CN104276569B - A kind of method improving asphalt-base globular active carbon crushing strength - Google Patents
A kind of method improving asphalt-base globular active carbon crushing strength Download PDFInfo
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- CN104276569B CN104276569B CN201410560489.8A CN201410560489A CN104276569B CN 104276569 B CN104276569 B CN 104276569B CN 201410560489 A CN201410560489 A CN 201410560489A CN 104276569 B CN104276569 B CN 104276569B
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Abstract
A kind of method improving asphalt-base globular active carbon crushing strength is by after high softening point bitumen, naphthalene, iodide Homogeneous phase mixing, obtains modifying asphalt in 230-350 DEG C of reaction; Joining containing concentration is afterwards in the autoclave of 1-5wt% polyvinyl alcohol water solution, at 85-150 DEG C, stir 0.5-3h, obtains bitumen ball; Bitumen ball is not melted through peroxidation, and carbonization-activation process obtains product.The present invention has and can be mass-produced, the advantage that crushing strength is high.
Description
Technical field
The present invention relates to a kind of preparation method of gac, relate in particular to a kind of method improving asphalt-base globular active carbon crushing strength.
Background technology
Spheric active carbon can be applicable to a lot of field, is wherein asphalt-base globular active carbon prepared by raw material obtains researchist favor because material cost is cheap, starting material are easy to get with pitch, is therefore mainly manifested in following several respects to its research:
(1) aspect is prepared: if application number is 201310673124.1 " preparing the method for ball shape active carbon with water-soluble pitch ", CN97101617.8 " a kind of preparation method of spheric active carbon ", CN98104975.3 " preparation method of asphalt-base globular active carbon " and CN200910241779.5 " a kind of activated carbon microballon and preparation method thereof ";
(2) accelerating oxidation does not melt maybe need not be oxidized and does not melt aspect: CN201110108729.7 " a kind of preparation method of the asphalt-base spherical activated carbon without the need to molten treatment process ", CN201210317727.3 " the low power consuming preparation method of asphalt-base spherical activated carbon ", CN96102663.4 " promote the method for non-melting process of asphalt balls ";
(3) holes of products structure regulating aspect: CN201410071680.6 " a kind of preparation method of asphalt-base spherical activated carbon of mesoporous prosperity ", CN03178572.7 " is rich in the preparation method of the asphalt-base globular active carbon of mesopore ", CN98104731.9 " adds the method that metal inorganic salt prepares asphalt-base globular active carbon ", CN200810037092.5 " method of preparing mesopore pitch-based spherical activated carbon by post-carbonizing impregnated metal salts ", CN98123530.1 " a kind of preparation method of mesopore asphalt-base globular active carbon ", CN99102012.X " a kind of method controlling porous structure of spherical asphalt-base activated carbon ",
(4) gac aftertreatment aspect: CN201010583089.0 " a kind of preparation method protecting the asphalt ball impregnation carbon of H2S, NH3 ", CN200810041080.X " a kind of spherical active carbon fuel oil adsorption desulfurizing and preparation method thereof ", CN200810040665.X " a kind of novel globular active carbon and the application at desulfuration field thereof ";
(5) starting material modification aspect: CN200610127621.1 " a kind of method preparing the low ball shape active carbon of heavy metal content ", CN200810037093.X " a kind of preparation method of nitrogen-containing asphalt-base spherical activated ";
(6) product yield aspect: CN200810037093.X " a kind of preparation method of high-carbon yield asphalt group spherical absorbent charcoal " is improved.
Although carried out above-mentioned research, in the crushing strength improving asphalt-base globular active carbon, there is no pertinent literature.
Summary of the invention
The object of this invention is to provide one can be mass-produced, the method for the raising asphalt-base globular active carbon crushing strength that crushing strength is high.
Preparation method of the present invention comprises the steps:
(1) preparation of modifying asphalt: be 1:(0.2-05 by mass ratio): after the high softening point bitumen of (0.1-0.3), naphthalene, iodide Homogeneous phase mixing, in 230-350 DEG C of reaction 3-5h, obtain modifying asphalt;
(2) preparation of bitumen ball: modifying asphalt obtains 0.1-2mm pitch particle after crushing and screening, joining containing concentration is afterwards in the autoclave of 1-5wt% polyvinyl alcohol water solution, wherein the quality of polyvinyl alcohol is the 5-15% of pitch, at 85-150 DEG C, stir 0.5-3h, obtains bitumen ball; Concrete preparation method is prepared according to CN97101617.8 " a kind of preparation method of spheric active carbon ";
(3) oxidation of bitumen ball is not melted: with 30-120 DEG C/h temperature rise rate from room temperature to 230-350 DEG C, stops 2-5h, obtains oxidized bitumen ball; Concrete oxidation is not melted method and is processed according to patent 201310227294.7 " bitumen ball is oxidized non-fusible method ";
(4) carbonization-activation of ball is oxidized: with 3-10 DEG C/min temperature rise rate DEG C stop 0.5-2h from room temperature to 800-1000 in an inert atmosphere, switch to water vapour or CO afterwards
2activation 1-5h, obtain product, concrete preparation method is prepared according to CN97101617.8 " a kind of preparation method of spheric active carbon ".
