CN103936004B - A kind of preparation method of resin base spheric active carbon of controllable hole structure - Google Patents
A kind of preparation method of resin base spheric active carbon of controllable hole structure Download PDFInfo
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- CN103936004B CN103936004B CN201410139231.0A CN201410139231A CN103936004B CN 103936004 B CN103936004 B CN 103936004B CN 201410139231 A CN201410139231 A CN 201410139231A CN 103936004 B CN103936004 B CN 103936004B
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Abstract
A kind of preparation method of resin base spheric active carbon of controllable hole structure is that 1:2-6 is added to the water by phenols and aldehydes according to mol ratio, the catalyzer of phenols molar weight 0.7%-1% is added in above-mentioned solution, 85-90 DEG C is heated under the condition stirred, then the dispersion agent of phenols molar weight 10%-30% is added, continue to stir after 20-60 minute and add the solidifying agent of phenols molar weight 1%-3% and the pore-forming material of phenols molar weight 0-5%, continue to stir 2-5 hour, cool to room temperature, filters and obtains resin balls; By the resin balls of preparation, in nitrogen protection charing, then activate, be cooled to room temperature, obtain alkyd resin based spheric active carbon.The present invention has the advantage that aperture is controlled, operational condition is gentle, with low cost.
Description
Technical field
The invention belongs to a kind of method preparing the controlled alkyd resin based spheric active carbon of pore structure.
Background technology
Spheric active carbon has the advantages such as good sphericity, adsorptive capacity is large, tamped density is even, resistance is little, in catalysis, chemical separating, environmental protection, medical treatment etc., have important effect.The raw material preparing spheric active carbon at present comprises pitch, resol, polystyrene spheres etc.Because the raw material of resol is cheap and easy to get, and synthesis is convenient, and carbonization yield is high, and impure amount is low and have good physical strength and resistance toheat, and becomes the main precursor preparing spheric active carbon.
Yang Junbing (patent No. CN98115717.3) etc. are by after resol, solidifying agent, solvent, removal of solvent under reduced pressure, carry out fragmentation again, sieve the particle obtaining predetermined particle size, by this particle and the aqueous solution adding tensio-active agent, emulsion process is utilized to prepare resin base bead, the resin base bead obtained carries out carbonizing again, activate after obtain alkyd resin based spheric active carbon, this method process is complicated, poor reproducibility.Wang Furong (patent No. CN200410012346.X) with water and alcohol mixture for solvent, polyvinyl alcohol is tensio-active agent, heating resol obtains resin beads, but the method is suitable for preparing micron order bead, and when producing the bead of more than 0.3mm, sphere diameter distribution broadens.Pre-treatment material adds in the alcoholic solution of resol by Li Kaixi (patent No. 101157451B) etc., then adds tensio-active agent, mixture in autoclave heated and stirred to 110-140 DEG C.These methods all well can not regulate and control the aperture of spheric active carbon above, and react in autoclave, and condition is harsh.
Summary of the invention
The object of the present invention is to provide the alkyd resin based spheric active carbon preparation method that a kind of aperture is controlled, operational condition is gentle, with low cost.
The invention process process is as follows:
Be 1:(2-6 by phenols and aldehydes according to mol ratio) be added to the water, the catalyzer of phenols molar weight 0.7%-1% is added in above-mentioned solution, 85-90 DEG C is heated under the condition stirred, then the dispersion agent of phenols molar weight 10%-30% is added, continue to stir after 20-60 minute and add the solidifying agent of phenols molar weight 1%-3% and the pore-forming material of phenols molar weight 0-5%, continue to stir 2-5 hour, cool to room temperature, filter and obtain resin balls; By the resin balls of preparation, under nitrogen protection by room temperature to 700-1000 DEG C of charing, and then pass into carbonic acid gas or water vapour activates, Temperature fall, to room temperature, obtains alkyd resin based spheric active carbon.
