resin base porous carbon material rupture - Google Patents
Weaken the preparation method of resin base porous carbon material rupture Download PDFInfo
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- CN107857264A CN107857264A CN201711087546.5A CN201711087546A CN107857264A CN 107857264 A CN107857264 A CN 107857264A CN 201711087546 A CN201711087546 A CN 201711087546A CN 107857264 A CN107857264 A CN 107857264A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of furfural
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of method for weakening the rupture of resin base porous carbon material, meta induced by alkyl hydroxybenzene and aldehydes are added in deionized water and are configured to solution, add triethanolamine and heat to 95 100 DEG C under conditions of stirring as catalyst, then polyvinyl alcohol and aniline are added respectively, continue to stir 3 6h, cool down and be filtrated to get resin；Resin is well mixed with binder, deionized water under 450 650r/min mixing speeds, then cylinder is squeezed under 15 35MPa pressure with flat die rolling granulator, obtains forming charcoal；Forming charcoal is put into carbonization-activation stove, 650 850 DEG C of charings, and the 2h of constant temperature 0.5 are risen to by room temperature under nitrogen protection；Then pass to vapor constant temperature and activate 1 4h, be naturally cooling to room temperature, obtain resin base porous carbon material.The present invention have it is simple to operate, it is easily controllable；Weaken in preparation process resin in heat treatment process it is cracked to prepare the smooth activated carbon in surface the advantages of.
Description
Technical field
It is specially a kind of to weaken what resin base porous carbon ruptured the invention belongs to the preparing technical field of porous carbon material
Preparation method.
Background technology
Resin matrix activated carbon because of the features such as its surface is smooth, loading density is uniform, flow resistance is small, turn into industry, national defence,
The study hotspot of the application field such as medical and health and environmental protection.Preparing the raw material of resin matrix activated carbon at present includes phenolic aldehyde tree
Fat, polystyrene, polydivinylbenezene, polyacrylonitrile, polyvinylidene chloride, poly- phthalimide etc..Contain because phenolic resin has
The features such as impurity level is low, carbonization yield is high and is easy to activate pore-creating, and turn into the preferred presoma for preparing resin matrix activated carbon.
Youth Liu（Patent No. CN98115717.3）After phenolic resin, curing agent and solvent are mixed, removal of solvent under reduced pressure
Obtain the particle of prescribed particle size with broken, screening, prepare resin using emulsion process afterwards, then carbonized, activate after obtain phenol
Urea formaldehyde matrix activated carbon.Liang Xiao is pleased（Patent No. CN101721972A）Deng to patent CN98115717.3 progress sustained improvements, general
Phenolic resin ethanol solution, curing agent and dispersant, which are disposably added in autoclave, to be emulsified, and then carries out microwave curing to resin,
The resin after solidification is finally subjected to high temperature carbonization and activation obtains activated carbon.The above method can prepare phenolic resin
Matrix activated carbon, but surface has a large amount of crackles, or even rupture, breakage rate is up to more than 50%, seriously restricts it and applies model
Enclose.
The content of the invention
The present invention is intended to provide a kind of weakening moulding resin is cracked smooth to prepare surface in heat treatment process
Activated carbon method.
The present invention, which carries, adopts the following technical scheme that realization：
A kind of preparation method for weakening the rupture of resin base porous carbon, comprises the following steps：
（1）, by mol ratio be 1:3-8 meta induced by alkyl hydroxybenzene adds in deionized water with aldehydes and is configured to solution, adds phenols
Mole 1%-3% triethanolamine heats to 95-100 DEG C as catalyst under conditions of stirring, then adds respectively
Phenols mole 5%-15% polyvinyl alcohol and the 3%-6% aniline of phenols mole, continue to stir 3-6h, cool down and be filtrated to get
Resin.
（2）, by step（1）The resin of gained is with binder, deionized water using mass ratio as 65-80:15-30:10-20 exists
It is well mixed under 450-650r/min mixing speeds, is then squeezed into cylinder under 15-35MPa pressure with flat die rolling granulator
Shape, obtain forming charcoal.
