CN109796007A - Micro-nano size biomass fiber and the suspension mixed preparation method of carbon nanotube - Google Patents

Micro-nano size biomass fiber and the suspension mixed preparation method of carbon nanotube Download PDF

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Publication number
CN109796007A
CN109796007A CN201910121823.2A CN201910121823A CN109796007A CN 109796007 A CN109796007 A CN 109796007A CN 201910121823 A CN201910121823 A CN 201910121823A CN 109796007 A CN109796007 A CN 109796007A
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suspension
biomass fiber
carbon nanotube
micro
nano
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CN109796007B (en
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张靠民
李如燕
王文俊
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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Abstract

The invention discloses a kind of micro-nano size biomass fibers and the suspension mixed preparation method of carbon nanotube, the method of the present invention is that biomass fiber powder is made to micro-nano biomass fiber suspension, carbon nanotube is added in micro-nano biomass fiber suspension again and is dispersed, micro-nano size biomass fiber and carbon nanotube mixing suspension is made;The mixing suspension can keep for a long time stable, provide material foundation for nanocomposite preparation, prepare for high-performance, functionalized nano composite material and provide a kind of simple process, nontoxic, the green low-cost technologies that are easy to implement.

Description

Micro-nano size biomass fiber and the suspension mixed preparation method of carbon nanotube
Technical field
The present invention relates to the processing of biomass fiber micro-nano and carbon nanotube to disperse suspension preparation field, specifically a kind of micro- Receive size biomass fiber and the suspension mixed preparation process of carbon nanotube.
Background technique
Carbon nanotube is all very high nano material of intensity and modulus, while also having electromagnetic property, in aerospace Material, automotive material and field of electronic devices have broad application prospects.As other nano materials, carbon nanotube, which has, to be held It is easy to reunite, be difficult to the characteristics of dispersing, this prepares associated materials for scale application carbon nanotube and brings difficulty, carbon nanotube it is equal Even dispersion is the main bugbear for restricting the application of its mass;Since being found from carbon nanotube, the equal of carbon nanotube how has been solved Even the dispersion just becomes the key problem that numerous researchers consider.
The dispersion of current carbon nanotube is mainly realized by following three kinds of modes.First is that acted on by strength mechanical shearing, The Van der Waals force between carbon nanotube is destroyed, has the function that dispersion.When the carbon nano tube dispersion liquid that this method obtains is stablized Between it is short, carbon nanotube can reunite again after a certain period of time;Second is that promote carbon nanotube to disperse by specific dispersing agent, this side Method dispersion effect is good, but due to introducing dispersing agent in carbon nano tube dispersion liquid, limits the application of carbon nanotube;Three It is that chemical modification is carried out to carbon nanotube, introduces function functional group, such as carboxyl, hydroxyl on its surface, pass through the work of functional group With dispersibility of the carbon nanotube in related solvents is increased, this method is limited to dispersion effect is increased.
Biomass fiber is widely present in tellurian plant, is from a wealth of sources, nexhaustible green resource.It is raw Material fibrils are mainly by three kinds of material compositions, and cellulose, hemicellulose and lignin, cellulose and hemicellulose are containing a large amount of The natural polymer of hydroxy functional group is the main raw material(s) of paper, biological plastics;The present invention is contained largely using biomass fiber The characteristics of cellulose and hemicellulose, prepares the biomass of micro-nano size using the method that chemical treatment and mechanical shearing combine Fibrous suspension prepares micro-nano size biomass fiber and carbon nanotube is mixed using this suspension as the dispersing agent of carbon nanotube Suspension is closed, provides material foundation to prepare biomass fiber and carbon nanotube as the polymer matrix composite of reinforced phase. The present invention is characterized in that the biomass fiber suspension that micro-nano is handled is used as the dispersing agent of carbon nanotube, this and other dispersions Agent will not influence the performance of carbon nanotube the difference is that biomass fiber can be used as a kind of component of material.
