CN101214944A - Method for preparing high-strength coal tar asphalt carbon foam material - Google Patents
Method for preparing high-strength coal tar asphalt carbon foam material Download PDFInfo
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- CN101214944A CN101214944A CNA2007101731269A CN200710173126A CN101214944A CN 101214944 A CN101214944 A CN 101214944A CN A2007101731269 A CNA2007101731269 A CN A2007101731269A CN 200710173126 A CN200710173126 A CN 200710173126A CN 101214944 A CN101214944 A CN 101214944A
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Abstract
The invention relates to a method for preparing high-intensity coal tar pitch carbon foam material including (1) pyrolyzing the coal tar pitch to prepare pitch with intermediate phase, and adding in toluene solution for extracting and drying after being crashed, (2) adding the dried pitch with intermediate phase to a high-pressure autoclave, increasing the temperature to reach above the softening point of the pitch via pumping vacuum and charging inactive gas, keeping 120-240 minutes under the temperature of 350-500 DEG C and the pressure of 6-80kg/cm 2, then releasing the pressure foams, cooling to the room temperature, then obtaining the pitch foam material, (3) carbonizing the pitch foam material under the protection of nitrogen with 1300-1600 DEG C to obtain pitch carbon foam material. The pitch carbon foam material obtained by using the method of the invention has the advantages of high-intensity, is capable of being used in relative fields of high load and high charge and the like, and is suitable to high commercial process.
Description
Technical field
The invention belongs to the preparation method field of carbon foam, particularly relate to a kind of preparation method of high-strength coal tar asphalt carbon foam material.
Background technology
Asphalt foam material is that a kind of calorifics is stable, high temperature resistant, the novel material of light specific gravity, specific surface area, it has excellent heat-insulating property and mechanical property, it is applied in the parts such as aerospace, navigation, nuclear power as protecting hot material, can be to the miniaturization of device, the change that lightness is brought leap.
U.S. Ultramet`s company develops a kind of reticulated carbon foam, has low-down thermal conductivity, can reach 0.085W/m.K, but compressive strength only is 0.763MPa, must improve intensity through technologies such as precipitated metals.
The U.S. inferior university of west Buddhist guinea has developed a kind of coal that utilizes and has prepared the carbon foam with higher-strength as persursor material, compressive strength can reach 15MPa, thermal conductivity scope 0.4～17.5W/m.k, but this carbon foam needs oxidation-stabilized processing, and the process complexity is restive.
Its principal character of USP 6033506 (J.W. Klett, Process For Making Carbon Foam) is that its defective is that intensity is low with bituminous material expanded forming in high pressure, and power consumption is high, the Working environment poor stability.
USP 6398994 B (J.W Klett, 2002.6.4) disclosed a kind of technology of utilizing, it is characterized in that adopting after petroleum pitch and the whipping agent blend expanded the forming of foaming in lower pressure, but its defective is that two kinds of phase material mixing uniformity are poor, the hole interface distributions and the lack of homogeneity of Xing Chenging thus, thus make the homogeneity of function of carbon foam also relatively poor.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of high-strength coal tar asphalt carbon foam material, to remedy the deficiencies in the prior art and defective, satisfies the needs of production and association area development.Adopt the asphalt foam material of method preparation of the present invention to have high strength, can be used for association areas such as high year high loading, be suitable for suitability for industrialized production.
The preparation method of a kind of high-strength coal tar asphalt carbon foam material of the present invention comprises the steps:
(1) coal-tar pitch is prepared mesophase pitch through pyrolysis, join in the toluene solution after the pulverizing and extract, the pitch after the extraction is taken out drying;
(2) dried mesophase pitch adds autoclave, vacuumizes that to be warmed up to the bituminous softening temperature above and charge into rare gas element, at 350～500 ℃ temperature and 6～80kg/cm
2Pressure kept 120～240 minutes down, relief pressure foaming then, cool to room temperature obtains the asphalt foam material;
(3) the asphalt foam material was kept 120～180 minutes 1300～1600 ℃ the time, carbonization under the nitrogen protection, asphalt foam material.
Described pitch is a kind of or its mixture in coal-tar pitch or the petroleum pitch, and its bituminous softening temperature is 80～90 ℃, and pitch softening point is 200～300 ℃ after pyrolysis and after the toluene extraction, and intermediate phase content is 70%～95%.
Described pyrolysis preparation is 400 ℃～500 ℃ pyrolysis 4～6 hours, and preferred 400～450 ℃, pyrolysis prepares the reacting completely back nitrogen purging of mesophase pitch, removes the small molecule component that reacts with difficulty that generates in the dereaction.
Described toluene extraction temperature is 100～250 ℃, is incubated 30～60 minutes, and the density of the asphalt foam that makes after the toluene extraction is increased to 0.8g/cm
3
Rare gas element in the described step (2) is one or more in nitrogen, carbonic acid gas or the argon gas.