（3）, by step（2）The forming charcoal of gained rises to 650-850 DEG C of charing 0.5-2h in high temperature process furnances by room temperature,
Obtain carbide.
（4）And then by step（3）The carbide of gained is heated to 850-1000 DEG C, is passed through the work of 10-20mL/min vapor
Change 1-4h, be naturally cooling to room temperature and obtain porous carbon material.
In above-mentioned preparation method, induced by alkyl hydroxybenzene is 3- ethyl -phenols, 3- isopropyl-phenols, 3- tert-butyl phenols, 3,5- bis-
One or more mixtures of methylphenol or 3- methyl -5- ethyl -phenols.
In above-mentioned preparation method, aldehydes is formaldehyde or furfural.
In above-mentioned preparation method, step（2）Middle adhesive is resol or carboxymethyl cellulose.
The detection method of the present invention：
Arbitrarily choosing 50 activated carbons reading surface under ESEM has the activated carbon of crackle, is accounted for entirely according to there is crackle activated carbon
The percentage of portion's activated carbon calculates breakage rate, repeats 10 times and takes the mean.
Beneficial effects of the present invention：
The preparation method provided by the invention for weakening the rupture of resin base porous carbon, raw material is cheap and easy to get, the simple controllable, behaviour of technique
Make mild condition, it is aggregated successively, mixed using adhesive and deionized water as object specifically based on induced by alkyl hydroxybenzene and aldehydes
Conjunction, shaping, charing and steam activation, obtain being rich in porous Carbon Materials.
This method passes through to different phenolic aldehyde mol ratios, different adhesive adding proportions, different carbonization temperatures, different activation
The experiment of the conditions such as temperature, it is determined that test the processing of instrument equipment, experimental condition, determination step and measurement result.For
The preparation research and design of high intensity desulphurization denitration activated carbon provide theoretical foundation.
Embodiment
The present invention is further illustrated below by embodiment, but is not limited to following examples.
Embodiment 1
A kind of preparation method for weakening the rupture of resin base porous carbon, comprises the following steps：
1st, 2mol 3- ethyl -phenols and 6mol formaldehyde are added in deionized water and is configured to solution, add 0.02mol three ethanol
Amine heats to 95 DEG C under conditions of stirring；Then 0.1mol polyvinyl alcohol and 0.06mol aniline are added respectively, are continued
3h is stirred, cools down and be filtrated to get resin；
2nd, 13g resins are well mixed with 3g carboxymethyl celluloses, 4g deionized waters under 450r/min mixing speeds, Ran Houyong
Flat die rolling granulator is squeezed into cylinder under 15 MPa pressure, obtains forming charcoal；
3rd, above-mentioned forming charcoal is risen into 650 DEG C of charing 0.5h by room temperature in high temperature process furnances, temperature is then risen to 850 DEG C,
20mL/min steam activation 4h are passed through, room temperature is naturally cooling to and obtains porous carbon material.
After testing, the breakage rate of activated carbon is 2.1%.
Embodiment 2
A kind of preparation method for weakening the rupture of resin base porous carbon, comprises the following steps：
1st, 4mol 3- isopropyl-phenols and 12mol formaldehyde are added in deionized water and is configured to solution, add 0.6mol three second
Hydramine heats to 97 DEG C under conditions of stirring；Then 0.28mol polyvinyl alcohol and 0.06mol aniline are added respectively, after
Continuous stirring 5h, cools down and is filtrated to get resin；
2nd, 19.5g resins are well mixed with 4.5g carboxymethyl celluloses, 6g deionized waters under 500r/min mixing speeds, so
Cylinder is squeezed under 20MPa pressure with flat die rolling granulator afterwards, obtains forming charcoal；
3rd, above-mentioned forming charcoal is risen into 700 DEG C of charing 1.5h by room temperature in high temperature process furnances, temperature is then risen to 900 DEG C,
16mL/min steam activation 3h are passed through, room temperature is naturally cooling to and obtains porous carbon material.
