CN106929083A - A kind of petroleum base isotropy carbon fiber can spin the preparation method of pitch - Google Patents
A kind of petroleum base isotropy carbon fiber can spin the preparation method of pitch Download PDFInfo
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- CN106929083A CN106929083A CN201511008731.1A CN201511008731A CN106929083A CN 106929083 A CN106929083 A CN 106929083A CN 201511008731 A CN201511008731 A CN 201511008731A CN 106929083 A CN106929083 A CN 106929083A
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- pitch
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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
-
- 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
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- 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 isotropy carbon fiber can spin the preparation method of pitch, comprise the following steps：1. it is that raw material is purified by sedimentation, filtering with ethylene cracking tar；2. tar is flashed at 280 DEG C of -320 DEG C of temperature, normal pressure after purifying；3. the material after atmospheric flashing carries out vacuum flashing again；4. the material after vacuum flashing is fused and mixed in proportion with coumarone or other raw materials production mid temperature pitch；5. material after mixing melting is carried out into polycondensation reaction.It is an advantage of the invention that：1. process is simple is without the easy industrialized production of any catalyst.2. abundant raw material, cheap, low cost.3. without waste residue, waste liquid discharge, environmental protection is good.4. the hard pitch and modified pitch of multiple use can be prepared by the change of adjusting process parameter and the proportioning of raw material.
Description
Technical field
The present invention relates to petrochemical industry, specifically a kind of system of petroleum base hard pitch
Preparation Method.
Background technology
Petroleum base isotropy carbon fiber can spin pitch with one or more petroleum refining or oil
The heavy component discarded in product is raw material.It is sufficient with raw material, cheap, Residual carbon is high,
Oxidation activity is high, high-purity, modest viscosity, spinnability high the features such as, carbon fiber can be made,
Cathode of lithium battery covering material and other carbon materials, wherein carbon fiber have high temperature resistant, corrosion-resistant,
Thermal expansion is low advantage, and the composite made can be applied to aviation, building, military project, the people
With industry, high-quality thermal insulating material etc.；This pitch is also the production indispensable cladding material of lithium battery
Material, existing production method complex process, production cost is higher.
The content of the invention
In order to solve the above technical problems, it is an object of the invention to provide a kind of each phase of new petroleum base
Same sex carbon fiber can spin the preparation method of pitch, and concrete technical scheme is as follows：
A kind of petroleum base isotropy carbon fiber can spin the preparation method of pitch, it is characterised in that bag
Include following steps：
1. it is that raw material is purified by sedimentation, filtering with ethylene cracking tar；
2. tar is flashed at 280 DEG C of -320 DEG C of temperature, normal pressure after purifying；
3. the material after atmospheric flashing carries out vacuum flashing again, 280 DEG C -320 DEG C of flash temperature,
Vacuum 60-110kpa；
4. the material after vacuum flashing and coumarone or other raw materials production mid temperature pitch are pressed 1：
The ratio of 0-2 is fused and mixed, and it is 200 DEG C -240 DEG C to be fused and mixed temperature；
5. material after mixing melting is carried out into polycondensation reaction, reaction temperature is 320 DEG C -460 DEG C, vacuum
The 1-8 hours 50-500pa reaction time of degree.
Another technical scheme is：Step be 4. by with ethylene cracking tar mid temperature pitch with it is ancient
The grand resin of horse or other raw materials production petroleum base mid temperature pitch, press at a temperature of 200 DEG C -240 DEG C
1：The ratio of 0-2 is fused and mixed, at the same omit step 1. -3., ethylene cracking tar mid temperature pitch is soft
Change 90 DEG C -130 DEG C of point.
80 DEG C -130 DEG C described of other raw materials production mid temperature pitch softening point.
It is rapid be 4. by the material after vacuum flashing and the mid temperature pitch of catalytic cracked oil pulp production by
1：The ratio of 0.1-2 is fused and mixed, and it is 200 DEG C -240 DEG C to be fused and mixed temperature；
The present invention further discloses the application of the product：Dripped as petroleum-based carbon fibre spinnable
It is blue or green and as cathode of lithium battery covering material.
It is an advantage of the invention that：
1. process is simple is without the easy industrialized production of any catalyst.
2. abundant raw material, cheap, low cost.
3. without waste residue, waste liquid discharge, environmental protection is good.
4. multiple use can be prepared by the change of adjusting process parameter and the proportioning of raw material
Hard pitch and modified pitch.
Specific embodiment
Example 1：
1. it is that raw material is purified by sedimentation, filtering with ethylene cracking tar；
2. 10 tons of ethylene bottom oil after 1. step is refined is inserted agitator in atmospheric flashing kettle and is stirred
Mix, mixing speed 200 min, be warming up to 280 DEG C, normal pressure is stopped 5 hours；
3. the material after atmospheric flashing carries out vacuum flashing, 320 DEG C of flash temperature, agitator again
Stirring, stir speed (S.S.) 200r/min is vacuumized, vacuum 60kpa；
4. by the material after step 3. vacuum flashing and 6000kg coumarone indene resins, stirring is fused and mixed,
Stir speed (S.S.) 300 min, 230 DEG C of temperature, stop 2 hours after filtering be placed in polycondensation vessel stir,
Stopped at 100pa.430 DEG C of vacuum and obtain within 6.5 hours hard pitch, softening point is 264.5
℃。
Embodiment 2
1. it is that raw material is purified by sedimentation, filtering with ethylene cracking tar；
2. 10 tons of ethylene bottom oil after 1. step is refined is inserted agitator in atmospheric flashing kettle and is stirred
Mix, be warming up to 320 DEG C, normal pressure is stopped 6 hours；
3. the material after atmospheric flashing carries out vacuum flashing, 280 DEG C of flash temperature, agitator again
Stirring, stir speed (S.S.) 220r/min is vacuumized, vacuum 110kpa；
4. by fire stons oil in 100 DEG C of the material after step 3. vacuum flashing and 6000kg softening points
Pitch is fused and mixed stirring, is fused and mixed stirring, and stir speed (S.S.) 300r/min, 240 DEG C of temperature stops 2
Filtering is placed in polycondensation vessel and stirs after hour, is stopped 8 hours at 100pa.430 DEG C of vacuum
To hard pitch, softening point is 264.5 DEG C.
Embodiment 3
1. it is that raw material is purified by sedimentation, filtering with ethylene cracking tar；
2. 10 tons of ethylene bottom oil after 1. step is refined is inserted agitator in atmospheric flashing kettle and is stirred
Mix, be warming up to 300 DEG C, normal pressure is stopped 6 hours；
3. the material after atmospheric flashing carries out vacuum flashing, 280 DEG C of flash temperature, agitator again
Stirring, stir speed (S.S.) 220r/min is vacuumized, vacuum 110kpa；
4. by the material after step 3. vacuum flashing and 3000kg coumarone indene resins, 300kg100
Fire stons oil asphalt in DEG C, is fused and mixed stirring, is fused and mixed stirring, stir speed (S.S.) 300r/min, temperature
200 DEG C, filtering is placed in polycondensation vessel and stirs after stopping 2 hours, at 50pa.460 DEG C of vacuum
Stop obtains hard pitch for 1 hour, and softening point is 264.5 DEG C.
Embodiment 4
1. it is that raw material is purified by sedimentation, filtering with ethylene cracking tar；
2. tar is flashed in 300 DEG C of temperature under normal pressure after 100kg is purified；
3. the material after atmospheric flashing carries out vacuum flashing, 300 DEG C of flash temperature, vacuum again
100kpa；
4. fire stons oil asphalt in the material after vacuum flashing and 2000kg100 DEG C is fused and mixed, is fused and mixed
Temperature is 220 DEG C；
5. material after mixing melting is carried out into polycondensation reaction, reaction temperature is 320 DEG C, vacuum 200pa
8 hours reaction time obtained hard pitch, and softening point is 265 DEG C.
Embodiment 5
1. it is that raw material is purified by sedimentation, filtering with ethylene cracking tar；
2. tar is flashed in 320 DEG C of temperature under normal pressure after 100kg is purified；
3. the material after atmospheric flashing carries out vacuum flashing, 280 DEG C of flash temperature, vacuum again
60kpa；
4. the material after vacuum flashing and 2000kg coumarone indene resins are fused and mixed, being fused and mixed temperature is
200℃；
5. material after mixing melting is carried out into polycondensation reaction, reaction temperature is 360 DEG C, vacuum 260pa
7 hours reaction time obtained hard pitch, and softening point is 265 DEG C.
Example 6, will be fused and mixed tank and allocates coumarone indene resin 5000kg, 5000kg catalytic cracked oil pulp into,
Be fused and mixed stirring, stir speed (S.S.) 300 min, 200 DEG C of temperature, stop 5 hours after filtering be placed in contracting
Stirred in poly- kettle, stopped at 300pa.350 DEG C of vacuum and obtain hard pitch in 7 hours, softened
Point is 266 DEG C.
Example 7, will be fused and mixed tank and allocates 110 DEG C of oil mid temperature pitch .2500kg of 2500kg softening points into
Coumarone indene resin, be fused and mixed stirring, stir speed (S.S.) 300 min, 230 DEG C of temperature, stop 5 hours
Filtering afterwards is placed in polycondensation vessel and stirs, and is stopped at 200pa.430 DEG C of vacuum and obtained for 6.5 hours
Hard pitch, softening point is 267 DEG C.
Example 8, will be fused and mixed tank and allocates 100 DEG C of oil mid temperature pitch 1500kg of 3500kg softening points into
Catalytic cracked oil pulp, is fused and mixed stirring, stir speed (S.S.) 300 min, 230 DEG C of temperature stops 5 small
When after filtering be placed in polycondensation vessel and stir, stopped at 300pa.440 DEG C of vacuum and obtained for 6 hours
Hard pitch, softening point is 265 DEG C.
