CN114455571A - Method for preparing carbon nanotubes by taking waste express packaging bags as carbon sources - Google Patents
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- CN114455571A CN114455571A CN202210107834.7A CN202210107834A CN114455571A CN 114455571 A CN114455571 A CN 114455571A CN 202210107834 A CN202210107834 A CN 202210107834A CN 114455571 A CN114455571 A CN 114455571A
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Abstract
The invention relates to the technical field of carbon nanotube preparation, and particularly discloses a method for preparing a carbon nanotube by taking a waste express delivery packaging bag as a carbon source. The method for preparing the carbon nano tube by taking the waste express packaging bag as the carbon source comprises the following steps: (1) cleaning and shearing the waste express packaging bags, adding the cut waste express packaging bags and a cracking catalyst into a first quartz tube, then placing the quartz tube in a reaction furnace, and introducing protective atmosphere to carry out pyrolysis reaction to obtain a pyrolysis product; (2) and introducing the pyrolysis product into a second quartz tube with a metal catalyst, performing catalytic reaction in a protective atmosphere, and obtaining the carbon nano tube after the reaction is finished. The application of the method can solve the problem of a large number of waste plastic bags, provide a carbon source with unlimited sources and transportation for the preparation of the carbon nano tube, and the carbon nano tube prepared by the method has the advantages of high yield, good performance and the like.
Description
Technical Field
The invention relates to the technical field of carbon nanotube preparation, in particular to a method for preparing a carbon nanotube by taking a waste express packaging bag as a carbon source.
Background
In recent years, with the rapid development of the internet, a great number of electric merchants are coming into the market, and online shopping becomes an option for many people to shop, so that the rapid growth of logistics in China is also driven. People receive and dispatch express items every day, using a large number of express packages and express fillers. The packaging of the express industry at present mainly comprises express waybills, woven bags, plastic bags, envelopes, packing cases (corrugated boxes), adhesive tapes and the like; meanwhile, a large amount of buffer fillers are arranged in the express package. The result is that the waste and improper recycling of a large amount of packages, in which the cartons can be recycled, but the recycling system of plastic products needs to be perfect, which leads to the disposal of the plastic products and the landfill of the plastic products as common garbage, and leads to the mass production of plastic garbage.
At present, the waste plastics mainly have three directions: firstly, the power is generated by burning, and accounts for about 42%; secondly, landfill, which accounts for about 27%; thirdly, recycling, which accounts for about 31 percent. In the recovery, 99% is mechanical recovery (new product without destroying original molecular structure), and only 1% is thermal decomposition recovery. The thermal decomposition recovery can pyrolyze and gasify the waste plastics to produce various petrochemical products, and effectively convert the waste plastics into high value-added products, but the application is not wide at present, which is related to that the method is directly incinerated, and the landfill method has higher cost and complex flow. However, with the progress of research, the thermal decomposition recovery process is gradually optimized, and the process has great potential to become a large-scale waste plastic recovery mode in the future. In recent years, many researchers have attempted to produce hydrogen gas using waste plastics as a hydrogen source, and researchers have also found that waste plastics can also serve as a source of carbon materials under a suitable catalyst.
The carbon nano tube has excellent mechanical, thermal and electrical properties and has high specific strength due to the advantage of low density. Carbon nanotubes of different structures have different applications in engineering, and are ideal application materials in fields requiring low density, low weight, high tensile strength or elastic modulus (e.g., transportation, structural materials, high-tech applications, etc.).
Carbon nanotubes can be synthesized from gaseous or liquid hydrocarbons, aromatic compounds (such as toluene, benzene, etc.), ethylene, acetylene, etc. are traditionally used in synthesis, and these petroleum-related products are controlled, i.e., the sources are limited, and the transportation is inconvenient. The common synthesis method of carbon nanotubes is Chemical Vapor Deposition (CVD), Catalytic Chemical Vapor Deposition (CCVD), arc discharge, laser ablation, and other preparation techniques, and is performed in a reactor such as an autoclave, a muffle furnace, or a fluidized bed. Different modes and reactors have great influence on the forming of the carbon nano tube, and meanwhile, the problems of catalyst poisoning, over-high energy consumption and the like often occur in the existing reaction technology, so that new improvement is needed.
In summary, the current requirements should be: 1. the problem of a large amount of discarded express packaging plastic bags is solved, a proper recycling mode is found, and the additional value of the waste plastic bags is improved. 2. High quality carbon nanotubes are sought to be produced using suitable methods, distinguished from sources and carbon sources that are limited in transportation.
Disclosure of Invention
In order to overcome the technical problems in the prior art, the invention provides a method for preparing carbon nanotubes by taking waste express packaging bags as carbon sources.