Iodide as above are one in potassiumiodide, sodium iodide, ammonium iodide or two kinds.
The softening point range of high softening point bitumen as above is at 200-300 DEG C.
Crushing strength of the present invention measures and adopts patent 200820105920.X " instrument for testing crushed strength of simple-grain spherical particles " method: choose the spheric active carbon 26 that diameter is 0.8mm, intensity meter is measured the single pellet crush strength of spheric active carbon, cast out maximum, each three of minimum value, calculate the mean value of 20.Repeat 3 times, then average as the crushing strength of simple grain.
Tool of the present invention has the following advantages:
Due to this patent i.e. properties-correcting agent in doping in starting material, thus table can be obtained mutually and body modification uniformly mutually, cause the high strength that the performance of the finished product can reach invented;
By the method for invention, can significantly promote with pitch is the crushing strength of spheric active carbon prepared by raw material; This patent can further genralrlization be also the strength enhancing aspect of gac prepared by raw material with pitch to other, as columnar activated carbon, Alveolate activated carbon capable, amorphous gac etc.
This patent method is simple, and properties-correcting agent is conventional chemical reagent, is easy to buy in a large number.
Embodiment
Embodiment 1
Be after 300 DEG C of softening point asphalts of 1:0.5:0.1, naphthalene, potassiumiodide Homogeneous phase mixing by mass ratio, in 230 DEG C of reaction 5h, obtain modifying asphalt; Modifying asphalt obtains 0.1mm pitch particle after crushing and screening, and joining containing concentration is afterwards in the aqueous solution of 1wt% polyvinyl alcohol, and wherein the quality of polyvinyl alcohol is 5% of pitch, at 85 DEG C, stir 3h, obtains bitumen ball; Bitumen ball from room temperature to 230 DEG C, stops 5h with 120 DEG C/h temperature rise rate, obtains oxidized bitumen ball; Air is switched to N
2after with 10 DEG C/min temperature rise rate from room temperature to 800 DEG C stop 2h, switch to steam activation 3h afterwards, obtain product.
The single particle crushing strength of this product is 10.2N, and specific surface area is 1450m
2/ g, sphere diameter is between 0.08-0.12mm.
Embodiment 2
Be after 240 DEG C of softening point asphalts of 1:0.2:0.3, naphthalene, sodium iodide Homogeneous phase mixing by mass ratio, in 350 DEG C of reaction 3h, obtain modifying asphalt; Modifying asphalt obtains 0.5mm pitch particle after crushing and screening, and joining containing concentration is afterwards in the aqueous solution of 5wt% polyvinyl alcohol, and wherein the quality of polyvinyl alcohol is 10% of pitch, at 150 DEG C, stir 1h, obtains bitumen ball; Bitumen ball from room temperature to 330 DEG C, stops 2h with 30 DEG C/h temperature rise rate, obtains oxidized bitumen ball; Air is switched to N
2after with 3 DEG C/min temperature rise rate from room temperature to 1000 DEG C stop 0.5h, switch to steam activation 0.5h afterwards, obtain product.
The single particle crushing strength of this product is 13.3N, and specific surface area is 1140m
2/ g, sphere diameter is between 0.3-0.65mm.
Embodiment 3
Be after 200 DEG C of softening point asphalts of 1:0.3:0.2, naphthalene, ammonium iodide Homogeneous phase mixing by mass ratio, in 320 DEG C of reaction 4h, obtain modifying asphalt; Modifying asphalt obtains 1.5mm pitch particle after crushing and screening, and joining containing concentration is afterwards in the aqueous solution of 3wt% polyvinyl alcohol, and wherein the quality of polyvinyl alcohol is 15% of pitch, at 145 DEG C, stir 0.5h, obtains bitumen ball; Bitumen ball from room temperature to 350 DEG C, stops 5h with 60 DEG C/h temperature rise rate, obtains oxidized bitumen ball; Air is switched to N
2after with 4 DEG C/min temperature rise rate from room temperature to 900 DEG C stop 1h, switch to CO afterwards
2activation 5h, obtains product.
