CN115367728A - Non-porous formed carbon material and preparation method thereof - Google Patents
Non-porous formed carbon material and preparation method thereof Download PDFInfo
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- CN115367728A CN115367728A CN202110549077.4A CN202110549077A CN115367728A CN 115367728 A CN115367728 A CN 115367728A CN 202110549077 A CN202110549077 A CN 202110549077A CN 115367728 A CN115367728 A CN 115367728A
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 235000013312 flour Nutrition 0.000 claims abstract description 44
- 239000002245 particle Substances 0.000 claims abstract description 27
- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 24
- 235000009566 rice Nutrition 0.000 claims abstract description 24
- 241000209140 Triticum Species 0.000 claims abstract description 20
- 235000021307 Triticum Nutrition 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000004898 kneading Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000010025 steaming Methods 0.000 claims abstract description 9
- 239000008187 granular material Substances 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 244000275012 Sesbania cannabina Species 0.000 claims abstract 3
- 238000000034 method Methods 0.000 claims description 30
- 241000209094 Oryza Species 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 229920000945 Amylopectin Polymers 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 102000004169 proteins and genes Human genes 0.000 claims description 5
- 108090000623 proteins and genes Proteins 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 4
- 230000000391 smoking effect Effects 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 2
- 240000007594 Oryza sativa Species 0.000 abstract 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 241000219782 Sesbania Species 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000003223 protective agent Substances 0.000 description 3
- 229920002472 Starch Polymers 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 238000004438 BET method Methods 0.000 description 1
- 241000219793 Trifolium Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000003958 fumigation Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Classifications
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Cereal-Derived Products (AREA)
Abstract
The invention provides a non-porous formed carbon material and a preparation method thereof. The non-porous formed carbon material has the following properties: has regular particle shape, the particles contain 5-50 μm through channels, and the specific surface area is less than 25m 2 (iv) the granules have a crush strength of 8-20N/mm. The preparation method comprises the following steps: (1) Pasting glutinous rice flour and water, then uniformly mixing the pasted material with baking powder, wheat flour and sesbania powder, and kneading to form a plastic body; (2) And (3) after the plastic body is sealed and stored for a certain time, kneading the plastic body again, then extruding and molding, steaming and fumigating the molded body under a sealed condition, and then drying and roasting to obtain the molded carbon material. The non-porous formed carbon material has the advantages of low specific surface area, large-size through channels in the granules, high crushing strength of the granules, high pressure bearing capacity, low chemical action strength with blocked impurities, and simple recovery, utilization or treatment of waste agents, and is an environment-friendly material.
Description
Technical Field
The invention belongs to the field of non-metallic functional materials, and relates to a non-porous formed carbon material and a preparation method thereof.
Background
In some special fields, such as the field of fixed bed residue hydrogenation, the protective agent loaded on the upper layer of the series of catalysts for intercepting the physical impurities in the feed generally uses an inert ceramic filter material, which has a very low specific surface area and large through holes. However, the ceramic filter material has high density, heavy weight and inconvenient assembly and disassembly, and meanwhile, the used waste filter material has high treatment difficulty and difficult recycling, and can bring serious environmental pollution if being directly buried.
CN201720249177.4 provides a special residual oil hydrogenation protective agent which has large specific surface area and high stacking void ratio and can effectively improve the pollutant interception and filtration effect. The protective agent has large specific surface area, has chemical reaction activity after loading active metal, but can not completely replace the interception effect of filter materials on feed impurities, and the used carrier is a ceramic component, so that the waste agent is difficult to recover, utilize and treat, and the environmental protection problem is prominent.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a non-porous formed carbon material and a preparation method thereof. The non-porous formed carbon material has specific particle shape, low specific surface area, large-size through passages in the particles, high crushing strength of the particles, high pressure bearing capacity, low chemical action strength with blocked impurities, and simple recovery, utilization or treatment of waste agents, and is an environment-friendly material. As used herein, "non-porous" means having a specific surface area of not more than 25m according to the BET specific surface area test method 2 /g。
The non-porous formed carbon material of the invention has the following properties: has regular particle shape, the particles contain 5-50 μm through channels, and the specific surface area is less than 25m 2 G, more preferably less than 15m 2 (iv) the granules have a crushing strength of 8 to 20N/mm.
