CN1188074A - Method for preparing globular active carbon - Google Patents
Method for preparing globular active carbon Download PDFInfo
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- CN1188074A CN1188074A CN97101617A CN97101617A CN1188074A CN 1188074 A CN1188074 A CN 1188074A CN 97101617 A CN97101617 A CN 97101617A CN 97101617 A CN97101617 A CN 97101617A CN 1188074 A CN1188074 A CN 1188074A
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Abstract
The preparation method of spherical active carbon includes the following steps: uniformly mixing 100 portions of asphalt with high softenig point and 10-50 portions of additive at 100-300 deg.C to make eutectic body; using eutectic body with correspondent grain size and pass through the process of emulsification treatment to obtain asphalt spheres containing additive, then making the obtained asphalt spheres pass through such processes of removing additive, nonconsumable treatment and carbonization and activation so as to obtain the invented spherical active carbon whose grain size can be directly controlled. According to the requirement for use, said invention can be used to prepare asphalt-base spherical active carbon with narrow sphere diameter distribution.
Description
The invention belongs to the preparation of gac.
Spheric active carbon, asphalt-base globular active carbon particularly, owing to have good sphericity, high loading capacity, packing density, high a series of excellent properties such as physical strength uniformly, defectives such as present employed ordinary granular gac physical strength is low, filling is inhomogeneous, absorption property is not good have been overcome, thereby be subjected to people's attention, be expected to obtain widespread use in medical science medicine, military affairs, senior environmental protection, catalysis, chemical separating, along with development of science and technology, spheric active carbon preparation method and technology are updated, and new purposes also constantly is developed.
GB 1468982 provides a kind of preparation method of spheric active carbon, this method is that pitch is placed the autoclave that has whipping appts with additive (naphthalene), under certain pressure and temperature, it is mixed fully, add half saponified polyvinyl acetate suspension then and obtain mixture.Under certain pressure, temperature and stirring velocity, make this mixture be dispersed into small droplets and be suspended in the water.After disperseing to finish,, with solvent additive is removed again and made the porous asphalt ball making bitumen ball after mixture cooling, the separation.The last atmospheric oxidation of carrying out the porous asphalt ball in converter is not melted, charing, activation make spheric active carbon.The preparation method of the spheric active carbon among the US 3917806 places the autoclave that has whipping appts with pitch with additive (naphthalene), under certain pressure and temperature, it is mixed fully, in mixture, add polyvinyl alcohol water solution then, under certain temperature and stirring velocity, mixture is scattered in the liquid.Make bitumen ball after mixture cooling, the separation, with solvent additive is removed again and made the porous asphalt ball.The last atmospheric oxidation of carrying out the porous asphalt ball in ebullated bed is not melted, charing, activation make spheric active carbon.Above-mentioned two kinds of methods prepare bitumen ball by dispersion method, can not control the granularity of spheric active carbon, therefore can't make the spheric active carbon that narrow sphere diameter distributes.
The purpose of this invention is to provide a kind of is raw material with the coal-tar pitch, and can prepare the method for asphalt-base globular active carbon according to the desired globule size of reality.
The preparation method of spheric active carbon of the present invention carries out as follows:
With high softening point bitumen and additive with 100: the ratio of 10-50 mixes under 100-300 ℃, makes eutectic, and is standby after broken, screening,
2. the eutectic of getting the corresponding granularity in screening back places reactor, add emulsion, in temperature is 130～150 ℃, under the pressure 0.4-0.8MPa, make the bitumen ball that contains additive by emulsion process, remove additive with solvent extraction process again and make the porous asphalt ball, then through not melting, after charcoal activation (charing and activation are finished synchronously) handles, obtaining product.
Being fit to raw material of the present invention can be coal-tar pitch, also can be all kinds of pitches of petroleum slag wet goods.Pitch can adopt heat treating method commonly used to obtain softening temperature at 200-300 ℃ high softening point bitumen.
Employed additive can be selected one or more in the aromatic compounds such as benzene, toluene, naphthalene, naphthane, anthracene among the present invention.
