CN115947334B - A high-density charcoal and a method for rapidly preparing the charcoal under pressure - Google Patents
A high-density charcoal and a method for rapidly preparing the charcoal under pressure Download PDFInfo
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- CN115947334B CN115947334B CN202211429980.8A CN202211429980A CN115947334B CN 115947334 B CN115947334 B CN 115947334B CN 202211429980 A CN202211429980 A CN 202211429980A CN 115947334 B CN115947334 B CN 115947334B
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- 239000003610 charcoal Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 132
- 229910052742 iron Inorganic materials 0.000 claims abstract description 66
- 238000000197 pyrolysis Methods 0.000 claims abstract description 34
- 239000002023 wood Substances 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims description 43
- 238000001816 cooling Methods 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 32
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 239000011148 porous material Substances 0.000 abstract description 7
- 239000012263 liquid product Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000004134 energy conservation Methods 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 239000012071 phase Substances 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 description 16
- 239000002296 pyrolytic carbon Substances 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000003990 capacitor Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Solid Fuels And Fuel-Associated Substances (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The invention discloses a method for preparing high-density charcoal and pressurizing quickly, placing dry wood raw material in an iron tank, placing load above the iron tank, low-temperature pyrolysis is carried out under a certain pressure within a certain temperature range, so that charcoal slowly releases pyrolysis gas-phase products and liquid-phase products and volume shrinkage. After the low-temperature pyrolysis process is finished, the iron tank, the charcoal and the external load are transferred to a box-type furnace together, the pyrolysis to charcoal process is further finished under the protective atmosphere condition, and finally the high-density charcoal product is obtained. Aiming at the problems that the charcoal structure has more pores and cracks caused by rapid escape of charcoal pyrolysis gas-liquid products, the improvement of charcoal density is affected, the production time of the existing high-density charcoal is extremely long, and the like, the pressurizing pyrolysis method is innovatively adopted, so that the generation of the pores and the cracks is avoided, the density of the charcoal is greatly improved, the preparation time is obviously shortened compared with the traditional process flow, the energy conservation and emission reduction can be realized, the production efficiency is improved, the production cost is reduced, and the method has good application prospect.
Description
Technical Field
The invention belongs to the technical field of preparation and application of carbonaceous materials, and mainly relates to a method for rapidly preparing high-density charcoal under pressure.
Background
Charcoal is a black solid phase product obtained by pyrolysis of wood raw materials. The cell cavity structure of the wood is reserved in the conventional pyrolysis process, and a large amount of gas and liquid are generated to escape, so that the pyrolytic carbon has more pores and cracks, and the density of the charcoal is usually only 0.4-0.6 g/cm 3. With the current technological development, there is an increasing demand for high density charcoal, for example, when activated charcoal is further activated to obtain activated charcoal for use in capacitors, more charcoal can be filled per unit volume, thereby improving capacitor performance or effectively reducing capacitor volume. The production of traditional high-density charcoal (density higher than 1.0g/cm 3) often requires extremely slow heating rate to ensure slow escape of pyrolysis products such as gas and the like, and slow shrinkage of the charcoal framework structure, thereby obtaining a compact product. The process often needs more than ten days and even tens of days, and has lower production efficiency and high energy consumption. Therefore, reducing the production time of high density charcoal is of great importance for further broadening the application market.
Aiming at the two problems that the density of the pyrolytic carbon of the wood raw material obtained by the conventional method is low and the production time of high-density charcoal is extremely long, the invention applies pressure at 160-260 ℃ which is caused by the escape of a large amount of gas-liquid products to destroy the cell cavity structure and the pores and cracks generated by the escape of the pyrolytic products, thereby greatly improving the density of the obtained charcoal. Meanwhile, the method can shorten the preparation time of charcoal to within 72 hours, obviously reduce the production energy consumption and cost and improve the production efficiency.
Disclosure of Invention
The invention aims to provide a method for rapidly preparing high-density charcoal under pressure.
The invention provides high-density charcoal, which enables a dry wood raw material to simultaneously generate pyrolysis reaction and volume shrinkage under a certain pressure condition, and finally obtains the high-density charcoal with the density exceeding 1g/cm 3 after the pyrolysis reaction.
The method for rapidly preparing the high-density charcoal under pressure comprises the following steps:
firstly, drying and preprocessing a wood raw material to constant weight;
Secondly, placing the pretreated wood raw material in an iron tank, placing a load above the iron tank to provide pressure, and performing heat treatment on the wood raw material under the pressure to perform low-temperature pyrolysis reaction;
and thirdly, cooling after the heat treatment is finished, transferring the iron tank loaded with the wood and the additional load into a box-type atmosphere furnace, slowly heating under the protection of nitrogen to further complete the pyrolysis to form carbon, and cooling to obtain a final product.
The drying pretreatment temperature is 105-120 ℃.
The pyrolysis reaction temperature range is 160-260 ℃ and the reaction time is 6-10 h.
The pressure range applied by the load is 4-10 MPa.
The reaction temperature range of pyrolysis to charcoal is 400-600 ℃, the heating rate is 2-10 ℃ per minute, and the reaction time is 6-10 h.