After testing, the breakage rate of activated carbon is 1.6%.
Embodiment 3
A kind of preparation method for weakening the rupture of resin base porous carbon, comprises the following steps：
1st, 6mol 3- tert-butyl phenols and 24mol formaldehyde are added in deionized water and is configured to solution, add 0.9mol three second
Hydramine heats to 96 DEG C under conditions of stirring；Then 0.6mol polyvinyl alcohol and 0.24mol aniline are added respectively, after
Continuous stirring 4.5h, cools down and is filtrated to get resin；
2nd, 21g resins are well mixed with 6g carboxymethyl celluloses, 3g deionized waters under 550r/min mixing speeds, Ran Houyong
Flat die rolling granulator is squeezed into cylinder under 30MPa pressure, obtains forming charcoal；
3rd, above-mentioned forming charcoal is risen into 750 DEG C of charing 2h by room temperature in high temperature process furnances, temperature is then risen to 900 DEG C, led to
Enter 14mL/min steam activation 2.5h, be naturally cooling to room temperature and obtain porous carbon material.
After testing, the breakage rate of activated carbon is 2%.
Embodiment 4
A kind of preparation method for weakening the rupture of resin base porous carbon, comprises the following steps：
1st, 5mol MXs and 25mol furfurals are added in deionized water and is configured to solution, add 0.15mol's
Triethanolamine heats to 98 DEG C under conditions of stirring；Then 0.75mol polyvinyl alcohol and 0.3mol benzene are added respectively
Amine, continue to stir 6h, cool down and be filtrated to get resin；
2nd, 34g resins are well mixed with 2g resols, 4g deionized waters under 650r/min mixing speeds, Ran Houyong
Flat die rolling granulator is squeezed into cylinder under 35MPa pressure, obtains forming charcoal；
3rd, above-mentioned forming charcoal is risen into 850 DEG C of charing 2h by room temperature in high temperature process furnances, temperature is then risen to 1000 DEG C, led to
Enter 12mL/min steam activation 1h, be naturally cooling to room temperature and obtain porous carbon material.
After testing, the breakage rate of activated carbon is 1.8%.
Embodiment 5
A kind of preparation method for weakening the rupture of resin base porous carbon, comprises the following steps：
1st, 4mol 3- methyl -5- ethyl -phenols and 32mol furfurals are added in deionized water and is configured to solution, add 0.1mol
Triethanolamine 100 DEG C are heated under conditions of stirring；Then 0.64mol polyvinyl alcohol and 0.2mol are added respectively
Aniline, continue to stir 5h, cool down and be filtrated to get resin；
2nd, 30g resins are well mixed with 4g resols, 6g deionized waters under 600r/min mixing speeds, Ran Houyong
Flat die rolling granulator is squeezed into cylinder under 35MPa pressure, obtains forming charcoal；
3rd, above-mentioned forming charcoal is risen into 820 DEG C of charing 1.5h by room temperature in high temperature process furnances, temperature is then risen to 950 DEG C,
15mL/min steam activation 1.5h are passed through, room temperature is naturally cooling to and obtains porous carbon material.
After testing, the breakage rate of activated carbon is 1.3%.
Embodiment 6
A kind of preparation method for weakening the rupture of resin base porous carbon, comprises the following steps：
1st, 3mol MXs and 24mol furfurals are added in deionized water and is configured to solution, add 0.75mol's
Triethanolamine heats to 96 DEG C under conditions of stirring；Then 0.42mol polyvinyl alcohol and 0.18mol benzene are added respectively
Amine, continue to stir 5h, cool down and be filtrated to get resin；
2nd, 51g resins are well mixed with 3g resols, 6g deionized waters under 600r/min mixing speeds, Ran Houyong
Flat die rolling granulator is squeezed into cylinder under 30MPa pressure, obtains forming charcoal；
3rd, above-mentioned forming charcoal is risen into 830 DEG C of charing 2h by room temperature in high temperature process furnances, temperature is then risen to 950 DEG C, led to
Enter 17mL/min steam activation 2h, be naturally cooling to room temperature and obtain porous carbon material.
