CN1285389A - Method for increasing soluble composition of toluene insoluble pyridine in asphalt - Google Patents
Method for increasing soluble composition of toluene insoluble pyridine in asphalt Download PDFInfo
- Publication number
- CN1285389A CN1285389A CN 99117613 CN99117613A CN1285389A CN 1285389 A CN1285389 A CN 1285389A CN 99117613 CN99117613 CN 99117613 CN 99117613 A CN99117613 A CN 99117613A CN 1285389 A CN1285389 A CN 1285389A
- Authority
- CN
- China
- Prior art keywords
- asphalt
- pitch
- toluene insoluble
- soluble composition
- pyridine
- 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
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
To raw material asphalt 5-15% of toluene-p-sulfonic acid is added, they are uniformly mixed and placed in reactor, then the nitrogen gas is introduced, and the temp. is risen to 150-250 deg.C, and stirred and reacted for 5-20 hr, and naturally cooled so as to obtain the asphalt whose toluene insoluble and pyridine soluble component content is high. Said invented method is simple, raw material source is extensive, it can expand application of asphalt.
Description
The invention belongs to a kind of method of optimizing the pitch component, relate in particular to a kind of method that improves soluble composition of toluene insoluble pyridine in the pitch.
The height of soluble composition of toluene insoluble pyridine content is very big to the bituminous performance impact, especially as binder pitch and dipping agent bitumen, wish that its soluble composition of toluene insoluble pyridine content can be higher, can improve the bituminous adhesiveproperties like this and improve the bituminous coking value.But the soluble composition of toluene insoluble pyridine reactive behavior is stronger in the pitch, in the bitumen production process, since normal through high-temperature heat treatment, soluble composition of toluene insoluble pyridine content lower (generally about 10%) in the pitch caused, and be difficult to control, therefore influenced the final use properties of bituminous.So adopt heat treating method to be difficult to effectively improve the content of soluble composition of toluene insoluble pyridine in the pitch.In addition, Japan's hillside plot is repaiied to succeed to wait and is utilized supercritical extraction method separate bitumen component to control the toluene insoluble quinoline solubles content of coal-tar pitch, (hillside plot is repaiied heir etc. with modulation mesophase pitch raw material, the 15 time plain nd Annual Meeting collection of Japanese charcoal, 1989, P1-4), but this method complex technical process, complex operation.On the other hand, purified compound catalyzed polymerization also can obtain the higher synthetic asphalts of soluble composition of toluene insoluble pyridine content, holding Tian Xun etc. as Japan is that raw material is Preparation of Catalyst mesophase pitch (I.Mochida through HF/BF3 with the naphthalene, K.Shimiza, et al, Hightemperature, High pressure, 22,671 (1990)), the beard monarch of Chinese Academy of Sciences Shanxi coalification institute utilizes ZrO
2/ SO
4 2-Solid superacid is made catalyzer and naphthalene is carried out catalyzed polymerization is prepared mesophase pitch (Shanxi coalification institute of Chinese Academy of Sciences Ph D dissertation, 1997).Both all can obtain the higher synthetic asphalts of soluble composition of toluene insoluble pyridine content (can obtain the pitch of soluble composition of toluene insoluble pyridine content between 20-30% as the latter) in the process of preparation mesophase pitch.Yet these class methods utilize super acid to make catalyzer, and are higher to equipment requirements, and Working environment is relatively poor, and the pure compound cost is higher, and complicated operation is unfavorable for the scale operation of general pitch binder applied and impregnating pitch.
The purpose of this invention is to provide that a kind of cost is low, technology is simple, mild condition, can effectively improve the method for soluble composition of toluene insoluble pyridine in the pitch.
The concrete steps of the method for raising soluble composition of toluene insoluble pyridine in asphalt of the present invention are as follows:
1. in material asphalt, add the tosic acid of 5-15%, mix;
2. mixture is packed in the reactor, under nitrogen protection, rise to 150-250 ℃ temperature with the rate of temperature rise speed of 2-5 ℃/min;
3. stir down and under 150-250 ℃ of temperature, reacted 5-20 hour;
4. go out still behind the naturally cooling, getting soluble composition of toluene insoluble pyridine content is the pitch of 20-40%.
