CN112028054A - Method for preparing ultra-long multi-walled carbon nano-tube by two-step microwave treatment of biomass - Google Patents
Method for preparing ultra-long multi-walled carbon nano-tube by two-step microwave treatment of biomass Download PDFInfo
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Abstract
The invention discloses a method for preparing an ultralong multi-walled carbon nanotube by biomass through two-step microwave treatment, which comprises the following steps: (1) separating a cellulose sample from the biomass by a chemical pretreatment process; (2) pyrolyzing the cellulose sample by low-temperature microwave to generate a biochar sample containing carbon nanotubes; (3) and (3) pyrolyzing the biochar sample by high-temperature microwave to prepare the ultra-long multi-walled carbon nanotube. According to the invention, a thin metal (Ni, Mo, Fe, Co and the like) substrate is not needed, biomass is used for replacing various hydrocarbons (ethane, methane, acetylene, xylene or a mixture of the ethane, the methane, the acetylene and the xylene), and only microwave heating is adopted to prepare the ultra-long multi-walled carbon nanotube with high graphene crystal content of about 0.97, length of more than or equal to 1cm and diameter of 200-400 nm. The method solves the problems of complex process, high cost, short carbon nano tube, more defects and the like in the prior art for preparing the ultra-long multi-walled carbon nano tube.
Description
Technical Field
The invention relates to a method for directly converting biomass into an ultralong multi-walled carbon nanotube by using microwaves, and relates to the technical field of efficient and clean utilization of biomass resources.
Background
Carbon nanotubes are hollow "microtubes" made by winding hexagonal grids similar to graphite structures, and are classified into single-walled tubes and multi-walled tubes. The multi-wall pipe is formed by a plurality of coaxial cylindrical sleeves with the layer spacing of about 0.34 nanometer. The diameter of the common carbon nano tube is from dozens of nanometers to hundreds of nanometers, the length is in micrometer unit, and the length of the ultra-long carbon nano tube can reach centimeter level or even decimeter level. Carbon nanotubes and composites thereof are widely used in various aspects such as field emission, multifunctional composites, catalyst materials, hydrogen storage materials, sensors, biomedicine, adsorption materials, electrochemistry and the like due to their unique properties, and are known as one of the most important materials in the 21 st century.
Carbon nanotubes are typically produced by arc discharge, laser ablation, Chemical Vapor Deposition (CVD), Plasma Enhanced Chemical Vapor Deposition (PECVD), or Catalytic Chemical Vapor Deposition (CCVD). The carbon nanotubes prepared by the arc method and the laser evaporation method have high crystallinity, but relatively low yield. Chemical vapor deposition is an effective method for realizing industrial mass production of carbon nanotubes, but the prepared carbon nanotubes usually contain more crystal structure defects and are accompanied with more catalyst impurities which are difficult to remove. In addition, the service life and the growth temperature of the nano catalyst determine the growth length of the carbon nano tube, and the length of the prepared carbon nano tube is very short and takes a micron as a unit. Meanwhile, the above preparation method requires the use of thin metals (Ni, Mo, Fe, Co, etc.), substrates, various hydrocarbons (ethane, methane, acetylene, xylene or their mixtures), etc., and has complicated processes and high raw material costs. With the widening of the application field of the carbon nano tube, the development of the preparation technology of the ultra-long carbon nano tube with simple process and low cost has important significance.