After testing, the breakage rate of activated carbon is 1.2%.
Embodiment 7
A kind of preparation method for weakening the rupture of resin base porous carbon, comprises the following steps：
1st, 6mol 3- methyl -5- ethyl -phenols and 12mol formaldehyde are added in deionized water and is configured to solution, add 0.12mol
Triethanolamine 98 DEG C are heated under conditions of stirring；Then 0.6mol polyvinyl alcohol and 0.27mol benzene are added respectively
Amine, continue to stir 5h, cool down and be filtrated to get resin；
2nd, 41g resins are well mixed with 12g carboxymethyl celluloses, 6g deionized waters under 600r/min mixing speeds, then
Cylinder is squeezed under 35MPa pressure with flat die rolling granulator, obtains forming charcoal；
3rd, above-mentioned forming charcoal is risen into 800 DEG C of charing 1.5h by room temperature in high temperature process furnances, temperature is then risen to 900 DEG C,
20mL/min steam activation 2h are passed through, room temperature is naturally cooling to and obtains porous carbon material.
After testing, the breakage rate of activated carbon is 1.4%.
Comparative example 1
1st, 6mol phenol and 24mol formaldehyde are added in deionized water and is configured to solution, the triethanolamine for adding 0.06mol exists
96 DEG C are heated under conditions of stirring；Then 0.42mol polyvinyl alcohol and 0.36mol aniline are added respectively, continue to stir
4h, cool down and be filtrated to get resin；
2nd, 26g resins are well mixed with 6g carboxymethyl celluloses, 8g deionized waters under 550r/min mixing speeds, Ran Houyong
Flat die rolling granulator is squeezed into cylinder under 30MPa pressure, obtains forming charcoal；
3rd, above-mentioned forming charcoal is risen into 800 DEG C of charing 1h by room temperature in high temperature process furnances, temperature is then risen to 900 DEG C, led to
Enter 18mL/min steam activation 3h, be naturally cooling to room temperature and obtain porous carbon material.
After testing, the breakage rate of activated carbon is 44%.
Comparative example 2
1st, 8mol phenol and 48mol furfurals are added in deionized water and is configured to solution, the triethanolamine for adding 0.16mol is stirring
98 DEG C are heated under conditions of mixing；Then 0.96mol polyvinyl alcohol and 0.4mol aniline are added respectively, continue to stir 5h,
Cool down and be filtrated to get resin；
2nd, 42g resins are well mixed with 12g carboxymethyl celluloses, 6g deionized waters under 600r/min mixing speeds, then
Cylinder is squeezed under 25MPa pressure with flat die rolling granulator, obtains forming charcoal；
3rd, above-mentioned forming charcoal is risen into 850 DEG C of charing 1.5h by room temperature in high temperature process furnances, temperature is then risen to 950 DEG C,
20mL/min steam activation 2.5h are passed through, room temperature is naturally cooling to and obtains porous carbon material.
After testing, the breakage rate of activated carbon is 56%.
In a word, the present invention has simple to operate, easily controllable；Weaken resin in preparation process in heat treatment process to occur
The advantages of crackle is to prepare the smooth activated carbon in surface.
The inventive method is started with from the raw material of novolak resin ball, from meta induced by alkyl hydroxybenzene such as 3- ethyl -phenols, 3-
Isopropyl-phenol, 3- tert-butyl phenols, MX or 3- methyl -5- ethyls are reaction monomers, are suspended with formaldehyde poly-
Conjunction prepares alkyl phenolic resin ball, and fracture base of different sizes is produced by the pyrolysis of meta methyl, ethyl, isopropyl and the tert-butyl group
Group, is discharged in the form of gaseous state small molecule, and group is bigger, and the duct left is more, increases activator molecule and carbon matrix
Contact probability increase, resin balls is fully activated, form equally distributed hole, and then keep the spheroid of activated carbon ball
Completely, without crackle.