The preparation method of the non-porous formed carbon material comprises the following steps:
(1) Pasting glutinous rice flour and water, then uniformly mixing the pasted material with baking powder, wheat flour and sesbania powder, and kneading to form a plastic body;
(2) And (3) after the plastic body is sealed and stored for a certain time, kneading the plastic body again, then extruding and molding, steaming and smoking the molded object under a sealed condition, and then drying and roasting to obtain the molded carbon material.
In the method of the invention, the baking powder in the step (1) is a commercial product. The amount of the baking powder is 1-5% of the total amount of the glutinous rice flour and the wheat flour by mass.
In the method, the glutinous rice flour in the step (1) accounts for 10-30% of the total amount of the wheat flour and the glutinous rice flour.
In the method of the invention, the mass content of the protein in the wheat flour in the step (1) is 5-15 percent,
in the method, the amylopectin content in the glutinous rice flour in the step (1) is not less than 70% by mass.
In the method, the amount of the water used in the step (1) is 20-60% of the total amount of the wheat flour and the glutinous rice flour by mass.
In the method, the sesbania powder in the step (1) accounts for 1-5% of the amount of the wheat flour and the glutinous rice flour by mass.
In the method, the gelatinization conditions of the glutinous rice flour in the step (1) are as follows: adding glutinous rice flour into 1.5-5 times of water, heating to 58-100 deg.C under stirring, and holding for 10-60 min.
In the method, the temperature for sealing and storing the plastic body in the step (1) is 25-45 ℃, and the storage time is 0.1-2 hours. The sealed preservation generally adopts a solid sealed container or other modes which can prevent the plastic body from exchanging substances with the outside, such as a dryer, a sealed bag package and the like.
In the method, the re-kneading time in the step (2) is 15-60 minutes, the ambient temperature is room temperature, and the room temperature is generally 15-35 ℃.
In the method, the shape of the extruded and molded particles in the step (2) is cylindrical, clover and other shapes suitable for being extruded by a bar extruder.
In the method, the steaming and smoking treatment in the step (2) is carried out in a closed pressure-resistant container, water does not directly contact with the formed product, the temperature is 100-200 ℃, the time is 0.5-5 hours, and the pressure is the autogenous pressure under the closed condition.
In the method of the present invention, the drying condition in the step (3) is drying at 60-200 ℃ for 1-48 hours, preferably drying at 100-150 ℃ for 3-24 hours.
In the method of the invention, the roasting conditions in the step (3) are as follows: keeping the temperature of 250-350 ℃ for 2-5 hours under the inert atmosphere, and then heating to 650-950 ℃ for roasting for 1-5 hours; the inert atmosphere is one or more of nitrogen, argon or helium.
The baking powder used in the invention reacts with water to generate carbon dioxide, the protein in the wheat flour has ductility and can form a three-dimensional network to seal the carbon dioxide in the plastic body, and the carbon dioxide flows in the plastic body in series to form three-dimensional through holes. The wheat flour particles absorb water and swell under the action of water, and form a three-dimensional staggered structure with protein. The three-dimensional structure is more stable and compact through two times of kneading. The starch and protein can be hardened by the fumigation hydrothermal treatment, so that the shape of the plastic body is fixed. The mixed glutinous rice flour generally has high proportion of starch with branched structure, is equivalent to a binder after pasting, can further enhance the strength of a formed body, and can be converted into carbon in the carbonization process.
The carbon material has the advantages of low specific surface area, large-size through pore passages, high crushing strength, low chemical bonding strength between the material and blocked impurities, convenient acid washing regeneration or direct incineration treatment, and environmental pollution caused by direct landfill can be avoided.
Drawings
FIG. 1 is a photograph of an optical camera of the non-porous shaped carbon material prepared in example 1.
FIG. 2 is a scanning electron micrograph of a non-porous shaped carbon material prepared according to example 1.
