CN110317623A - A kind of preparation method for extracting ultra-fine carbon material from pitch - Google Patents
A kind of preparation method for extracting ultra-fine carbon material from pitch Download PDFInfo
- Publication number
- CN110317623A CN110317623A CN201910728390.7A CN201910728390A CN110317623A CN 110317623 A CN110317623 A CN 110317623A CN 201910728390 A CN201910728390 A CN 201910728390A CN 110317623 A CN110317623 A CN 110317623A
- Authority
- CN
- China
- Prior art keywords
- carbon material
- fine carbon
- additive
- ultra
- preparation
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- 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)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Civil Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The invention discloses a kind of to extract the preparation method of ultra-fine carbon material from pitch, comprising the following steps: prepares maltha, prepares refined bitumen, dissolved dilution, addition additive, hot melt separation, dry milling and removing additive；Preparation method of the invention is more scientific and reasonable, this extracts the preparation method of ultra-fine carbon material from pitch, refined bitumen is prepared by the way that addition modified additive cooperation is high temperature modified, using refined bitumen as raw material, aromatic solvent is added and carries out dissolved dilution, by adding additive, increase QI partial size, the method separated using thermosol, solid powder containing QI is recycled, ultra-fine carbon material has been obtained after removing additive, obtained ultra-fine carbon material can meet fineness requirement, purity is high, quality is considerable, and the efficiency of production is higher, process equipment requires low, it is worthy to be popularized.
Description
Technical field
The present invention relates to field of bitumen technology, specially a kind of preparation method that ultra-fine carbon material is extracted from pitch.
Background technique
When removing QI prepares refined bitumen, contain the solid powder of QI as a kind of ultra-fine carbon material, for downstream
Producer uses, and is the excellent raw material for producing high-density high-strength carbon material, solves and generate during refined bitumen
The problem of solid waste, while benefit is increased, but the method efficiency that tradition extracts ultra-fine carbon material from pitch is relatively low,
The purity of extraction is not high and fineness of product not enough requires；For this purpose, it is proposed that a kind of extract ultra-fine carbon material from pitch
Preparation method.
Summary of the invention
The purpose of the present invention is to provide a kind of to extract the preparation method of ultra-fine carbon material from pitch, to solve background
The problem of being proposed in technology.
To achieve the above object, the invention provides the following technical scheme: a kind of extract ultra-fine carbon material from pitch
Preparation method, comprising the following steps:
S1: washing oil is added in the mid temperature pitch that softening point is 60-95 DEG C or containing luxuriant and rich with fragrance Residual oil, obtaining softening point after mixing is
45-65 DEG C of maltha；
S2: maltha is added in stirred autoclave, and is sequentially added modified additive into reaction kettle and be modified, will be anti-
It answers temperature to improve to 150 DEG C -180 DEG C, 4-8 hour of isothermal reaction, obtains refined bitumen；
S2: it is added to using refined bitumen as raw material in Mixer pot and is heated to complete molten condition, be then added into Mixer pot
15-30% aromatic solvent carries out dissolved dilution；
S3: being added into the refined bitumen after dissolved dilution and additive and stir evenly, and temperature control is in 130-150 when stirring
DEG C, additive divides 3-5 addition, and each interval time is 5-15 minutes, adds temperature every time and increases 2-4 DEG C, by adding
Add agent to increase the partial size of QI；
S4: the refined bitumen for adding additive is put into hot melt seperator and carries out hot melt separation, is divided from refined bitumen
Separate out the slag body containing QI；
S5: the slag body isolated is launched in drying equipment, 6-12 hours dry under conditions of 80-95 DEG C, then
It is ground into fixed powder by grinder, the solid powder recycling containing QI is spare；
S6: using the additive in solvent extraction process removing solid powder, ultra-fine carbon material can be obtained.
Preferably, modified additive includes epoxy resin 5.5-7.5%, carbon black 3.6-5.2% and glycerol in the S2
1.7-3.4%。
Preferably, the additive in the S3 is any one of vinyl-based siloxanes, unsaturated acids or light diesel.
Preferably, QI content is 25-40wt% in the slag body isolated in the S4.
Preferably, the partial size that powder is fixed in the S5 is 80-90 mesh.
Preferably, the partial size of ultra-fine carbon material obtained is 90 mesh or more in the S6.
It compared with prior art, should be from the beneficial effects of the present invention are: preparation method of the invention is more scientific and reasonable
The preparation method that ultra-fine carbon material is extracted in pitch cooperates high temperature modified prepare to refine drip by addition modified additive
Blueness is added aromatic solvent and carries out dissolved dilution using refined bitumen as raw material, by adding additive, increases QI partial size, using heat
Molten isolated method, the solid powder containing QI is recycled, and has been obtained ultra-fine carbon material after removing additive, has been obtained
To ultra-fine carbon material can meet that fineness requirement, purity is high, quality are considerable, and the efficiency produced is higher, process equipment requirement
It is low, it is worthy to be popularized.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment one:
A kind of preparation method for extracting ultra-fine carbon material from pitch, comprising the following steps:
S1: washing oil is added in the mid temperature pitch that softening point is 70 DEG C, obtains the maltha that softening point is 45 DEG C after mixing；
S2: maltha is added in stirred autoclave, and is sequentially added modified additive into reaction kettle and be modified, will be anti-
It answers temperature to improve to 150 DEG C, 5 hours of isothermal reaction, obtains refined bitumen；
S2: it is added to using refined bitumen as raw material in Mixer pot and is heated to complete molten condition, be then added into Mixer pot
18% aromatic solvent carries out dissolved dilution；
S3: being added into the refined bitumen after dissolved dilution and additive and stir evenly, and temperature control adds at 130 DEG C when stirring
Agent is added to be added three times, each interval time is 5 minutes, adds temperature every time and increases 2 DEG C, increases QI by addition additive
Partial size；
S4: the refined bitumen for adding additive is put into hot melt seperator and carries out hot melt separation, is divided from refined bitumen
From contain QI slag body；
S5: the slag body isolated is launched in drying equipment, 6 hours dry under conditions of 80 DEG C, then by grinding
Grinding machine is ground into fixed powder, and the solid powder recycling containing QI is spare；
S6: using the additive in solvent extraction process removing solid powder, ultra-fine carbon material can be obtained.
Further, modified additive includes epoxy resin 5.5%, carbon black 3.6% and glycerol 1.7% in S2.
Further, the additive in S3 is vinyl-based siloxanes.
Further, QI content is 30wt% in the slag body isolated in S4.
Further, the partial size that powder is fixed in S5 is 80 mesh.
Further, the partial size of ultra-fine carbon material obtained is 100 in S6.
Embodiment two:
A kind of preparation method for extracting ultra-fine carbon material from pitch, comprising the following steps:
S1: washing oil is added in the mid temperature pitch that softening point is 80 DEG C, obtains the maltha that softening point is 55 DEG C after mixing；
S2: maltha is added in stirred autoclave, and is sequentially added modified additive into reaction kettle and be modified, will be anti-
It answers temperature to improve to 170 DEG C, 6 hours of isothermal reaction, obtains refined bitumen；
S2: it is added to using refined bitumen as raw material in Mixer pot and is heated to complete molten condition, be then added into Mixer pot
25% aromatic solvent carries out dissolved dilution；
S3: being added into the refined bitumen after dissolved dilution and additive and stir evenly, and temperature control adds at 140 DEG C when stirring
Add 4 additions of agent point, each interval time is 10 minutes, adds temperature every time and increases 3 DEG C, increases QI by addition additive
Partial size；
S4: the refined bitumen for adding additive is put into hot melt seperator and carries out hot melt separation, is divided from refined bitumen
Separate out the slag body containing QI；
S5: the slag body isolated is launched in drying equipment, 9 hours dry under conditions of 90 DEG C, then by grinding
Grinding machine is ground into fixed powder, and the solid powder recycling containing QI is spare；
S6: using the additive in solvent extraction process removing solid powder, ultra-fine carbon material can be obtained.
Further, modified additive includes epoxy resin 6.5%, carbon black 4.3% and glycerol 2.8% in S2.
Further, the additive in S3 is light diesel.
Further, QI content is 35wt% in the slag body isolated in S4.
Further, the partial size that powder is fixed in S5 is 80 mesh.
Further, the partial size of ultra-fine carbon material obtained is 110 mesh in S6.
Embodiment three:
A kind of preparation method for extracting ultra-fine carbon material from pitch, comprising the following steps:
S1: it is added in the mid temperature pitch that softening point is 95 DEG C containing luxuriant and rich with fragrance Residual oil, obtains the soft drip that softening point is 65 DEG C after mixing
It is green；
S2: maltha is added in stirred autoclave, and is sequentially added modified additive into reaction kettle and be modified, will be anti-
It answers temperature to improve to 180 DEG C, 8 hours of isothermal reaction, obtains refined bitumen；
S2: it is added to using refined bitumen as raw material in Mixer pot and is heated to complete molten condition, be then added into Mixer pot
30% aromatic solvent carries out dissolved dilution；
S3: being added into the refined bitumen after dissolved dilution and additive and stir evenly, and temperature control adds at 150 DEG C when stirring
Add 5 additions of agent point, each interval time is 15 minutes, adds temperature every time and increases 4 DEG C, increases QI by addition additive
Partial size；
S4: the refined bitumen for adding additive is put into hot melt seperator and carries out hot melt separation, is divided from refined bitumen
Separate out the slag body containing QI；
S5: the slag body isolated is launched in drying equipment, 12 hours dry under conditions of 95 DEG C, then by grinding
Grinding machine is ground into fixed powder, and the solid powder recycling containing QI is spare；
S6: using the additive in solvent extraction process removing solid powder, ultra-fine carbon material can be obtained.
Further, modified additive includes epoxy resin 7.5%, carbon black 5.2% and glycerol 3.4% in S2.
Further, the additive in S3 is unsaturated acids.
Further, QI content is 40wt% in the slag body isolated in S4.
Further, the partial size that powder is fixed in S5 is 90 mesh.
Further, the partial size of ultra-fine carbon material obtained is 120 mesh in S6.
Above three groups of embodiments are preparation method of the invention, wherein using embodiment two as most preferably, it is of the invention
Preparation method is more scientific and reasonable, and the preparation method of ultra-fine carbon material should be extracted from pitch, passes through the modified addition of addition
Agent cooperation is high temperature modified to prepare refined bitumen, using refined bitumen as raw material, aromatic solvent is added and carries out dissolved dilution, by adding
Doping increases QI partial size, and the method separated using thermosol is recycled the solid powder containing QI, adds in removing
Ultra-fine carbon material has been obtained after agent, it is considerable that obtained ultra-fine carbon material can meet fineness requirement, purity is high, quality, and
The efficiency of production is higher, process equipment requirement is low, is worthy to be popularized.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of preparation method for extracting ultra-fine carbon material from pitch, which comprises the following steps:
S1: washing oil is added in the mid temperature pitch that softening point is 60-95 DEG C or containing luxuriant and rich with fragrance Residual oil, obtaining softening point after mixing is
45-65 DEG C of maltha；
S2: maltha is added in stirred autoclave, and is sequentially added modified additive into reaction kettle and be modified, will be anti-
It answers temperature to improve to 150 DEG C -180 DEG C, 4-8 hour of isothermal reaction, obtains refined bitumen；
S2: it is added to using refined bitumen as raw material in Mixer pot and is heated to complete molten condition, be then added into Mixer pot
15-30% aromatic solvent carries out dissolved dilution；
S3: being added into the refined bitumen after dissolved dilution and additive and stir evenly, and temperature control is in 130-150 when stirring
DEG C, additive divides 3-5 addition, and each interval time is 5-15 minutes, adds temperature every time and increases 2-4 DEG C, by adding
Add agent to increase the partial size of QI；
S4: the refined bitumen for adding additive is put into hot melt seperator and carries out hot melt separation, is divided from refined bitumen
Separate out the slag body containing QI；
S5: the slag body isolated is launched in drying equipment, 6-12 hours dry under conditions of 80-95 DEG C, then
It is ground into fixed powder by grinder, the solid powder recycling containing QI is spare；
S6: using the additive in solvent extraction process removing solid powder, ultra-fine carbon material can be obtained.
2. a kind of preparation method for extracting ultra-fine carbon material from pitch according to claim 1, it is characterised in that: institute
Stating modified additive in S2 includes epoxy resin 5.5-7.5%, carbon black 3.6-5.2% and glycerol 1.7-3.4%.
3. a kind of preparation method for extracting ultra-fine carbon material from pitch according to claim 1, it is characterised in that: institute
State any one that the additive in S3 is vinyl-based siloxanes, unsaturated acids or light diesel.
4. a kind of preparation method for extracting ultra-fine carbon material from pitch according to claim 1, it is characterised in that: institute
Stating QI content in the slag body isolated in S4 is 25-40wt%.
5. a kind of preparation method for extracting ultra-fine carbon material from pitch according to claim 1, it is characterised in that: institute
Stating and fixing the partial size of powder in S5 is 80-90 mesh.
6. a kind of preparation method for extracting ultra-fine carbon material from pitch according to claim 1, it is characterised in that: institute
The partial size for stating ultra-fine carbon material obtained in S6 is 90 mesh or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910728390.7A CN110317623B (en) | 2019-08-08 | 2019-08-08 | Preparation method for extracting superfine carbon material from asphalt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910728390.7A CN110317623B (en) | 2019-08-08 | 2019-08-08 | Preparation method for extracting superfine carbon material from asphalt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110317623A true CN110317623A (en) | 2019-10-11 |
| CN110317623B CN110317623B (en) | 2021-06-25 |
Family
ID=68125736
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910728390.7A Active CN110317623B (en) | 2019-08-08 | 2019-08-08 | Preparation method for extracting superfine carbon material from asphalt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110317623B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040228789A1 (en) * | 2000-12-13 | 2004-11-18 | Alfred Stiller | Method of controlling swelling and shrinkage during synthesis of coke |
| CN101591819A (en) * | 2009-06-25 | 2009-12-02 | 神华集团有限责任公司 | A kind of asphalt base carbon fiber that utilizes the coal directly-liquefied residue preparation and preparation method thereof |
| CN102766478A (en) * | 2012-07-23 | 2012-11-07 | 辽宁科技大学 | Method for producing low-Na+ high-QI (quinoline insoluble) mid-temperature pitch |
| CN102952561A (en) * | 2011-08-31 | 2013-03-06 | 上海宝钢化工有限公司 | Method for preparing adjustable high-quinoline-insoluble (QI) coal tar |
| CN104861676A (en) * | 2015-06-11 | 2015-08-26 | 山东大学 | Waste superpolymer based comprehensive asphaltic-mixture modifier and preparation method and application thereof |
| KR101646845B1 (en) * | 2014-12-02 | 2016-08-16 | 오씨아이 주식회사 | Highly efficient method for manufacturing pitch as carbonaceous raw material |
-
2019
- 2019-08-08 CN CN201910728390.7A patent/CN110317623B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040228789A1 (en) * | 2000-12-13 | 2004-11-18 | Alfred Stiller | Method of controlling swelling and shrinkage during synthesis of coke |
| CN101591819A (en) * | 2009-06-25 | 2009-12-02 | 神华集团有限责任公司 | A kind of asphalt base carbon fiber that utilizes the coal directly-liquefied residue preparation and preparation method thereof |
| CN102952561A (en) * | 2011-08-31 | 2013-03-06 | 上海宝钢化工有限公司 | Method for preparing adjustable high-quinoline-insoluble (QI) coal tar |
| CN102766478A (en) * | 2012-07-23 | 2012-11-07 | 辽宁科技大学 | Method for producing low-Na+ high-QI (quinoline insoluble) mid-temperature pitch |