Summary of the invention
The present invention provides a kind of micro-nano size biomass fiber and the suspension mixed preparation method of carbon nanotube, this hairs Bright method has many advantages, such as that simple process, manufacturing cost be low, green non-pollution, for preparing High-performance green polymer composite Material has important practical usage.
Steps are as follows for micro-nano size biomass fiber of the present invention and the suspension mixed preparation method of carbon nanotube:
(1) biomass fiber is mechanically pulverized, is sieved, obtains biomass fiber powder of the partial size less than 200 μm;
(2) step (1) biomass fiber powder is subjected to swelling treatment, biomass fiber powder mixed liquor is made;
(3) step (2) biomass fiber powder mixed liquor is placed into 10~40min at -3 DEG C~-12 DEG C;
(4) high speed shear processing will be carried out through the mixed liquor of step (3) freezing processing, will then carry out mixed liquor at grinding shearing Reason, obtains micro-nano biomass fiber suspension;
(5) aqueous solution of step (4) micro-nano biomass fiber suspension deionized water or low molecule alcohol compound is handled, Obtaining pH value is neutral suspension, is then allowed to stand, supernatant is taken out spare;
It is handled and is referred to deionized water or low molecule alcohol compound with the aqueous solution of deionized water or low molecule alcohol compound Aqueous solution by micro-nano biomass fiber suspension dilute 2~3 times, then filter, filter residue deionized water or low molecule alcohol The aqueous solution of compound dilutes, filtering, until suspension is in neutrality;
(6) carbon nanotube is added in step (5) supernatant, then carries out decentralized processing, until carbon nanotube is evenly dispersed Until, obtain finely dispersed carbon nano tube suspension;
(7) step (6) carbon nano tube suspension is added in step (5) after taking out supernatant in remaining suspension, is carried out Decentralized processing obtains micro-nano size biomass fiber and carbon nanotube mixing suspension until carbon nanotube is evenly dispersed, Wherein mass fraction of the carbon nanotube in mixing suspension is 0.01%~0.6%, and micro-nano size biomass fiber is outstanding in mixing Mass fraction in supernatant liquid is 0.1%~6%.
Swelling treatment is to prepare the mixed aqueous solution of sodium hydroxide and urea, the quality of sodium hydroxide in the step (2) Score is 3%~12%, the mass fraction of urea is 1.5%~7%;Then biomass fiber powder is added to sodium hydroxide and urine 30~60min is handled in the mixed aqueous solution of element, and biomass fiber powder mixed liquor, the quality point of biomass fiber powder is made Number is 0.1%~6%.
High speed shear processing be in the case where high-speed shearing machine revolving speed is the r/min of 2000r/min~12000 processing 3~ 5min。
The aqueous solution of the low molecule alcohol compound is methanol aqueous solution or ethanol water.
The biomass fiber powder can be the various plant fiber powders such as wood powder, coffee shell powder, sisal hemp powder, ramie powder End.
It is the biomass fiber containing nano-scale in the micro-nano size biomass fiber suspension, also contains micron meter Very little biological paper fiber.
The grinding shear treatment can be accomplished in several ways, such as but be not limited to following method: grinder is ground Mill, homogenizer homogenizing etc..
The decentralized processing can realize through various ways, such as but be not limited to following method: ultrasonic treatment, machinery stir It mixes.
The advantages of the method for the present invention and technical effect:
The present invention provides a kind of simple process, manufacturing cost is low, carbon nanotube of green non-pollution and biomass fiber mixing Suspension manufacturing methods, mixing suspension made from the method for the present invention can keep for a long time stable, and biomass fiber is both carbon The decentralized medium of nanotube, while being a kind of green material again, this provides material foundation for nanocomposite preparation, simplifies Preparation process, for high-performance, the preparation of functionalized nano composite material provide a kind of simple process, it is nontoxic, be easy to implement Green low-cost technologies.
Specific embodiment
Below by embodiment, invention is further described in detail, but the scope of the present invention is not limited in described Hold.