It should be pointed out that for the those skilled in the art of the art, under the premise without departing from the principles of the invention,
Some improvement and application can also be made, these are improved and application is also considered as protection scope of the present invention.
Claims (4)
- A kind of 1. preparation method for weakening the rupture of resin base porous carbon material, it is characterised in that：Comprise the following steps：（1）, by mol ratio be 1:3-8 meta induced by alkyl hydroxybenzene adds in deionized water with aldehydes and is configured to solution, adds phenols Mole 1%-3% triethanolamine heats to 95-100 DEG C as catalyst under conditions of stirring, then adds respectively Phenols mole 5%-15% polyvinyl alcohol and the 3%-6% aniline of phenols mole, continue to stir 3-6h, cool down and be filtrated to get Resin；（2）, by step（1）The resin of gained is with binder, deionized water using mass ratio as 65-80:15-30:10-20 is in 450- It is well mixed under 650 r/min mixing speeds, is then squeezed into cylinder under 15-35MPa pressure with flat die rolling granulator, Obtain forming charcoal；（3）, by step（2）The forming charcoal of gained rises to 650-850 DEG C of charing 0.5-2h in high temperature process furnances by room temperature, obtains Carbide；（4）And then by step（3）The carbide of gained is heated to 850-1000 DEG C, is passed through 10-20mL/min steam activations 1- 4h, it is naturally cooling to room temperature and obtains porous carbon material.
- 2. the preparation method according to claim 1 for weakening the rupture of resin base porous carbon material, it is characterised in that：The alkane Base phenols is 3- ethyl -phenols, 3- isopropyl-phenols, 3- tert-butyl phenols, 3,5- xylenols or 3- methyl -5- ethylo benzenes One or more mixtures of phenol.
- 3. the preparation method according to claim 1 for weakening the rupture of resin base porous carbon material, it is characterised in that：The aldehyde Class is formaldehyde or furfural.
- 4. the preparation method according to claim 1 for weakening the rupture of resin base porous carbon material, it is characterised in that：Step （2）Described in adhesive be resol or carboxymethyl cellulose.
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| CN201711087546.5A CN107857264A (en) | 2017-11-08 | 2017-11-08 | Weaken the preparation method of resin base porous carbon material rupture |
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| CN201711087546.5A CN107857264A (en) | 2017-11-08 | 2017-11-08 | Weaken the preparation method of resin base porous carbon material rupture |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774567A (en) * | 2010-01-12 | 2010-07-14 | 山东理工大学 | Method for preparing multilevel pore carbon electrode material of super capacitor |
| CN103936004A (en) * | 2014-04-09 | 2014-07-23 | 中国科学院山西煤炭化学研究所 | Preparation method of resin-based spherical activated carbon with controllable pore structure |
| CN104098095A (en) * | 2013-04-11 | 2014-10-15 | 济南圣泉集团股份有限公司 | Method for preparing active carbon from phenolic foam wastes |
| CN106185919A (en) * | 2016-07-16 | 2016-12-07 | 中国科学院山西煤炭化学研究所 | A kind of method preparing functional resin base spheric active carbon |
-
2017
- 2017-11-08 CN CN201711087546.5A patent/CN107857264A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774567A (en) * | 2010-01-12 | 2010-07-14 | 山东理工大学 | Method for preparing multilevel pore carbon electrode material of super capacitor |
| CN104098095A (en) * | 2013-04-11 | 2014-10-15 | 济南圣泉集团股份有限公司 | Method for preparing active carbon from phenolic foam wastes |
| CN103936004A (en) * | 2014-04-09 | 2014-07-23 | 中国科学院山西煤炭化学研究所 | Preparation method of resin-based spherical activated carbon with controllable pore structure |
| CN106185919A (en) * | 2016-07-16 | 2016-12-07 | 中国科学院山西煤炭化学研究所 | A kind of method preparing functional resin base spheric active carbon |
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Application publication date: 20180330 |