CN105884356A - Preparation method of carbon nanorod aerogel based on nanocellulose - Google Patents
Preparation method of carbon nanorod aerogel based on nanocellulose Download PDFInfo
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- CN105884356A CN105884356A CN201610233211.9A CN201610233211A CN105884356A CN 105884356 A CN105884356 A CN 105884356A CN 201610233211 A CN201610233211 A CN 201610233211A CN 105884356 A CN105884356 A CN 105884356A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/524—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/624—Sol-gel processing
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
Abstract
The invention discloses a preparation method of carbon nanorod aerogel based on nanocellulose and belongs to the field of preparation of capacitive deionized electrode materials. According to the preparation method, nanocellulose hydrogel is taken as a precursor, and ultralight carbon nanorod aerogel adopting a layered pore structure is obtained through freeze drying and high-temperature carbonization. The preparation method has the advantages as follows: (1) the nanocellulose hydrogel is taken as the precursor and has the advantages of being low in cost, high in content in nature, inexhaustible and the like; (2) the preparation method is simple, the process is short, the conditions are mild, and industrial production is facilitated; (3) the carbon nanorod aerogel has excellent capacitive deionization performance.
Description
Technical field
The present invention relates to capacitive deionization electrode material field, particularly to a kind of carbon nano rod based on nano-cellulose
Aeroge application in capacitive deionization field.
Background technology
Capacitive deionization (Capacitive deionization, CDI) is also referred to as electro-adsorption, be the sixties in last century with
Come along with porous carbon materials fast-developing start that one the most in widespread attention is efficient, energy-conservation, sustainable, low cost,
Eco-friendly novel desalting technology.Along with population expansion expands rapidly with industrial and agricultural production scale, whole world fresh water dosage is at full speed
Increase.Fresh water imbalance between supply and demand becomes increasingly conspicuous.But, the water resource in the whole world more than 98% is all the sea water or hardship not directly utilized
Salt water, this allows for desalinization becomes the approach being hopeful most to solve World Water crisis.Traditional desalting technology include flash distillation,
The methods such as reverse osmosis, electrodialysis and ion exchange, owing to its high energy consumption, secondary pollution, film fouling and water use efficiency are too low etc.
Problem makes too high Financial cost become its obstacle realizing desalinization.CDI technology is with its high efficiency, low energy consumption, environment
The advantages such as friendly, high water use efficiency become one of the most promising desalting technology.Electrode material as CDI technological core affect because of
Element receives mondial extensive concern all the time.Therefore, CDI technology based on new electrode materials is carried out further
Theory and applied research, the most important scientific value, the broad prospect of application more having in human social development and
Realistic meaning.
Cellulose is one of most important natural polymer of finding so far, and one is the most inexhaustible especially, use
Inexhaustible raw material, this has also become a kind of continuable material being excellently suitable for industrialized production.Nanocrystalline fiber
Element, also referred to as Cellulose nanocrystal body, it is common that the bar-like single crystal cellulose of a diameter of 1-100nm, generally led to by natural fiber
The strong acid hydrolysis such as persulfuric acid and obtain.Have environmental friendliness, low cost, specific surface is high, functional group is numerous and mechanical strength is high etc. excellent
Gesture.But, for conventional carbon material, the electric conductivity of nano-cellulose is relatively poor, then, and some research and utilization nanometers
Cellulose prepares carbon nanomaterial as template or carbon source, and be applied to lithium ion battery and ultracapacitor (J. Solid State Electrochem., 2013, 17, 575-581；Angew. Chem. Int. Ed., 2011, 50, 10991- 10995; Electrochim. Acta, 2014, 138, 139-147; J. Mater. Chem. A, 2014, 2, 5915-5921).Such as, Shopsowitz etc. utilize nano-cellulose to be prepared for Jie of high-ratio surface for stay in place form and carbon source
Hole C film the electrode material as ultracapacitor, it is thus achieved that the ratio electric capacity of 170 F/g.Afterwards, Pan et al. utilizes nanometer
Cellulose is prepared for carbon nano rod as template, and is applied to CDI field as electrode material, has obtained preferable electricity and has inhaled
Attached performance (Chem. Commun., 2015, 51, 12020-12023).But, up to the present, also not about based on receiving
The relevant report of the carbon nano rod aeroge of rice cellulose.