Embodiment 1: using sisal fiber and carbon nanotube prepares micro-nano size biomass fiber as raw material and carbon nanotube is mixed Suspension is closed, steps are as follows:
(1) sisal fiber is crushed in plant pulverizer, then crosses the sieve of 100 mesh, obtains sisal hemp of the partial size less than 200 μm Powder;
(2) mixed aqueous solution of sodium hydroxide and urea is prepared, the mass fraction of sodium hydroxide is 4%, the mass fraction of urea is 2%;
(3) it by the sisal hemp powder of step (1), is added in the mixed aqueous solution of sodium hydroxide and urea and handles 40min, life is made Material fibrils powder mixed liquor, the mass fraction of biomass fiber powder are 3%;
(4) step (3) biomass fiber powder mixed liquor is placed under -12 DEG C of environment and places 20min;
(5) mixed liquor through step (4) freezing processing the progress high speed shear at 2000r/min is placed in high-speed shearing machine to mix 3min is closed, is subsequently placed in planetary ball mill and grinds, drum's speed of rotation 500r/min, milling time 4h;Obtain micro-nano ruler Very little sisal fiber suspension;
(6) after suspension being diluted 2 times by step (5) micro-nano size sisal fiber suspension deionized water, filtering, then be resuspended Filtration washing is then allowed to stand, supernatant is taken out spare until obtaining pH value is neutral suspension;
(6) carbon nanotube is added in step (5) supernatant, then carries out decentralized processing, until carbon nanotube is evenly dispersed Until, obtain finely dispersed carbon nano tube suspension;
(7) step (6) carbon nano tube suspension is added in step (5) after taking out supernatant in remaining suspension, is carried out Decentralized processing obtains micro-nano size biomass fiber and carbon nanotube mixing suspension until carbon nanotube is evenly dispersed, Wherein mass fraction of the carbon nanotube in mixing suspension is 0.05%, and micro-nano size biomass fiber is in mixing suspension Mass fraction be 3%.
Through observing, the micro-nano size biomass fiber and carbon nanotube mixing suspension of above-mentioned preparation have good stability, room The lower standing of temperature is still uniformly dispersed for 24 hours.
Embodiment 2: using wood powder and carbon nanotube prepares micro-nano size biomass fiber as raw material and carbon nanotube is mixed and hanged Supernatant liquid, steps are as follows:
(1) wood-fibred is crushed in plant pulverizer, then crosses the sieve of 100 mesh, obtains wood powder of the partial size less than 200 μm;
(2) mixed aqueous solution of sodium hydroxide and urea is prepared, the mass fraction of sodium hydroxide is 8%, the mass fraction of urea is 5%;
(3) it by the wood powder of step (1), is added in the mixed aqueous solution of sodium hydroxide and urea and handles 50min, biomass is made Fiber dust mixed liquor, the mass fraction of biomass fiber powder are 0.5%;
(4) step (3) biomass fiber powder mixed liquor is placed under -6 DEG C of environment and places 30min;
(5) mixed liquor through step (4) freezing processing the progress high speed shear at 500r/min is placed in high-speed shearing machine to mix 5min is closed, is subsequently placed in planetary ball mill and grinds, drum's speed of rotation 800r/min, milling time 3h;Obtain micro-nano ruler Very little wood-fibred suspension;
(6) after suspension being diluted 3 times by step (5) micro-nano sized wood fiber suspension ethanol water, filtering, then be resuspended Filtration washing is then allowed to stand, supernatant is taken out spare until obtaining pH value is neutral suspension;
(6) carbon nanotube is added in step (5) supernatant, then carries out decentralized processing, until carbon nanotube is evenly dispersed Until, obtain finely dispersed carbon nano tube suspension;
(7) step (6) carbon nano tube suspension is added in step (5) after taking out supernatant in remaining suspension, is carried out Decentralized processing obtains micro-nano size biomass fiber and carbon nanotube mixing suspension until carbon nanotube is evenly dispersed, Wherein mass fraction of the carbon nanotube in mixing suspension is 0.1%, and micro-nano size biomass fiber is in mixing suspension Mass fraction is 0.5%.