Intensification in the described step (2) is in room temperature to 280 ℃, and keeping temperature rise rate is 4 ℃/min, is incubated 60 minutes, is raised to 350～500 ℃ at the further temperature rise rate with 2 ℃/min.
Prepared asphalt foam material directly carries out carbonizing treatment without oxidation-stabilized processing under nitrogen protection, preferred 1300～1400 ℃ of carbonization temperature, and temperature rise rate is 3 ℃/min.
Principle of the present invention is mainly to be that the content of toluene insolubles reduces in the mesophase pitch, has improved intermediate phase content greatly through after the toluene extraction, and the increase of intermediate phase content is to the material impact that is formed with of carbon foam ligament structure in the later stage foaming process.The increase of intermediate phase content, the amount of isotropic material reduces, and makes abscess more even in forming process, regular, and the foam crackle significantly reduces, and the foam ligament structure is also compact more thereupon, and intensity improves obviously, so the foamy physical strength is greatly improved.
Beneficial effect of the present invention:
Adopt method of the present invention to prepare asphalt foam material, the product that is obtained, mechanical property is good, can keep high physical strength under high temperature and high load condition, and Working environment is safe and reliable, is suitable for suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
(1) pitch (coal-tar base pitch) was prepared mesophase pitch in 4 hours through 400 ℃ of pyrolysis, wherein, the softening temperature of mesophase pitch is 240 ℃ after the pyrolysis, intermediate phase content 70%;
(2) the mesophase pitch pulverizing is joined in the toluene solution, be heated to 100 ℃ of extractions 30 minutes, the pitch after the extraction is taken out after drying, the softening temperature of mesophase pitch is 270 ℃ after the extraction, intermediate phase content 85%;
(3) dried mesophase pitch is added autoclave, vacuumize that to be warmed up to the bituminous softening temperature above and charge into nitrogen, fill nitrogen pressure 6Kg/cm
2, in room temperature to 280 ℃, keeping temperature rise rate is 4 ℃/min, is incubated 60 minutes; Be raised to 350 ℃ at further temperature rise rate, be incubated 240 minutes with 2 ℃/min, relief pressure foaming then, the cold room temperature of getting obtains the asphalt foam material:
(4) with the asphalt foam material 1300 ℃ of following carbonizations 120 minutes, wherein temperature rise rate is 3 ℃/min, obtains carbon foam.
The performance index of the carbon foam that makes see Table 1.
The carbon foam index that table 1 is produced
| Embodiment 1 | Embodiment 2 | Comparative Examples | |
| Volume density g/cm 3 | 0.54～0.6 | 0.75～0.8 | 0.44～0.53 |
| Thermal expansivity ppM/ ℃ | 4.2 | 3.1 | 5.4 |
| Compressive strength MPa | 21.6 | 29.7 | 4.5 |
Embodiment 2
Preparation process is as embodiment 1, but the preparation of pyrolysis wherein is 450 ℃ of pyrolysis 4 hours, the softening temperature of mesophase pitch is 240 ℃ after the pyrolysis, intermediate phase content 70%: 250 ℃ of toluene extraction temperature, be incubated 60 minutes, the softening temperature of toluene extraction back mesophase pitch is 285 ℃, intermediate phase content 95%; Fill nitrogen pressure 6Kg/cm
2, 400 ℃ of blowing temperatures, foamed time 240 minutes, the performance index of the carbon foam that makes see Table 1.
Comparative Examples
Preparation process is as embodiment 1, but without the toluene extraction, directly foams, wherein, 240 ℃ of the softening temperatures of mesophase pitch after the pyrolysis, intermediate phase content 70%, the carbon foam index of producing sees Table 1.
This shows, material of the present invention is compared with the material of Comparative Examples, use the carbon foam that the present invention adopts the preparation of toluene extraction mesophase pitch, keep high mechanical strength properties to prepare carbon foamy performance under the particularly high temperature and high load condition and all be significantly improved than ordinary method.
Claims (9)
1. the preparation method of a high-strength coal tar asphalt carbon foam material comprises the steps:
(1) coal-tar pitch is prepared mesophase pitch through pyrolysis, join in the toluene solution after the pulverizing and extract, the pitch after the extraction is taken out drying;
(2) dried mesophase pitch adds autoclave, vacuumizes that to be warmed up to the bituminous softening temperature above and charge into rare gas element, at 350～500 ℃ temperature and 6～80kg/cm
2Pressure kept 120～240 minutes down, relief pressure foaming then, cool to room temperature obtains the asphalt foam material;
(3), get asphalt foam material with the carbonization under 1300～1600 ℃ of nitrogen protections of asphalt foam material.