Summary of the invention
It is an object of the invention to propose a kind of method that technique is simple, experiment flow is short, preparation condition is gentle and prepare carbon
Nanometer rods aeroge, and it is applied to capacitive deionization field.Additionally, the present invention utilize raw material be environmental friendliness, cost
Nano cellulose material low, that specific surface is high, functional group is numerous and mechanical strength is high, is a significant benefit to this carbon nano rod aeroge
The realization of industrialization.
The concrete technical scheme realizing the object of the invention is:
The preparation method of a kind of carbon nano rod aeroge based on nano-cellulose, feature is that the method includes walking in detail below
Rapid:
(1) utilize ultrasonic cell disrupte machine to be dispersed in deionized water in nano-cellulose powder, obtain transparent nanometer
Cellulose aquagel；Wherein, nano-cellulose weight content is 20-50wt%, ultrasonic procedure: within the most ultrasonic 20 minutes, suspend 5 points
Clock, ultrasonic five circulations；
(2) the nanofiber hydrogel obtained is placed in quick freeze in-35 to-50 DEG C of ultra cold storage freezers, and keeps freezing
24～48 hours, the sample freezed being transferred quickly in freezer dryer lyophilization 24～48 hours afterwards, temperature sets
Being set to-53 DEG C, pressure is set to 5～10pa, obtains nano-cellulose aerogel；
(3) nano-cellulose aerogel obtained is slit into rectangle, circle or rhombus earnestly, is subsequently placed in tube furnace
Carry out ladder-elevating temperature carbonization, with 2 DEG C/min of ramp to after 250 DEG C, rise to target temperature with the heating rate of 5 DEG C/min
Degree, and it is incubated 2 hours, finally give described carbon nano rod aeroge；Described target temperature is 600-1000 DEG C.
Carbon nano rod aeroge prepared by the present invention is a kind of efficient capacitive deionization electrode material.
It is an advantage of the current invention that:
(1) present invention utilizes nanofiber hydrogel as presoma, has low cost, nature content high, inexhaustible
The advantage such as nexhaustible；
(2) preparation method of the carbon nano rod aeroge of the present invention is simple, and flow process is short, mild condition, is suitable for industrialized production.
(3) this carbon nano rod aeroge has the capacitive deionization performance of excellence.
Accompanying drawing explanation
Fig. 1 is the carbon nano rod aeroge digital photograph figure that the embodiment of the present invention 1 obtains；
Fig. 2 is the carbon nano rod aeroge stereoscan photograph figure that the embodiment of the present invention 1 obtains；
Fig. 3 is the carbon nano rod aeroge transmission electron microscope photo figure that the embodiment of the present invention 1 obtains；
Fig. 4 is the Raman spectrogram of the carbon nano rod aeroge that different carburizing temperatures obtain in embodiment of the present invention 1-3；
Fig. 5 is the N of the carbon nano rod aeroge that different carburizing temperatures obtain in embodiment of the present invention 1-32Adsorption/desorption curve chart；
Fig. 6 is the carbon nano rod aeroge of 600 DEG C of carbonization acquisitions electricity in variable concentrations NaCl solution in the embodiment of the present invention 1
Hold deionization performance chart；
The carbon nano rod aeroge of 800 DEG C of carbonization acquisitions electric capacity in variable concentrations NaCl solution in Fig. 7 embodiment of the present invention 2
Deionization performance chart；
The carbon nano rod aeroge of 1000 DEG C of carbonization acquisitions electricity in variable concentrations NaCl solution in Fig. 8 embodiment of the present invention 3
Hold deionization performance chart.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further elaborated.Should be understood that these embodiments are only used for
The bright present invention rather than be used for limiting the scope of the present invention.