| KR101646845B1 (en) * | 2014-12-02 | 2016-08-16 | 오씨아이 주식회사 | Highly efficient method for manufacturing pitch as carbonaceous raw material |
| CN104861676A (en) * | 2015-06-11 | 2015-08-26 | 山东大学 | Waste superpolymer based comprehensive asphaltic-mixture modifier and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110317623B (en) | 2021-06-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105038262B (en) | A kind of environment-friendly type regeneration softening agent and preparation method thereof | |
| CN107946593A (en) | A kind of method that coal tar pitch prepares lithium cell negative pole material needle coke | |
| CN104789248B (en) | Method for preparing mesophase pitch by coal-tar pitch | |
| CN112830867A (en) | Preparation method of energy-saving environment-friendly flame retardant tetrabromo double-part A | |
| CN109504416B (en) | Production process of coal-based needle coke | |
| CN103740400A (en) | Method for preparing high-quality needle coke raw material by removing QI (Quinoline Insolubles) in coal tar | |
| CN110317623A (en) | A kind of preparation method for extracting ultra-fine carbon material from pitch | |
| CN108998203A (en) | A kind of method that ultrasound on extracting-squeezing combines extraction sesame oil | |
| CN109504415B (en) | Production method of needle coke | |
| CN104479707B (en) | A kind of method for preparing needle coke | |
| CN103772309B (en) | The method of preparation 2,2 '-(4,4 '-diphenylethyllene) dibenzoxazine fine work | |
| CN103396309B (en) | A kind of method of pressurization production high-purity gallic acid propyl ester | |
| CN101747303A (en) | Method for producing maleopimaric anhydride | |
| CN103421196A (en) | Method for extracting high-purity eucommea rubber from eucommea samara | |
| CN107805405B (en) | A method of improving capsanthin smell | |
| CN106085584A (en) | A kind of processing method improving oil Paeonia suffruticosa oil yield | |
| CN102041018B (en) | Processing method of coal and oil co-refining | |
| CN101665402B (en) | Method for preparing refined fluorene | |
| CN105733630B (en) | A kind of preparation method and its device of homogeneous needle coke | |
| CN104987945B (en) | A kind of technical method that rapeseed oil residue viscosity is reduced using ultrasonic assistant | |
| CN104211658A (en) | Novel preparation method of rubber vulcanization accelerator MBT | |
| CN108658758A (en) | Preparation method, paraphthaloyl chloride and the application of paraphthaloyl chloride, the preparation method and p-phenylenediamine of p-phenylenediamine | |
| CN110713862A (en) | Ultrahigh continuous degumming method and device for illegal cooking oil | |
| CN103173283A (en) | Solvent de-acidifying method for edible idesia oil | |
| CN102899171B (en) | Method for refining and recycling waste wax in wax printing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20210219 Address after: Tang Cheng Zhen Tang Cheng Cun, Anze County, Linfen City, Shanxi Province 042500 Applicant after: Shanxi Yongxin Coal Coking Co.,Ltd. Address before: No.7 Renmin Road, Shilong District, Pingdingshan City, Henan Province Applicant before: PINGDINGSHAN DONGSHENG HI-TECH INDUSTRIAL Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230118 Address after: 042500 Tangcheng Industrial Park, Anze Economic Development Zone, Linfen City, Shanxi Province Patentee after: Kexin Carbon Materials Co.,Ltd. Address before: Tang Cheng Zhen Tang Cheng Cun, Anze County, Linfen City, Shanxi Province 042500 Patentee before: Shanxi Yongxin Coal Coking Co.,Ltd. |
|
| TR01 | Transfer of patent right |