CN103289719B - Process for preparing asphalt sphere - Google Patents
Process for preparing asphalt sphere Download PDFInfo
- Publication number
- CN103289719B CN103289719B CN201310227822.9A CN201310227822A CN103289719B CN 103289719 B CN103289719 B CN 103289719B CN 201310227822 A CN201310227822 A CN 201310227822A CN 103289719 B CN103289719 B CN 103289719B
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- China
- Prior art keywords
- autoclave
- pitch
- temperature
- asphalt
- stir
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000010426 asphalt Substances 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title description 2
- 238000003756 stirring Methods 0.000 claims abstract description 35
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000011295 pitch Substances 0.000 claims description 32
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 5
- -1 polyoxyethylene Polymers 0.000 claims description 5
- QQXDYWHKPKEBJU-UHFFFAOYSA-N CCCCCCCCCCCCCCCCCC[Na] Chemical compound CCCCCCCCCCCCCCCCCC[Na] QQXDYWHKPKEBJU-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 7
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 150000002790 naphthalenes Chemical class 0.000 description 4
- 238000004945 emulsification Methods 0.000 description 3
- 239000011280 coal tar Substances 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 239000011339 hard pitch Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011338 soft pitch Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000006353 environmental stress Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000011269 tar Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Working-Up Tar And Pitch (AREA)
Abstract
一种沥青球制备工艺是按每1升高压釜体积中放入0.2-0.4公斤重量的沥青，将沥青放入高压釜内，之后按每公斤沥青每小时需要10-20升的空气量通入空气，然后升温，待温度升到150-200℃时开启搅拌，搅拌速率为200-400转/分，继续升温到300-380℃进行氧化1-5h；之后高压釜在搅拌下降温到180-250℃，加入沥青重量20-35%的萘，在该温度下搅拌1-3h，然后降温到80-95℃；再将沥青重量0.1-1wt%的分散剂加入高压釜，同时将水加入到高压釜体积的60-80%，在100-150℃下以300-500转/分的转速搅拌1-5h后降温到室温，固液分离即得0.5-1.5mm的沥青球。本发明具有无污染，不经破碎或挤条直接在同一套反应釜内完成制备沥青球工艺的优点。A kind of asphalt ball preparation process is to put 0.2-0.4 kilograms of asphalt into the autoclave per 1 liter of volume, put the asphalt into the autoclave, and then feed in an air volume of 10-20 liters per hour per kilogram of asphalt Air, then heat up, start stirring when the temperature rises to 150-200°C, the stirring rate is 200-400 rpm, continue to heat up to 300-380°C for oxidation for 1-5h; after that, the autoclave is cooled down to 180- 250°C, add 20-35% of asphalt weight naphthalene, stir at this temperature for 1-3h, then cool down to 80-95°C; then add 0.1-1wt% asphalt dispersant into the autoclave, and add water to the autoclave at the same time 60-80% of the volume of the autoclave is stirred at 100-150°C at a speed of 300-500 rpm for 1-5 hours, then cooled to room temperature, and solid-liquid separation is performed to obtain pitch balls of 0.5-1.5 mm. The invention has the advantages of no pollution, and the process of preparing asphalt balls can be directly completed in the same set of reaction kettle without crushing or extruding.
Description
Technical field
The invention belongs to a kind of preparation technology of bitumen ball.
Background technology
Spheric active carbon is a kind of important absorbent charcoal material, and compared with the gac of other types, the research report of ball-type gac is less, especially sphere diameter be the millimetre-sized spheric active carbon taking pitch as raw material still less.What prepare this spheric active carbon is pitch containing carbon matrix precursor, needs first pitch to be carried out being prepared as bead by emulsification method again after modification, and the modification of pitch and balling-up become indispensable step for this reason.
The patent of preparing grade spheric active carbon taking pitch as presoma is more, Chinese invention patent 03178572 " is rich in the preparation method of the asphalt-base globular active carbon of mesopore " and is pitch, the atmospheric oxidation of coal tar wet goods are obtained adding aromatic hydrocarbon small molecules to carry out modification to it after the pitch of softening temperature 200-300 DEG C again, afterwards by adding dispersion agent to make balling-up pitch, final emulsion balling-up, makes bitumen ball thereby also need to obtain the emulsification balling-up that balling-up pitch just can carry out next step; It is by heavy hydrocarbon oil level raw materials such as the residues of petroleum tar, coal tar, low softening point asphalt or petroleum naphtha ethene processed that Chinese invention patent 200410100531 " is prepared the method for spherical activated carbon ", by using oxygenant as HNO
3, air etc. is oxidized and makes oxidized bitumen, carries out modification afterwards with the aromatic hydrocarbons of naphthalene one class, and at a certain temperature extrusion, be broken into clavate fragment, then emulsification balling-up.Visible, its pitch for balling-up is the fragment after fragmentation; Chinese invention patent 200610127621 " a kind of method of preparing the ball shape active carbon that heavy metal content is low ", Chinese invention patent 200810035853 " a kind of preparation method of nitrogen-containing asphalt-base spherical activated " and Chinese invention patent 201210317727 " the low power consuming preparation method of asphalt-base spherical activated carbon " etc. all need the pitch that makes in advance balling-up could finally obtain corresponding bitumen ball, so virtually not only need many complete equipments but also technological process is lengthened, simultaneously inevitable generation environmental pollution in acquisition balling-up pitch process.
Summary of the invention
The object of this invention is to provide one pollution-free, directly in same set of reactor, complete without fragmentation or extrusion the technique of preparing bitumen ball.
Preparation technology of the present invention realizes as follows:
In long-pending by every 1 liter of autoclave body, put into the pitch of 0.2-0.4 kilogram weight, pitch is put into autoclave, the air capacity rising by the per kilogram pitch 10-20 of needs per hour afterwards passes into air, then heat up, in the time that temperature is raised to 150-200 DEG C, opens and stir, stir speed (S.S.) is 200-400 rev/min, continues to be warmed up to 300-380 DEG C and is oxidized 1-5h; Autoclave under agitation cools to 180-250 DEG C afterwards, adds the naphthalene of pitch weight 20-35%, at this temperature, stirs 1-3h, then cools to 80-95 DEG C; Again the dispersion agent of pitch weight 0.1-1wt% is added to autoclave, water is joined to the 60-80% of autoclave volume simultaneously, at 100-150 DEG C, to cool to room temperature after the rotating speed stirring 1-5h of 300-500 rev/min, solid-liquid separation obtains the bitumen ball of 0.5-1.5mm.
The present invention's pitch used is that softening temperature is 35～75 DEG C of soft pitches, 75～95 DEG C of mid-temperature pitches or 95～120 DEG C of hard pitches.
Dispersion agent as above is polyvinyl alcohol, polyoxyethylene glycol or octadecyl sodium sulfonate.
Advantage of the present invention:
(1) all reaction masses all react in same set of equipment, and its utilization ratio is greatly improved, very favourable to reducing production costs;
(2) owing to operating in same set of reactor, can not produce a large amount of waste gas and waste residue, alleviate environmental stress;
(3) the present invention all operates in a set of reactor, and floor space reduces greatly, and equipment cost significantly reduces.
Embodiment
Embodiment 1
The soft pitch of putting into 35～75 DEG C of softening temperatures of 4 kilograms in 10 liters of autoclaves, blasts 40 liters/h air, then heats up, and in the time that temperature is raised to 150 DEG C, opens and stirs, and stir speed (S.S.) is 200 revs/min, continues to be warmed up to 300 DEG C and is oxidized 5h; Reactor under agitation cools to 180 DEG C afterwards, add 0.8 kilogram of naphthalene, at this temperature, stir 3h, then cool to 80 DEG C, now add the polyvinyl alcohol of asphalt quality 1wt%, water is joined simultaneously kettle long-pending 60%, cool to room temperature stir 1h with the rotating speed of 300 revs/min at 150 DEG C after, solid-liquid separation obtains bitumen ball.The sphere diameter of gained bitumen ball more than 90% is 1.5mm, and sphericity reaches 95%.
