CN104310374A - Preparation method of foam carbon based on hydrophobic component in coal - Google Patents
Preparation method of foam carbon based on hydrophobic component in coal Download PDFInfo
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- CN104310374A CN104310374A CN201410526402.5A CN201410526402A CN104310374A CN 104310374 A CN104310374 A CN 104310374A CN 201410526402 A CN201410526402 A CN 201410526402A CN 104310374 A CN104310374 A CN 104310374A
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Abstract
The invention discloses a preparation method of foam carbon based on a hydrophobic component in coal, belonging to the preparation method of foam carbon. The preparation method comprises the following steps: (1) taking the hydrophobic component separated from a coal component as a raw material; (2) putting the raw material into a solvent A for extraction, and regulating molecular components; (3) washing the hydrophobic component obtained by extracting by use of a solvent B at the room temperature; (4) drying the hydrophobic component in an air medium with a certain temperature, relative humidity and flow velocity, so that a foam structure with a film foam wall is further formed in the hydrophobic component; (5) grinding the dried hydrophobic component, and pressing to form a tablet; (6), putting the sample subjected to the tabletting into a high-temperature carbonization furnace for heating in an inert atmosphere to obtain semi-foam carbon, and performing carbonation and heating, naturally cooling in the presence of inert gas, and cooling to the room temperature to obtain the foam carbon. The preparation method has the advantages that the raw material source is simple and low in cost, the method is simple and does not need sealed pressuring equipment, the foam carbon is rich in cellular structure, and very low in volume density and apparent density.
Description
Technical field
The present invention relates to a kind of preparation method of Carbon foam, particularly a kind of Carbon foam preparation method based on dredging middle matter component in coal.
Background technology
Carbon foam take carbonaceous material as raw material, a kind of D light endoplasmic reticular structure be made up of abscess and bubble wall obtained through foaming, solidification, charing and greying supervisor, and can carry out suitable modification to strengthen the Carbon Materials of certain particular item performance according to purposes.Carbon foam is prepared from primarily of organic polymer, pitch, mesophase pitch, coal and coal measures thing, and different starting material determine its different character.The technique of the preparation Carbon foam reported often requires High Temperature High Pressure, or add whipping agent, or add the artificial bubble process of making such as template, and be though that raw material can prepare better performance Carbon foam with mesophase pitch, very harsh to the requirement of technology and equipment by asphalt modulation mesophase pitch.Based on initial feed cheap and easy to get, adopt easy operational path, excellent and one of the target that stable foam carbon material is people to be pursued of processability.
And patent of invention " based on extraction and the gentleness coal-family component separation method of stripping ", number of patent application: 200710022120.1, coal is separated into four kinds of Group Component under field conditions (factors), thin middle matter component is wherein that subparticle is agglomerated into short texture body, volatile matter is high, ash content very low (can be close to ashless after reinforcing process), the foam carbon material of excellent property can be prepared by relatively simple technique, thus open up a new way for the Carbon foam preparation taking coal as raw material.
Summary of the invention
The object of this invention is to provide a kind of Carbon foam preparation method based on middle matter component thin in coal that raw material high-quality is easy to get, preparation technology is simple, with low cost, solve prior art obtain at raw material and prepare the complicacy of Carbon foam process aspect, obtain excellent Carbon foam.