Above-mentioned pitch is medium temperature coal pitch, petroleum pitch.
The present invention has following advantage:
1. raw material sources are extensive, low price.
2. technological process is simple, the reaction conditions gentleness, and energy consumption is low, saves time, and is laborsaving.
3. in the modifying asphalt, soluble composition of toluene insoluble pyridine content can arbitrarily be adjusted between 15-40%.
Most preferred embodiment of the present invention is as follows:
Embodiment 1
Take by weighing 95.0g medium temperature coal pitch (TI-PS component content 12.1%) and 5.0g tosic acid; mix in the reactor of packing into; under nitrogen protection; temperature rise rate with 2 ℃/min rises to 150 ℃ of constant temperature, and stirring reaction 5 hours is after reaction finishes; naturally cooling; go out still, get modifying asphalt, its TI-PS component content 25.8%.
The mensuration of soluble composition of toluene insoluble pyridine (being called for short the TI-PS component): solvent thermosoling.With toluene is solvent, every 1g pitch with 20ml toluene 65 ℃ of thermosols 4 hours, isolate toluene soluble part (TS), the toluene insoluble part is that solvent is isolated the insoluble part with pyridine of toluene insoluble pyridine soluble part (TI-PS) (PI) at 65 ℃ of thermosols 4 hours (every 1g toluene insolubles 20ml pyridine) again with the pyridine.
Embodiment 2
Take by weighing 95.0g medium temperature coal pitch (TI-PS component content 12.1%) and 5.0g tosic acid; mix in the reactor of packing into; under nitrogen protection; temperature rise rate with 2 ℃/min rises to 150 ℃ of constant temperature, and stirring reaction 10 hours is after reaction finishes; naturally cooling; go out still, get modifying asphalt, its TI-PS component content 21.6%.
Embodiment 3
Take by weighing 90.0g medium temperature coal pitch (TI-PS component content 12.1%) and 10.0g tosic acid; mix in the reactor of packing into; under nitrogen protection; temperature rise rate with 2 ℃/min rises to 150 ℃ of constant temperature, and stirring reaction 5 hours is after reaction finishes; naturally cooling; go out still, get modifying asphalt, its TI-PS component content 36.1%.
Embodiment 4
Take by weighing 90.0g medium temperature coal pitch (TI-PS component content 12.1%) and 10.0g tosic acid; mix in the reactor of packing into; under nitrogen protection; temperature rise rate with 3 ℃/min rises to 190 ℃ of constant temperature, and stirring reaction 10 hours is after reaction finishes; naturally cooling; go out still, get modifying asphalt, its TI-PS component content 32.8%.
Embodiment 5
Take by weighing 90.0g medium temperature coal pitch (TI-PS component content 12.1%) and 10.0g tosic acid; mix in the reactor of packing into; under nitrogen protection; temperature rise rate with 4 ℃/min rises to 250 ℃ of constant temperature, and stirring reaction 10 hours is after reaction finishes; naturally cooling; go out still, get modifying asphalt, its TI-PS component content 31.0%.
Embodiment 6
Take by weighing 85.0g medium temperature coal pitch (TI-PS component content 12.1%) and 15.0g tosic acid; mix in the reactor of packing into; under nitrogen protection; temperature rise rate with 2 ℃/min rises to 150 ℃ of constant temperature, and stirring reaction 5 hours is after reaction finishes; naturally cooling; go out still, get modifying asphalt, its TI-PS component content 37.2%.
Embodiment 7
Take by weighing fire stons oily bitumen among the 95.0g (TI-PS component content 13.8%) and 5.0g tosic acid; mix in the reactor of packing into; under nitrogen protection; temperature rise rate with 2 ℃/min rises to 150 ℃ of constant temperature, and stirring reaction 5 hours is after reaction finishes; naturally cooling; go out still, get modifying asphalt, its TI-PS component content 28.5%.