The beneficial effects are that:
1. the pyrolysis pressure is increased under the low-temperature condition (160-260 ℃), and the solid-phase product can be extruded while the gas-liquid product slowly escapes by adopting a slow temperature rising method (1-2 ℃) so as to effectively reduce cracks and pores generated by escape of the gas product and destroy the cell cavity structure, so that the density of the solid-phase product is obviously improved compared with that of the product obtained under the non-pressure condition.
2. After pyrolysis at low temperature, the product has a certain density, and high-density pyrolytic carbon can be obtained after pyrolysis at a higher temperature. The method can obtain the target product within 72 hours, and compared with the prior art (more than ten days and even tens of days), the consumption is greatly shortened, and the method is very beneficial to energy conservation, emission reduction and production cost reduction.
Drawings
Fig. 1 is a schematic diagram of a low-temperature pyrolysis stage device, wherein 1 is a press, 2 is an iron block, 3 is a heating belt, 4 is a wood block raw material, and 5 is an iron tank.
FIG. 2 shows the density of the pressurized pyrolytic carbon compared with that of the unpressurized pyrolytic carbon, a is that of the unpressurized pyrolytic carbon and floats on the water surface, and b is that of the pressurized pyrolytic carbon and sinks on the water bottom.
Fig. 3 is an SEM photograph of pressurized pyrolytic carbon and non-pressurized pyrolytic carbon, a is non-pressurized pyrolytic carbon, and b is an SEM photograph of pressurized pyrolytic carbon.
Detailed Description
A method for rapidly preparing high-density charcoal under pressure comprises the following specific steps:
(1) The wood raw material was divided into blocks of suitable size and dried to constant weight at 105 ℃. Cooling, weighing, placing in an iron tank, and placing an iron block with the size similar to that of the iron tank above to provide a certain pressure. And (3) winding a heating belt outside the iron tank, placing the iron tank in a small press, and carrying out low-temperature pyrolysis in a certain temperature range under certain pressure to slowly release pyrolysis gas-phase products and liquid-phase products from the wood raw materials, and generating remarkable volume shrinkage to obtain the preheated charcoal.
(2) After the low-temperature pyrolysis process is finished, the iron tank, the pre-pyrolysis charcoal and the externally added iron blocks are transferred to a box furnace together, the pyrolysis charcoal forming process is further finished under the protective atmosphere condition, and finally the high-density charcoal product is obtained.
The method for preparing the high-density charcoal rapidly under pressure comprises the steps of firstly carrying out drying pretreatment on wood raw materials, then enabling the wood raw materials to simultaneously carry out pyrolysis reaction and remarkable volume shrinkage under a certain pressure condition, and finally obtaining the high-density charcoal with the density exceeding 1g/cm 3 after about 8 hours.
The drying treatment temperature is 105-120 ℃.
The low-temperature pyrolysis reaction temperature range is 160-260 ℃ and the reaction time is 6-10 h.
The applied pressure ranges from 4 MPa to 10MPa.
The pyrolysis carbonization reaction temperature range is 400-600 ℃, the heating rate is 1-10 ℃ per minute, and the reaction time is 6-10 hours.
Aiming at the problems that the charcoal structure has more pores and cracks caused by rapid escape of charcoal pyrolysis gas-liquid products, the improvement of charcoal density is affected, the production time of the existing high-density charcoal is extremely long, and the like, the pressurizing pyrolysis method is innovatively adopted, so that the generation of the pores and the cracks is avoided, the density of the charcoal is greatly improved, the preparation time is obviously shortened compared with the traditional process flow, the energy conservation and emission reduction can be realized, the production efficiency is improved, the production cost is reduced, and the method has good application prospect.
Example 1:
The raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 4MPa, and the temperature is raised to 160 ℃ and maintained for 6 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 400℃at a rate of 2℃/min for 6h. The density of the charcoal product obtained was 0.97g/cm 3.
Example 2:
the raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 6MPa, and the temperature is raised to 180 ℃ and maintained for 8 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 400℃at a rate of 2℃/min for 8h. The density of the charcoal product obtained was 1.03g/cm 3.
Example 3:
The raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 6MPa, and the temperature is raised to 180 ℃ and maintained for 8 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 500℃at a rate of 1℃/min for 10h. The density of the charcoal product obtained was 1.06g/cm 3.
Example 4:
The raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 6MPa, and the temperature is raised to 200 ℃ and maintained for 10 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 500℃at a rate of 2℃/min for 10h. The density of the charcoal product obtained was 1.10g/cm 3.
Example 5:
The raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 6MPa, and the temperature is raised to 220 ℃ and maintained for 10 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 600℃at a rate of 1℃/min for 10h. The density of the charcoal product obtained was 1.14g/cm 3.
Example 6:
The raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 8MPa, and the temperature is raised to 220 ℃ and maintained for 10 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 600℃at a rate of 2℃/min for 10h. The density of the charcoal product obtained was 1.12g/cm 3.
Example 7:
The raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 10MPa, and the temperature is raised to 220 ℃ and maintained for 6 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 500℃at a rate of 5℃/min for 10h. The density of the charcoal product obtained was 1.16g/cm 3. .