The object of the present invention is achieved like this, and its step comprises the preparation of dredging middle matter group:
Described preparation of dredging middle matter group has following steps:
1. be that 10-300 object coal sample is placed in extractor by granularity, then add mixed solvent, add-on is the mixed solvent of every gram of coal sample 20-300 milliliter, and mixed solvent is solvent orange 2 A and solvent B is the mixture of 1:0.2 to 1:2 preparation by volume; At room temperature stir 10-300 minute, extraction process completes, and is extracted solidliquid mixture;
2. to step 1. in extraction extraction solidliquid mixture carry out solid-liquid separation, be extracted liquid and extract remainder respectively after solid-liquid separation;
3. to step 2. in extraction liquid process, extraction liquid is put into stripper, strippant is added again in stripper, the amount adding strippant equals between 1:0.1 to 1:2 by extraction liquid than strippant, described ratio is volume ratio, stirred at ambient temperature 5-60 minute, reextraction end of processing, obtains reextraction solidliquid mixture after reextraction process;
4. to step 3. in reextraction solidliquid mixture process, to reextraction solidliquid mixture leave standstill after carry out solid-liquid separation, obtain dredge in matter group;
5. described solvent orange 2 A is: dithiocarbonic anhydride, chloroform, methylene dichloride, benzene, methyl alcohol, phenol, ether; Described solvent B is: METHYLPYRROLIDONE, cyclohexanone, dimethyl sulfoxide (DMSO), tetrahydrofuran (THF), dimethyl formamide, N,N-DIMETHYLACETAMIDE, quadrol, tricresyl phosphate second fat, quinoline, pyridine; Described strippant is: water, normal hexane; In same technological process, solvent orange 2 A, solvent B and strippant must select three kinds of different vehicle substances;
Further comprising the steps of:
1. thin middle matter group is carried out at 45-100 DEG C the solvent extraction of 1-20 hour by solvent C, extract small-molecule substance wherein; Solvent D is at room temperature used with 20-150mL/ (gmin), the thin middle matter group after extracting to be carried out to the washing of 0.5-4h; Temperature 50-110 DEG C, relative humidity 20-50%, flow velocity 0.5-2m/s air dielectric under to the dry 2-20h of matter group in dredging, in making to dredge, matter group forms the balloon-shaped structure with thin film bubble wall further;
2. by after in dried dredging matter group is ground to 100-200 order, be pressed into the lamellar body of thick about 1-40mm with 5-20MPa pressure, form particulate interspaces and all less thin film bubble wall foam structure of abscess;
3. the sample after compressing tablet is placed in high temperature carbonization furnace, under an inert atmosphere, with constant temperature 1-20h at temperature rise rate 1-5 DEG C/min, carbonization temperature 400-800 DEG C, obtains half Carbon foam; Constant temperature 0-3h under 800-1200 DEG C of carbonization temperature again, then stops heating, under an inert gas below Temperature fall to 300 DEG C, namely obtains Carbon foam after being cooled to room temperature;
4. the specific surface area of Carbon foam that 3. process that measures obtains and aperture and microscopic optical structure etc. also carry out respective table and levy;
5. described solvent C is: chloroform, normal hexane, methyl alcohol, dithiocarbonic anhydride.Described solvent D is: acetone, ethanol, water.
Beneficial effect: owing to have employed such scheme, the raw material preparing Carbon foam is re-used as by dredging after middle matter group is separated of Carbon foam can be prepared in coal, avoid the meaningless consumption of other components when directly preparing Carbon foam by coal, prepare Carbon foam energy consumption by matter group in dredging lower simultaneously.Matter component in dredging in coal is utilized to be agglomerated into short texture body for subparticle, volatile matter is high, ash content is very low waits key character, by it from coal after high efficiency separation, again through solvent extraction, small-molecule substance is wherein fallen in extracting, adjustment molecular composition, and by washing, dry, grinding, the operations such as compressing tablet, make it to form particulate interspaces and all less thin film bubble wall foam structure of abscess, thus the High Temperature High Pressure overcome required by general preparation Carbon foam technique, or add whipping agent, or add the complexity such as template and harsh bubble process of making, there iing good practicality in the art.
Advantage: the method furthermore achieved that the efficient and rational utilization of coal-family component " each its ability to the greatest extent "; (1) in dredging, matter group is as the quality matetrial of preparation Carbon foam, and raw material sources are simple, with low cost; (2) method is simple, does not need airtight pressure exerting device; (3) prepare Carbon foam process simple, Carbon foam foam structure enriches, and total pore volume is maximum reaches 4.7cm
3/ g, porosity reaches as high as 83.5%, and volume density, apparent density are all very low.