Comparative Examples 1
Take by weighing in 100.0g medium temperature coal pitch (the TI-PS component content 12.1%) reactor of packing into, under nitrogen protection, rise to 380 ℃ of constant temperature with the temperature rise rate of 4 ℃/min; stirring reaction 6 hours, after reaction finishes, naturally cooling; go out still, get modifying asphalt, its TI-PS component content 14.7%.
Comparative Examples 2
Take by weighing in 100.0g medium temperature coal pitch (the TI-PS component content 12.1%) reactor of packing into; under nitrogen protection; temperature rise rate with 4 ℃/min rises to 420 ℃ of constant temperature; in normal pressure stirring reaction 12 hours; after reaction finished, naturally cooling went out still; get modifying asphalt, its TI-PS component content 11.5%.
Comparative Examples 3
Take by weighing in 100.0g medium temperature coal pitch (the TI-PS component content 12.1%) reactor of packing into; under nitrogen protection; temperature rise rate with 4 ℃/min rises to 400 ℃ of constant temperature; maintenance system pressure 0.7MPa, stirring reaction 6 hours is after reaction finishes; naturally cooling; go out still, get modifying asphalt, its TI-PS component content 13.0%.
Claims (2)
1. method that improves soluble composition of toluene insoluble pyridine in asphalt is characterized in that concrete steps are as follows:
(1) tosic acid of interpolation 5-15% in material asphalt mixes;
(2) mixture is packed in the reactor, under nitrogen protection, rise to 150-250 ℃ temperature with the rate of temperature rise speed of 2-5 ℃/min;
(3) stirring was reacted 5-20 hour under 150-250 ℃ of temperature down;
(4) go out still behind the naturally cooling, getting soluble composition of toluene insoluble pyridine content is the pitch of 20-40%.
2. a kind of method that improves soluble composition of toluene insoluble pyridine in asphalt as claimed in claim 1 is characterized in that described pitch is medium temperature coal pitch, petroleum pitch.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99117613A CN1089109C (en) | 1999-08-18 | 1999-08-18 | Method for increasing soluble composition of toluene insoluble pyridine in asphalt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99117613A CN1089109C (en) | 1999-08-18 | 1999-08-18 | Method for increasing soluble composition of toluene insoluble pyridine in asphalt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1285389A true CN1285389A (en) | 2001-02-28 |
| CN1089109C CN1089109C (en) | 2002-08-14 |
Family
ID=5280165
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99117613A Expired - Fee Related CN1089109C (en) | 1999-08-18 | 1999-08-18 | Method for increasing soluble composition of toluene insoluble pyridine in asphalt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1089109C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649911A (en) * | 2012-05-16 | 2012-08-29 | 海工英派尔工程有限公司 | Preparation method for hard petroleum asphalt |
| CN102676196A (en) * | 2011-03-18 | 2012-09-19 | 北京三聚创洁科技发展有限公司 | Coal tar pitch for preparing needle coke, method for preparing same and solvent used in preparation process of coal tar pitch |
| CN103043656A (en) * | 2012-12-19 | 2013-04-17 | 中国平煤神马集团开封炭素有限公司 | Method for manufacturing ultra-high power graphite electrode joint by using asphalt additive |
| CN103834422A (en) * | 2014-03-24 | 2014-06-04 | 武汉科技大学 | Modified coal tar and preparation method thereof |
| CN108976833A (en) * | 2018-07-05 | 2018-12-11 | 太原理工大学 | It is a kind of to build the road with the modified preparation method that pitch is blended |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076384C (en) * | 1997-08-07 | 2001-12-19 | 中国科学院山西煤炭化学研究所 | Preparation of intermediate phase asphalt with solid superacid |
-
1999
- 1999-08-18 CN CN99117613A patent/CN1089109C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102676196A (en) * | 2011-03-18 | 2012-09-19 | 北京三聚创洁科技发展有限公司 | Coal tar pitch for preparing needle coke, method for preparing same and solvent used in preparation process of coal tar pitch |
