CN103289719A - Process for preparing asphalt sphere - Google Patents
Process for preparing asphalt sphere Download PDFInfo
- Publication number
- CN103289719A CN103289719A CN2013102278229A CN201310227822A CN103289719A CN 103289719 A CN103289719 A CN 103289719A CN 2013102278229 A CN2013102278229 A CN 2013102278229A CN 201310227822 A CN201310227822 A CN 201310227822A CN 103289719 A CN103289719 A CN 103289719A
- Authority
- CN
- China
- Prior art keywords
- temperature
- asphalt
- pitch
- stirring
- 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.)
- Granted
Links
Abstract
The invention relates to a process for preparing an asphalt sphere, and the process comprises the following steps of: placing asphalt into a high-pressure kettle by placing 0.2-0.4 kilograms of the asphalt into each 1 liter of volume of the high-pressure kettle; then introducing air by introducing 10-20 liters of the air to each kilogram of the asphalt per hour; then increasing temperature; starting to stir at the stirring speed of 200-400 rpm (revolutions per minute) when the temperature is increased to 150-200 DEG C; continuously increasing the temperature to 300-380 DEG C, and oxidizing for 1-5 hours; then reducing the temperature of the high-pressure kettle to 180-250 DEG C while stirring, adding naphthalene which accounts for 20wt%-35wt% of the asphalt, stirring at the temperature for 1-3 hours, and then reducing the temperature to 80-95 DEG C; then adding a dispersing agent which accounts for 0.1%-1% of the weight of the asphalt to the high-pressure kettle, adding water to 60%-80% of the volume of the high-pressure kettle at the same time, stirring at 100-150 DEG C at the rotation speed of 300-500 turns/minute for 1-5 hours, then reducing the temperature to room temperature, and carrying out solid-liquid separation to obtain the asphalt sphere of 0.5-1.5 mm. The process disclosed by the invention is pollution-free and can directly complete the process for preparing the asphalt sphere in a same reaction kettle without crushing or extruding strips.
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, compares with the gac of other types, and the research of ball-type gac report is less, especially sphere diameter be millimetre-sized with pitch be raw material spheric active carbon still less.The carbon matrix precursor that contains for preparing this spheric active carbon is pitch, needs earlier pitch to be carried out being prepared as bead by emulsification method again after the modification, and the modification of pitch and balling-up become indispensable step for this reason.
The patent that with pitch is presoma preparation millimeter level spheric active carbon is more, Chinese invention patent 03178572 " is rich in the preparation method of the asphalt-base globular active carbon of mesopore " and is and pitch, coal tar wet goods obtained adding the aromatic hydrocarbon small molecules again behind softening temperature 200-300 ℃ the pitch with atmospheric oxidation it is carried out modification, make balling-up pitch by adding dispersion agent afterwards, the final emulsion balling-up makes bitumen ball thereby also namely need to obtain the emulsification balling-up that balling-up pitch just can carry out next step; Chinese invention patent 200410100531 " method for preparing spherical activated carbon " is the heavy hydrocarbon oil level raw materials such as residue with petroleum tar, coal tar, low softening point asphalt or petroleum naphtha ethene processed, by using oxygenant such as HNO
3, air etc. carries out oxidation and makes oxidized bitumen, the aromatic hydrocarbons with naphthalene one class carries out modification afterwards, and at a certain temperature extrusion, be broken into the clavate fragment, emulsification balling-up then.As seen, its pitch that is used for balling-up is the fragment after the fragmentation; The pitch that Chinese invention patent 200610127621 " a kind of method for preparing the low ball shape active carbon of heavy metal content ", Chinese invention patent 200810035853 " a kind of preparation method of nitrogenous asphalt-base spherical activated carbon " and Chinese invention patent 201210317727 " the low power consuming preparation method of asphalt-base spherical activated carbon " etc. all need to make balling-up in advance could finally obtain corresponding bitumen ball, not only need many complete equipments but also make technological process lengthen so virtually, inevitable generation environmental pollution in obtaining balling-up pitch process simultaneously.
Summary of the invention
The purpose of this invention is to provide a kind of pollution-freely, directly in same set of reactor, finish the technology of preparation bitumen ball without fragmentation or extrusion.