The single particle crushing strength of this product is 15.4N, and specific surface area is 1320m
2/ g, sphere diameter is between 1.3-1.62mm.
Embodiment 4
Be after 280 DEG C of softening point asphalts of 1:0.25:0.15, naphthalene, potassiumiodide and sodium iodide (the two is 1:1 in mass ratio) Homogeneous phase mixing by mass ratio, in 300 DEG C of reaction 4h, obtain modifying asphalt; Modifying asphalt obtains 2mm pitch particle after crushing and screening, and joining containing concentration is afterwards in the aqueous solution of 2wt% polyvinyl alcohol, and wherein the quality of polyvinyl alcohol is 12% of pitch, at 140 DEG C, stir 01h, obtains bitumen ball; Bitumen ball from room temperature to 350 DEG C, stops 5h with 30 DEG C/h temperature rise rate, obtains oxidized bitumen ball; Air is switched to N
2after with 3 DEG C/min temperature rise rate from room temperature to 950 DEG C stop 2h, switch to steam activation 1h afterwards, obtain product.
The single particle crushing strength of this product is 13.9N, and specific surface area is 1410m
2/ g, sphere diameter is between 1.8-2.0mm.
Embodiment 5
Be after 300 DEG C of softening point asphalts of 1:0.4:0.25, naphthalene, potassiumiodide and ammonium iodide (the two is 2:1 in mass ratio) Homogeneous phase mixing by mass ratio, in 280 DEG C of reaction 5h, obtain modifying asphalt; Modifying asphalt obtains 0.8mm pitch particle after crushing and screening, and joining containing concentration is afterwards in the aqueous solution of 4wt% polyvinyl alcohol, and wherein the quality of polyvinyl alcohol is 8% of pitch, at 90 DEG C, stir 2h, obtains bitumen ball; Bitumen ball from room temperature to 260 DEG C, stops 3h with 100 DEG C/h temperature rise rate, obtains oxidized bitumen ball; Air is switched to N
2after with 8 DEG C/min temperature rise rate from room temperature to 850 DEG C stop 2h, switch to CO afterwards
2activation 5h, obtains product.
The single particle crushing strength of this product is 18.1N, and specific surface area is 1120m
2/ g, sphere diameter is between 0.6-1.2mm.
Embodiment 6
Be after 260 DEG C of softening point asphalts of 1:0.35:0.3, naphthalene, sodium iodide and ammonium iodide (the two is 3:1 in mass ratio) Homogeneous phase mixing by mass ratio, in 300 DEG C of reaction 3h, obtain modifying asphalt; Modifying asphalt obtains 1.3mm pitch particle after crushing and screening, and joining containing concentration is afterwards in the aqueous solution of 5wt% polyvinyl alcohol, and wherein the quality of polyvinyl alcohol is 10% of pitch, at 130 DEG C, stir 1h, obtains bitumen ball; Bitumen ball from room temperature to 320 DEG C, stops 4h with 60 DEG C/h temperature rise rate, obtains oxidized bitumen ball; Air is switched to N
2after with 5 DEG C/min temperature rise rate from room temperature to 930 DEG C stop 1h, switch to CO afterwards
2activation 4h, obtains product.
The single particle crushing strength of this product is 18.8N, and specific surface area is 1520m
2/ g, sphere diameter is between 1.0-1.2mm.
Embodiment 7
Be after 270 DEG C of softening point asphalts of 1:0.5:0.2, naphthalene, potassiumiodide Homogeneous phase mixing by mass ratio, in 330 DEG C of reaction 3h, obtain modifying asphalt; Modifying asphalt obtains 0.5mm pitch particle after crushing and screening, and joining containing concentration is afterwards in the aqueous solution of 3wt% polyvinyl alcohol, and wherein the quality of polyvinyl alcohol is 5% of pitch, at 85 DEG C, stir 2h, obtains bitumen ball; Bitumen ball from room temperature to 230 DEG C, stops 3h with 120 DEG C/h temperature rise rate, obtains oxidized bitumen ball; Air is switched to N
2after with 10 DEG C/min temperature rise rate from room temperature to 900 DEG C stop 0.5h, switch to CO afterwards
2activation 3h, obtains product.
The single particle crushing strength of this product is 12.4N, and specific surface area is 1620m
2/ g, sphere diameter is between 0.3-0.6mm.
Embodiment 8
Be after 290 DEG C of softening point asphalts of 1:0.25:0.25, naphthalene, ammonium iodide Homogeneous phase mixing by mass ratio, in 350 DEG C of reaction 5h, obtain modifying asphalt; Modifying asphalt obtains 1.2mm pitch particle after crushing and screening, and joining containing concentration is afterwards in the aqueous solution of 4wt% polyvinyl alcohol, and wherein the quality of polyvinyl alcohol is 7% of pitch, at 145 DEG C, stir 1h, obtains bitumen ball; Bitumen ball from room temperature to 330 DEG C, stops 5h with 50 DEG C/h temperature rise rate, obtains oxidized bitumen ball; Air is switched to N
2after with 3 DEG C/min temperature rise rate from room temperature to 930 DEG C stop 2h, switch to CO afterwards
2activation 5h, obtains product.
The single particle crushing strength of this product is 22.1N, and specific surface area is 1180m
2/ g, sphere diameter is between 0.8-1.3mm.
Comparative example
Be after 290 DEG C of softening point asphalts of 1:0.25, naphthalene Homogeneous phase mixing by mass ratio, in 350 DEG C of reaction 5h, obtain modifying asphalt; Modifying asphalt obtains 1.2mm pitch particle after crushing and screening, and joining containing concentration is afterwards in the aqueous solution of 4wt% polyvinyl alcohol, and wherein the quality of polyvinyl alcohol is 7% of pitch, at 145 DEG C, stir 1h, obtains bitumen ball; Bitumen ball from room temperature to 330 DEG C, stops 5h with 50 DEG C/h temperature rise rate, obtains oxidized bitumen ball; Air is switched to N
2after with 3 DEG C/min temperature rise rate from room temperature to 930 DEG C stop 2h, switch to CO afterwards
2activation 5h, obtains product.
The single particle crushing strength of this product is 7.1N, and specific surface area is 1150m
2/ g, sphere diameter is between 0.8-1.2mm.
Claims (3)
1. improve a method for asphalt-base globular active carbon crushing strength, it is characterized in that comprising the steps:
(1) preparation of modifying asphalt: be after the high softening point bitumen of 1:0.2-0.5:0.1-0.3, naphthalene, iodide Homogeneous phase mixing by mass ratio, in 230-350 DEG C of reaction 3-5h, obtains modifying asphalt;
(2) preparation of bitumen ball: modifying asphalt obtains 0.1-2mm pitch particle after crushing and screening, joining containing concentration is afterwards in the autoclave of 1-5wt% polyvinyl alcohol water solution, wherein the quality of polyvinyl alcohol is the 5-15% of pitch, at 85-150 DEG C, stir 0.5-3h, obtains bitumen ball;
(3) oxidation of bitumen ball is not melted: with 30-120 DEG C/h temperature rise rate from room temperature to 230-350 DEG C, stops 2-5h, obtains oxidized bitumen ball;
(4) carbonization-activation of ball is oxidized: with 3-10 DEG C/min temperature rise rate DEG C stop 0.5-2h from room temperature to 800-1000 in an inert atmosphere, switch to water vapour or CO afterwards
2activation 1-5h, obtains product.
2. a kind of method improving asphalt-base globular active carbon crushing strength as claimed in claim 1, is characterized in that described iodide are one in potassiumiodide, sodium iodide, ammonium iodide or two kinds.
3. a kind of method improving asphalt-base globular active carbon crushing strength as claimed in claim 1, is characterized in that the softening point range of described high softening point bitumen is at 200-300 DEG C.
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| CN104909365B (en) * | 2015-06-09 | 2017-12-19 | 中国科学院山西煤炭化学研究所 | Bitumen ball aoxidizes nonfused promotion method |
| CN105253884B (en) * | 2015-11-12 | 2017-09-26 | 山西新华化工有限责任公司 | Do not melt method for the oxidation for industrializing bitumen ball activated carbon |
| CN106318425B (en) * | 2016-08-30 | 2019-01-11 | 中国科学院山西煤炭化学研究所 | One kind micro mist containing naphthalene pitch prepares grade bitumen ball method |
| JPWO2020246448A1 (en) * | 2019-06-03 | 2020-12-10 | ||
| CN111422869A (en) * | 2020-03-04 | 2020-07-17 | 山西新华化工有限责任公司 | Preparation method for industrially improving crushing strength of asphalt balls |
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| JPS5571613A (en) * | 1978-11-27 | 1980-05-29 | Toho Rayon Co Ltd | Production of fibrous activated carbon |
| CN1057278C (en) * | 1997-01-17 | 2000-10-11 | 中国科学院山西煤炭化学研究所 | Method for preparing globular active carbon |
| CN101492162B (en) * | 2009-03-11 | 2011-02-02 | 煤炭科学研究总院 | Modified active coke, production and uses thereof |
| CN103272533B (en) * | 2013-06-08 | 2015-01-07 | 中国科学院山西煤炭化学研究所 | Pitch sphere oxidative stabilization method |
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