Embodiment 2
The hard pitch of putting into 95～120 DEG C of softening temperatures of 20 kilograms in 100 liters of autoclaves, blasts 400 liters/h air, then heats up, and in the time that temperature is raised to 200 DEG C, opens and stirs, and stir speed (S.S.) is 300 revs/min, continues to be warmed up to 350 DEG C and is oxidized 3h; Reactor under agitation cools to 230 DEG C afterwards, add 7 kilograms of naphthalenes, at this temperature, stir 3h, then cool to 90 DEG C, now add the octadecyl sodium sulfonate of asphalt quality 5wt%, water is joined simultaneously kettle long-pending 70%, cool to room temperature stir 3h with the rotating speed of 400 revs/min at 120 DEG C after, solid-liquid separation obtains bitumen ball.The sphere diameter of gained bitumen ball more than 92% is 1.1mm, and sphericity reaches 93%.
Embodiment 3
The mid-temperature pitch of putting into 75～95 DEG C of softening temperatures of 400 kilograms in 1000 liters of autoclaves, blasts 6000 liters/h air, then heats up, and in the time that temperature is raised to 180 DEG C, opens and stirs, and stir speed (S.S.) is 400 revs/min, continues to be warmed up to 380 DEG C and is oxidized 1h; Reactor under agitation cools to 250 DEG C afterwards, add 120 kg naphthalene, at this temperature, stir 2h, then cool to 95 DEG C, now add the polyoxyethylene glycol of asphalt quality 10wt%, add simultaneously water to kettle long-pending 80%, cool to room temperature stir 5h with the rotating speed of 500 revs/min at 100 DEG C after, solid-liquid separation obtains bitumen ball.The sphere diameter of gained bitumen ball more than 92% is 0.5mm, and sphericity reaches 97%.
Embodiment 4
The soft pitch of putting into 35～75 DEG C of softening temperatures of 20 kilograms in 50 liters of autoclaves, blasts 300 liters/h air, then heats up, and in the time that temperature is raised to 160 DEG C, opens and stirs, and stir speed (S.S.) is 250 revs/min, continues to be warmed up to 320 DEG C and is oxidized 2h; Reactor under agitation cools to 220 DEG C afterwards, add 5 kilograms of naphthalenes, at this temperature, stir 2h, then cool to 90 DEG C, now add the polyoxyethylene glycol of asphalt quality 3wt%, add simultaneously water to kettle long-pending 75%, cool to room temperature stir 3h with the rotating speed of 400 revs/min at 120 DEG C after, solid-liquid separation obtains bitumen ball.The sphere diameter of gained bitumen ball more than 92% is 1.1mm, and sphericity reaches 92%.
Embodiment 5
The hard pitch of putting into 95～120 DEG C of softening temperatures of 180 kilograms in 500 liters of autoclaves, blasts 3000 liters/h air, then heats up, and in the time that temperature is raised to 190 DEG C, opens and stirs, and stir speed (S.S.) is 400 revs/min, continues to be warmed up to 340 DEG C and is oxidized 2h; Reactor under agitation cools to 250 DEG C afterwards, add 50 kilograms of naphthalenes, at this temperature, stir 2h, then cool to 85 DEG C, now add the octadecyl sodium sulfonate of asphalt quality 8wt%, add simultaneously water to kettle long-pending 65%, cool to room temperature stir 2h with the rotating speed of 450 revs/min at 130 DEG C after, solid-liquid separation obtains bitumen ball.The sphere diameter of gained bitumen ball more than 94% is 0.8mm, and sphericity reaches 94%.
Embodiment 6
The mid-temperature pitch of putting into 75～95 DEG C of softening temperatures of 4 kilograms in 10 liters of autoclaves, blasts 72 liters/h air, then heats up, and in the time that temperature is raised to 170 DEG C, opens and stirs, and stir speed (S.S.) is 350 revs/min, continues to be warmed up to 350 DEG C and is oxidized 2h; Reactor under agitation cools to 200 DEG C afterwards, add 1.4 kilograms of naphthalenes, at this temperature, stir 3h, then cool to 90 DEG C, now add the polyvinyl alcohol of asphalt quality 6wt%, add simultaneously water to kettle long-pending 60%, cool to room temperature stir 2h with the rotating speed of 400 revs/min at 120 DEG C after, solid-liquid separation obtains bitumen ball.The sphere diameter of gained bitumen ball more than 90% is 1.2mm, and sphericity reaches 95%.