Phenols used described above be between ethylphenol, a tert.-butyl phenol, 1-naphthols, one or more mixing in 1,5-dihydroxy naphthlene; Aldehydes is formaldehyde, paraformaldehyde; Catalyzer is triethylamine, ammoniacal liquor, sodium hydroxide, hydrated barta; Dispersion agent is polyvinyl alcohol, sodium laurylsulfonate, gum arabic; Solidifying agent is hexamethyl tetramine, trimeric cyanamide, aniline; Pore-forming material is polyoxyethylene glycol, ethylene glycol.
Carbonization condition as above is: temperature rise rate is 1-5 DEG C/min, and carbonization temperature is 700-1000 DEG C, and carbonization time is 0-1h.
Activation condition as above is: activation temperature is 700-1000 DEG C, and soak time is 1-3h.
Advantage of the present invention
1, from the aperture of molecule roofing control spheric active carbon.
2, with low cost, prepare phenolic resin balls with more basic raw material.
3, operational condition is gentle, and balling-up reaction is carried out at ambient pressure.
Embodiment
Embodiment 1
Between inciting somebody to action, ethylphenol and formaldehyde are that 1:4 is added to the water according to mol ratio, a triethylamine for ethylphenol molar weight 0.75% is added in above-mentioned solution, 85 DEG C are heated under the condition stirred, then the polyvinyl alcohol of ethylphenol molar weight 23% between adding, continue stirring adds a hexamethylenetetramine of ethylphenol molar weight 3% and an ethylphenol molar weight 2.5% ethylene glycol after 30 minutes, continue stirring 3 hours, after cool to room temperature, filter and obtain resin balls.By the resin balls of preparation, under nitrogen protection by room temperature to 850 DEG C charing 1h, and then pass into water vapour and carry out activation 2h, Temperature fall, to room temperature, obtains alkyd resin based spheric active carbon.
Embodiment 2
Between inciting somebody to action, ethylphenol and formaldehyde are that 1:4 is added to the water according to mol ratio, a triethylamine for ethylphenol molar weight 0.75% is added in above-mentioned solution, 90 DEG C are heated under the condition stirred, then the polyvinyl alcohol of ethylphenol molar weight 23% between adding, continue stirring adds a hexamethylenetetramine of ethylphenol molar weight 3% and an ethylphenol molar weight 2.8% polyoxyethylene glycol after 30 minutes, continue stirring 3 hours, after cool to room temperature, filter and obtain resin balls.By the resin balls of preparation, under nitrogen protection by room temperature to 1000 DEG C charing 1h, and then pass into water vapour and carry out activation 2h, Temperature fall, to room temperature, obtains alkyd resin based spheric active carbon, and its Pore Characteristics is in table 1.
Embodiment 3
Between inciting somebody to action, ethylphenol and formaldehyde are that 1:2 is added to the water according to mol ratio, between inciting somebody to action, ethylphenol molar weight 0.85% triethylamine adds in above-mentioned solution, 90 DEG C are heated under the condition stirred, then the polyvinyl alcohol of ethylphenol molar weight 23% between adding, continue stirring and after 60 minutes, add a hexamethylenetetramine for ethylphenol molar weight 3%, continue stirring 2 hours, after cool to room temperature, filter and obtain resin balls.By the resin balls of preparation, under nitrogen protection by room temperature to 700 DEG C, do not carbonize, and then pass into water vapour and carry out activation 1h, Temperature fall, to room temperature, obtains alkyd resin based spheric active carbon, and its Pore Characteristics is in table 1.
Embodiment 4
Between inciting somebody to action, tert.-butyl phenol and formaldehyde are that 1:6 is added to the water according to mol ratio, an ammoniacal liquor of tert.-butyl phenol molar weight 0.75% is added in above-mentioned solution, 90 DEG C are heated under the condition stirred, then the sodium laurylsulfonate of tert.-butyl phenol molar weight 30% between adding, continue stirring and after 20 minutes, add a trimeric cyanamide for tert.-butyl phenol molar weight 1%, continue stirring 5 hours, after cool to room temperature, filter and obtain resin balls.By the resin balls of preparation, under nitrogen protection by room temperature to 900 DEG C charing 1h, and then pass into CO
2carry out activation 2h, Temperature fall, to room temperature, obtains alkyd resin based spheric active carbon, and its Pore Characteristics is in table 1.