The biomass is a clean and renewable natural carbon resource with stable property and lower production cost. Microwave heating is a process in which electromagnetic fields interact with material particles during propagation in a material to produce various electromagnetic losses that convert electromagnetic energy into thermal energy. Compared with the traditional heating method, the microwave heating has the characteristics of high heating speed, uniform heating, easy control, selective heating, low energy consumption, safety, harmlessness and the like. The preparation process of developing the carbon nano tube by taking the microwave as a heat source and the biomass as a raw material is concerned. Zeng et al (A route to Rapid carbon nanotube growth) pass CH in a microwave field4/N2The chemical vapor phase cracking deposition method synthesizes carbon nano-tubes with different forms, and the result shows the reaction temperature and CH4/N2The mixing proportion and the total gas flow speed have large influence on the form of the carbon nano tube, and Raman spectrum detection results show that the prepared carbon nano tube has low graphitization degree. Nie et al (Growth and morphology of carbon nanostructures by microwave-induced heating of a mixture of ferrocene and carbon fiber for 15s to prepare carbon nanotubes, but the catalyst ferrocene used in the method is difficult to separate from the carbon nanotubes. Patent CN 104787747a "a method for preparing multi-walled carbon nanotubes by microwave enhanced fast pyrolysis of biomass and/or carbon-containing organic waste" discloses that biomass or carbon-containing organic waste or a mixture of the two is uniformly mixed with a microwave absorbent, and multi-walled carbon nanotubes are prepared under the action of microwaves. However, the carbon nanotube prepared by the method has low graphene crystal content of about 0.70 and an imperfect structure.
Disclosure of Invention
The invention aims to provide a method for preparing an ultralong multi-walled carbon nanotube by two-step microwave treatment of biomass, which solves the technical problems that a catalyst is used in the prior art, the separation of the catalyst and the carbon nanotube is difficult, the carbon nanotube has many structural defects, the preparation process is complex and the like; the invention effectively reduces the preparation cost of the carbon nano tube, improves the production efficiency and the quality of the carbon nano tube, can be produced in a large scale, and is an economic and efficient preparation method of the ultra-long multi-walled carbon nano tube.
In order to achieve the purpose, the invention is realized by the following technical scheme:
(1) separation of cellulose samples from biomass by chemical pretreatment methods
Firstly, putting biomass into a vacuum drying oven, and drying at 100-110 ℃ for 10-14 h to remove moisture; adding strong base into the dried biomass, continuously stirring for 1.5-2.5 h at 85-95 ℃, dissolving lignin in the biomass, filtering and separating, and washing residues after alkali treatment with warm water; adding strong acid into the alkaline washing residue, heating for 1.5-2.5 h at 85-95 ℃, dissolving hemicellulose in the biomass, filtering and separating, washing the residue after acid treatment with warm water, putting the obtained residue into a vacuum drying oven, and drying for 20-30 h at 75-85 ℃ to obtain a cellulose sample;
(2) low-temperature microwave pyrolysis for generating biochar sample containing carbon nano-tubes
Uniformly mixing the cellulose sample obtained in the step (1) with a microwave absorbent, placing the mixture into a quartz reactor, placing the quartz reactor into microwave heating equipment, introducing nitrogen into the quartz reactor to remove air in the quartz reactor, and continuously introducing nitrogen in the reaction process, wherein the heating rate is controlled to be 10-100 ℃/min, the heating temperature is controlled to be 400-700 ℃, and the constant temperature is kept for 25-35 min to obtain a biochar sample containing carbon nanotubes;
(3) preparation of ultralong multi-walled carbon nanotubes by high-temperature microwave pyrolysis
And (3) putting the biochar sample containing the carbon nano tube obtained in the step (2) into a quartz reactor, then putting the quartz reactor into microwave heating equipment, introducing nitrogen into the quartz reactor to remove air in the quartz reactor, and continuously introducing the nitrogen in the reaction process, wherein the heating rate is controlled to be 8-12 ℃/min, the temperature is controlled to be 1000-1500 ℃, and the temperature is kept constant for 25-35 min, so that the ultra-long carbon nano tube is obtained.
The biomass is coconut shell or pine nut shell.
The strong base is 0.5 +/-0.05 mol/L sodium hydroxide or 0.5 +/-0.05 mol/L potassium hydroxide; the mass ratio of the biomass to the sodium hydroxide or the potassium hydroxide is 2: 1-5: 1.