Example 8:
The raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 4MPa, and the temperature is raised to 240 ℃ and maintained for 8 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 500℃at a rate of 2℃/min for 8h. The density of the charcoal product obtained was 1.14g/cm 3.
Example 9:
The raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 4MPa, and the temperature is raised to 240 ℃ and maintained for 10 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 600℃at a rate of 2℃/min for 8h. The charcoal product density was 1.18g/cm 3.
Example 10:
The raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 6MPa, and the temperature is raised to 240 ℃ and maintained for 10 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 500℃at a rate of 5℃/min for 10h. The density of the charcoal product obtained was 1.10g/cm 3.
Example 11:
The raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 8MPa, and the temperature is raised to 240 ℃ and maintained for 8 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 600℃at a rate of 5℃/min for 10h. The density of the charcoal product obtained was 1.08g/cm 3.
Example 12:
The raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 4MPa, and the temperature is raised to 260 ℃ and maintained for 10 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 600℃at a rate of 5℃/min for 10h. The density of the charcoal product obtained was 1.05g/cm 3.
Example 13:
The raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 6MPa, and the temperature is raised to 260 ℃ and maintained for 8 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 600℃at a rate of 10℃/min for 10h. The density of the charcoal product obtained was 1.10g/cm 3.
Example 14:
the raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 8MPa, and the temperature is raised to 260 ℃ and maintained for 10 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 600℃at a rate of 5℃/min for 10h. The density of the charcoal product obtained was 1.17g/cm 3.
Example 15:
the raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 10MPa, and the temperature is raised to 260 ℃ and maintained for 10 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 600℃at a rate of 5℃/min for 10h. The density of the charcoal product obtained was 1.14g/cm 3.
Example 16:
the raw material wood blocks are dried at 105 ℃ and then placed in an iron tank, the iron blocks are added and then placed in a press, and a heating belt is wound on the outer ring of the iron tank. The pressure is regulated to 10MPa, and the temperature is raised to 260 ℃ and maintained for 10 hours. After cooling, the heating belt was unwound, transferred to a box-type resistance furnace, charged with N 2, and raised to 600℃at a rate of 10℃/min for 10h. The density of the charcoal product obtained was 1.09g/cm 3.
Claims (4)
1. A method of pressurizing a rapid high density charcoal, comprising the steps of:
firstly, drying and preprocessing a wood raw material to constant weight;
Secondly, placing the pretreated wood raw material in an iron tank, placing a load above the iron tank to provide pressure, and performing heat treatment on the wood raw material under the pressure to perform low-temperature pyrolysis reaction, wherein the pressure range applied by the load is 4-10 MPa, and the low-temperature pyrolysis reaction temperature range is 160-260 ℃;
and thirdly, cooling after the heat treatment is finished, transferring the iron tank loaded with the wood and the additional load into a box-type atmosphere furnace, slowly heating under the protection of nitrogen to further complete the pyrolysis to form charcoal, and cooling to obtain a final product, namely the high-density charcoal with the density exceeding 1 g/cm 3.
2. The method of claim 1, wherein the drying pretreatment temperature is 105-120 ℃.
3. The method of claim 1, wherein the low temperature pyrolysis reaction time is 6 to 10 hours.
4. The method of claim 1, wherein the pyrolysis to char is carried out at a reaction temperature in the range of 400 to 600 ℃, a temperature rise rate of 2 to 10 ℃ per minute, and a reaction time of 6 to 10 hours.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4005107B1 (en) * | 2006-09-25 | 2007-11-07 | ジスコム株式会社 | Hard white coal and method for producing the same |
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| JP3759372B2 (en) * | 1999-09-08 | 2006-03-22 | 東京瓦斯株式会社 | Method for producing activated carbon |
| RU2217468C1 (en) * | 2002-04-27 | 2003-11-27 | Данилов Владимир Николаевич | Method of production of charcoal and device for realization of this method |
| FR2931162B1 (en) * | 2008-05-13 | 2010-08-20 | Carbonex | CARBONIZATION METHOD AND DEVICE |
| KR100912663B1 (en) * | 2008-09-05 | 2009-08-17 | 주식회사 우일 이알에스 | Molded charcoal using palm keratin and its manufacturing method |
| WO2010128650A2 (en) * | 2009-05-06 | 2010-11-11 | 株式会社インキュベーション・アライアンス | Carbon material and manufacturing method therefor |
| KR101220325B1 (en) * | 2010-12-22 | 2013-01-09 | 한국화학연구원 | Preparation of high density and high porous activated carbon |
| CN106276898A (en) * | 2016-08-12 | 2017-01-04 | 南京林大活性炭有限公司 | A kind of method utilizing urban landscaping rubbish to prepare agglomerated activated carbon |
| CN112058222B (en) * | 2020-08-18 | 2021-12-03 | 大连理工大学 | Device and method for preparing in-situ formed high-specific-surface-area biochar |
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| JP4005107B1 (en) * | 2006-09-25 | 2007-11-07 | ジスコム株式会社 | Hard white coal and method for producing the same |
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