Claims (1)
1. a bitumen ball preparation technology, is characterized in that comprising the steps:
In long-pending by every 1 liter of autoclave body, put into the pitch of 0.2-0.4 kilogram weight, pitch is put into autoclave, the air capacity rising by the per kilogram pitch 10-20 of needs per hour afterwards passes into air, then heat up, in the time that temperature is raised to 150-200 DEG C, opens and stir, stir speed (S.S.) is 200-400 rev/min, continues to be warmed up to 300-380 DEG C and is oxidized 1-5h; Autoclave under agitation cools to 180-250 DEG C afterwards, adds the naphthalene of pitch weight 20-35%, at this temperature, stirs 1-3h, then cools to 80-95 DEG C; Again the dispersion agent of pitch weight 0.1-1wt% is added to autoclave, water is joined to the 60-80% of autoclave volume simultaneously, at 100-150 DEG C, to cool to room temperature after the rotating speed stirring 1-5h of 300-500 rev/min, solid-liquid separation obtains the bitumen ball of 0.5-1.5mm;
Described pitch is that softening temperature is 35～75 DEG C of soft pitches, 75～95 DEG C of mid-temperature pitches or 95～120 DEG C of hard pitches;
Described dispersion agent is polyvinyl alcohol, polyoxyethylene glycol or octadecyl sodium sulfonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310227822.9A CN103289719B (en) | 2013-06-08 | 2013-06-08 | Process for preparing asphalt sphere |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310227822.9A CN103289719B (en) | 2013-06-08 | 2013-06-08 | Process for preparing asphalt sphere |
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| Publication Number | Publication Date |
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| CN103289719A CN103289719A (en) | 2013-09-11 |
| CN103289719B true CN103289719B (en) | 2014-11-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201310227822.9A Active CN103289719B (en) | 2013-06-08 | 2013-06-08 | Process for preparing asphalt sphere |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103695019B (en) * | 2013-12-09 | 2015-04-29 | 中国科学院山西煤炭化学研究所 | Low energy one-step method for preparing asphalt balls |
| CN106350089B (en) * | 2016-08-30 | 2021-10-26 | 中国科学院山西煤炭化学研究所 | Process for preparing asphalt balls by continuous method |
| CN110451475B (en) * | 2019-07-05 | 2021-03-26 | 北京化工大学 | Preparation method of asphalt-based carbon microspheres and application of asphalt-based carbon microspheres as sodium ion battery electrode material |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1188136A (en) * | 1997-01-17 | 1998-07-22 | 中国科学院山西煤炭化学研究所 | Method for preparing narrow size distribution asphalt ball |
| CN1057276C (en) * | 1996-02-02 | 2000-10-11 | 中国科学院山西煤炭化学研究所 | Method for improving non-melting process of asphalt balls |
| CN1480398A (en) * | 2003-07-18 | 2004-03-10 | 中国科学院山西煤炭化学研究所 | Preparation method of pitch-based spherical activated carbon rich in mesopores |
| CN101792678A (en) * | 2010-04-07 | 2010-08-04 | 中国海洋石油总公司 | Preparation method of bitumen balls |
-
2013
- 2013-06-08 CN CN201310227822.9A patent/CN103289719B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1057276C (en) * | 1996-02-02 | 2000-10-11 | 中国科学院山西煤炭化学研究所 | Method for improving non-melting process of asphalt balls |
| CN1188136A (en) * | 1997-01-17 | 1998-07-22 | 中国科学院山西煤炭化学研究所 | Method for preparing narrow size distribution asphalt ball |
| CN1480398A (en) * | 2003-07-18 | 2004-03-10 | 中国科学院山西煤炭化学研究所 | Preparation method of pitch-based spherical activated carbon rich in mesopores |
| CN101792678A (en) * | 2010-04-07 | 2010-08-04 | 中国海洋石油总公司 | Preparation method of bitumen balls |
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| CN103289719A (en) | 2013-09-11 |
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