CN100374367C - Technical method and schedule for preparation of foam carbon material used asphalt as raw material - Google Patents
Technical method and schedule for preparation of foam carbon material used asphalt as raw material Download PDFInfo
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- CN100374367C CN100374367C CNB2003101050531A CN200310105053A CN100374367C CN 100374367 C CN100374367 C CN 100374367C CN B2003101050531 A CNB2003101050531 A CN B2003101050531A CN 200310105053 A CN200310105053 A CN 200310105053A CN 100374367 C CN100374367 C CN 100374367C
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Abstract
The present invention relates to a preparation method for a carbon foam material using coal-based medium temperature pitch and petroleum-based mesophase pitch as raw materials by self-reacting foaming, which belongs to the technical field of coal chemical industry materials, petrochemical industry materials and carbon materials. The present invention is characterized in that the method comprises the following steps: milling pitch material for modification to form a precursor; heating the pitch material in a reaction vessel to form a sticky fluid and form foam during volatile gas release, and continuously heating the sticky fluid to a certain temperature for solidification to shape the foam; taking out the solidified sticky fluid, and carrying out high temperature carbonization. The carbon foam material with different foam pore structures can be prepared by controlling the technological conditions of foaming which mainly comprise the heating rate and reaction pressure, and the carbon foam material of the present invention has correspondingly uniform pore size distribution when observed with SEM. The present invention has the advantages and effects that the preparation cost is reduced, the defect that polymers are not easy to graphite when used to prepare the carbon foam material is overcome, and the performance of the carbon foam material is enhanced, thereby laying a foundation of the application of the carbon foam material in high technology fields, such as aerospace, etc.
Description
Technical field
The invention belongs to Coal Chemical Industry, petrochemical complex and carbon material technical field, relating to a kind of is raw material with coal-based mid-temperature pitch and petroleum base mesophase pitch, through the technological method of autoreaction foaming preparation foam carbon material.
Background technology
The porous material that Carbon foam is made up of hole bubble and mutual banded hole bubble wall with tridimensional network, this particular structure feature makes it have low density, high specific tenacity, good high temperature resistant and excellent acid-alkali-corrosive-resisting performance, and characteristics such as surperficial oxide-free impurity, is a kind of light porous property material.According to the difference of selected raw material and treatment process, the capacity of heat transmission of Carbon foam has the distribution range of broad, and (0.05～210W/mK), common Carbon foam is the same with other foam materials, and the capacity of heat transmission is lower, can be used as heat preserving and insulating material; And by the Carbon foam of mesophase pitch preparation after greying, has the capacity of heat transmission higher 4～6 times than metallic copper, use the thermal characteristics and the mechanical property of Carbon foam uniqueness, make matrix material, be with a wide range of applications in high-tech sectors such as aerospace with " sandwich " structure.The Carbon foam surface is polynuclear plane, the hole bubble has opening and remains silent two kinds, the higher Carbon foam of open porosity can be used as sorbent material or support of the catalyst is used, also can be used as good thermally conductive material and be used for the dissipate occasion of most of heat of needs, as highly integrated computer chip, the scatterer of automobile etc.; The porous foam carbon material can be used for the processing of vehicle exhaust and dust because of it has the better gas flowability; Utilize the porous and the conductivity of Carbon foam, also can be used as the effect of fuel cell electrode.In brief, the application prospect of foam carbon material is extremely extensive.
Early stage Carbon foam is a kind of reticulated structure vitreous state Carbon foam (RVC) that has, American Walter ford at first made (US patent 3121050) by the polymkeric substance pyrolysis charring in 1964, because of its unique physical and chemical performance has obtained Application and Development (US Patent:4795763 and 5397809) rapidly.This Carbon foam needs to add raw materials such as whipping agent, catalyzer and tensio-active agent in preparation process, and the product ultimate compression strength that makes is lower, difficult greying, limited its use range, therefore need its performance is improved, one of method is to add fibrous additive and utilize the CVI technology to obtain the top coat (US Patent 6183854) of refractory metal oxide and carbide in organic polymer, improves the physical strength and high temperature resistant, the corrosive nature of Carbon foam; Just increased the cost of Carbon foam product so widely, it is more complicated that preparation technology also becomes.
With the petroleum base mesophase pitch is raw material, adds whipping agent, and preparation foaming pitch carries out charing, greying (2300 ℃) then after oxidation-stabilized, can make the graphited Carbon foam of foam wall high orientation.1997, people such as U.S. Oak Ridge laboratory James.Klett utilize the method for the volatilization autoreaction foaming of low molecular compound in the mesophase pitch heat-processed to prepare graphited Carbon foam, the pore size distribution average out to 300 μ m of Carbon foam, and have the higher specific tenacity and the capacity of heat transmission (US Patent 6033506).
Coal is a kind of important energy raw material, is the traditional way of coal utilization as the direct combustion heat supplying of primary energy source and generating, worldwide has coal over half to be used in this aspect at present.Along with science and technology development, the comprehensive utilization of coal is developed rapidly, and chemistry, industrial chemicals and the high-carbon material of producing high added value as starting material with coal receive much attention.Utilize coal and derivative thereof successfully to make multiple carbon material through hot-work, as: coal-tar pitch based carbon fiber, intermediate phase charcoal microballon, coal activated carbon, coal charcoal processing molecular sieve etc.Rich coal resources in China is that the feedstock production carbon material has not only been expanded the range of application of coal beyond energy field with the coal, and can reduces the cost of carbon material greatly that its development prospect is wide.
Gas discharges in viscous fluid and produces foams, foams are finalized the design after fluid solidifies and are generated foam materials, high volatile volatile bituminous coal will produce a large amount of volatile gaseses between 350～550 ℃, itself is fluid state coal, begin gradually later on to solidify when temperature is higher than 500 ℃, control reaction system and pressure release will make raw material expand and produce foam.The A.H.Stiller people such as (1999) of U.S. West Virginia university is raw material with bituminous coal, through dissolution with solvents, coal-tar pitch is isolated in extracting, under 325～500 ℃, rare gas element (argon gas or the nitrogen) condition of 50～1000psi (hot pressing), foam, making density again through high temperature carbonization, greying is 0.2～2g/cm3, aperture Carbon foam (US Patent 5888469) comparatively uniformly, and to have studied with charcoal fiber and carbon nanotube be that additive strengthens Carbon foam (US Patent 6183154).And the Touchstone institute of West Virginia university is a raw material with high volatile volatile bituminous coal directly, and having prepared density under 400～600 ℃, the inert gas conditions of 0～500psi (colding pressing) is 0.16～0.8g/cm
3The Carbon foam of low heat conductivity, and the degree of graphitization of Carbon foam after the choosing of bituminous coal, preparation technology and the thermal treatment carried out more careful discussion, also deep research has been carried out in the aspects such as mechanical property, thermal characteristics and electrical property of Carbon foam, for the business development of Carbon foam product is laid a good foundation.
Summary of the invention
The purpose of this invention is to provide a kind of is the method for feedstock production Carbon foam with pitch.Preparation process is by under certain temperature and pressure, and volatile gases discharges the generation foam in viscous liquid realizes through charing, has overcome to add the shortcoming that whipping agent prepares the Carbon foam complex process.
The present invention is a raw material with coal-based mid-temperature pitch or petroleum base mesophase pitch respectively, and raw material by control temperature rise rate and pressure regime, is prepared the Carbon foam with different holes bubble structure and pore size distribution after upgrading is handled.Be characterized in not needing to add whipping agent, also aerobicization stabilizing treatment not, thus simplified production process, shortened the production cycle, reduced production cost, be convenient to the production of product.
The present invention has been feedstock production with the mid-temperature pitch and had a cancellated vitreous state Carbon foam, for the exploitation of this series products provides cheap more raw material and the processing method of more simplifying.
Technical scheme of the present invention is:
Material asphalt thermal degradation in autoclave produces gas and liquid, and the spontaneous infusion of gas release is equipped with foam materials, carries out charing under nitrogen protection, and utilizes the structural form of SEM and XRD analysis Carbon foam.
With pitch is that the feedstock production Carbon foam roughly can be divided following step:
1, the upgrading of asphalt stock: with the raw material grinding, cross 80 mesh sieves, (1) coal-based mid-temperature pitch is constant temperature 4h under about 400 ℃, the inert gas conditions of 3MPa, naturally cool to room temperature after, take out grinding, cross 80 mesh sieves; (2) ratio with 10: 1 adds iron nitrate in the mesophase pitch, and is even through ground and mixed, 100 ℃ of constant temperature 1h in baking oven.
2, asphalt foaming prepares Carbon foam: the raw material behind the upgrading is put into the high alumina ceramic former, place in the autoclave then, sequencing heats up under argon gas (or nitrogen) condition of 1～4MPa, temperature rise rate is that 2～5 ℃/min rises to 300 ℃, and constant temperature 1h, 1 ℃/min rise to 460 ℃, constant temperature 3h, 0.5 ℃/min rises to 550 ℃, and constant temperature 3h naturally cools to room temperature.
3, the carbonization process of Carbon foam: Carbon foam is placed the intensification of tubular type charring furnace internal program, rise to 500 ℃ with 5 ℃/min, constant temperature 30min rises to 1000 ℃ with 1 ℃/min, and constant temperature 3h naturally cools to room temperature.Whole carbonization process carries out under nitrogen protection.
4, the preparation of cancellated vitreous state Carbon foam and charing: through the mid-temperature pitch of step 1 upgrading, not needing grinding directly to put into the sequencing of tubular type charring furnace with mould heats up, rise to 400 ℃ with 2 ℃/min, constant temperature 30min, rise to 1000 ℃ with 8～10 ℃/min, constant temperature 3h naturally cools to room temperature.Whole foaming carbonization process carries out under nitrogen protection.
Effect of the present invention and benefit are as follows:
1, coal-based mid-temperature pitch and the petroleum base mesophase pitch with cheapness is raw material, do not add whipping agent, need not oxidation-stabilized in the preparation process, directly discharge volatile gases and make the viscous fluid foaming, continue to heat up fluid solidifies by temperature programming, lather styling forms Carbon foam, production technique is simple, and cost is low, is easy to produce.
2, by to the control of gaseous tension in the reactor, can prepare have different holes bubble sizes (200～800 μ m), Carbon foam that extent of opening is different, and hole bubble distribution uniform.
3, add iron nitrate in the petroleum base mesophase pitch, not only increased the quantity of Carbon foam hole bubble generation and the homogeneity of hole bubble, and help the catalyzed graphitization of Carbon foam, improve the performance of foam carbon material.
4, coal-based mid-temperature pitch is the feedstock production Carbon foam, has enriched the approach of the utilization of coal resources in China, for the coal-based carbon cellulosic material of preparation high added value is laid a good foundation.
5, be feedstock production with coal-based mid-temperature pitch and had cancellated vitreous state Carbon foam, reduced production cost, and be difficult for graphited shortcoming when having improved by this series products of polymer production.
6, Carbon foam has favorable mechanical performance and unique thermal characteristics, many again a kind of high performance materials applicatory in high-tech sectors such as aerospace.
Description of drawings
Fig. 1, the 2nd is raw material issues the Carbon foam that infusion is equipped with respectively in the condition of 4MPa, 2.8MPa scanning electron microscope (SEM) photo with the petroleum base mesophase pitch.As can be known when pressure diminishes, the hole of the Carbon foam of preparation bubble size is less by contrast, about average 400 μ m, and the obvious attenuation of thickness of hole bubble wall, and hole bubble quantity and open pore bubble rate (as arrow) improve, and helps the formation of hole bubble.
Fig. 3 is, and to be raw material with coal-based mid-temperature pitch issue scanning electron microscope (SEM) photo of the Carbon foam that infusion is equipped with in the condition of 4MPa.
Fig. 4 is to be scanning electron microscope (SEM) photo of the cancellated vitreous state Carbon foam of having of feedstock production with coal-based mid-temperature pitch.This Carbon foam of the clear demonstration of photo has higher open porosity (as arrow), is reticulated structure.
Embodiment
The invention will be further described below by embodiment.
Embodiment 1
With coal-based mid-temperature pitch is the feedstock production Carbon foam, and the softening temperature of used coal-based mid-temperature pitch is 80 ℃, pulverizes through speed muller, and it is standby to cross 80 mesh sieves.The upgrading process is to get about above-mentioned raw materials 2g, puts into the high alumina ceramic former, places in the autoclave, and reactor is put into crucible oven; Open inflation valve, under the pressure of 1MPa, charge into argon gas, the tensimeter on the observing response still, when showing that pressure is consistent with reducing valve pressure, close charging valve, open the venting valve, the gas in the reactor is emitted, close the venting valve, repeat aforesaid operations more once, with the air in the emptying still, the pressure with reducing valve increases to 3MPa (colding pressing) then, charge in the reactor, close inflation valve and reducing valve.Start program heats up, and 2 ℃/min rises to 400 ℃, and constant temperature 4h naturally cools to room temperature.Take out the pitch in the high alumina ceramic former, be reentered in the mould after the grinding, and place again in the reactor of crucible oven, get rid of the air in the reactor as stated above, and charge into argon gas to 4MPa (colding pressing).Start program heats up, and the temperature rise rate of foaming process is 2～5 ℃/min to 300 ℃, and constant temperature 1h, 1 ℃/min rise to 460 ℃, and constant temperature 3h, 0.5 ℃/min rise to 550 ℃, and constant temperature 3h naturally cools to room temperature.To put into the tubular type charring furnace after the mould taking-up, charing is carried out in temperature programming, and whole carbonization process carries out under nitrogen protection.The temperature rise rate of carbonization process is that 5 ℃/min rises to 500 ℃, and constant temperature 30min, 1 ℃/min rise to 1000 ℃, and constant temperature 3h naturally cools to room temperature.Sample is carried out phenetic analysis, the analysis of the line density of going forward side by side, void content, mechanical property and thermal characteristics etc. with scanning electronic microscope (SEM), X-ray diffractometer (XRD).
Embodiment 2
With the petroleum base mesophase pitch is the feedstock production Carbon foam, and the softening temperature of used petroleum base mesophase pitch is 220 ℃, pulverizes through speed muller, and it is standby to cross 80 mesh sieves.Get above-mentioned raw materials 10g, mix with 10: 1 ratios and iron nitrate, 100 ℃ of constant temperature 1h in baking oven cool off standby.Get above-mentioned raw materials 2g, by the mode of embodiment 1 pressure of reactor is added to 4MPa (colding pressing) fully, the temperature rise rate of foaming process and carbonization process and embodiment 1 are identical.For investigating the influence of pressure to the hole bubble structure, the pressure-controlling during foaming can obtain the different Carbon foam of hole bubble structure in the scope of 0.5～4MPa (colding pressing).Sample is carried out phenetic analysis, the analysis of the line density of going forward side by side, void content, mechanical property and thermal characteristics etc. with scanning electronic microscope (SEM), X-ray diffractometer (XRD).
Embodiment 3
With coal-based mid-temperature pitch is that feedstock production has cancellated vitreous state Carbon foam, used mid-temperature pitch and upgrading process thereof and embodiment 1 are just the same, mid-temperature pitch behind the upgrading need not grind after taking out, directly put into tubular type charring furnace temperature programming charing, whole carbonization process carries out under condition of nitrogen gas.2 ℃/the min of temperature rise rate of carbonization process rises to 400 ℃, and constant temperature 30min, 8～10 ℃/min rise to 1000 ℃, and constant temperature 3h naturally cools to room temperature.Sample is carried out phenetic analysis, the analysis of the line density of going forward side by side, void content, mechanical property and thermal characteristics etc. with scanning electronic microscope (SEM), X-ray diffractometer (XRD).
Claims (6)
1. one kind is the method for feedstock production Carbon foam with coal-based mid-temperature pitch or petroleum base mesophase pitch, the preparation technology who it is characterized in that Carbon foam comprises the asphalt stock grinding, sieve, coal-based mid-temperature pitch carries out upgrading by thermal treatment, perhaps the petroleum base mesophase pitch carries out upgrading by adding catalyzer, pack into behind the raw material grinding behind the upgrading in the high alumina ceramic former, put into reactor then, colding pressing is under the inert gas conditions of the high pure nitrogen of 0.5～8MPa or argon gas, temperature rise rate with 2～5 ℃/min is heated to 300 ℃, constant temperature 1h, 1 ℃/min rise to 460 ℃, constant temperature 3h, 0.5 ℃/min rises to 550 ℃, constant temperature 3h naturally cools to room temperature afterwards, makes the Carbon foam presoma, from reactor, take out the back and under nitrogen, carry out the charing processing, make the Carbon foam goods.
2. the method for preparing Carbon foam according to claim 1, it is characterized in that coal-based mid-temperature pitch carries out upgrading by thermal treatment, its modifying process is that the high alumina ceramic former that coal-based mid-temperature pitch is housed is put into reactor, rise to 400 ℃ with 2 ℃/min, be incubated 2～8h under the inert gas conditions of colding pressing for 3MPa.
3. the method for preparing Carbon foam according to claim 1, it is characterized in that the petroleum base mesophase pitch carries out upgrading by adding catalyzer, promptly in the petroleum base mesophase pitch, add iron nitrate, nickelous nitrate, Xiao Suangu, aluminum nitrate, saltpetre, iron trichloride, aluminum chloride or boron as catalyzer, 100 ℃ of constant temperature 1h in baking oven with 10: 1 ratio.
4. the method for preparing Carbon foam according to claim 1; it is characterized in that Carbon foam carries out charing and handle; charring process is that the Carbon foam presoma is put into atmosphere furnace; rise to 500 ℃ with 2～5 ℃/min; behind the constant temperature 30min; rise to 1000 ℃ with 1 ℃/min again, constant temperature 3h, whole carbonization process carries out under nitrogen protection.
5. the method for preparing Carbon foam according to claim 1, it is characterized in that the control of reaction pressure to hole bubble size, control is reflected under pressure 1～4MPa to be carried out, and obtains the hole bubble and is evenly distributed, and hole bubble size is 200～800 μ m Carbon foam different with extent of opening.
6. the method for preparing Carbon foam according to claim 2, it is characterized in that behind the coal-based mid-temperature pitch upgrading, directly put into charring furnace without grinding, rise to 400 ℃ with 2 ℃/min, constant temperature 30min, rise to 1000 ℃ with 8～10 ℃/min, constant temperature 3h, whole foaming carbonization process carries out under nitrogen protection; The Carbon foam that makes is reticulated structure, and has high open porosity, and the hole bubble size of Carbon foam is at 1～2mm.
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| CNB2003101050531A CN100374367C (en) | 2003-11-07 | 2003-11-07 | Technical method and schedule for preparation of foam carbon material used asphalt as raw material |
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| CN105462602A (en) * | 2015-11-19 | 2016-04-06 | 贵州大学 | A method of preparing foamy carbon from coal-tar pitch |
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| CN108190853B (en) * | 2018-01-18 | 2021-03-26 | 中国科学院山西煤炭化学研究所 | Preparation method of honeycomb foam wall hollow carbon ball |
| CN109553084B (en) * | 2019-01-31 | 2022-10-18 | 东北大学 | Method for preparing high-strength blocky porous carbon by pyrolysis |
| CN110745808B (en) * | 2019-12-04 | 2023-01-24 | 西安科技大学 | Method for preparing foam carbon based on heavy tar generated by pyrolysis of rich coal |
| CN113036164B (en) * | 2019-12-24 | 2022-05-27 | 大连大学 | Preparation method and application of composite electrode based on mesoporous carbon foam |
| CN114232215B (en) * | 2021-12-20 | 2022-11-29 | 西安工程大学 | Preparation method and application of asphalt-based carbon nanofiber multistage non-woven fabric with three-dimensional cavity structure |
| CN114956042A (en) * | 2022-06-17 | 2022-08-30 | 武汉科技大学 | High-thermal-conductivity foam carbon precursor, foam carbon and preparation method thereof |
| CN115072699B (en) * | 2022-06-29 | 2024-01-12 | 鞍钢化学科技有限公司 | Low-cost coal tar pitch-based foam carbon and preparation method of precursor thereof |
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