| CN102676196B (en) * | 2011-03-18 | 2015-01-21 | 北京宝塔三聚能源科技有限公司 | Coal tar pitch for preparing needle coke, method for preparing same and solvent used in preparation process of coal tar pitch |
| CN102649911A (en) * | 2012-05-16 | 2012-08-29 | 海工英派尔工程有限公司 | Preparation method for hard petroleum asphalt |
| CN102649911B (en) * | 2012-05-16 | 2013-10-30 | 海工英派尔工程有限公司 | Preparation method for hard petroleum asphalt |
| CN103043656A (en) * | 2012-12-19 | 2013-04-17 | 中国平煤神马集团开封炭素有限公司 | Method for manufacturing ultra-high power graphite electrode joint by using asphalt additive |
| CN103834422A (en) * | 2014-03-24 | 2014-06-04 | 武汉科技大学 | Modified coal tar and preparation method thereof |
| CN103834422B (en) * | 2014-03-24 | 2015-04-01 | 武汉科技大学 | Modified coal tar and preparation method thereof |
| CN108976833A (en) * | 2018-07-05 | 2018-12-11 | 太原理工大学 | It is a kind of to build the road with the modified preparation method that pitch is blended |
| CN108976833B (en) * | 2018-07-05 | 2020-11-27 | 太原理工大学 | Preparation method of modified blended asphalt for road building |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1089109C (en) | 2002-08-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101768141B (en) | Method for preparing alpha-acetyl-gamma-butyrolactone | |
| CN103265966B (en) | Preparation method of mesophase pitch with high mesophase content | |
| CN110003932B (en) | Method for preparing high-quality mesophase pitch by ternary co-carbonization | |
| CN108485694B (en) | Method for preparing high-quality mesophase pitch by co-carbonization method | |
| CN1089109C (en) | Method for increasing soluble composition of toluene insoluble pyridine in asphalt | |
| CN108728147A (en) | A kind of method that heavy oil fast pyrogenation pretreatment-catalyzed polycondensation prepares mesophase pitch and carbon fiber | |
| CN113621130A (en) | Preparation method of high-quality spinning asphalt, product and application thereof | |
| CN111575053B (en) | Method for preparing mesophase pitch by size exclusion separation-thermal polycondensation and application thereof | |
| CN103923681B (en) | Mesophase pitch and utilize gelatin liquefaction refined asphaltic bitumen to prepare the method for mesophase pitch | |
| CN114437020B (en) | Preparation method of glycolide | |
| CN114272932B (en) | Nickel-cerium biochar catalyst and preparation method and application thereof | |
| CN108611113B (en) | Method for preparing mesophase pitch and carbon fiber by deep oxidation-catalytic polycondensation | |
| CN104498072A (en) | Method of preparing mesophase pitch by means of naphthene-based vacuum gas oil co-carbonization | |
| KR101543534B1 (en) | Preparation method of pitch for carbon fiber | |
| CN110540855B (en) | Petroleum-series impregnating asphalt and preparation method thereof | |
| CN110628449B (en) | Method for preparing spinning-grade synthetic mesophase pitch | |
| CN1944572A (en) | Process for preparing thick oil hydrothermally catalytic cracking viscosity reducer containing amphiphilic structure | |
| CN108264915A (en) | A kind of preparation method for spinning mesophase pitch | |
| CN1418930A (en) | Method for preparing needle coke using petrolium and coal series raw material | |
| CN112538362B (en) | Method for improving rheological property of coal tar pitch | |
| CN113046045B (en) | EVA emulsion type crude oil pour point depressant and preparation method thereof | |
| CN112574770B (en) | Preparation method of high-quality coal-based needle coke | |
| CN1076384C (en) | Preparation of intermediate phase asphalt with solid superacid | |
| CN105838408A (en) | Method for preparing mesophase pitch from residue derived from coal liquefaction and prepared mesophase pitch | |
| CN115403554B (en) | Method for directly recycling lactide from polylactic acid waste |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |