CN107488456A - A kind of preparation method of high β resin modified asphalts - Google Patents
A kind of preparation method of high β resin modified asphalts Download PDFInfo
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- CN107488456A CN107488456A CN201710640155.5A CN201710640155A CN107488456A CN 107488456 A CN107488456 A CN 107488456A CN 201710640155 A CN201710640155 A CN 201710640155A CN 107488456 A CN107488456 A CN 107488456A
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- preparation
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- resin modified
- mass flow
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/04—Working-up pitch, asphalt, bitumen by chemical means reaction by blowing or oxidising, e.g. air, ozone
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/026—Working-up pitch, asphalt, bitumen by chemical means reaction with organic compounds
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The invention discloses a kind of preparation method of high β resin modified asphalts, using mid temperature pitch as raw material, the refined bitumen of low quinoline insolubles content is obtained by solvent extraction sedimentation separation, then thermal polymerization air oxidation modification is carried out to refined bitumen, obtains the modified pitch of high β resin contents.After the processing of specific thermal polymerization condition, the influence of reaction temperature, oxidization time and the air mass flow in air oxidation stage to asphalt modification have studied.Test result indicates that in the air oxidation stage, when oxidizing temperature is 290 DEG C, oxidization time 2.5h, air mass flow 0.05m3During/h, can obtain softening point be 218 DEG C, toluene insolubles 62.35%, quinoline insolubles 4.46%, coking value 79.85%, β resin contents be 58.08% high-quality modified pitch.
Description
Technical field
The present invention relates to a kind of preparation method of high β resin modified asphalts.
Background technology
Coal tar pitch is the residue after coal tar distillation extraction cut, and its yield accounts for the 50%~60% of coal tar total amount,
It is the quality raw materials of carbon material industry, available for the novel charcoal material of manufacture high added value, graphite electrode adhesive and prevents
Water construction material etc..At present, modifying agent of the high quality asphalt as commercial Li-ion battery graphite cathode material so that pitch
Very important status is occupied in lithium ion battery negative material industry.
By the way that pitch can be reduced effectively to the specific surface area of graphite to native graphite by one or many liquid phase coatings,
So as to increase substantially the reversible capacity first of graphite cathode material and coulombic efficiency, improve the cycle performance of battery.Coal tar pitch
The height of middle β resin contents is one of important indicator for evaluating asphalt quality, directly affects the quality of novel charcoal material.
Therefore, high β resin modified asphalts are researched and developed to have important practical significance.
The content of the invention
Goal of the invention：In order to improve β resin contents in coal tar pitch, the present invention is extracted using mid temperature pitch as raw material by solvent
Take sedimentation separation to obtain the refined bitumen of low quinoline insolubles content, then thermal polymerization-air oxidation is carried out to refined bitumen and is modified
Processing, obtains the modified pitch of high β resin contents.After the processing of specific thermal polymerization condition, the reaction in air oxidation stage is studied
The influence of temperature, oxidization time and air mass flow to asphalt modification, comprehensive analysis determine optimal preparation technology.
Technical scheme：In order to solve above-mentioned performance issue, the technical solution adopted in the present invention is：A kind of high β resins change
The preparation method of property pitch, comprises the following steps：The refined bitumen for weighing certain mass is added in 0.5L stainless steel cauldrons,
The heat polymerization of refined bitumen is completed under certain condition, then adjusts the oxidizing temperature of reactor, into kettle by certain empty
Throughput blasts air, and for a period of time, reaction stops being passed through air constant temperature oxidation after terminating, and question response kettle takes after being cooled to room temperature
Go out product in kettle, obtain modified pitch.
Further, the oxidizing temperature is 260 DEG C, 270 DEG C, 280 DEG C, 290 DEG C, 300 DEG C.
Further, the air mass flow is 0.03m3/h、0.04m3/h、0.05m3/h、0.06m3/h、0.07m3/h。
Further, the oxidization time is 1.0h, 1.5h, 2.0h, 2.5h, 3.0h.
Beneficial effect：A kind of preparation method of high β resin modified asphalts provided by the invention, using mid temperature pitch as raw material,
The refined bitumen of low quinoline insolubles content is obtained by solvent extraction sedimentation separation, then thermal polymerization-sky is carried out to refined bitumen
Gas oxidation modification is handled, and obtains the modified pitch of high β resin contents.After the processing of specific thermal polymerization condition, air oxygen have studied
Influence of reaction temperature, oxidization time and the air mass flow in change stage to asphalt modification.Test result indicates that in air oxidation rank
Section, when oxidizing temperature is 290 DEG C, oxidization time 2.5h, air mass flow 0.05m3During/h, softening point can be obtained as 218
DEG C, toluene insolubles 62.35%, quinoline insolubles 4.46%, coking value 79.85%, β resin contents be 58.08%
High-quality modified pitch.
Embodiment
With reference to embodiment, the present invention is described in further detail：
Embodiment 1：
A kind of preparation method of high β resin modified asphalts, comprises the following steps：The refined bitumen for weighing certain mass adds
Into 0.5L stainless steel cauldrons, the heat polymerization of refined bitumen is completed under certain condition, then adjusts the temperature of reactor
Degree presses air mass flow 0.03m into kettle to 260 DEG C3/ h blasts air, constant temperature oxidation 1h, and reaction stops being passed through air after terminating,
Question response kettle takes out product in kettle after being cooled to room temperature, obtains modified pitch.
Embodiment 2：
A kind of preparation method of high β resin modified asphalts, comprises the following steps：The refined bitumen for weighing certain mass adds
Into 0.5L stainless steel cauldrons, the heat polymerization of refined bitumen is completed under certain condition, then adjusts the temperature of reactor
Degree presses air mass flow 0.05m into kettle to 270 DEG C3/ h blasts air, constant temperature oxidation 2h, and reaction stops being passed through air after terminating,
Question response kettle takes out product in kettle after being cooled to room temperature, obtains modified pitch.
Embodiment 3：
A kind of preparation method of high β resin modified asphalts, comprises the following steps：The refined bitumen for weighing certain mass adds
Into 0.5L stainless steel cauldrons, the heat polymerization of refined bitumen is completed under certain condition, then adjusts the temperature of reactor
Degree presses air mass flow 0.06m into kettle to 280 DEG C3/ h blasts air, constant temperature oxidation 2.5h, and reaction stops being passed through sky after terminating
Gas, question response kettle take out product in kettle after being cooled to room temperature, obtain modified pitch.
Finally it should be noted that：Above example only not limits technology described in the invention to illustrate the present invention
Scheme, therefore, although this specification with reference to above-mentioned various embodiments to present invention has been detailed description, this
Field it is to be appreciated by one skilled in the art that still can be modified to the present invention or equivalent substitution, and all do not depart from this
The technical scheme of the spirit and scope of invention and improvement, it all should cover in scope of the presently claimed invention.
Claims (4)
1. a kind of preparation method of high β resin modified asphalts, it is characterised in that comprise the following steps：Weigh the essence of certain mass
Pitch processed is added in 0.5L stainless steel cauldrons, is completed the heat polymerization of refined bitumen under certain condition, is then adjusted
The oxidizing temperature of reactor, air is blasted by certain air mass flow into kettle, for a period of time, reaction stops constant temperature oxidation after terminating
Air is passed through, question response kettle takes out product in kettle after being cooled to room temperature, obtains modified pitch.
2. the preparation method of high β resin modified asphalts according to claim 1, it is characterised in that：The oxidizing temperature is
260℃、270℃、280℃、290℃、300℃。
3. the preparation method of high β resin modified asphalts according to claim 1, it is characterised in that：The air mass flow is
0.03m3/h、0.04m3/h、0.05m3/h、0.06m3/h、0.07m3/h。
4. the preparation method of high β resin modified asphalts according to claim 1, it is characterised in that：The oxidization time is
1.0h、1.5h、2.0h、2.5h、3.0h。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710640155.5A CN107488456A (en) | 2017-07-31 | 2017-07-31 | A kind of preparation method of high β resin modified asphalts |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710640155.5A CN107488456A (en) | 2017-07-31 | 2017-07-31 | A kind of preparation method of high β resin modified asphalts |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107488456A true CN107488456A (en) | 2017-12-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710640155.5A Pending CN107488456A (en) | 2017-07-31 | 2017-07-31 | A kind of preparation method of high β resin modified asphalts |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112577848A (en) * | 2020-11-24 | 2021-03-30 | 本钢板材股份有限公司 | Method for determining quinoline insoluble substances in coal tar pitch |
| CN113563915A (en) * | 2021-08-31 | 2021-10-29 | 山东常任新材料有限公司 | Preparation method of coated asphalt |
| CN114317018A (en) * | 2021-11-23 | 2022-04-12 | 淮北矿业股份有限公司 | Method for improving coking property of low-coalification-degree coal |
Citations (5)
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|---|---|---|---|---|
| CN101838542A (en) * | 2010-05-19 | 2010-09-22 | 镇江新光冶金辅材厂 | Manufacturing method of ultra-temperature pitch |
| CN101323788B (en) * | 2008-07-31 | 2011-07-27 | 上海奥韦通工程技术有限公司 | Processing process for preparing various asphalt and fuel oil with coal tar |
| CN102391885A (en) * | 2011-09-22 | 2012-03-28 | 天津大学 | Coal tar pitch-based high-softening point spinning pitch and preparation method thereof |
| CN102399563A (en) * | 2010-09-10 | 2012-04-04 | 辽宁科技大学 | Method for preparing general type coal series asphalt with spinnability by solvent extraction and oxidative thermopolymerization |
| CN102477595A (en) * | 2010-11-22 | 2012-05-30 | 大连创达技术交易市场有限公司 | Pitch-based carbon fiber and preparation method thereof |
-
2017
- 2017-07-31 CN CN201710640155.5A patent/CN107488456A/en active Pending
Patent Citations (5)
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| CN101323788B (en) * | 2008-07-31 | 2011-07-27 | 上海奥韦通工程技术有限公司 | Processing process for preparing various asphalt and fuel oil with coal tar |
| CN101838542A (en) * | 2010-05-19 | 2010-09-22 | 镇江新光冶金辅材厂 | Manufacturing method of ultra-temperature pitch |
| CN102399563A (en) * | 2010-09-10 | 2012-04-04 | 辽宁科技大学 | Method for preparing general type coal series asphalt with spinnability by solvent extraction and oxidative thermopolymerization |
| CN102477595A (en) * | 2010-11-22 | 2012-05-30 | 大连创达技术交易市场有限公司 | Pitch-based carbon fiber and preparation method thereof |
| CN102391885A (en) * | 2011-09-22 | 2012-03-28 | 天津大学 | Coal tar pitch-based high-softening point spinning pitch and preparation method thereof |
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| 朱亚明: "热聚合-氧化法制备高 β 树脂改性沥青", 《化工进展》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112577848A (en) * | 2020-11-24 | 2021-03-30 | 本钢板材股份有限公司 | Method for determining quinoline insoluble substances in coal tar pitch |
| CN113563915A (en) * | 2021-08-31 | 2021-10-29 | 山东常任新材料有限公司 | Preparation method of coated asphalt |
| CN114317018A (en) * | 2021-11-23 | 2022-04-12 | 淮北矿业股份有限公司 | Method for improving coking property of low-coalification-degree coal |
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Application publication date: 20171219 |
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