2. the preparation method of high-strength coal tar asphalt carbon foam material according to claim 1, it is characterized in that: described pitch is coal-tar pitch or petroleum pitch a kind of or its mixture wherein, and its bituminous softening temperature is 80～90 ℃.
3. the preparation method of high-strength coal tar asphalt carbon foam material according to claim 1 is characterized in that: described after pyrolysis and toluene extraction back pitch softening point be 200～300 ℃, intermediate phase content is 70%～95%.
4. the preparation method of high-strength coal tar asphalt carbon foam material according to claim 1 is characterized in that: described pyrolysis preparation is 400 ℃～500 ℃ pyrolysis 4～6 hours.
5. the preparation method of high-strength coal tar asphalt carbon foam material according to claim 4, it is characterized in that: described pyrolysis preparation temperature is 400～450 ℃.
6. the preparation method of high-strength coal tar asphalt carbon foam material according to claim 1, it is characterized in that: described toluene extraction temperature is 100～250 ℃, is incubated 30～60 minutes, the density of the asphalt foam that makes after the toluene extraction is increased to 0.8g/cm
3
7. the preparation method of high-strength coal tar asphalt carbon foam material according to claim 1, it is characterized in that: the rare gas element in the described step (2) is one or more in nitrogen, carbonic acid gas or the argon gas.
8. the preparation method of high-strength coal tar asphalt carbon foam material according to claim 1, it is characterized in that: the intensification in the described step (2) is in room temperature to 280 ℃, keeping temperature rise rate is 4 ℃/min, be incubated 60 minutes, be raised to 350～500 ℃ at further temperature rise rate with 2 ℃/min.
9. the preparation method of high-strength coal tar asphalt carbon foam material according to claim 1, it is characterized in that: the carbonization in the described step (3) is 1300～1400 ℃ of carbonization temperatures, and temperature rise rate is 3 ℃/min, keeps 120～180 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101731269A CN101214944A (en) | 2007-12-26 | 2007-12-26 | Method for preparing high-strength coal tar asphalt carbon foam material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101731269A CN101214944A (en) | 2007-12-26 | 2007-12-26 | Method for preparing high-strength coal tar asphalt carbon foam material |
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| CN101214944A true CN101214944A (en) | 2008-07-09 |
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|---|---|---|---|
| CNA2007101731269A Pending CN101214944A (en) | 2007-12-26 | 2007-12-26 | Method for preparing high-strength coal tar asphalt carbon foam material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102870319A (en) * | 2010-03-26 | 2013-01-09 | 东洋炭素株式会社 | Carbon brush |
| CN102942945A (en) * | 2012-11-15 | 2013-02-27 | 四川创越炭材料有限公司 | Preparation method of soluble mesophase pitch |
| CN108584909A (en) * | 2018-06-21 | 2018-09-28 | 西安理工大学 | A method of high intensity Carbon foam is prepared using modified pitch |
| CN109867272A (en) * | 2019-04-08 | 2019-06-11 | 广东煤基碳材料研究有限公司 | A kind of foamy carbon and preparation method thereof |
| CN112048291A (en) * | 2020-09-14 | 2020-12-08 | 陕西博石源丰能源科技有限公司 | Asphalt-reinforced foam plugging agent suitable for selective water plugging of oil-water well and preparation method and application thereof |
-
2007
- 2007-12-26 CN CNA2007101731269A patent/CN101214944A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102870319A (en) * | 2010-03-26 | 2013-01-09 | 东洋炭素株式会社 | Carbon brush |
| CN102870319B (en) * | 2010-03-26 | 2016-02-17 | 东洋炭素株式会社 | Carbon brush |
| CN102942945A (en) * | 2012-11-15 | 2013-02-27 | 四川创越炭材料有限公司 | Preparation method of soluble mesophase pitch |
| CN102942945B (en) * | 2012-11-15 | 2014-05-28 | 四川创越炭材料有限公司 | Preparation method of soluble mesophase pitch |
| CN108584909A (en) * | 2018-06-21 | 2018-09-28 | 西安理工大学 | A method of high intensity Carbon foam is prepared using modified pitch |
| CN109867272A (en) * | 2019-04-08 | 2019-06-11 | 广东煤基碳材料研究有限公司 | A kind of foamy carbon and preparation method thereof |
| CN112048291A (en) * | 2020-09-14 | 2020-12-08 | 陕西博石源丰能源科技有限公司 | Asphalt-reinforced foam plugging agent suitable for selective water plugging of oil-water well and preparation method and application thereof |
| CN112048291B (en) * | 2020-09-14 | 2023-03-24 | 陕西博石源丰能源科技有限公司 | Asphalt-reinforced foam plugging agent suitable for selective water plugging of oil-water well and preparation method and application thereof |
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Open date: 20080709 |