Embodiment
The preparation method of the Carbon foam based on middle matter component thin in coal of the present invention, comprises the preparation of matter group in dredging, and the preparation process of described thin middle matter group is as follows:
1. be that 10-300 object coal sample is placed in extractor by granularity, then add mixed solvent, add-on is the mixed solvent of every gram of coal sample 20-300 milliliter, and mixed solvent is solvent orange 2 A and solvent B is the mixture of 1:0.2 to 1:2 preparation by volume; At room temperature stir 10-300 minute, extraction process completes, and is extracted solidliquid mixture;
2. to step 1. in extraction extraction solidliquid mixture carry out solid-liquid separation, be extracted liquid and extract remainder respectively after solid-liquid separation;
3. to step 2. in extraction liquid process, extraction liquid is put into stripper, strippant is added again in stripper, the amount adding strippant equals between 1:0.1 to 1:2 by extraction liquid than strippant, described ratio is volume ratio, stirred at ambient temperature 5-60 minute, reextraction end of processing, obtains reextraction solidliquid mixture after reextraction process;
4. to step 3. in reextraction solidliquid mixture process, to reextraction solidliquid mixture leave standstill after carry out solid-liquid separation, obtain dredge in matter group;
5. described solvent orange 2 A is: dithiocarbonic anhydride, chloroform, methylene dichloride, benzene, methyl alcohol, phenol, ether; Described solvent B is: METHYLPYRROLIDONE, cyclohexanone, dimethyl sulfoxide (DMSO), tetrahydrofuran (THF), dimethyl formamide, N,N-DIMETHYLACETAMIDE, quadrol, tricresyl phosphate second fat, quinoline, pyridine; Described strippant is: water, normal hexane; In same technological process, solvent orange 2 A, solvent B and strippant must select three kinds of different vehicle substances;
Further comprising the steps of:
1. thin middle matter group is carried out at 45-100 DEG C the solvent extraction of 1-20 hour by solvent C, extract small-molecule substance wherein; Solvent D is at room temperature used with 20-150mL/ (gmin), the thin middle matter group after extracting to be carried out to the washing of 0.5-4h; Temperature 50-110 DEG C, relative humidity 20-50%, flow velocity 0.5-2m/s air dielectric under to the dry 2-20h of matter group in dredging, in making to dredge, matter group forms the balloon-shaped structure with thin film bubble wall further;
2. by after in dried dredging matter group is ground to 100-200 order, be pressed into the lamellar body of thick about 1-40mm with 5-20MPa pressure, form particulate interspaces and all less thin film bubble wall foam structure of abscess;
3. the sample after compressing tablet is placed in high temperature carbonization furnace, under an inert atmosphere, with constant temperature 1-20h at temperature rise rate 1-5 DEG C/min, carbonization temperature 400-800 DEG C, obtains half Carbon foam; Constant temperature 0-3h under 800-1200 DEG C of carbonization temperature again, then stops heating, under an inert gas below Temperature fall to 300 DEG C, namely obtains Carbon foam after being cooled to room temperature;
4. the specific surface area of Carbon foam that 3. process that measures obtains and aperture and microscopic optical structure etc. also carry out respective table and levy;
5. described solvent C is: chloroform, normal hexane, methyl alcohol, dithiocarbonic anhydride.Described solvent D is: acetone, ethanol, water.
Embodiment 1:
Select carbon content C
dafbe 86.50% certain coal sample carry out fragmentation, by the total composition race separating technology of coal, coal sample is separated into four kinds of components, collect dredge in matter component for subsequent use.
1, at 65 DEG C, carrying out soxhlet extraction 20 hours by dredging middle matter group methanol solution, extracting small-molecule substance wherein;
2, at room temperature with water, 2 hours are washed to the middle matter group of dredging after extracting;
3, dry 20 hours of matter group in dredging under the air dielectric of temperature 110 DEG C, relative humidity 20%, flow velocity 2m/s;
4, suppress into about the thick right cylinder of 1mm with 5MPa pressure after matter group in dried dredging being ground to 200 orders;
5, sample compressing tablet is placed on crucible bottom and puts into tube furnace certain position, at inert component N
2in, under 5 DEG C/min temperature rise rate, be warming up to 450 DEG C, 550 DEG C, 650 DEG C, 800 DEG C, constant temperature 1 hour, then stop heating, Temperature fall to 300 DEG C under protection of inert gas, is cooled to room temperature and namely obtains Carbon foam.
The data of Carbon foam volume density, apparent density, porosity and mean pore size are as following table:
Temperature/DEG C | Volume density g/cm 3 | Apparent density g/cm 3 | Porosity % | Mean pore size μm |
450 | 0.2468 | 0.7244 | 65.9342 | 15.1593 |
550 | 0.1748 | 1.0226 | 82.9034 | 3.2652 |
650 | 0.1933 | 0.8318 | 76.7633 | 7.8715 |
800 | 0.2493 | 1.0139 | 75.4117 | 5.8482 |
Embodiment 2:
Select carbon content C
dafbe 85.0% certain coal sample carry out fragmentation, by the total composition race separating technology of coal, coal sample is separated into four kinds of components, collect dredge in matter component for subsequent use.
1, at 61 DEG C, soxhlet extraction is carried out 2 hours, extracting small molecules wherein by dredging middle matter group chloroformic solution;
2, at room temperature with ethanol, 4 hours are washed to the middle matter group of dredging after extracting;
3, dry 15 hours of matter group in dredging under the air dielectric of temperature 80 DEG C, relative humidity 30%, flow velocity 1m/s.