Embodiment 5
Be that 1:5 is added to the water by 1-naphthols and paraformaldehyde according to mol ratio, the ammoniacal liquor of 1-naphthols molar weight 1% is added in above-mentioned solution, 90 DEG C are heated under the condition stirred, then the gum arabic of 1-naphthols molar weight 20% is added, continue stirring adds 1-naphthols molar weight 12% aniline after 30 minutes, the ethylene glycol of 1-naphthols molar weight 15%, continue stirring 3 hours, after cool to room temperature, filter and obtain resin balls.By the resin balls of preparation, under nitrogen protection by room temperature to 800 DEG C charing 2h, and then pass into CO
2carry out activation 3h, Temperature fall, to room temperature, obtains alkyd resin based spheric active carbon, and its Pore Characteristics is in table 1.
Embodiment 6
Be that 1:2 is added to the water, by 1 by 1,5-dihydroxy naphthlene and formaldehyde according to mol ratio, the hydrated barta of 5-dihydroxy naphthlene molar weight 0.8% adds in above-mentioned solution, heats to 90 DEG C, then add 1 under the condition stirred, the polyvinyl alcohol of 5-dihydroxy naphthlene molar weight 10%, continue stirring adds 1,5-dihydroxy naphthlene molar weight 2% hexamethylenetetramine after 30 minutes, 1, the polyoxyethylene glycol of 5-dihydroxy naphthlene molar weight 5%, continue stirring 5 hours, after cool to room temperature, filter and obtain resin balls.By the resin balls of preparation, under nitrogen protection by room temperature to 900 degree Celsius charing 1h, and then pass into water vapour and carry out activation 2h, Temperature fall, to room temperature, obtains alkyd resin based spheric active carbon, and its Pore Characteristics is in table 1.
Embodiment 7
Be that 1:3 is added to the water by 1-naphthols and paraformaldehyde according to mol ratio, the triethylamine of 1-naphthols molar weight 10% is added in above-mentioned solution, 90 DEG C are heated under the condition stirred, then the gum arabic of 1-naphthols molar weight 30% is added, continue stirring adds 1-naphthols molar weight 1% trimeric cyanamide after 30 minutes, continue stirring 3 hours, after cool to room temperature, filter and obtain resin balls.By the resin balls of preparation, under nitrogen protection by room temperature to 800 DEG C charing 2h, and then pass into CO
2carry out activation 3h, Temperature fall, to room temperature, obtains alkyd resin based spheric active carbon, and its Pore Characteristics is in table 1.
Embodiment 8
Between inciting somebody to action, ethylphenol and paraformaldehyde are that 1:6 is added to the water according to mol ratio, a triethylamine for ethylphenol molar weight 0.75% is added in above-mentioned solution, 90 DEG C are heated under the condition stirred, then the polyvinyl alcohol of ethylphenol molar weight 23% between adding, continue stirring adds a hexamethylenetetramine of ethylphenol molar weight 3% and an ethylphenol molar weight 2.5% ethylene glycol after 30 minutes, continue stirring 3 hours, after cool to room temperature, filter and obtain resin balls.By the resin balls of preparation, under nitrogen protection by room temperature to 850 DEG C charing 1h, and then pass into water vapour and carry out activation 2h, Temperature fall, to room temperature, obtains alkyd resin based spheric active carbon, and its Pore Characteristics is in table 1.
Embodiment 9
Be that 1:4 is added to the water, by 1 by 1,5-dihydroxy naphthlene and paraformaldehyde according to mol ratio, the triethylamine of 5-dihydroxy naphthlene molar weight 0.8% adds in above-mentioned solution, under the condition stirred, heat to 90 DEG C, then add the polyvinyl alcohol of 1,5-dihydroxy naphthlene molar weight 23%, continue stirring and add 1 after 30 minutes, the hexamethylenetetramine of 5-dihydroxy naphthlene molar weight 3% and the polyoxyethylene glycol of 1,5-dihydroxy naphthlene molar weight 5%, continue stirring 3 hours, after cool to room temperature, filter and obtain resin balls.By the resin balls of preparation, under nitrogen protection by room temperature to 850 DEG C charing 1.5h, and then pass into water vapour and carry out activation 1.5h, Temperature fall, to room temperature, obtains alkyd resin based spheric active carbon, and its Pore Characteristics is in table 1.
The Pore Characteristics of spheric active carbon prepared by table 1
Claims (7)
1. a preparation method for the resin base spheric active carbon of controllable hole structure, is characterized in that comprising the steps:
Be that 1:2-6 is added to the water by phenols and aldehydes according to mol ratio, the catalyzer of phenols molar weight 0.7%-1% is added in above-mentioned solution, 85-90 DEG C is heated under the condition stirred, then the dispersion agent of phenols molar weight 10%-30% is added, continue to stir after 20-60 minute and add the solidifying agent of phenols molar weight 1%-3% and the pore-forming material of phenols molar weight 0-5%, wherein do not comprise 0 point, continue to stir 2-5 hour, cool to room temperature, filters and obtains resin balls; By the resin balls of preparation, under nitrogen protection by room temperature to 700-1000 DEG C of charing, and then pass into carbonic acid gas or water vapour activates, Temperature fall, to room temperature, obtains alkyd resin based spheric active carbon;
Described phenols be between ethylphenol, a tert.-butyl phenol, 1-naphthols, one or more mixing in 1,5-dihydroxy naphthlene;
Described pore-forming material is polyoxyethylene glycol or ethylene glycol.
2. the preparation method of the resin base spheric active carbon of a kind of controllable hole structure as claimed in claim 1, is characterized in that described aldehydes is formaldehyde or paraformaldehyde.
3. the preparation method of the resin base spheric active carbon of a kind of controllable hole structure as claimed in claim 1, is characterized in that described catalyzer is triethylamine, ammoniacal liquor, sodium hydroxide or hydrated barta.
4. the preparation method of the resin base spheric active carbon of a kind of controllable hole structure as claimed in claim 1, is characterized in that described dispersion agent is polyvinyl alcohol, sodium laurylsulfonate or gum arabic.
5. the preparation method of the resin base spheric active carbon of a kind of controllable hole structure as claimed in claim 1, is characterized in that described solidifying agent is hexamethyl tetramine, trimeric cyanamide or aniline.
6. the preparation method of the resin base spheric active carbon of a kind of controllable hole structure as claimed in claim 1, it is characterized in that temperature rise rate 1-5 DEG C/min of described charing, carbonization time is 0-1h.
7. the preparation method of the resin base spheric active carbon of a kind of controllable hole structure as claimed in claim 1, it is characterized in that the activation temperature of described activation is 700-1000 DEG C, soak time is 1-3h.
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Families Citing this family (6)
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| CN105293488B (en) * | 2015-10-23 | 2017-07-21 | 北京林业大学 | Lignin-Based Activated Carbon microballoon, its preparation method and application |
| CN105170092A (en) * | 2015-10-23 | 2015-12-23 | 蓝星（成都）新材料有限公司 | Resin-based activated carbon ball and preparation method thereof |
| CN106185919B (en) * | 2016-07-16 | 2018-12-21 | 中国科学院山西煤炭化学研究所 | A method of preparing functional resin base spheric active carbon |
| CN107857264A (en) * | 2017-11-08 | 2018-03-30 | 山西新华化工有限责任公司 | Weaken the preparation method of resin base porous carbon material rupture |
| CN108862240B (en) * | 2018-07-31 | 2021-07-16 | 大连理工大学 | Heteroatom-doped carbon nano-microsphere and preparation method thereof |
| 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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