The problems to be solved by the invention are solved by the following technical scheme:
a method for preparing carbon nanotubes by taking waste express packaging bags as carbon sources comprises the following steps:
(1) cleaning the waste express packaging bags, shearing the waste express packaging bags into pieces, adding the cut waste express packaging bags and a cracking catalyst into a first quartz tube, then placing the quartz tube into a reaction furnace, and introducing protective atmosphere to perform pyrolysis reaction to obtain pyrolysis products;
(2) and introducing the pyrolysis product into a second quartz tube with a metal catalyst, carrying out catalytic reaction under a protective atmosphere, and obtaining the carbon nano tube after the reaction is finished.
The waste express packaging bags are waste express packaging bags made of plastic materials; in particular to an express packaging bag made of waste PE.
Preferably, the cracking catalyst in step (1) is HF/Al2O3、BF3/Al2O3、H3PO4Diatomite, SiO2/Al2O3、B2O3/Al2O3Zeolite, AlPO4、BPO4、Fe2(SO4)3、CuSO4One or a combination of more than one of them.
Further preferably, the cracking catalyst is composed of zeolite, AlPO4And CuSO4Composition is carried out; wherein the zeolite is AlPO4And CuSO4The weight ratio of (A) to (B) is 5-10: 1-3: 2-4.
Most preferably, zeolite, AlPO4And CuSO4In a weight ratio of 8:2: 3.
Preferably, the addition amount of the cracking catalyst in the step (1) is 2-10 wt% of the amount of the waste express packaging bags.
Preferably, the specific conditions of the pyrolysis reaction in step (1) are: heating to 500-550 ℃ at a heating rate of 5-10 ℃/min, and reacting for 1.5-3 h.
Preferably, the metal catalyst in the step (2) is a catalyst in which a metal element is supported on an oxide;
the metal element is selected from one or more of Fe, Ni, Mo, Mn, Co, Mg, Cr, Pd, Au and Ti; the oxide is Al, Mg or Si oxide.
Most preferably, the metal catalyst is Fe/Ni/Al2O3Catalyst, Ni/Mn/Al2O3Catalyst or Ni/Mo/MgO catalyst. The weight ratio of the metal to the oxide in the metal catalyst is 1:1: 3.
Preferably, the addition amount of the metal catalyst is 2-10 wt% of the amount of the waste express packaging bags.
Most preferably, the specific conditions of the pyrolysis reaction in step (2) are: heating to 550-800 ℃ at a heating rate of 5-10 ℃/min and reacting for 1-2 h.
The further problem encountered in the process of preparing the carbon nano tube by using the waste express packaging bag as a carbon source by the inventor is how to improve the purity and the carbon conversion rate of the prepared carbon nano tube. The inventors have found through extensive experiments that this is closely related to the selection of the cracking catalyst in step (1) and the selection of the metal catalyst in step (2); the inventor shows through a large number of experiments that the zeolite and AlPO4And CuSO4Carrying out pyrolysis reaction under the cracking catalyst, and then adopting Ni/Mo/MgO catalyst as goldThe carbon nano tube obtained by catalytic reaction of the catalyst has higher purity and carbon conversion rate.
Has the advantages that: the invention provides a method for preparing carbon nanotubes by taking waste express packaging bags as carbon sources. The application of the method can solve the problem of a large number of waste plastic bags, provide a carbon source with unlimited sources and transportation for the preparation of the carbon nano tube, and the carbon nano tube prepared by the method has the advantages of high yield, good performance and the like. In addition, the method has the advantages of simple synthesis process and mild conditions, effectively reduces the preparation cost, and has the potential of large-scale generation.
Drawings
Fig. 1 shows the scanning electron microscope results of the carbon nanotube sample prepared in example 1 of the present invention.
Fig. 2 shows the transmission electron microscope results of the carbon nanotube sample prepared in example 1 of the present invention.
Detailed Description
The present invention is further explained below with reference to specific examples, which are not intended to limit the present invention in any way.
Example 1
(1) Carrying out primary cleaning and shearing treatment on the recycled express packaging bag made of the waste PE material, and adding 5g of sheet material and 0.25g of cracking catalyst into a first quartz tube; setting the temperature rise rate of a reaction furnace in which the first quartz tube is positioned at 5 ℃/min, raising the temperature to 500 ℃, keeping the temperature for 2h, and introducing protective atmosphere N into the furnace2A pyrolysis reaction occurs inside with the temperature rise;
(2) connecting the gas outlet of the pyrolysis product with a second quartz tube, placing 0.2g of metal catalyst in the second quartz tube, and introducing protective atmosphere N2Carrying out catalytic reaction; setting the temperature rise rate of 10 ℃/min in a reaction furnace in which the second quartz tube is positioned to 750 ℃ for reaction for 1h, and converting pyrolysis products into carbon nano tubes;
wherein the cracking catalyst in the step (1) is prepared from ZSM-5 zeolite and AlPO with the weight ratio of 8:2:34And CuSO4Composition of；
The metal catalyst in the step (1) is selected from Fe/Ni/Al2O3Catalyst, metal catalyst in Fe, Ni, Al2O3The weight ratio of (A) to (B) is 1:1: 3.