Detailed Description
The present invention will be described in further detail with reference to examples. The particle size is measured by a vernier caliper, the mechanical strength is measured by a DL3 type strength instrument, the microscopic morphology and the macroporous morphology are observed and measured by a scanning electron microscope, and the specific surface area is measured by a BET method.
Example 1
60 g of glutinous rice flour (with the mass content of amylopectin being 80%) and 150 g of water are heated to 80 ℃ for gelatinization and kept for 30 minutes, 6 g of baking powder, 6 g of sesbania powder and 500 g of wheat flour (with the protein content being 6.7%) are uniformly mixed, and the mixture is kneaded into a plastic body (a proper amount of supplementary materials can be provided when the water content is insufficient, and a proper amount of wheat flour can be added when the water content is excessive). And (2) sealing and storing for 2 hours at 35 ℃, kneading the plastic body for 45 minutes again, extruding the plastic body into a cylindrical strip, performing hydrothermal steaming and fumigating for 1.5 hours at 120 ℃, cooling, taking out, drying for 12 hours at 120 ℃, putting the cylindrical strip into a tubular furnace filled with nitrogen for protection, heating to 250 ℃, keeping for 5 hours, heating to 850 ℃, keeping for 3 hours, and cooling to obtain the low specific surface molded carbon particles.
The diameter of the obtained cylindrical carbon particles is 1.5mm. The specific surface area is 10.7m 2 In terms of/g, the particles can therefore be considered to be of low specific surface material. The crushing strength is 18N/mm, and the particles are observed by a scanning electron microscope to have large-size through channels of 5-47 mu m.
Example 2
100 g of glutinous rice flour (with the amylopectin content of 80%) and 200 g of water are heated to 90 ℃ for gelatinization and kept for 50 minutes, 10 g of baking powder, 6 g of sesbania powder and 500 g of wheat flour (with the protein content of 10%) are uniformly mixed and kneaded into a plastic body. And (2) sealing and storing for 2 hours at 35 ℃, kneading the plastic body for 60 minutes again, extruding the plastic body into a cylindrical strip, performing hydrothermal steaming and fumigating for 1.5 hours at 150 ℃, cooling, taking out, drying for 12 hours at 120 ℃, putting the cylindrical strip into a tubular furnace filled with nitrogen for protection, heating to 300 ℃ for 5 hours, heating to 850 ℃ for 3 hours, and cooling to obtain the low-specific-surface-area molded carbon particle.
The diameter of the obtained cylindrical carbon particles is 2mm. Proportion tableThe area is 14.7m 2 (iv) g. The crushing strength is 19N/mm, and the particles are observed by a scanning electron microscope to have large-size through channels of 12-45 mu m.
Example 3
150 g of glutinous rice flour (with the amylopectin content of 80%) and 250 g of water are heated to 85 ℃ for gelatinization and kept for 30 minutes, 7 g of baking powder and 500 g of wheat flour (with the protein content of 10%) are uniformly mixed and kneaded into a plastic body. Sealing and storing for 1 hour at 35 ℃, kneading the plastic body for 30 minutes again, extruding the plastic body into cylindrical strips, carrying out hydrothermal steaming and smoking for 2 hours at 150 ℃, taking out after cooling, drying for 12 hours at 120 ℃, putting the cylindrical strips into a tubular furnace filled with nitrogen for protection, heating to 300 ℃ for 5 hours, heating to 900 ℃ for 3 hours, and cooling to obtain the low specific surface area molding carbon particles.
The diameter of the obtained cylindrical carbon particles is 2.5mm. The specific surface area is 9.6m 2 (iv) g, crushing strength of 14N/mm, and observation by a scanning electron microscope revealed that the particles had large-sized through channels of 21 to 49 μm.
Comparative example 1
The method is the same as that in example 1, except that the amylopectin content in glutinous rice flour is 50 wt%, and other conditions are kept unchanged. The specific surface area of the obtained cylindrical carbon particles is 12.5m 2 G, but the crush strength of the material was reduced to 9.2N/mm.
Comparative example 2
The same as in example 1, except that the treated wheat flour was selected and its protein content was 2%, the other conditions were kept constant. The specific surface area of the obtained carbon particles is 13.2m 2 The granules are considered to be low specific surface materials with a crushing strength of 11N/mm, but the hardening effect is not good due to the reduced protein content, and it is difficult to form relatively regular pillars in the final shaped granules.
Comparative example 3
The same as example 1 except that the steaming treatment was not performed. The final shaped particles are difficult to form into more regular cylinders.
Comparative example 4
The same procedure as in example 1 was repeated except that the composition was sealed and stored, and then was directly extruded. The final formed particles are loose, and the crushing strength is reduced to 7N/mm.
Comparative example 5
As in example 1, only one stage of calcination, i.e., direct heating to 850 ℃ for 3 hours, was used for calcination. The material has low carbon conversion rate, still contains polymerized organic matters, and finally has loose formed particles and the crushing strength reduced to 3N/mm.
Claims (15)
1. A non-porous shaped carbon material characterized by the following properties: has regular particle shape, the particles contain 5-50 μm through channels, and the specific surface area is less than 25m 2 A further preferred value is less than 15 m/g 2 (iv) the granules have a crushing strength of 8 to 20N/mm.
2. A method for preparing the non-porous shaped carbon material according to claim 1, comprising the steps of: (1) Pasting glutinous rice flour and water, then uniformly mixing the pasted material with baking powder, wheat flour and sesbania powder, and kneading to form a plastic body; (2) And (3) after the plastic body is sealed and stored for a certain time, kneading the plastic body again, then extruding and molding, steaming and smoking the molded object under a sealed condition, and then drying and roasting to obtain the non-porous molded carbon material.
3. The method of claim 2, wherein: the baking powder in the step (1) is 1-5% of the total amount of the glutinous rice flour and the wheat flour by mass.
4. The method of claim 2, wherein: the glutinous rice flour in the step (1) accounts for 10-30 wt% of the total amount of the wheat flour and the glutinous rice flour.
5. The method of claim 2, wherein: the mass content of the protein in the wheat flour in the step (1) is 5wt% -15wt%.
6. The method of claim 2, wherein: the mass content of the amylopectin in the glutinous rice flour in the step (1) is not less than 70wt%.
7. The method of claim 2, wherein: the amount of the water used in the step (1) is 20-60 wt% of the total amount of the wheat flour and the glutinous rice flour by mass.
8. The method of claim 2, wherein: the sesbania powder in the step (1) accounts for 1-5 wt% of the wheat flour and the glutinous rice flour by mass.
9. The method of claim 2, wherein: the gelatinization conditions of the glutinous rice flour in the step (1) are as follows: adding glutinous rice flour into 1.5-5 times of water, heating to 58-100 deg.C under stirring, and holding for 10-60 min.
10. The method of claim 2, wherein: the temperature for sealing and storing the plastic body in the step (1) is 25-45 ℃, and the storage time is 0.1-2 hours.
11. The method of claim 2, wherein: the time for re-kneading in the step (2) is 15-60 minutes.
12. The method of claim 2, wherein: the shape of the granules extruded and molded in the step (2) is cylindrical, clover-shaped or other shapes suitable for being extruded by a strip extruder.
13. The method of claim 2, wherein: the steaming treatment in the step (2) is carried out in a closed pressure-resistant container, water does not directly contact with the formed product, the temperature is 100-200 ℃, the time is 0.5-5 hours, and the pressure is the autogenous pressure under the closed condition.
14. The method of claim 2, wherein: the drying condition in the step (3) is drying for 1-48 hours at 60-200 ℃.
15. The method of claim 2, wherein: the roasting conditions in the step (3) are as follows: keeping the temperature of 250-350 ℃ for 2-5 hours under inert atmosphere, and then heating to 650-950 ℃ for roasting for 1-5 hours; the inert atmosphere is one or more of nitrogen, argon or helium.
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|---|---|---|---|---|
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2021
- 2021-05-20 CN CN202110549077.4A patent/CN115367728B/en active Active
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| Title |
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Effective date of registration: 20231124 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Applicant after: CHINA PETROLEUM & CHEMICAL Corp. Applicant after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Applicant before: CHINA PETROLEUM & CHEMICAL Corp. Applicant before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |
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