Preparation technology of the present invention realizes as follows:
Put into 0.2-0.4 kilogram weight pitch in long-pending by per 1 rising pressure kettle, pitch is put into autoclave, the air capacity bubbling air that per hour needs the 10-20 liter afterwards by per kilogram pitch, heat up then, treat to open when temperature is raised to 150-200 ℃ and stir, stir speed (S.S.) is 200-400 rev/min, continues to be warmed up to 300-380 ℃ and carries out oxidation 1-5h; Autoclave under agitation cools to 180-250 ℃ afterwards, adds the naphthalene of pitch weight 20-35%, stirs 1-3h under this temperature, cools to 80-95 ℃ then; Again the dispersion agent of pitch weight 0.1-1wt% is added autoclave, simultaneously water is joined the 60-80% of autoclave volume, cool to room temperature after stirring 1-5h with 300-500 rev/min rotating speed under 100-150 ℃, solid-liquid separation namely gets the bitumen ball of 0.5-1.5mm.
The used pitch of the present invention is that softening temperature is 35～75 ℃ of soft pitches, 75～95 ℃ of mid-temperature pitches or 95～120 ℃ of hard pitches.
Aforesaid dispersion agent is polyvinyl alcohol, polyoxyethylene glycol or octadecyl sodium sulfonate.
Advantage of the present invention:
(1) all at same set of equipment internal reaction, its utilization ratio is greatly improved all reaction masses, and is very favourable to reducing production costs;
(2) owing in same set of reactor, operate, can not produce a large amount of waste gas and waste residue, alleviate environmental stress;
(3) the present invention all operates in a cover reactor, and floor space reduces greatly, and equipment cost significantly reduces.
Embodiment
Embodiment 1
Put into the soft pitch of 35～75 ℃ of softening temperatures of 4 kilograms in 10 liters of autoclaves, blast 40 liters/h air, heat up then, treat to open when temperature is raised to 150 ℃ and stir, stir speed (S.S.) is 200 rev/mins, continues to be warmed up to 300 ℃ and carries out oxidation 5h; Reactor under agitation cools to 180 ℃ afterwards, add 0.8 kilogram of naphthalene, under this temperature, stir 3h, cool to 80 ℃ then, add the polyvinyl alcohol of asphalt quality 1wt% this moment, simultaneously water is joined kettle long-pending 60%, after stirring 1h with 300 rev/mins rotating speed under 150 ℃, cool to room temperature, solid-liquid separation namely gets bitumen ball.The sphere diameter of gained bitumen ball is 1.5mm more than 90%, and sphericity reaches 95%.
Embodiment 2
Put into the hard pitch of 95～120 ℃ of softening temperatures of 20 kilograms in 100 liters of autoclaves, blast 400 liters/h air, heat up then, treat to open when temperature is raised to 200 ℃ and stir, stir speed (S.S.) is 300 rev/mins, continues to be warmed up to 350 ℃ and carries out oxidation 3h; Reactor under agitation cools to 230 ℃ afterwards, add 7 kilograms of naphthalenes, under this temperature, stir 3h, cool to 90 ℃ then, add the octadecyl sodium sulfonate of asphalt quality 5wt% this moment, simultaneously water is joined kettle long-pending 70%, after stirring 3h with 400 rev/mins rotating speed under 120 ℃, cool to room temperature, solid-liquid separation namely gets bitumen ball.The sphere diameter of gained bitumen ball is 1.1mm more than 92%, and sphericity reaches 93%.
Embodiment 3
Put into the mid-temperature pitch of 75～95 ℃ of softening temperatures of 400 kilograms in 1000 liters of autoclaves, blast 6000 liters/h air, heat up then, treat to open when temperature is raised to 180 ℃ and stir, stir speed (S.S.) is 400 rev/mins, continues to be warmed up to 380 ℃ and carries out oxidation 1h; Reactor under agitation cools to 250 ℃ afterwards, add the 120 kg naphthalene, under this temperature, stir 2h, cool to 95 ℃ then, add the polyoxyethylene glycol of asphalt quality 10wt% this moment, add water simultaneously kettle long-pending 80%, after stirring 5h with 500 rev/mins rotating speed under 100 ℃, cool to room temperature, solid-liquid separation namely gets bitumen ball.The sphere diameter of gained bitumen ball is 0.5mm more than 92%, and sphericity reaches 97%.