The strong acid is hydrochloric acid with the volume ratio of 10% or sulfuric acid with the volume ratio of 10%; the mass ratio of the biomass to the hydrochloric acid or sulfuric acid is 1: 2-1: 5.
The granularity of the biomass is 150-280 μm.
The nitrogen flow is 300 ml/min-500 ml/min.
The mass ratio of the cellulose sample to the microwave absorbent is 10: 20-10: 0.1. The microwave absorbent is one or a mixture of any of activated carbon, silicon carbide and semicoke.
The length of the super-long carbon nano tube is more than or equal to 1cm, and the diameter of the super-long carbon nano tube is 200 nm-400 nm.
The cellulose pyrolysis is carried out by adopting a temperature programming microwave oven, the maximum output power is 2000W, and the frequency is 2.45 GHz.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention overcomes the problems that the traditional methods of arc discharge, laser ablation, Chemical Vapor Deposition (CVD), Plasma Enhanced Chemical Vapor Deposition (PECVD) or Catalytic Chemical Vapor Deposition (CCVD) and the like need to use thin metal (Ni, Mo, Fe, Co and the like), a substrate, various hydrocarbons (ethane, methane, acetylene, dimethylbenzene or a mixture thereof) and the like to prepare the carbon nano tube, the process is complex, the cost of raw materials is high, the prepared carbon nano tube is short in length, and the like. The invention adopts biomass as raw material, prepares the multi-wall carbon nano-tube with higher quality by chemical pretreatment and two-step microwave treatment, and is a method which has simple preparation process and low cost and can produce the high-quality ultra-long multi-wall carbon nano-tube in large scale.
(2) The existing microwave preparation technology of the carbon nano tube has the problem that the catalyst and the carbon nano tube are difficult to separate; the method for preparing the carbon nano tube by directly performing one-step microwave treatment on the biomass has the problems of more structural defects (about 0.70 of graphene crystal content), short length and the like. The inventor finds that the cellulose biological component is a high-quality raw material for preparing the carbon nano tube, and the quality of the prepared ultra-long carbon nano tube is higher when the content of the cellulose biological component is higher. The lignocellulose biomass is used as a raw material, cellulose components in the biomass are separated by a chemical pretreatment method, and the biomass is processed into the high-performance ultra-long carbon nano tube by two-stage microwave technology step by step, wherein the content of graphene crystals is high, about 0.97, the length is more than or equal to 1cm, and the diameter is 200nm to 400 nm.
Drawings
FIG. 1 is a flow chart of a process for preparing an ultra-long multi-walled carbon nanotube by using biomass through two-step microwave treatment.
FIG. 2 is a schematic diagram of an apparatus for two-step microwave treatment of biomass to produce ultra-long multi-walled carbon nanotubes, wherein (a) is a low-temperature microwave pyrolysis apparatus; FIG. (b) is a high-temperature microwave heat treatment apparatus; wherein (1) a thermocouple; (2) a microwave control panel; (3) a microwave oven; (4) a quartz reactor; (5) an inner chamber of the microwave oven; (6) a conduit; (7) an exhaust pipe; (8) a condensation bottle; (9) a water bath cooler; (10) an air inlet pipe; (11) a ceramic gasket; (12) a high temperature thermocouple; (13) a quartz reactor; (14) a ceramic reactor.
FIG. 3 SEM pictures of a biomass sample before and after treatment; wherein (a) the biomass PKS; (b) PKS caustic wash residue (c) PKS acid wash residue; (d) a PKS biochar sample at 600 ℃; (e)1200 ℃ ultra-long multi-walled carbon nanotubes; (f)1300 ℃ ultra-long multi-walled carbon nano-tubes; (g)1400 ℃ ultra-long multi-walled carbon nanotubes.
FIG. 4 is a Raman spectrum of an ultra-long multi-walled carbon nanotube.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not to be considered in a limiting sense, the invention being thus defined which, to the extent possible, is intended to be within the scope of the appended claims.
The process flow diagram for preparing the ultra-long carbon nano-tube by using Malaysia Palm Kernel Shell (PKS) biomass is shown in figure 1, and figure 2 is a structure diagram of microwave equipment.
(1) Separation of cellulose samples from biomass by chemical pretreatment methods
Putting the PKS sample with the particle size of 150-280 microns into a vacuum drying oven, and drying at 105 ℃ for 12h to remove water; adding 250 ml of NaOH (0.5mol/L) into 10g of a dried PKS sample, continuously stirring for 2h at 90 ℃, dissolving lignin in the biomass, filtering and separating, and washing residues after alkali treatment by using warm water; to the caustic wash residue was added 100ml of 10% v/v H2SO4Heating at 90 ℃ for 2h to dissolve hemicellulose in the biomass, filtering and separating, washing the residue after acid treatment with warm water, putting the obtained residue into a vacuum drying oven, and drying at 80 ℃ for 24h to obtain a cellulose sample.
(2) Low-temperature microwave pyrolysis for generating biochar sample containing carbon nano-tubes
Uniformly mixing a cellulose sample and 300-600 mu m microwave wave absorbing agent silicon carbide in a ratio of 10:2, putting the mixture into a quartz reactor, and then putting the quartz reactor into a microwave oven. And introducing nitrogen into the quartz reactor at a flow rate of 400ml/min to remove air in the quartz reactor, continuously introducing nitrogen in the reaction process, controlling the heating temperature at 600 ℃, controlling the heating rate at 10 ℃/min, and keeping the temperature for 30min to obtain the biochar sample containing the carbon nano tube.
(3) Preparation of ultralong multi-walled carbon nanotubes by high-temperature microwave pyrolysis
Putting 5g of a biochar sample into a quartz reactor, then putting the quartz reactor into a microwave oven, introducing nitrogen into the quartz reactor at the flow rate of 400ml/min to remove the air in the quartz reactor, continuously introducing the nitrogen in the reaction process, controlling the heating rate at 10 ℃/min, setting the heating final temperature at 1200 ℃, 1300 ℃ and 1400 ℃, and keeping the temperature for 30min to obtain the ultra-long multi-walled carbon nanotube.
FIGS. 3a-c characterize the change in PKS structure during chemical pretreatment. (a) Biomass PKS, (b) PKS caustic wash residue, (c) PKS acid wash residue, and (d) PKS biochar sample. FIGS. 3e-g Carbon Nanotubes (CNTs) obtained at 1200 deg.C, 1300 deg.C and 1400 deg.C, respectively. It can be seen that the CNTs form is changed from a twisted, bent and linear form to a linear form along with the increase of the temperature, and the ultra-long carbon nano tube with the length of 1cm and the diameter of 300nm is prepared. Experimental results show that the carbon order degree in the carbon nano-fiber is increased after the microwave high-temperature heat treatment, the graphene crystal content is increased, the length is obviously increased, and the carbon nano-fiber is directly converted into the ultra-long multi-walled carbon nano-tube with a perfect carbon structure.
Ratio of D Peak to G Peak (I)D/IG) Has been widely used for researching the microcrystalline structure of the carbon material, which is a method for quantifying the carbon sequence of the ultra-long multi-wall carbon nano tube. Fig. 4 shows the raman spectra of the ultra-long multi-walled carbon nanotubes, i.e. the variation of the graphitization (G) intensity and the disorder (D) intensity. It can be seen from fig. 4 that the G peak of the ultra-long multi-walled carbon nanotube increases with increasing temperature, the D peak intensity decreases, and the ID/IG ratio decreases with increasing temperature, at 1200 ℃, 1300 ℃ and 1400 ℃, 0.97, 0.87 and 0.84, respectively. The results show that the sample has better carbon order degree and higher graphitization degree at 1200 ℃.