4, suppress into about the thick right cylinder of 2mm with 8MPa pressure after matter group in dried dredging being ground to 100 orders;
5, sample is placed in crucible bottom and puts into tube furnace certain position, at inert component N
2in, under 1 DEG C/min temperature rise rate, be warming up to 550 DEG C, constant temperature 1h, 2h, 3h, then stop heating, Temperature fall to 300 DEG C under protection of inert gas, is cooled to room temperature and namely obtains Carbon foam.
The data of Carbon foam volume density, apparent density, porosity and mean pore size are as following table:
One section of constant temperature time/h | Volume density g/cm 3 | Apparent density g/cm 3 | Porosity % | Mean pore size μm |
1 | 0.2277 | 1.1935 | 80.9205 | 12.4477 |
2 | 0.3189 | 1.6569 | 80.7529 | 17.1159 |
3 | 0.2665 | 0.9989 | 73.3188 | 5.5019 |
Embodiment 3:
Select carbon content C
dafbe 87.0% certain coal sample carry out fragmentation, by the total composition race separating technology of coal, coal sample is separated into four kinds of components, collect dredge in matter component for subsequent use.
1, at 46 DEG C, soxhlet extraction is carried out 6 hours, extracting small molecules wherein by dredging middle matter group dithiocarbonic anhydride solution;
2, at room temperature with acetone, 3 hours are washed to the middle matter group of dredging after extracting;
3, dry 8 hours of matter group in dredging under the air dielectric of temperature 70 C, relative humidity 50%, flow velocity 1.5m/s;
4, suppress into about the thick right cylinder of 1mm with 20MPa pressure after matter group in dried dredging being ground to 200 orders;
5, sample be placed in crucible bottom and put into tube furnace certain position, at inert component N
2in, under 3 DEG C/min temperature rise rate, be warming up to 550 DEG C, constant temperature 1h, then under 1 DEG C/min temperature rise rate, be warming up to 1100 DEG C, constant temperature 0h, 1h, 2h, stop heating, Temperature fall to 300 DEG C under protection of inert gas, is cooled to room temperature and namely obtains Carbon foam.
The data of Carbon foam volume density, apparent density, porosity and mean pore size are as following table:
Two sections of constant temperature time/h | Volume density g/cm 3 | Apparent density g/cm 3 | Porosity % | Mean pore size μm |
0 | 0.2277 | 1.1935 | 80.9205 | 12.4477 |
1 | 0.2456 | 1.3345 | 81.5961 | 6.0164 |
2 | 0.2273 | 1.2452 | 81.7446 | 8.0961 |
Embodiment 4:
Select carbon content C
dafbe 84.50% certain coal sample carry out fragmentation, by the total composition race separating technology of coal, coal sample is separated into four kinds of components, collect dredge in matter component for subsequent use.
1, soxhlet extraction is carried out 15 hours at 98 DEG C, extracting small molecules wherein by dredging middle matter group hexane solution;
2, at room temperature with acetone, 0.5 hour is washed to the middle matter group of dredging after extracting;
3, dry 2 hours of matter group in dredging under the air dielectric of temperature 70 C, relative humidity 40%, flow velocity 0.5m/s;
4, suppress into about the thick right cylinder of 2mm with 15MPa pressure after matter group in dried dredging being ground to 100 orders;
5, sample be placed in crucible bottom and put into tube furnace certain position, at inert component N
2in, under 2 DEG C/min temperature rise rate, be warming up to 550 DEG C, constant temperature 1h, then under 5 DEG C/min temperature rise rate, be warming up to 1100 DEG C, constant temperature 0h, 2h, 3h, stop heating, Temperature fall to 300 DEG C under protection of inert gas, is cooled to room temperature and namely obtains Carbon foam.