Embodiment 1
1) preparation of carbon nano rod aeroge
Nano-cellulose powder utilizes ultrasonic cell disrupte machine be dispersed in deionized water at normal temperatures, and (30 wt% surpass
Sound process: suspend 5 minutes in the most ultrasonic 20 minutes, ultrasonic five circulations), obtain transparent nanofiber hydrogel.Will preparation
Good nanofiber hydrogel is placed in quick freeze in ultra cold storage freezer (-50 DEG C), and keeps freezing 48 hours, afterwards will
The sample freezed is transferred quickly to lyophilization in freezer dryer, and within 48 hours, (temperature is set to-53 DEG C, and pressure is set to
8pa), nano-cellulose aerogel is obtained.The rectangle that the nano-cellulose aerogel prepared cuts into 8 × 8 cm is placed in
In tube furnace, be warming up to 250 DEG C with 2 DEG C/min, after rise to 600 DEG C with the heating rate of 5 DEG C/min, and be incubated 2 hours,
Obtaining carbon nano rod aeroge eventually, be labeled as CNRA600, its digital photograph is shown in Fig. 1, uses field emission scanning electron microscope
(FESEM, Hitachi S-4800) and transmission electron microscope (TEM, M200) are to the pattern of carbon nano rod aeroge and structure
Characterizing, stereoscan photograph is shown in that Fig. 2, transmission electron microscope photo are shown in Fig. 3.
2) capacitive deionization experiment
The carbon nano rod aeroge prepared is entered among CDI device directly as electrode assembling.Subsequently, respectively by the beginning of 50 ml
Beginning concentration is that the NaCl solution of 100,200,500 mg/l is circulated in CDI device with 50 flow velocitys of ml/ minute, additional
Voltage is set to 1.2 V.Indirectly recorded the concentration of solution by the electrical conductivity of detection solution, experimental result is shown in Fig. 6.
Embodiment 2
1) preparation of carbon nano rod aeroge
Nano-cellulose powder utilizes ultrasonic cell disrupte machine be dispersed in deionized water at normal temperatures, and (50 wt% surpass
Sound process: suspend 5 minutes in the most ultrasonic 20 minutes, ultrasonic five circulations), finally give transparent nanofiber hydrogel.Will
The nanofiber hydrogel prepared is placed in quick freeze in ultra cold storage freezer (-50 DEG C), and keeps freezing 40 hours, afterwards
The sample freezed is transferred quickly to lyophilization in freezer dryer, and within 40 hours, (temperature is set to-53 DEG C, and pressure is set to
10pa), nano-cellulose aerogel is obtained.The nano-cellulose aerogel prepared is cut into the rectangle juxtaposition of 8 × 8 cm
In tube furnace, be warming up to 250 DEG C with 2 DEG C/min, after rise to 800 DEG C with the heating rate of 5 DEG C/min, and it is little to be incubated 2
Time, finally give carbon nano rod aeroge, be labeled as CNRA800.
2) capacitive deionization experiment
The carbon nano rod aeroge prepared is entered among CDI device directly as electrode assembling.Subsequently, respectively by the beginning of 50 ml
Beginning concentration is that the NaCl solution of 100,200,500 mg/l is circulated in CDI device with 50 flow velocitys of ml/ minute, additional
Voltage is set to 1.2 V.Recording the concentration of solution between the electrical conductivity by detection solution, experimental result is shown in Fig. 7.
Embodiment 3
1) preparation of carbon nano rod aeroge
Nano-cellulose powder utilizes ultrasonic cell disrupte machine be dispersed in deionized water at normal temperatures, and (30 wt% surpass
Sound process: suspend 5 minutes in the most ultrasonic 20 minutes, ultrasonic five circulations), finally give transparent nanofiber hydrogel.Will
The nanofiber hydrogel prepared is placed in quick freeze in ultra cold storage freezer (-35 DEG C), and keeps freezing 38 hours, afterwards
The sample freezed is transferred quickly to lyophilization in freezer dryer, and within 38 hours, (temperature is set to-53 DEG C, and pressure is arranged
For 8pa), obtain nano-cellulose aerogel.The nano-cellulose aerogel prepared is cut into the rectangle juxtaposition of 8 × 8 cm
In tube furnace, be warming up to 250 DEG C with 2 DEG C/min, after rise to 1000 DEG C with the heating rate of 5 DEG C/min, and it is little to be incubated 2
Time, finally give carbon nano rod aeroge, be labeled as CNRA1000.
2) capacitive deionization experiment
The carbon nano rod aeroge prepared is entered among CDI device directly as electrode assembling.Subsequently, respectively by the beginning of 50 ml
Beginning concentration is that the NaCl solution of 100,200,500 mg/l is circulated in CDI device with 50 flow velocitys of ml/ minute, additional
Voltage is set to 1.2 V.Indirectly recorded the concentration of solution by the electrical conductivity of detection solution, experimental result is shown in Fig. 8.
Raman spectrum (Raman, Renishaw in Via) is used to analyze different carburizing temperature carbon nano rod aeroge
Defect and crystal structure, result is shown in Fig. 4.The mode that the surface apertures of carbon nano rod aeroge utilizes nitrogen adsorption to be desorbed uses
ASAP2020 surface area and pore analysis instrument (Micrometitics, Norcross, GA) are characterized, and result is shown in Fig. 5 and Biao
1。
The different specific surface areas of carbon nano rod aeroge, total pore volume and average pore size in table 1 embodiment of the present invention.
Claims (1)
1. the preparation method of a carbon nano rod aeroge based on nano-cellulose, it is characterised in that the method includes following tool
Body step:
(1) utilize ultrasonic cell disrupte machine to be dispersed in deionized water in nano-cellulose powder, obtain transparent nanometer
Cellulose aquagel；Wherein, nano-cellulose is 20-50wt%, ultrasonic procedure: within the most ultrasonic 20 minutes, suspend 5 minutes, ultrasonic five
Individual circulation；
(2) the nanofiber hydrogel obtained is placed in quick freeze in-35 to-50 DEG C of ultra cold storage freezers, and keeps freezing
24～48 hours, the sample freezed being transferred quickly in freezer dryer lyophilization 24～48 hours afterwards, temperature sets
Being set to-53 DEG C, pressure is set to 5～10pa, obtains nano-cellulose aerogel；
(3) nano-cellulose aerogel obtained is slit into rectangle, circle or rhombus earnestly, is subsequently placed in tube furnace
Carry out ladder-elevating temperature carbonization, with 2 DEG C/min of ramp to after 250 DEG C, rise to target temperature with the heating rate of 5 DEG C/min
Degree, and it is incubated 2 hours, finally give described carbon nano rod aeroge；Described target temperature is 600-1000 DEG C.
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Cited By (6)
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|---|---|---|---|---|
| CN106495671A (en) * | 2016-10-12 | 2017-03-15 | 武汉理工大学 | Cellulose nanocrystal modified ceramic base substrate and preparation method thereof |
| CN106824080A (en) * | 2017-03-03 | 2017-06-13 | 中国科学院理化技术研究所 | A kind of high absorption property carbon aerogels and its preparation method and application |
| CN110606747A (en) * | 2019-10-16 | 2019-12-24 | 西北工业大学 | Preparation method of isotropic ceramic nanowire preform |
| CN111204831A (en) * | 2020-01-19 | 2020-05-29 | 陕西科技大学 | CNF-based homologous heterogeneous photothermal material for seawater desalination and preparation method thereof |
| CN111613828A (en) * | 2020-06-04 | 2020-09-01 | 武汉理工大学 | Batch preparation method of micro energy storage devices on flexible film substrate |
| CN114853126A (en) * | 2022-04-29 | 2022-08-05 | 青岛科技大学 | Carbon fiber aerogel protected bismuth nanocluster and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106495671A (en) * | 2016-10-12 | 2017-03-15 | 武汉理工大学 | Cellulose nanocrystal modified ceramic base substrate and preparation method thereof |
| CN106495671B (en) * | 2016-10-12 | 2019-04-30 | 武汉理工大学 | Cellulose nanocrystal modified ceramic green body and preparation method thereof |
| CN106824080A (en) * | 2017-03-03 | 2017-06-13 | 中国科学院理化技术研究所 | A kind of high absorption property carbon aerogels and its preparation method and application |
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| CN110606747A (en) * | 2019-10-16 | 2019-12-24 | 西北工业大学 | Preparation method of isotropic ceramic nanowire preform |
| CN110606747B (en) * | 2019-10-16 | 2021-09-07 | 西北工业大学 | Preparation method of isotropic ceramic nanowire preform |
| CN111204831A (en) * | 2020-01-19 | 2020-05-29 | 陕西科技大学 | CNF-based homologous heterogeneous photothermal material for seawater desalination and preparation method thereof |
| CN111613828A (en) * | 2020-06-04 | 2020-09-01 | 武汉理工大学 | Batch preparation method of micro energy storage devices on flexible film substrate |
| CN114853126A (en) * | 2022-04-29 | 2022-08-05 | 青岛科技大学 | Carbon fiber aerogel protected bismuth nanocluster and preparation method thereof |
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Application publication date: 20160824 |