CN114715877A - High-specific-surface-area porous carbon material and preparation method thereof - Google Patents
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Abstract
The invention relates to the technical field of carbon material preparation, and particularly discloses a porous carbon material with a high specific surface area and a preparation method thereof. The preparation method of the porous carbon material with high specific surface area comprises the following steps: (1) mixing polypropylene with a catalyst and a thermal decomposition inorganic substance, and then performing melt extrusion granulation by a double screw extruder to obtain composite polypropylene particles; (2) and (2) placing the composite polypropylene particles prepared in the step (1) into a heating device, heating to 600-900 ℃, reacting for 1-3 h, and washing a product after the reaction is finished to obtain the porous carbon material with the high specific surface area. The method has simple preparation process and lower requirement on equipment, and the prepared porous carbon material has higher specific surface area.
Description
Technical Field
The invention relates to the technical field of carbon material preparation, in particular to a porous carbon material with a high specific surface area and a preparation method thereof.
Background
The carbon nano tube is a one-dimensional nano material and has a plurality of abnormal mechanical, electrical and chemical properties; in recent years, the extensive application prospect of the carbon nano-tube and the nano-material is continuously shown along with the research of the carbon nano-tube and the nano-material.
Chinese patent 200410011337.9 discloses a method for synthesizing carbon nanotubes by burning polyolefin; the method comprises the following steps: polyolefin, a compatibilizer, organic modified montmorillonite and a nickel-loaded catalyst are melted and mixed in an internal mixer or a double-screw extruder according to a certain composition ratio, and then the mixture is placed into a crucible and heated by gas flame, so that the mixture is combusted at 660-850 ℃ to prepare the carbon nano tube. The method can be completed by adopting common processing equipment, and has the advantages of simple production method and lower cost. However, the carbon nano tube prepared by the method has smaller specific surface area.
Polypropylene is a polymer obtained by addition polymerization of propylene, and is widely used in the fields of fiber products such as clothing and blankets, medical instruments, automobiles, bicycles, parts, conveying pipelines, chemical containers, food and medicine packaging, and the like. As the amount of polypropylene used increases, the processing pressure of the waste polypropylene plastic also increases. Therefore, the method for preparing the carbon material by using the polypropylene as the raw material, particularly the method for preparing the carbon material with high specific surface area has important application value.
Disclosure of Invention
In order to overcome at least one technical problem in the prior art, the invention provides a porous carbon material with high specific surface area and a preparation method thereof.
The technical scheme of the invention is as follows: a preparation method of a high specific surface area porous carbon material comprises the following steps:
(1) mixing polypropylene with a catalyst and a thermal decomposition inorganic substance, and then carrying out melt extrusion granulation by a double-screw extruder to obtain composite polypropylene particles;
(2) and (2) placing the composite polypropylene particles prepared in the step (1) into a heating device, heating to 600-900 ℃, reacting for 1-3 h, and washing a product after the reaction is finished to obtain the porous carbon material with the high specific surface area.
The porous carbon material is successfully prepared by using the polypropylene as a raw material and adopting the preparation method, and the preparation method is simple in preparation process and low in equipment requirement.
Preferably, the weight ratio of the polypropylene to the catalyst and the thermally decomposed inorganic substance in the step (1) is 100:1 to 10:10 to 20.
Most preferably, the weight ratio of polypropylene to catalyst and thermally decomposed inorganic substance in step (1) is 100:5: 15.
Preferably, the catalyst is nickel carbonate.
Preferably, the thermally decomposable inorganic substance is composed of sodium bicarbonate and calcium bicarbonate.
Preferably, the weight ratio of the sodium bicarbonate to the calcium bicarbonate is 1: 1-3.
Most preferably, the weight ratio of sodium bicarbonate to calcium bicarbonate is 1: 2.
In the process of preparing the porous carbon material by using polypropylene as a raw material and adopting the method, the specific surface area of the prepared porous carbon material can be improved by adding the thermal decomposition inorganic substance. The inventors have surprisingly found in further studies that the specific surface area of the porous carbon material prepared using a thermally decomposed inorganic substance consisting of sodium bicarbonate and calcium bicarbonate is significantly higher than that of the porous carbon material prepared using sodium bicarbonate alone or calcium bicarbonate alone.
Preferably, a dispersant is also added in step (1).