Example 2
(1) Carrying out primary cleaning and shearing treatment on the recycled and obtained express packaging bag made of the waste PE material, and adding 5g of sheet material and 0.4g of cracking catalyst into a first quartz tube; setting the temperature rise rate of a reaction furnace in which the first quartz tube is positioned at 5 ℃/min, raising the temperature to 550 ℃, preserving the temperature for 1.5h, and simultaneously introducing protective atmosphere N into the furnace2A pyrolysis reaction occurs inside with the temperature rise;
(2) connecting the gas outlet of the pyrolysis product with a second quartz tube, placing 0.4g of metal catalyst in the second quartz tube, and introducing protective atmosphere N2Carrying out catalytic reaction; setting a reaction furnace in which the second quartz tube is arranged to be heated to 600 ℃ at a heating rate of 10 ℃/min for reacting for 2 hours, and converting pyrolysis products into carbon nano tubes;
wherein the cracking catalyst in the step (1) is prepared from ZSM-5 zeolite and AlPO with the weight ratio of 10:1:44And CuSO4Forming;
the metal catalyst in the step (1) is selected from Ni/Mn/Al2O3Catalyst, Ni, Mn, Al in metal catalyst2O3The weight ratio of (A) to (B) is 1:1: 3.
Example 3
(1) Carrying out primary cleaning and shearing treatment on the recycled express packaging bag made of the waste PE material, and adding 5g of sheet material and 0.25g of cracking catalyst into a first quartz tube; setting the temperature rise rate of a reaction furnace in which the first quartz tube is positioned at 5 ℃/min, raising the temperature to 500 ℃, keeping the temperature for 2h, and introducing protective atmosphere N into the furnace2A pyrolysis reaction occurs inside with the temperature rise;
(2) connecting the gas outlet of the pyrolysis product with a second quartz tube, placing 0.2g of metal catalyst in the second quartz tube, and introducing protective atmosphere N2Carrying out catalytic reaction; setting the temperature rise rate of 10 ℃/min in a reaction furnace in which the second quartz tube is positioned to 750 ℃ for reaction for 1h, and converting pyrolysis products into carbon nano tubes;
wherein the cracking catalyst in the step (1) is prepared from ZSM-5 zeolite and AlPO with the weight ratio of 8:2:34And CuSO4Composition is carried out;
the metal catalyst in the step (1) is selected from Ni/Mo/MgO catalyst, and the weight ratio of Ni, Mo and MgO in the metal catalyst is 1:1: 3.
Example 4
(1) Carrying out primary cleaning and shearing treatment on the recycled express packaging bag made of the waste PE material, and adding 5g of sheet material and 0.25g of cracking catalyst into a first quartz tube; setting the temperature rise rate of a reaction furnace in which the first quartz tube is positioned at 5 ℃/min, raising the temperature to 500 ℃, keeping the temperature for 2h, and introducing protective atmosphere N into the furnace2A pyrolysis reaction occurs inside with the temperature rise;
(2) connecting the gas outlet of the pyrolysis product with a second quartz tube, placing 0.2g of metal catalyst in the second quartz tube, and introducing protective atmosphere N2Carrying out catalytic reaction; setting the temperature rise rate of 10 ℃/min in a reaction furnace in which the second quartz tube is positioned to 750 ℃ for reaction for 1h, and converting pyrolysis products into carbon nano tubes;
wherein the cracking catalyst in the step (1) is prepared from ZSM-5 zeolite and CuSO with the weight ratio of 8:54Composition is carried out;
the metal catalyst in the step (1) is selected from Fe/Ni/Al2O3Catalyst, metal catalyst in Fe, Ni, Al2O3The weight ratio of (A) to (B) is 1:1: 3.
Example 5
(1) Carrying out primary cleaning and shearing treatment on the recycled and obtained express packaging bag made of the waste PE material, and adding 5g of sheet material and 0.25g of cracking catalyst into a first quartz tube; setting the temperature rise rate of a reaction furnace in which the first quartz tube is positioned at 5 ℃/min, raising the temperature to 500 ℃, keeping the temperature for 2h, and introducing protective atmosphere N into the furnace2A pyrolysis reaction occurs inside with the temperature rise;
(2) connecting the gas outlet of the pyrolysis product with a second quartz tube, placing 0.2g of metal catalyst in the second quartz tube, and introducing protective atmosphere N2Carrying out catalytic reaction; setting the temperature rise rate of a reaction furnace in which the second quartz tube is arranged to be 10 ℃/min to be 750 ℃ for reaction1h, converting the pyrolysis product into the carbon nano tube;
wherein the cracking catalyst in the step (1) is prepared from ZSM-5 zeolite and AlPO with the weight ratio of 8:54Composition is carried out;
the metal catalyst in the step (1) is selected from Fe/Ni/Al2O3Catalyst, Fe, Ni, Al in metal catalyst2O3The weight ratio of (A) to (B) is 1:1: 3.
TABLE 1 purity and carbon conversion of carbon nanotubes
| Purity of | Carbon conversion | |
| Example 1 preparation of the obtained carbon nanotubes | 80.6％ | 49.7％ |
| Example 2 preparation of the resulting carbon nanotubes | 74.2％ | 41.1％ |
| Example 3 preparation of the resulting carbon nanotubes | 91.1％ | 70.5％ |
| Example 4 preparation of the resulting carbon nanotubes | 57.2％ | 32.7％ |
| Example 5 preparation of the resulting carbon nanotubes | 61.3％ | 34.6％ |
As can be seen from the purity and carbon conversion in table 1, the purity and carbon conversion of the obtained carbon nanotubes are greatly different due to the different selection of the cracking catalyst in step (1) and the different selection of the metal catalyst in step (2); however, the purity of the carbon nanotube prepared in example 3 reaches more than 90%, and the carbon conversion rate reaches more than 70%; the effect is very remarkable far more than other embodiments. This indicates that: using waste express packaging bags as a carbon source, zeolite and AlPO4And CuSO4The carbon nano tube obtained by carrying out pyrolysis reaction under the cracking catalyst and then carrying out catalytic reaction by using Ni/Mo/MgO catalyst as a metal catalyst has very high purity and carbon conversion rate.
Claims (10)
1. A method for preparing carbon nanotubes by taking waste express packaging bags as carbon sources is characterized by comprising the following steps:
(1) cleaning the waste express packaging bags, shearing the waste express packaging bags into pieces, adding the cut waste express packaging bags and a cracking catalyst into a first quartz tube, then placing the quartz tube into a reaction furnace, and introducing protective atmosphere to perform pyrolysis reaction to obtain pyrolysis products;
(2) and introducing the pyrolysis product into a second quartz tube with a metal catalyst, performing catalytic reaction under a protective atmosphere, and obtaining the carbon nano tube after the reaction is finished.
2. The method for preparing carbon nanotubes by using waste express packaging bags as a carbon source according to claim 1, wherein the cracking catalyst in the step (1) is HF/Al2O3、BF3/Al2O3、H3PO4Diatomite, SiO2/Al2O3、B2O3/Al2O3Zeolite, AlPO4、BPO4、Fe2(SO4)3、CuSO4One or a combination of more than one of them.
3. The method for preparing carbon nanotubes by using waste express packaging bags as a carbon source according to claim 2, wherein the cracking catalyst is zeolite or AlPO4And CuSO4Composition is carried out; wherein the zeolite is AlPO4And CuSO4The weight ratio of (A) to (B) is 5-10: 1-3: 2-4.
4. The method for preparing carbon nanotubes by using waste express packaging bags as a carbon source according to claim 3, wherein the carbon nanotubes are zeolite and AlPO4And CuSO4In a weight ratio of 8:2: 3.
5. The method for preparing carbon nanotubes by using the waste express packaging bags as a carbon source according to claim 1, wherein the addition amount of the cracking catalyst in the step (1) is 2-10 wt% of the use amount of the waste express packaging bags.
6. The method for preparing carbon nanotubes by using the waste express packaging bags as a carbon source according to claim 1, wherein the specific conditions of the pyrolysis reaction in the step (1) are as follows: heating to 500-550 ℃ at a heating rate of 5-10 ℃/min, and reacting for 1.5-3 h.
7. The method for preparing carbon nanotubes by using the waste express packaging bags as a carbon source according to claim 1, wherein the metal catalyst in the step (2) is a catalyst in which a metal element is supported on an oxide;
the metal element is selected from one or more of Fe, Ni, Mo, Mn, Co, Mg, Cr, Pd, Au and Ti; the oxide is Al, Mg or Si oxide.
8. The method for preparing carbon nano-particles by using waste express packaging bags as carbon sources according to claim 1The method of the tube is characterized in that the metal catalyst is Fe/Ni/Al2O3Catalyst, Ni/Mn/Al2O3Catalyst or Ni/Mo/MgO catalyst.
9. The method for preparing the carbon nanotube by using the waste express packaging bags as the carbon source according to claim 1, wherein the addition amount of the metal catalyst is 2-10 wt% of the consumption amount of the waste express packaging bags.
10. The method for preparing carbon nanotubes by using the waste express packaging bags as a carbon source according to claim 1, wherein the specific conditions of the pyrolysis reaction in the step (2) are as follows: heating to 550-800 ℃ at a heating rate of 5-10 ℃/min and reacting for 1-2 h.
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