The data of Carbon foam volume density, apparent density, porosity and mean pore size are as following table:
Two sections of constant temperature time/h | Volume density g/cm 3 | Apparent density g/cm 3 | Porosity % | Mean pore size μm |
0 | 0.2384 | 1.4453 | 83.5044 | 10.9242 |
2 | 0.2380 | 1.1635 | 79.5473 | 8.7550 |
3 | 0.2935 | 1.2856 | 77.1714 | 2.7302 |
Claims (1)
1. based on a Carbon foam preparation method for middle matter component thin in coal, this preparation method comprises the preparation of dredging middle matter group, and the described preparation of dredging middle matter group has following steps:
1. be that 10-300 object coal sample is placed in extractor by granularity, then add mixed solvent, add-on is the mixed solvent of every gram of coal sample 20-300 milliliter, and mixed solvent is solvent orange 2 A and solvent B is the mixture of 1:0.2 to 1:2 preparation by volume; At room temperature stir 10-300 minute, extraction process completes, and is extracted solidliquid mixture;
2. to step 1. in extraction extraction solidliquid mixture carry out solid-liquid separation, be extracted liquid and extract remainder respectively after solid-liquid separation;
3. to step 2. in extraction liquid process, extraction liquid is put into stripper, strippant is added again in stripper, the amount adding strippant equals between 1:0.1 to 1:2 by extraction liquid than strippant, described ratio is volume ratio, stirred at ambient temperature 5-60 minute, reextraction end of processing, obtains reextraction solidliquid mixture after reextraction process;
4. to step 3. in reextraction solidliquid mixture process, to reextraction solidliquid mixture leave standstill after carry out solid-liquid separation, obtain dredge in matter group;
5. described solvent orange 2 A is: dithiocarbonic anhydride, chloroform, methylene dichloride, benzene, methyl alcohol, phenol, ether; Described solvent B is: METHYLPYRROLIDONE, cyclohexanone, dimethyl sulfoxide (DMSO), tetrahydrofuran (THF), dimethyl formamide, N,N-DIMETHYLACETAMIDE, quadrol, tricresyl phosphate second fat, quinoline, pyridine; Described strippant is: water, normal hexane; In same technological process, solvent orange 2 A, solvent B and strippant must select three kinds of different vehicle substances;
It is characterized in that: further comprising the steps of:
1. thin middle matter group is carried out at 45-100 DEG C the solvent extraction of 1-20 hour by solvent C, extract small-molecule substance wherein; Solvent D is at room temperature used with 20-150mL/ (gmin), the thin middle matter group after extracting to be carried out to the washing of 0.5-4h; Temperature 50-110 DEG C, relative humidity 20-50%, flow velocity 0.5-2m/s air dielectric under to the dry 2-20h of matter group in dredging, in making to dredge, matter group forms the balloon-shaped structure with thin film bubble wall further;
2. by after in dried dredging matter group is ground to 100-200 order, be pressed into the lamellar body of thick about 1-40mm with 5-20MPa pressure, form particulate interspaces and all less thin film bubble wall foam structure of abscess;
3. the sample after compressing tablet is placed in high temperature carbonization furnace, under an inert atmosphere, with constant temperature 1-20h at temperature rise rate 1-5 DEG C/min, carbonization temperature 400-800 DEG C, obtains half Carbon foam; Constant temperature 0-3h under 800-1200 DEG C of carbonization temperature again, then stops heating, under an inert gas below Temperature fall to 300 DEG C, namely obtains Carbon foam after being cooled to room temperature;
4. the specific surface area of Carbon foam that 3. process that measures obtains and aperture and microscopic optical structure etc. also carry out respective table and levy;
5. described solvent C is: chloroform, normal hexane, methyl alcohol, dithiocarbonic anhydride.Described solvent D is: acetone, ethanol, water.
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Cited By (1)
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CN106398736A (en) * | 2016-10-17 | 2017-02-15 | 天津工业大学 | Preparation method of mesophase pitch |
Citations (4)
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US6797251B1 (en) * | 2000-12-13 | 2004-09-28 | West Virginia University | Method of making carbon foam at low pressure |
CN1541939A (en) * | 2003-11-07 | 2004-11-03 | 大连理工大学 | Technical method and schedule for preparation of foam carbon material used asphalt as raw material |
CN101070495A (en) * | 2007-04-30 | 2007-11-14 | 中国矿业大学 | Mild coal-family component separation method based on extraction and back extraction |
CN102431995A (en) * | 2011-10-10 | 2012-05-02 | 中国矿业大学 | Method for preparing carbon foam based on clean coal group component in coal |
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2014
- 2014-10-08 CN CN201410526402.5A patent/CN104310374B/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6797251B1 (en) * | 2000-12-13 | 2004-09-28 | West Virginia University | Method of making carbon foam at low pressure |
CN1541939A (en) * | 2003-11-07 | 2004-11-03 | 大连理工大学 | Technical method and schedule for preparation of foam carbon material used asphalt as raw material |
CN101070495A (en) * | 2007-04-30 | 2007-11-14 | 中国矿业大学 | Mild coal-family component separation method based on extraction and back extraction |
CN102431995A (en) * | 2011-10-10 | 2012-05-02 | 中国矿业大学 | Method for preparing carbon foam based on clean coal group component in coal |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106398736A (en) * | 2016-10-17 | 2017-02-15 | 天津工业大学 | Preparation method of mesophase pitch |
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