Preferably, the weight ratio of the polypropylene to the catalyst, the thermally decomposed inorganic substance and the dispersant is 100: 1-10: 10-20: 5-10.
Most preferably, the weight ratio of polypropylene to catalyst, thermally decomposed inorganic substance and dispersant is 100:5:15: 7.
Preferably, the dispersant consists of sorbitan laurate and pentaerythritol stearate.
Preferably, the weight ratio of the sorbitan laurate to the pentaerythritol stearate is 2-3: 1.
The inventor further researches and discovers that the porous carbon material can be prepared by the method; but the specific surface area of the prepared porous carbon material is still not high; in order to further increase the surface area of the porous carbon material prepared by the above method, the inventors surprisingly found during a number of tests that: in the preparation process, a dispersing agent consisting of sorbitan laurate and pentaerythritol stearate is further added, so that the specific surface area of the prepared carbon material can be further greatly increased. The inventors here need to emphasize that the choice of the dispersing agent is critical and that the choice of the dispersing agent, not at will, can further increase the specific surface area of the carbon material produced to a great extent; studies have shown that the use of other dispersants alone or in combination does not greatly increase the specific surface area of the carbon material produced.
Has the advantages that: the invention provides a brand-new preparation method of a porous carbon material with high specific surface area, the preparation method is simple in preparation process and low in equipment requirement, and the prepared porous carbon material has high specific surface area.
Detailed Description
The present invention is further illustrated below with reference to examples, which are not intended to limit the invention in any way.
The polypropylene used in the following examples is a petrochemical polypropylene having a designation of B8101.
Example 1 preparation of high specific surface area porous carbon Material
(1) Mixing polypropylene with a catalyst and a thermal decomposition inorganic substance, and then carrying out melt extrusion granulation by a double-screw extruder to obtain composite polypropylene particles;
(2) and (2) placing the composite polypropylene particles prepared in the step (1) into a crucible, heating the crucible to 800 ℃, carrying out combustion reaction for 2 hours, washing a product after the reaction is finished, and drying the product to obtain the porous carbon material with the high specific surface area.
In the step (1), the weight ratio of the polypropylene to the catalyst to the thermal decomposition inorganic matter is 100:5: 15; the catalyst is nickel carbonate; the thermal decomposition inorganic substance consists of sodium bicarbonate and calcium bicarbonate with the weight ratio of 1: 2.
Example 2 preparation of high specific surface area porous carbon Material
(1) Mixing polypropylene with a catalyst, a thermal decomposition inorganic substance and a dispersing agent, and then carrying out melt extrusion granulation by a double-screw extruder to obtain composite polypropylene particles;
(2) and (2) placing the composite polypropylene particles prepared in the step (1) into a crucible, heating the crucible to 800 ℃, carrying out combustion reaction for 2 hours, washing a product after the reaction is finished, and drying the product to obtain the porous carbon material with the high specific surface area.
In the step (1), the weight ratio of the polypropylene to the catalyst, the thermal decomposition inorganic substance and the dispersant is 100:5:15: 7; the catalyst is nickel carbonate; the thermal decomposition inorganic matter consists of sodium bicarbonate and calcium bicarbonate with the weight ratio of 1: 2; the dispersing agent consists of sorbitan laurate and pentaerythritol stearate in a weight ratio of 3: 1.
Comparative example 1 preparation of high specific surface area porous carbon Material
(1) Mixing polypropylene with a catalyst, and then carrying out melt extrusion granulation by a double-screw extruder to obtain composite polypropylene particles;
(2) and (2) placing the composite polypropylene particles prepared in the step (1) into a crucible, heating the crucible to 800 ℃, carrying out combustion reaction for 2 hours, washing a product after the reaction is finished, and drying the product to obtain the porous carbon material with the high specific surface area.
In the step (1), the weight ratio of the polypropylene to the catalyst is 100: 5; the catalyst is nickel carbonate.
Comparative example 1 is different from example 1 in that comparative example 1 does not add thermally decomposed inorganic substances, whereas example 1 adds thermally decomposed inorganic substances.
Comparative example 2 preparation of high specific surface area porous carbon Material
(1) Mixing polypropylene with a catalyst and a thermal decomposition inorganic substance, and then carrying out melt extrusion granulation by a double-screw extruder to obtain composite polypropylene particles;
(2) and (2) placing the composite polypropylene particles prepared in the step (1) into a crucible, heating the crucible to 800 ℃, carrying out combustion reaction for 2 hours, washing a product after the reaction is finished, and drying the product to obtain the porous carbon material with the high specific surface area.
In the step (1), the weight ratio of the polypropylene to the catalyst to the thermal decomposition inorganic matter is 100:5: 15; the catalyst is nickel carbonate; the thermal decomposition inorganic substance is sodium bicarbonate.
Comparative example 2 is different from example 1 in that the thermally decomposed inorganic substance of comparative example 2 uses only sodium bicarbonate; the thermally decomposed inorganic material of example 1 consisted of sodium bicarbonate and calcium bicarbonate.
Comparative example 3 preparation of high specific surface area porous carbon Material
(1) Mixing polypropylene with a catalyst and a thermal decomposition inorganic substance, and then carrying out melt extrusion granulation by a double-screw extruder to obtain composite polypropylene particles;
(2) and (2) placing the composite polypropylene particles prepared in the step (1) into a crucible, heating the crucible to 800 ℃, carrying out combustion reaction for 2 hours, washing a product after the reaction is finished, and drying the product to obtain the porous carbon material with the high specific surface area.
In the step (1), the weight ratio of the polypropylene to the catalyst to the thermal decomposition inorganic matter is 100:5: 15; the catalyst is nickel carbonate; the thermal decomposition inorganic substance is calcium bicarbonate.
Comparative example 3 is different from example 1 in that the thermally decomposed inorganic substance of comparative example 3 uses only calcium bicarbonate; the thermally decomposed inorganic material of example 1 consisted of sodium bicarbonate and calcium bicarbonate.
Comparative example 4 preparation of porous carbon Material with high specific surface area
(1) Mixing polypropylene with a catalyst, a thermal decomposition inorganic substance and a dispersing agent, and then carrying out melt extrusion granulation by a double-screw extruder to obtain composite polypropylene particles;
(2) and (2) placing the composite polypropylene particles prepared in the step (1) into a crucible, heating the crucible to 800 ℃, performing combustion reaction for 2 hours, washing a product after the reaction is finished, and drying the product to obtain the porous carbon material with the high specific surface area.
In the step (1), the weight ratio of the polypropylene to the catalyst, the thermal decomposition inorganic substance and the dispersant is 100:5:15: 7; the catalyst is nickel carbonate; the thermal decomposition inorganic matter consists of sodium bicarbonate and calcium bicarbonate with the weight ratio of 1: 2; the dispersant is sorbitan laurate.
Comparative example 4 differs from example 2 in that the dispersant is different; comparative example 4 only sorbitan laurate was used as the dispersant; in contrast, comparative example 2 used sorbitan laurate and pentaerythritol stearate together as the dispersant.
Comparative example 5 preparation of porous carbon Material with high specific surface area
(1) Mixing polypropylene with a catalyst, a thermal decomposition inorganic substance and a dispersing agent, and then carrying out melt extrusion granulation by a double-screw extruder to obtain composite polypropylene particles;
(2) and (2) placing the composite polypropylene particles prepared in the step (1) into a crucible, heating the crucible to 800 ℃, carrying out combustion reaction for 2 hours, washing a product after the reaction is finished, and drying the product to obtain the porous carbon material with the high specific surface area.
In the step (1), the weight ratio of the polypropylene to the catalyst, the thermal decomposition inorganic substance and the dispersant is 100:5:15: 7; the catalyst is nickel carbonate; the thermal decomposition inorganic matter consists of sodium bicarbonate and calcium bicarbonate with the weight ratio of 1: 2; the dispersing agent is pentaerythritol stearate.
Comparative example 5 differs from example 2 in that the dispersant is different; comparative example 5 only pentaerythritol stearate was used as the dispersant; in contrast, comparative example 2 used sorbitan laurate and pentaerythritol stearate together as the dispersant.
Comparative example 6 preparation of porous carbon Material with high specific surface area
(1) Mixing polypropylene with a catalyst, a thermal decomposition inorganic substance and a dispersing agent, and then carrying out melt extrusion granulation by a double-screw extruder to obtain composite polypropylene particles;
(2) and (2) placing the composite polypropylene particles prepared in the step (1) into a crucible, heating the crucible to 800 ℃, carrying out combustion reaction for 2 hours, washing a product after the reaction is finished, and drying the product to obtain the porous carbon material with the high specific surface area.
In the step (1), the weight ratio of the polypropylene to the catalyst, the thermal decomposition inorganic substance and the dispersant is 100:5:15: 7; the catalyst is nickel carbonate; the thermal decomposition inorganic matter consists of sodium bicarbonate and calcium bicarbonate with the weight ratio of 1: 2; the dispersing agent is ethylene bis stearamide.
Comparative example 6 differs from example 2 in that the dispersant is different; comparative example 6 ethylene bis stearamide was used as a dispersant; in contrast, comparative example 2 used sorbitan laurate and pentaerythritol stearate together as the dispersant.
Comparative example 7 preparation of porous carbon Material with high specific surface area
(1) Mixing polypropylene with a catalyst, a thermal decomposition inorganic substance and a dispersing agent, and then carrying out melt extrusion granulation by a double-screw extruder to obtain composite polypropylene particles;
(2) and (2) placing the composite polypropylene particles prepared in the step (1) into a crucible, heating the crucible to 800 ℃, carrying out combustion reaction for 2 hours, washing a product after the reaction is finished, and drying the product to obtain the porous carbon material with the high specific surface area.
In the step (1), the weight ratio of the polypropylene to the catalyst, the thermal decomposition inorganic substance and the dispersant is 100:5:15: 7; the catalyst is nickel carbonate; the thermal decomposition inorganic matter consists of sodium bicarbonate and calcium bicarbonate with the weight ratio of 1: 2; the dispersing agent consists of ethylene bis stearamide and pentaerythritol stearate in a weight ratio of 3: 1.
Comparative example 7 differs from example 2 in that the dispersant is different; comparative example 7 ethylene bis stearamide and pentaerythritol stearate were used together as a dispersant; in contrast, comparative example 2 used sorbitan laurate and pentaerythritol stearate together as the dispersant.
Comparative example 8 preparation of porous carbon Material with high specific surface area
(1) Mixing polypropylene with a catalyst, a thermal decomposition inorganic substance and a dispersing agent, and then carrying out melt extrusion granulation by a double-screw extruder to obtain composite polypropylene particles;
(2) and (2) placing the composite polypropylene particles prepared in the step (1) into a crucible, heating the crucible to 800 ℃, carrying out combustion reaction for 2 hours, washing a product after the reaction is finished, and drying the product to obtain the porous carbon material with the high specific surface area.
In the step (1), the weight ratio of the polypropylene to the catalyst, the thermal decomposition inorganic substance and the dispersant is 100:5:15: 7; the catalyst is nickel carbonate; the thermal decomposition inorganic matter consists of sodium bicarbonate and calcium bicarbonate with the weight ratio of 1: 2; the dispersing agent consists of sorbitan laurate and ethylene bis stearamide in a weight ratio of 3: 1.
Comparative example 8 differs from example 2 in that the dispersant is different; comparative example 8 sorbitan laurate and ethylene bis stearamide together were used as the dispersant; in contrast, comparative example 2 used sorbitan laurate and pentaerythritol stearate together as the dispersant.
Specific surface areas of the high specific surface area porous carbon materials prepared in examples 1 to 2 and comparative examples 1 to 8 were analyzed by a specific surface analyzer, and the results are shown in table 1.
TABLE 1 specific surface area of porous carbon Material
| Specific surface area | |
| Example 1 porous carbon material with high specific surface area prepared | 987m2/g |
| Example 2 porous carbon material with high specific surface area prepared | 1641m2/g |
| Comparative example 1 prepared porous carbon material with high specific surface area | 432m2/g |
| Comparative example 2 prepared porous carbon material with high specific surface area | 528m2/g |
| Comparative example 3 porous carbon material with high specific surface area | 577m2/g |
| Comparative example 4 the porous carbon material with high specific surface area | 1092m2/g |
| Comparative example 5 the porous carbon material with high specific surface area | 1145m2/g |
| Comparative example 6 the porous carbon material with high specific surface area | 1037m2/g |
| Comparative example 7 prepared porous carbon material with high specific surface area | 1088m2/g |
| Comparative example 8 prepared porous carbon material with high specific surface area | 1059m2/g |
As can be seen from the experimental data in Table 1, the specific surface area of the porous carbon material prepared by using polypropylene as a raw material and adopting the method of the invention without heating to decompose inorganic matters is only 432m2(ii)/g; and do not have excellent porosity properties. However, the specific surface area of example 1 reached 987m compared with that of comparative example 12(iv)/g, is significantly improved; this indicates that: the method of the invention is adopted by taking polypropylene as a raw material, and inorganic substances composed of sodium bicarbonate and calcium bicarbonate are added for thermal decomposition, so that the specific surface area of the prepared porous carbon material can be obviously improved.
As can be seen from the experimental data in table 1, the specific surface area of the porous carbon materials prepared in comparative examples 2 and 3 is not obviously improved compared with that of comparative example 1, and is far smaller than that of example 1; this indicates that: in the method of the invention, the specific surface area of the prepared porous carbon material can be obviously improved by not adding inorganic substances for thermal decomposition randomly; the specific surface area of the prepared porous carbon material can be obviously improved only by adding the inorganic substance consisting of sodium bicarbonate and calcium bicarbonate for thermal decomposition.
Slave watch1 experimental data can also show that the specific surface area of the sample 2 reaches 1641m compared with the sample 12(iv)/g, is further greatly improved; this indicates that: by adopting polypropylene as a raw material and adding a dispersing agent consisting of sorbitan laurate and pentaerythritol stearate, the method can further greatly improve the specific surface area of the prepared porous carbon material; the prepared porous carbon material has very high specific surface area.
As can be seen from the experimental data in Table 1, the specific surface area of the comparative examples 4 to 6 is not obviously improved compared with that of the example 1; and the specific surface area is also far smaller than that of the embodiment 2; this indicates that: by adopting the method of the invention with polypropylene as the raw material, the specific surface area of the prepared porous carbon material can be further greatly improved without adding a dispersing agent randomly; the specific surface area of the prepared porous carbon material can be further greatly improved only by adding a dispersing agent consisting of sorbitan laurate and pentaerythritol stearate; the specific surface area of the prepared porous carbon material cannot be further greatly increased by adding a single dispersing agent or a combination of other dispersing agents.
Claims (10)
1. A preparation method of a porous carbon material with high specific surface area is characterized by comprising the following steps:
(1) mixing polypropylene with a catalyst and a thermal decomposition inorganic substance, and then carrying out melt extrusion granulation by a double-screw extruder to obtain composite polypropylene particles;
(2) and (2) placing the composite polypropylene particles prepared in the step (1) into a heating device, heating to 600-900 ℃, reacting for 1-3 h, and washing a product after the reaction is finished to obtain the porous carbon material with the high specific surface area.
2. The method for preparing a porous carbon material with a high specific surface area according to claim 1, wherein the weight ratio of the polypropylene to the catalyst and the thermally decomposed inorganic substance in the step (1) is 100:1 to 10:10 to 20;
most preferably, the weight ratio of polypropylene to catalyst and thermally decomposed inorganic substance in step (1) is 100:5: 15.
3. The method according to claim 1, wherein the catalyst is nickel carbonate.
4. The method for preparing a porous carbon material with high specific surface area according to claim 1, wherein the thermally decomposed inorganic substance is composed of sodium bicarbonate and calcium bicarbonate.
5. The method for preparing a porous carbon material with a high specific surface area according to claim 4, wherein the weight ratio of sodium bicarbonate to calcium bicarbonate is 1: 1-3;
most preferably, the weight ratio of sodium bicarbonate to calcium bicarbonate is 1: 2.
6. The method for preparing a porous carbon material with a high specific surface area according to claim 1, wherein a dispersant is further added in the step (1).
7. The method for preparing a porous carbon material with a high specific surface area according to claim 6, wherein the weight ratio of the polypropylene to the catalyst, the thermally decomposed inorganic substance and the dispersant is 100: 1-10: 10-20: 5-10;
most preferably, the weight ratio of polypropylene to catalyst, thermally decomposed inorganic substance and dispersant is 100:5:15: 7.
8. The method for preparing a porous carbon material with high specific surface area according to claim 1, wherein the dispersant is composed of sorbitan laurate and pentaerythritol stearate.
9. The method for producing a porous carbon material with a high specific surface area according to claim 1, wherein the weight ratio of sorbitan laurate to pentaerythritol stearate is 2 to 3: 1.
10. The porous carbon material prepared by the method for preparing a porous carbon material with a high specific surface area according to any one of claims 1 to 9.
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| CN117619347A (en) * | 2023-11-27 | 2024-03-01 | 嘉应学院 | Porous carbon material, preparation method thereof and application thereof in sewage treatment |
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