The used emulsion of the present invention is made up of tensio-active agent and dispersion medium.Tensio-active agent can be half saponified polyvinyl acetate, methylcellulose gum, polyoxyethylene glycol, polyvinyl alcohol, starch etc., and dispersion medium can be silicone oil, glycerol, hydro carbons higher-boiling compound, water etc.
Used solvent extraction process, emulsion process, non-method of fusion, the charcoal activation method of present method is technology commonly used in the existing chemical field.Charing and activation are carried out in low speed circulating fluidized bed.
Compared with the prior art method of the present invention has following advantage:
(1) is the feedstock production asphalt-base globular active carbon with the coal-tar pitch, enlarged raw material sources.
(2) adopt emulsion process, control the size of bitumen ball by the size of control eutectic crushed particles, and then reach the globule size of control asphalt-base globular active carbon.
(3) in low speed circulating fluidized bed, carry out the not charing and the activation of molten asphalt ball, make the spheric active carbon of high mechanical strength.
It is following that the example that provides will the present invention is described in detail.
Embodiment 1
With coal-tar pitch (70 ℃ of softening temperatures) is raw material, under 300 ℃, by atmospheric oxidation 2 hours, makes high softening point bitumen (247 ℃ of softening temperatures).
Getting high softening point bitumen (softening temperature is 247 ℃) 130 gram, add naphthalene 70 grams, is that 150 ℃, pressure are 0.6MPa modulated pitch eutectic in temperature, standby after cooling, broken, screening.
Embodiment 2
Getting embodiment 1 granularity is the eutectic of 0.15-0.35mm, under 132 ℃ of temperature, pressure 0.6MPa, adopts the emulsion process balling-up.The concentration of emulsion is 4%, (weight ratio of surface active agent polyvinyl alcohol and dispersion medium water is 4: 96).Bitumen ball is carried out the solvent impregnated porous asphalt ball of making, again through 300 ℃ of melt processed not, in low speed circulating fluidized bed, carry out the not charing of molten asphalt ball in 900 ℃, and under this temperature with steam activation 3 hours, make the coal-tar pitch base spheric active carbon of 0.15-0.35mm, its specific surface area S
BET=1016m
2/ g, sphericity 0.95, intensity 95wt%.Specific surface area and pore volume by ASAP absorption instrument according to gac at low temperatures (77K) adsorption isothermal line of nitrogen is recorded, sphericity is the minor semi-axis of spheric active carbon and the ratio of semi-major axis, intensity is to record according to Chinese national standard GB7702.3-87.
Embodiment 3
Getting embodiment 1 granularity is the eutectic of 0.35-0.45mm, under 132 ℃ of temperature, pressure 0.6MPa, employing concentration is 4% emulsion (Emulsion is with embodiment 2), make the bitumen ball of 0.35-0.45mm by emulsion process, bitumen ball is carried out the solvent impregnated porous asphalt ball of making, again through 300 ℃ of melt processed not, in low speed circulating fluidized bed, carry out the not charing of molten asphalt ball in 900 ℃, and under this temperature with steam activation 2 hours, make the coal-tar pitch base spheric active carbon of 0.15-0.45, its specific surface area S
BET=1300m
2/ g, total pore volume is 0.64ml/g, sphericity 0.95, intensity 94wt%.
Embodiment 4
Getting embodiment 1 granularity is the eutectic of 0.6-1.0mm, under 132 ℃ of temperature, pressure 0.6MPa, employing concentration is 4% emulsion, make the bitumen ball of 0.60-1.0mm by emulsion process, bitumen ball is carried out the solvent impregnated porous asphalt ball of making, again through 300 ℃ of melt processed not, in low speed circulating fluidized bed, carry out the not charing of molten asphalt ball in 900 ℃, and under this temperature, use steam activation 2 hours, make the coal-tar pitch base spheric active carbon of 0.45-0.85mm, its specific surface area S
BET=1170m
2/ g, total pore volume is 0.48ml/g, sphericity 0.95, intensity 95wt%.
Claims (9)
1. method for preparing spheric active carbon is characterized in that carrying out as follows:
(1) with high softening point bitumen and additive with 100: the ratio of 10-50 mixes under 100-300 ℃, makes eutectic, and is standby after broken, screening,
(2) get the eutectic of sieving the corresponding granularity in back and place reactor, add emulsion, in temperature is 130-150 ℃, under the pressure 0.4-0.8MPa, make the bitumen ball that contains additive by emulsion process, remove additive with solvent extraction process again and make the porous asphalt ball, then through do not melt, after charcoal activation (charing and activation are finished synchronously) handles, product.
2. the method for claim 1 is characterized in that the softening temperature of described high softening point bitumen is preferably 200-300 ℃.
3. the method for claim 1, feature is that described additive can be selected one or more in naphthalene benzene, toluene, the naphthane anthracene.
4. the method for claim 1, it is characterized in that described emulsion is made up of tensio-active agent and dispersion medium, tensio-active agent can be half saponified polyvinyl acetate, methylcellulose gum, polyoxyethylene glycol, polyvinyl alcohol, starch, and dispersion medium can be silicone oil, glycerol, hydro carbons higher-boiling compound, water.
5. the method for claim 1 is characterized in that the charing of described not molten asphalt ball and activation treatment are to carry out in low speed circulating fluidized bed.
6. method as claimed in claim 2 is characterized in that described pitch is coal-tar pitch.
7. method as claimed in claim 3 is characterized in that preferably naphthalene of described additive.
8. method as claimed in claim 4 is characterized in that preferably polyvinyl alcohol of described tensio-active agent.
9. method as claimed in claim 4 is characterized in that preferably water of described dispersion medium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97101617A CN1057278C (en) | 1997-01-17 | 1997-01-17 | Method for preparing globular active carbon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97101617A CN1057278C (en) | 1997-01-17 | 1997-01-17 | Method for preparing globular active carbon |
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| CN1188074A true CN1188074A (en) | 1998-07-22 |
| CN1057278C CN1057278C (en) | 2000-10-11 |
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| CN97101617A Expired - Fee Related CN1057278C (en) | 1997-01-17 | 1997-01-17 | Method for preparing globular active carbon |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1084293C (en) * | 1998-10-07 | 2002-05-08 | 中国科学院山西煤炭化学研究所 | Preparation of middle-pore asphalt-base globular active carbon |
| CN100371241C (en) * | 2004-11-24 | 2008-02-27 | 中国科学院金属研究所 | Apparatus for producing isotropic pyrolyzed carbon materials of large-size machinery seal |
| CN100462302C (en) * | 2006-08-31 | 2009-02-18 | 华东理工大学 | Method for preparing spherical active carbon with low content of beary metal |
| CN1956919B (en) * | 2004-05-20 | 2011-08-03 | 可乐丽化学株式会社 | Spherical active carbon and process for producing the same |
| CN102218297A (en) * | 2011-04-28 | 2011-10-19 | 孔亦周 | Preparation method of asphalt based spherical active carbon without infusibility processing technology |
| US8247072B2 (en) | 2006-02-14 | 2012-08-21 | Eastman Chemical Company | Resol beads, methods of making them and methods of using them |
| CN104084195A (en) * | 2014-07-11 | 2014-10-08 | 中国船舶重工集团公司第七一八研究所 | Load type spherical active carbon catalyst and preparation method thereof |
| CN104232135A (en) * | 2014-09-25 | 2014-12-24 | 四川创越炭材料有限公司 | Purification method for coal pitch with high softening point |
| CN104276569A (en) * | 2014-10-21 | 2015-01-14 | 中国科学院山西煤炭化学研究所 | Method for improving crushing strength of asphalt-based spherical activated carbon |
| CN105836747A (en) * | 2016-03-21 | 2016-08-10 | 邵武市金寿活性炭有限公司 | Spherical activated carbon and preparation method thereof |
| CN106517199A (en) * | 2015-12-21 | 2017-03-22 | 山东晨阳新型碳材料股份有限公司 | Preparation method for spherical active carbon with hollow shell-core structure |
| CN108516547A (en) * | 2018-05-16 | 2018-09-11 | 辽宁科技大学 | The preparation method of carbon black-coal tar pitch complex spherical activated carbon |
| CN108940135A (en) * | 2018-06-20 | 2018-12-07 | 东南大学 | Coal pitch spheres aoxidize infusible stepped heating difference frequency vibratory liquefaction system and method |
| CN109399632A (en) * | 2018-09-29 | 2019-03-01 | 中国科学院山西煤炭化学研究所 | A method of preparing asphalt-base globular active carbon |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6114110A (en) * | 1984-06-26 | 1986-01-22 | Kawasaki Steel Corp | Manufacture of fine and hollow body of carbon |
-
1997
- 1997-01-17 CN CN97101617A patent/CN1057278C/en not_active Expired - Fee Related
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1084293C (en) * | 1998-10-07 | 2002-05-08 | 中国科学院山西煤炭化学研究所 | Preparation of middle-pore asphalt-base globular active carbon |
| CN1956919B (en) * | 2004-05-20 | 2011-08-03 | 可乐丽化学株式会社 | Spherical active carbon and process for producing the same |
| CN100371241C (en) * | 2004-11-24 | 2008-02-27 | 中国科学院金属研究所 | Apparatus for producing isotropic pyrolyzed carbon materials of large-size machinery seal |
| US8247072B2 (en) | 2006-02-14 | 2012-08-21 | Eastman Chemical Company | Resol beads, methods of making them and methods of using them |
| US8557381B2 (en) | 2006-02-14 | 2013-10-15 | Eastman Chemical Company | Resol beads, methods of making them, and methods of using them |
| CN100462302C (en) * | 2006-08-31 | 2009-02-18 | 华东理工大学 | Method for preparing spherical active carbon with low content of beary metal |
| CN102218297A (en) * | 2011-04-28 | 2011-10-19 | 孔亦周 | Preparation method of asphalt based spherical active carbon without infusibility processing technology |
| CN104084195A (en) * | 2014-07-11 | 2014-10-08 | 中国船舶重工集团公司第七一八研究所 | Load type spherical active carbon catalyst and preparation method thereof |
| CN104232135A (en) * | 2014-09-25 | 2014-12-24 | 四川创越炭材料有限公司 | Purification method for coal pitch with high softening point |
| CN104276569A (en) * | 2014-10-21 | 2015-01-14 | 中国科学院山西煤炭化学研究所 | Method for improving crushing strength of asphalt-based spherical activated carbon |
| CN106517199A (en) * | 2015-12-21 | 2017-03-22 | 山东晨阳新型碳材料股份有限公司 | Preparation method for spherical active carbon with hollow shell-core structure |
| CN106517199B (en) * | 2015-12-21 | 2018-09-18 | 济宁碳素集团有限公司 | A kind of preparation method of hollow nucleocapsid spherical activated charcoal |
| CN105836747A (en) * | 2016-03-21 | 2016-08-10 | 邵武市金寿活性炭有限公司 | Spherical activated carbon and preparation method thereof |
| CN105836747B (en) * | 2016-03-21 | 2019-01-29 | 邵武市金寿活性炭有限公司 | A kind of spherical activated charcoal and preparation method thereof |
| CN108516547A (en) * | 2018-05-16 | 2018-09-11 | 辽宁科技大学 | The preparation method of carbon black-coal tar pitch complex spherical activated carbon |
| CN108940135A (en) * | 2018-06-20 | 2018-12-07 | 东南大学 | Coal pitch spheres aoxidize infusible stepped heating difference frequency vibratory liquefaction system and method |
| CN109399632A (en) * | 2018-09-29 | 2019-03-01 | 中国科学院山西煤炭化学研究所 | A method of preparing asphalt-base globular active carbon |
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| CN1057278C (en) | 2000-10-11 |
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