Example 9, will be fused and mixed tank and allocates 100 DEG C of oil mid temperature pitches of 2000kg softening points, 4000kg into
Catalytic cracked oil pulp, is fused and mixed stirring, stir speed (S.S.) 300 min, 230 DEG C of temperature stops 5 small
When after filtering be placed in polycondensation vessel and stir, stopped at 350pa.380 DEG C of vacuum and obtained for 7 hours
Hard pitch, softening point is 264 DEG C of
Embodiment 1 and the petroleum-based carbon fibre spinnable pitch of embodiment 7, through domestic manufacturer's spinning system
Obtain carbon fiber indices ----compare with same kind of products at abroad such as table 1
Table 1
Lithium cell negative pole covering material is applied to, contrast indices is carried out better than it with external producer,
External product can be replaced completely.As the material that is produced with the product of the embodiment of the present invention 1 with
Foreign material is to such as table 2；
Table 2
Claims (6)
1. a kind of petroleum base isotropy carbon fiber can spin the preparation method of pitch, it is characterised in that comprise the following steps：
1. it is that raw material is purified by sedimentation, filtering with ethylene cracking tar；
2. tar is flashed at 280 DEG C of -320 DEG C of temperature, normal pressure after purifying；
3. the material after atmospheric flashing carries out vacuum flashing, 280 DEG C -320 DEG C of flash temperature, vacuum 60-110kpa again；
4. the material after vacuum flashing and coumarone or other raw materials production mid temperature pitch are pressed 1：The ratio of 0-2 is fused and mixed, and it is 200 DEG C -240 DEG C to be fused and mixed temperature；
5. material after mixing melting is carried out into polycondensation reaction, reaction temperature is 320 DEG C -460 DEG C, 1-8 hours vacuum 50-500pa reaction time.
2. preparation method according to claim 1, it is characterised in that：
4. step is that will produce petroleum base mid temperature pitch with ethylene cracking tar mid temperature pitch and coumarone indene resin or other raw materials, 1 is pressed at a temperature of 200 DEG C -240 DEG C：The ratio of 0-2 is fused and mixed, at the same omit step 1. -3., 90 DEG C -120 DEG C of ethylene cracking tar mid temperature pitch softening point.
3. preparation method according to claim 1, it is characterised in that：80 DEG C -130 DEG C described of other raw materials production mid temperature pitch softening point.
4. preparation method according to claim 1, it is characterised in that：4. step is by 1 by the material after vacuum flashing and catalytic cracked oil pulp：The ratio of 0-2 is fused and mixed, and it is 200 DEG C -240 DEG C to be fused and mixed temperature.
5. the application of product according to claim 1 or claim 2, it is characterised in that：As petroleum-based carbon fibre spinnable pitch.
6. the application of product according to claim 1 or claim 2, it is characterised in that：As cathode of lithium battery covering material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511008731.1A CN106929083A (en) | 2015-12-29 | 2015-12-29 | A kind of petroleum base isotropy carbon fiber can spin the preparation method of pitch |
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| CN201511008731.1A CN106929083A (en) | 2015-12-29 | 2015-12-29 | A kind of petroleum base isotropy carbon fiber can spin the preparation method of pitch |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109233305A (en) * | 2017-07-11 | 2019-01-18 | 宝武炭材料科技有限公司 | Preparation method of coated asphalt for carbon negative electrode material |
| CN109913253A (en) * | 2019-02-26 | 2019-06-21 | 王志明 | Lithium battery coats special asphalt and preparation method |
| CN114989850A (en) * | 2022-06-06 | 2022-09-02 | 中建安装集团有限公司 | High-efficiency conversion process and device for heavy ethylene tar |
| CN115093872A (en) * | 2022-06-22 | 2022-09-23 | 中国石油大学(华东) | Coated asphalt and preparation method and application thereof |
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| CN102690672A (en) * | 2012-06-18 | 2012-09-26 | 辽宁科技大学 | Preparing method for coal tar refined pitch |
| CN102925187A (en) * | 2012-11-15 | 2013-02-13 | 四川创越炭材料有限公司 | Method for continuously producing spinning 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 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109233305A (en) * | 2017-07-11 | 2019-01-18 | 宝武炭材料科技有限公司 | Preparation method of coated asphalt for carbon negative electrode material |
| CN109233305B (en) * | 2017-07-11 | 2020-12-08 | 宝武炭材料科技有限公司 | Preparation method of coated asphalt for carbon negative electrode material |
| CN109913253A (en) * | 2019-02-26 | 2019-06-21 | 王志明 | Lithium battery coats special asphalt and preparation method |
| CN114989850A (en) * | 2022-06-06 | 2022-09-02 | 中建安装集团有限公司 | High-efficiency conversion process and device for heavy ethylene tar |
| CN114989850B (en) * | 2022-06-06 | 2024-05-03 | 中建安装集团有限公司 | High-efficiency conversion process and device for heavy ethylene tar |
| CN115093872A (en) * | 2022-06-22 | 2022-09-23 | 中国石油大学(华东) | Coated asphalt and preparation method and application thereof |
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Application publication date: 20170707 |