Claims (8)
1. A method for preparing an ultralong multi-wall carbon nanotube by biomass through two-step microwave treatment is characterized by comprising the following steps:
(1) separation of cellulose samples from biomass by chemical pretreatment methods
Firstly, putting biomass into a vacuum drying oven, and drying at 100-110 ℃ for 10-14 h to remove moisture; adding strong base into the dried biomass, continuously stirring for 1.5-2.5 h at 85-95 ℃, dissolving lignin in the biomass, filtering and separating, and washing residues after alkali treatment with warm water; adding strong acid into the alkaline washing residue, heating for 1.5-2.5 h at 85-95 ℃, dissolving hemicellulose in the biomass, filtering and separating, washing the residue after acid treatment with warm water, putting the obtained residue into a vacuum drying oven, and drying for 20-30 h at 75-85 ℃ to obtain a cellulose sample;
(2) low-temperature microwave pyrolysis for generating biochar sample containing carbon nano-tubes
Uniformly mixing the cellulose sample obtained in the step (1) with a microwave absorbent, placing the mixture into a quartz reactor, placing the quartz reactor into microwave heating equipment, introducing nitrogen into the quartz reactor to remove air in the quartz reactor, and continuously introducing nitrogen in the reaction process, wherein the heating rate is controlled to be 10-100 ℃/min, the heating temperature is controlled to be 400-700 ℃, and the constant temperature is kept for 25-35 min to obtain a biochar sample containing carbon nanotubes;
(3) preparation of ultralong multi-walled carbon nanotubes by high-temperature microwave pyrolysis
And (3) putting the biochar sample containing the carbon nano tube obtained in the step (2) into a quartz reactor, then putting the quartz reactor into microwave heating equipment, introducing nitrogen into the quartz reactor to remove air in the quartz reactor, and continuously introducing the nitrogen in the reaction process, wherein the heating rate is controlled to be 8-12 ℃/min, the temperature is controlled to be 1000-1500 ℃, and the temperature is kept constant for 25-35 min, so that the ultra-long carbon nano tube is obtained.
2. The method for preparing the ultra-long multi-walled carbon nanotubes by the two-step microwave treatment of the biomass according to claim 1, wherein the biomass is coconut shells or pine nut shells.
3. The method for preparing the ultra-long multi-walled carbon nanotubes by two-step microwave treatment of biomass according to claim 1, wherein the strong base is 0.5 +/-0.05 mol/L sodium hydroxide or 0.5 +/-0.05 mol/L potassium hydroxide; the mass ratio of the biomass to the sodium hydroxide or the potassium hydroxide is 2: 1-5: 1.
4. The method for preparing ultra-long multi-walled carbon nanotubes from biomass through two-step microwave treatment according to claim 1, wherein the strong acid is 10% hydrochloric acid by volume or 10% sulfuric acid by volume; the mass ratio of the biomass to the hydrochloric acid or sulfuric acid is 1: 2-1: 5.
5. The method for preparing the ultra-long multi-walled carbon nanotubes by the biomass through two-step microwave treatment according to claim 1, wherein the particle size of the biomass is 150-280 μm.
6. The method for preparing the ultra-long multi-wall carbon nano-tubes by the two-step microwave treatment of the biomass as claimed in claim 1, wherein the nitrogen flow is 300ml/min to 500 ml/min.
7. The method for preparing the ultra-long multi-walled carbon nanotube by the two-step microwave treatment of the biomass as claimed in claim 1, wherein the mass ratio of the cellulose sample to the microwave absorbent is 10: 20-10: 0.1; the microwave absorbent is one or a mixture of any of activated carbon, silicon carbide and semicoke.
8. The method for preparing the ultra-long multi-walled carbon nanotube by the two-step microwave treatment of the biomass as claimed in claim 1, wherein the length of the ultra-long carbon nanotube is more than or equal to 1cm, and the diameter is 200nm to 400 nm.
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