Embodiment 4
Put into the soft pitch of 35～75 ℃ of softening temperatures of 20 kilograms in 50 liters of autoclaves, blast 300 liters/h air, heat up then, treat to open when temperature is raised to 160 ℃ and stir, stir speed (S.S.) is 250 rev/mins, continues to be warmed up to 320 ℃ and carries out oxidation 2h; Reactor under agitation cools to 220 ℃ afterwards, add 5 kilograms of naphthalenes, under this temperature, stir 2h, cool to 90 ℃ then, add the polyoxyethylene glycol of asphalt quality 3wt% this moment, add water simultaneously kettle long-pending 75%, after stirring 3h with 400 rev/mins rotating speed under 120 ℃, cool to room temperature, solid-liquid separation namely gets bitumen ball.The sphere diameter of gained bitumen ball is 1.1mm more than 92%, and sphericity reaches 92%.
Embodiment 5
Put into the hard pitch of 95～120 ℃ of softening temperatures of 180 kilograms in 500 liters of autoclaves, blast 3000 liters/h air, heat up then, treat to open when temperature is raised to 190 ℃ and stir, stir speed (S.S.) is 400 rev/mins, continues to be warmed up to 340 ℃ and carries out oxidation 2h; Reactor under agitation cools to 250 ℃ afterwards, add 50 kilograms of naphthalenes, under this temperature, stir 2h, cool to 85 ℃ then, add the octadecyl sodium sulfonate of asphalt quality 8wt% this moment, add water simultaneously kettle long-pending 65%, after stirring 2h with 450 rev/mins rotating speed under 130 ℃, cool to room temperature, solid-liquid separation namely gets bitumen ball.The sphere diameter of gained bitumen ball is 0.8mm more than 94%, and sphericity reaches 94%.
Embodiment 6
Put into the mid-temperature pitch of 75～95 ℃ of softening temperatures of 4 kilograms in 10 liters of autoclaves, blast 72 liters/h air, heat up then, treat to open when temperature is raised to 170 ℃ and stir, stir speed (S.S.) is 350 rev/mins, continues to be warmed up to 350 ℃ and carries out oxidation 2h; Reactor under agitation cools to 200 ℃ afterwards, add 1.4 kilograms of naphthalenes, under this temperature, stir 3h, cool to 90 ℃ then, add the polyvinyl alcohol of asphalt quality 6wt% this moment, add water simultaneously kettle long-pending 60%, after stirring 2h with 400 rev/mins rotating speed under 120 ℃, cool to room temperature, solid-liquid separation namely gets bitumen ball.The sphere diameter of gained bitumen ball is 1.2mm more than 90%, and sphericity reaches 95%.
Claims (3)
1. a bitumen ball preparation technology is characterized in that comprising the steps:
Put into 0.2-0.4 kilogram weight pitch in long-pending by per 1 rising pressure kettle, pitch is put into autoclave, the air capacity bubbling air that per hour needs the 10-20 liter afterwards by per kilogram pitch, heat up then, treat to open when temperature is raised to 150-200 ℃ and stir, stir speed (S.S.) is 200-400 rev/min, continues to be warmed up to 300-380 ℃ and carries out oxidation 1-5h; Autoclave under agitation cools to 180-250 ℃ afterwards, adds the naphthalene of pitch weight 20-35%, stirs 1-3h under this temperature, cools to 80-95 ℃ then; Again the dispersion agent of pitch weight 0.1-1wt% is added autoclave, simultaneously water is joined the 60-80% of autoclave volume, cool to room temperature after stirring 1-5h with 300-500 rev/min rotating speed under 100-150 ℃, solid-liquid separation namely gets the bitumen ball of 0.5-1.5mm.
2. a kind of bitumen ball preparation technology as claimed in claim 1 is characterized in that described pitch is that softening temperature is 35～75 ℃ of soft pitches, 75～95 ℃ of mid-temperature pitches or 95～120 ℃ of hard pitches.
3. a kind of bitumen ball preparation technology as claimed in claim 1 is characterized in that 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103289719A true CN103289719A (en) | 2013-09-11 |
| CN103289719B CN103289719B (en) | 2014-11-26 |
Family
ID=49091266
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310227822.9A Active CN103289719B (en) | 2013-06-08 | 2013-06-08 | Process for preparing asphalt sphere |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103289719B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103695019A (en) * | 2013-12-09 | 2014-04-02 | 中国科学院山西煤炭化学研究所 | Low energy one-step method for preparing asphalt balls |
| CN106350089A (en) * | 2016-08-30 | 2017-01-25 | 中国科学院山西煤炭化学研究所 | Process for preparing asphalt spheres by aid of continuous methods |
| CN110451475A (en) * | 2019-07-05 | 2019-11-15 | 北京化工大学 | A kind of preparation method of Pitch-based Carbon microballoon and its application 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 | Method for preparing spherical active cardon with base of asphaltum riched 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 | Method for preparing spherical active cardon with base of asphaltum riched in mesopores |
| CN101792678A (en) * | 2010-04-07 | 2010-08-04 | 中国海洋石油总公司 | Preparation method of bitumen balls |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103695019A (en) * | 2013-12-09 | 2014-04-02 | 中国科学院山西煤炭化学研究所 | Low energy one-step method for preparing asphalt balls |
| CN106350089A (en) * | 2016-08-30 | 2017-01-25 | 中国科学院山西煤炭化学研究所 | Process for preparing asphalt spheres by aid of continuous methods |
| CN110451475A (en) * | 2019-07-05 | 2019-11-15 | 北京化工大学 | A kind of preparation method of Pitch-based Carbon microballoon and its application as sodium ion battery electrode material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103289719B (en) | 2014-11-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102381705B (en) | Method for producing activated carbon by thermally activating coal tar dreg/ sludge fermentation body by using microwaves | |
| Jiang et al. | Acid functionalized, highly dispersed carbonaceous spheres: an effective solid acid for hydrolysis of polysaccharides | |
| CN103289719B (en) | Process for preparing asphalt sphere | |
| CN106698427A (en) | Activated carbon, preparation method thereof, and application of activated carbon in supercapacitor electrode | |
| CN101397136A (en) | Method for preparing high specific surface area granular activated carbon by physical activation process | |
| Sun et al. | Comparison of biodiesel production using a novel porous Zn/Al/Co complex oxide prepared from different methods: Physicochemical properties, reaction kinetic and thermodynamic studies | |
| CN103708455A (en) | Method for preparing calcium carbide | |
| CN101264879B (en) | Method for preparing biomass conductive charcoal | |
| CN106904625A (en) | A kind of charing method of the compound intercalated montmorillonite of cellulose | |
| CN102658109A (en) | Preparation method of nanometer strontium titanate catalyst | |
| CN104909365A (en) | Method for promoting asphalt sphere oxidation without melting | |
| CN112645304B (en) | Method for preparing high-performance mesocarbon microbeads from heavy oil | |
| CN103272533A (en) | Pitch sphere oxidative stabilization method | |
| CN102532045A (en) | Method for producing cyanuric acid from urea used as raw material | |
| CN111362265B (en) | VOCs adsorbent prepared from hypha solid waste resources and coal and preparation method thereof | |
| CN104326470A (en) | Method for preparing high specific surface area micron-scale spherical activated carbon from carboxymethyl cellulose | |
| CN101717084A (en) | Method for preparing mesoporous activated carbon from shell of jatropha curcas | |
| CN107188172A (en) | A kind of preparation method rich in mesopore pitch super active carbon | |
| CN104910941B (en) | A kind of revolving bed coal is catalyzed method for pyrolysis | |
| CN102689899A (en) | A preparation method for improving specific surface area of activated carbon | |
| CN102795624A (en) | Low-energy-consumption preparation method of pitch-based spherical active carbon | |
| CN103484137B (en) | Carbonizing apparatus and carbonizing method for waste solid organic matters | |
| CN103446977A (en) | Microwave assisted method for producing revertose by carrying out hydrothermal reaction on kitchen waste | |
| CN103896543A (en) | Unfired ceramsite by using lignite extracted germanium tailings as main raw material and preparation method of unfired ceramsite | |
| CN102850053A (en) | Preparation method of mineral insulated cable porcelain column |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |