CN108998062A - A kind of method that carbolineum prepares pitch - Google Patents
A kind of method that carbolineum prepares pitch Download PDFInfo
- Publication number
- CN108998062A CN108998062A CN201810907227.2A CN201810907227A CN108998062A CN 108998062 A CN108998062 A CN 108998062A CN 201810907227 A CN201810907227 A CN 201810907227A CN 108998062 A CN108998062 A CN 108998062A
- Authority
- CN
- China
- Prior art keywords
- carbolineum
- pitch
- prepares
- beaker
- flask
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 238000010792 warming Methods 0.000 claims abstract description 9
- 238000013019 agitation Methods 0.000 claims abstract description 5
- 238000009413 insulation Methods 0.000 claims abstract description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 15
- 239000005864 Sulphur Substances 0.000 claims description 15
- 239000011280 coal tar Substances 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000010426 asphalt Substances 0.000 abstract description 19
- 239000011295 pitch Substances 0.000 description 35
- 238000003760 magnetic stirring Methods 0.000 description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 22
- 230000035515 penetration Effects 0.000 description 12
- 238000001035 drying Methods 0.000 description 11
- 238000004321 preservation Methods 0.000 description 11
- 230000001105 regulatory effect Effects 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000003921 oil Substances 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
- 239000011331 needle coke Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000002685 polymerization catalyst Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000011294 coal tar pitch Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (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 present invention discloses a kind of method that carbolineum prepares pitch, after carbolineum is warming up to 200~300 DEG C, catalyst is added, catalyst accounts for the 10~30% of carbolineum and catalyst gross mass, magnetic agitation, and 4~30h of insulation reaction obtains pitch after cooling；The method of the present invention simple process, reaction condition is mild, and bitumen product yield is high, and economy is stronger, and the method for the present invention increases the carbolineum purposes of high value.
Description
Technical field
The present invention relates to a kind of methods that carbolineum prepares pitch, belong to coal tar pitch technical field of refinement.
Background technique
The product that carbolineum is coal tar after 250~370 DEG C of distillations, China are maximum coke production state and to disappear in the world
Fei Guo produces 600~8,000,000 tons of coal tar per year, accounts for about the 1/3 of the world, and about 1,000,000 tons of carbolineum.It is more due to scale and technical reason
Using roughing, it is mainly used as carbon black raw oil, fuel oil and pitch ready-mixed oil, added value is lower, and economic benefit is poor, as
Low-grade fuel oil environmental pollution is larger.Pitch has huge demand in China, has extensively in road pavement and needle coke etc.
General application.Traditional asphalt is mainly derived from petroleum coking, and coal tar asphalt cannot replace petroleum due to its special property
Pitch, and China's oil demand relies on import, and therefore, a kind of method for researching and developing carbolineum production novel asphalt is pendulum every
Glorious and arduous mission in face of a pitch scientific worker.
The conventionally employed oxidizing process of pitch is produced, chemical polymerization etc., the oxidizing process production time is longer, and step is many and diverse, chemistry
Polymerization catalyst is easy inactivation, requires harsh and yield not high reaction condition, limits its popularization and application.
Summary of the invention
In view of the problems of the existing technology and insufficient, the present invention provides a kind of method that carbolineum prepares pitch, more specifically
Be a kind of carbolineum catalytic polymerization production novel asphalt method, this method simple process, reaction condition is mild, and bitumen product
Have high yield and high softening point, lower needle penetration and stronger economy, increases carbolineum purposes.
The invention is realized by the following technical scheme:
A kind of method that carbolineum prepares pitch, after carbolineum is warming up to 200~300 DEG C, be added catalyst, catalyst account for carbolineum and
The 10~30% of catalyst gross mass, magnetic agitation, 4~30h of insulation reaction obtain pitch after cooling.
The carbolineum is product of the coal tar after 250~370 DEG C of distillations.
The heating rate is 4~6 DEG C/min.
The catalyst is sulphur.
The revolving speed of the magnetic agitation is 25~50 revs/min.
The method production pitch can be used for road asphalt or needle coke.
The beneficial effects of the present invention are:
1, the present invention use sulphur as polymerization catalyst production pitch, passes through the initial concentration of control sulphur, reaction temperature, when reaction
Between control the performance of pitch, increase the purposes of carbolineum.
2, the yield and production efficiency that the present invention greatly improves, reduce production cost, are conducive to the production of carbolineum catalytic polymerization
The industrialized production and application of novel asphalt.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of method that carbolineum prepares pitch, takes 120g carbolineum to pour into dried beaker, pours into three-necked flask, and three mouthfuls
An appropriately sized rotor is placed in flask, then three-necked flask is put into constant temperature blender with magnetic force, is opened recirculated water, is followed
For ring water by spherical condensating tube bottom in and top out, the revolving speed of regulating thermostatic magnetic stirring apparatus is 25 turns/min, is warming up to 5 DEG C/min
200 DEG C of reaction temperature, constant temperature to reaction terminates, logical after experimental temperature is stablized in the beaker after taking sulphur 13.33g to be placed in drying
It crosses funnel to be added from the side port of three-neck flask, after 200 DEG C of heat preservation 4h, closes magnetic stirring apparatus, stand disassembly reaction dress after 10min
It sets, the pitch in three-neck flask is poured into dried beaker and be placed in natural cooling in draught cupboard.
Acquired asphalt softening point is 42.5 DEG C, needle penetration 80.2, ductility 300mm.
Embodiment 2
A kind of method that carbolineum prepares pitch, takes 120g carbolineum to pour into dried beaker, pours into three-necked flask, and three mouthfuls
An appropriately sized rotor is placed in flask, then three-necked flask is put into constant temperature blender with magnetic force, is opened recirculated water, is followed
For ring water by spherical condensating tube bottom in and top out, the revolving speed of regulating thermostatic magnetic stirring apparatus is 40 turns/min, is warming up to 4 DEG C/min
200 DEG C of reaction temperature, constant temperature to reaction terminates, logical after experimental temperature is stablized in the beaker after taking sulphur 13.33g to be placed in drying
It crosses funnel to be added from the side port of three-neck flask, after 200 DEG C of heat preservation 4h, closes magnetic stirring apparatus, stand disassembly reaction dress after 10min
It sets, the pitch in three-neck flask is poured into dried beaker and be placed in natural cooling in draught cupboard.
Acquired asphalt softening point is 44 DEG C, needle penetration 79.4, ductility 298mm.
Embodiment 3
A kind of method that carbolineum prepares pitch, takes 120g carbolineum to pour into dried beaker, pours into three-necked flask, and three mouthfuls
An appropriately sized rotor is placed in flask, then three-necked flask is put into constant temperature blender with magnetic force, is opened recirculated water, is followed
For ring water by spherical condensating tube bottom in and top out, the revolving speed of regulating thermostatic magnetic stirring apparatus is 50 turns/min, is warming up to 5 DEG C/min
200 DEG C of reaction temperature, constant temperature to reaction terminates, logical after experimental temperature is stablized in the beaker after taking sulphur 13.33g to be placed in drying
It crosses funnel to be added from the side port of three-neck flask, after 200 DEG C of heat preservation 4h, closes magnetic stirring apparatus, stand disassembly reaction dress after 10min
It sets, the pitch in three-neck flask is poured into dried beaker and be placed in natural cooling in draught cupboard.
Acquired asphalt softening point is 45 DEG C, needle penetration 79.4, ductility 298mm.
Embodiment 4
A kind of method that carbolineum prepares pitch, takes 120g carbolineum to pour into dried beaker, pours into three-necked flask, and three mouthfuls
An appropriately sized rotor is placed in flask, then three-necked flask is put into constant temperature blender with magnetic force, is opened recirculated water, is followed
For ring water by spherical condensating tube bottom in and top out, the revolving speed of regulating thermostatic magnetic stirring apparatus is 40 turns/min, is warming up to 5 DEG C/min
250 DEG C of reaction temperature, constant temperature to reaction terminates, logical after experimental temperature is stablized in the beaker after taking sulphur 13.33g to be placed in drying
It crosses funnel to be added from the side port of three-neck flask, after 250 DEG C of heat preservation 4h, closes magnetic stirring apparatus, stand disassembly reaction dress after 10min
It sets, the pitch in three-neck flask is poured into dried beaker and be placed in natural cooling in draught cupboard.
Acquired asphalt softening point is 52.5 DEG C, needle penetration 64.2, ductility 282mm.
Embodiment 5
A kind of method that carbolineum prepares pitch, takes 120g carbolineum to pour into dried beaker, pours into three-necked flask, and three mouthfuls
An appropriately sized rotor is placed in flask, then three-necked flask is put into constant temperature blender with magnetic force, is opened recirculated water, is followed
For ring water by spherical condensating tube bottom in and top out, the revolving speed of regulating thermostatic magnetic stirring apparatus is 25 turns/min, is warming up to 6 DEG C/min
300 DEG C of reaction temperature, constant temperature to reaction terminates, logical after experimental temperature is stablized in the beaker after taking sulphur 13.33g to be placed in drying
It crosses funnel to be added from the side port of three-neck flask, after 300 DEG C of heat preservation 4h, closes magnetic stirring apparatus, stand disassembly reaction dress after 10min
It sets, the pitch in three-neck flask is poured into dried beaker and be placed in natural cooling in draught cupboard.
Acquired asphalt softening point is 80.2 DEG C, needle penetration 50.1, ductility 242mm.
Embodiment 6
A kind of method that carbolineum prepares pitch, takes 120g carbolineum to pour into dried beaker, pours into three-necked flask, and three mouthfuls
An appropriately sized rotor is placed in flask, then three-necked flask is put into constant temperature blender with magnetic force, is opened recirculated water, is followed
For ring water by spherical condensating tube bottom in and top out, the revolving speed of regulating thermostatic magnetic stirring apparatus is 40 turns/min, is warming up to 5 DEG C/min
250 DEG C of reaction temperature, constant temperature to reaction terminates, logical after experimental temperature is stablized in the beaker after taking sulphur 13.33g to be placed in drying
It crosses funnel to be added from the side port of three-neck flask, after 250 DEG C of heat preservation 5h, closes magnetic stirring apparatus, stand disassembly reaction dress after 10min
It sets, the pitch in three-neck flask is poured into dried beaker and be placed in natural cooling in draught cupboard.
Acquired asphalt softening point is 80.2 DEG C, needle penetration 50.1, ductility 242mm.
Embodiment 7
A kind of method that carbolineum prepares pitch, takes 120g carbolineum to pour into dried beaker, pours into three-necked flask, and three mouthfuls
An appropriately sized rotor is placed in flask, then three-necked flask is put into constant temperature blender with magnetic force, is opened recirculated water, is followed
Ring water is by spherical condensating tube bottom in and top out, and the revolving speed of regulating thermostatic magnetic stirring apparatus is 40 turns/min, and temperature is with 4 DEG C/min liter
Temperature arrives 200 DEG C of reaction temperature, and constant temperature to reaction terminates, in the beaker after taking sulphur 21.18g to be placed in drying, when experimental temperature is stablized
It is added afterwards by funnel from the side port of three-neck flask, after 200 DEG C of heat preservation 4h, closes magnetic stirring apparatus, disassembly is anti-after standing 10min
Device is answered, the pitch in three-neck flask is poured into dried beaker and is placed in natural cooling in draught cupboard.
Acquired asphalt softening point is 50.5 DEG C, needle penetration 75.2, ductility 292mm.
Embodiment 8
A kind of method that carbolineum prepares pitch, takes 120g carbolineum to pour into dried beaker, pours into three-necked flask, and three mouthfuls
An appropriately sized rotor is placed in flask, then three-necked flask is put into constant temperature blender with magnetic force, is opened recirculated water, is followed
Ring water is by spherical condensating tube bottom in and top out, and the revolving speed of regulating thermostatic magnetic stirring apparatus is 40 turns/min, and temperature is with 5 DEG C/min liter
Temperature arrives 200 DEG C of reaction temperature, and constant temperature to reaction terminates, in the beaker after taking sulphur 51.42g to be placed in drying, after experimental temperature is stablized
It is added by funnel from the side port of three-neck flask, after 200 DEG C of heat preservation 4h, closes magnetic stirring apparatus, dismantle reaction after standing 10min
Pitch in three-neck flask is poured into dried beaker and is placed in natural cooling in draught cupboard by device.
Acquired asphalt softening point is 98.3 DEG C, needle penetration 72.5, ductility 212mm.
Embodiment 9
A kind of method that carbolineum prepares pitch, takes 120g carbolineum to pour into dried beaker, pours into three-necked flask, and three mouthfuls
An appropriately sized rotor is placed in flask, then three-necked flask is put into constant temperature blender with magnetic force, is opened recirculated water, is followed
Ring water is by spherical condensating tube bottom in and top out, and the revolving speed of regulating thermostatic magnetic stirring apparatus is 40 turns/min, and temperature is with 5 DEG C/min liter
Temperature arrives 200 DEG C of reaction temperature, and constant temperature to reaction terminates, in the beaker after taking sulphur 13.33g to be placed in drying, experimental temperature and stabilization
It is added afterwards by funnel from the side port of three-neck flask, after 200 DEG C of heat preservation 10h, closes magnetic stirring apparatus, dismantled after standing 10min
Pitch in three-neck flask is poured into dried beaker and is placed in natural cooling in draught cupboard by reaction unit.
Acquired asphalt softening point is 50.5 DEG C, needle penetration 70.2, ductility 288mm.
Embodiment 10
A kind of method that carbolineum prepares pitch, takes 120g carbolineum to pour into dried beaker, pours into three-necked flask, and three mouthfuls
An appropriately sized rotor is placed in flask, then three-necked flask is put into constant temperature blender with magnetic force, is opened recirculated water, is followed
Ring water is by spherical condensating tube bottom in and top out, and the revolving speed of regulating thermostatic magnetic stirring apparatus is 40 turns/min, and temperature is with 5 DEG C/min liter
Temperature arrives 200 DEG C of reaction temperature, and constant temperature to reaction terminates, in the beaker after taking sulphur 13.33g to be placed in drying, experimental temperature and stabilization
It is added afterwards by funnel from the side port of three-neck flask, after 200 DEG C of heat preservation 20h, closes magnetic stirring apparatus, dismantled after standing 10min
Pitch in three-neck flask is poured into dried beaker and is placed in natural cooling in draught cupboard by reaction unit.
Acquired asphalt softening point is 63.5 DEG C, needle penetration 56.2, ductility 248mm.
Embodiment 11
A kind of method that carbolineum prepares pitch, takes 120g carbolineum to pour into dried beaker, pours into three-necked flask, and three mouthfuls
An appropriately sized rotor is placed in flask, then three-necked flask is put into constant temperature blender with magnetic force, is opened recirculated water, is followed
Ring water is by spherical condensating tube bottom in and top out, and the revolving speed of regulating thermostatic magnetic stirring apparatus is 40 turns/min, and temperature is with 5 DEG C/min liter
Temperature arrives 200 DEG C of reaction temperature, and constant temperature to reaction terminates, in the beaker after taking sulphur 13.33g to be placed in drying, experimental temperature and stabilization
It is added afterwards by funnel from the side port of three-neck flask, after 200 DEG C of heat preservation 30h, closes magnetic stirring apparatus, dismantled after standing 10min
Pitch in three-neck flask is poured into dried beaker and is placed in natural cooling in draught cupboard by reaction unit.
Acquired asphalt softening point is 66.5 DEG C, needle penetration 51.2, ductility 237mm.
Above the embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment party
Formula can also be made without departing from the purpose of the present invention within the knowledge of a person skilled in the art
Various change out.
Claims (5)
1. a kind of method that carbolineum prepares pitch, which is characterized in that after carbolineum is warming up to 200~300 DEG C, catalyst is added,
Catalyst accounts for the 10~30% of carbolineum and catalyst gross mass, magnetic agitation, and 4~30h of insulation reaction obtains pitch after cooling.
2. the method that carbolineum prepares pitch according to claim 1, which is characterized in that the carbolineum is coal tar 250~
Product after 370 DEG C of distillations.
3. the method that carbolineum prepares pitch according to claim 1, which is characterized in that the heating rate be 4~6 DEG C/
min。
4. the method that carbolineum prepares pitch according to claim 1, which is characterized in that the catalyst is sulphur.
5. the method that carbolineum prepares pitch according to claim 1, which is characterized in that the revolving speed of the magnetic agitation be 25~
50 revs/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810907227.2A CN108998062A (en) | 2018-08-10 | 2018-08-10 | A kind of method that carbolineum prepares pitch |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810907227.2A CN108998062A (en) | 2018-08-10 | 2018-08-10 | A kind of method that carbolineum prepares pitch |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108998062A true CN108998062A (en) | 2018-12-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810907227.2A Pending CN108998062A (en) | 2018-08-10 | 2018-08-10 | A kind of method that carbolineum prepares pitch |
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| Country | Link |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109536189A (en) * | 2018-12-29 | 2019-03-29 | 山东齐创石化工程有限公司 | The production technology of needle coke |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6228343B1 (en) * | 1996-09-06 | 2001-05-08 | Mitsubishi Gas Chemical Company, Inc. | Method for producing isotropic pitch, activated carbon fibers and carbon materials for non-aqueous secondary battery anodes |
| CN102977906A (en) * | 2012-11-15 | 2013-03-20 | 四川创越炭材料有限公司 | Preparing method of high-purity arene oligomerization asphalt |
| CN104593033A (en) * | 2015-01-12 | 2015-05-06 | 中钢集团鞍山热能研究院有限公司 | Preparation method of high-performance environment-friendly asphalt |
-
2018
- 2018-08-10 CN CN201810907227.2A patent/CN108998062A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6228343B1 (en) * | 1996-09-06 | 2001-05-08 | Mitsubishi Gas Chemical Company, Inc. | Method for producing isotropic pitch, activated carbon fibers and carbon materials for non-aqueous secondary battery anodes |
| CN102977906A (en) * | 2012-11-15 | 2013-03-20 | 四川创越炭材料有限公司 | Preparing method of high-purity arene oligomerization asphalt |
| CN104593033A (en) * | 2015-01-12 | 2015-05-06 | 中钢集团鞍山热能研究院有限公司 | Preparation method of high-performance environment-friendly asphalt |
Non-Patent Citations (1)
| Title |
|---|
| ADELA L. FERNANDEZ: "Carbon Precursors from Anthracene Oil. Insight into the Reactions of Anthracene Oil with Sulfur", 《ENERGY & FUELS》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109536189A (en) * | 2018-12-29 | 2019-03-29 | 山东齐创石化工程有限公司 | The production technology of needle coke |
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Application publication date: 20181214 |