Through observing, the micro-nano size wood powder fiber and carbon nano tube suspension of embodiment preparation have good stability, room temperature Lower standing is still uniformly dispersed for 24 hours.
Embodiment 3: using ramie and carbon nanotube prepares micro-nano size biomass fiber as raw material and carbon nanotube is mixed and hanged Supernatant liquid, steps are as follows:
(1) ramee is crushed in plant pulverizer, then crosses the sieve of 100 mesh, obtains ramie of the size less than 200 microns Numb powder;
(2) mixed aqueous solution of sodium hydroxide and urea is prepared, the mass fraction of sodium hydroxide is the mass fraction of 10%, urea It is 6%;
(3) it by the ramie powder of step (1), is added in the mixed aqueous solution of sodium hydroxide and urea and handles 60min, biology is made Matter fiber dust mixed liquor, the mass fraction of biomass fiber powder are 4%;
(4) step (3) biomass fiber powder mixed liquor is placed under -3 DEG C of environment and places 40min;
(5) mixed liquor through step (4) freezing processing the progress high speed shear at 8000r/min is placed in high-speed shearing machine to mix 4min is closed, then homogenizing is handled in homogenizer, and homogenization pressures are 15MPa~20MPa, obtains the suspension of micro-nano size ramee Liquid;
(6) after suspension being diluted 2 times by step (5) micro-nano size sisal fiber suspension deionized water, filtering, then be resuspended Filtration washing is then allowed to stand, supernatant is taken out spare until obtaining pH value is neutral suspension;
(6) carbon nanotube is added in step (5) supernatant, then carries out decentralized processing, until carbon nanotube is evenly dispersed Until, obtain finely dispersed carbon nano tube suspension;
(7) step (6) carbon nano tube suspension is added in step (5) after taking out supernatant in remaining suspension, is carried out Decentralized processing obtains micro-nano size biomass fiber and carbon nanotube mixing suspension until carbon nanotube is evenly dispersed, Wherein mass fraction of the carbon nanotube in mixing suspension is 0.6%, and micro-nano size biomass fiber is in mixing suspension Mass fraction is 4%.
Through observing, the micro-nano size ramee and carbon nano tube suspension of above-mentioned preparation have good stability, quiet at room temperature It sets 72 hours and is still uniformly dispersed.
Embodiment 4: using ramie and carbon nanotube prepares micro-nano size biomass fiber as raw material and carbon nanotube mixes second Alcohol suspension, steps are as follows:
(1) ramee is crushed in plant pulverizer, then crosses the sieve of 100 mesh, obtains ramie of the size less than 200 microns Numb powder;
(2) mixed aqueous solution of sodium hydroxide and urea is prepared, the mass fraction of sodium hydroxide is the mass fraction of 12%, urea It is 3%;
(3) it by the ramie powder of step (1), is added in the mixed aqueous solution of sodium hydroxide and urea and handles 45min, biology is made Matter fiber dust mixed liquor, the mass fraction of biomass fiber powder are 2%;
(4) step (3) biomass fiber powder mixed liquor is placed under -5 DEG C of environment and places 25min;
(5) mixed liquor through step (4) freezing processing is placed in high-speed shearing machine at 10000r/min and carries out high speed shear Mixing, then homogenizing is handled in homogenizer, and homogenization pressures are 15MPa~20MPa, obtains the suspension of micro-nano size ramee Liquid;
(6) after suspension being diluted 2 times by step (5) micro-nano size sisal fiber suspension ethanol water, filtering, then weigh Outstanding filtration washing is then allowed to stand, supernatant is taken out spare until obtaining pH value is neutral suspension;
(6) carbon nanotube is added in step (5) supernatant, then carries out decentralized processing, until carbon nanotube is evenly dispersed Until, obtain finely dispersed carbon nano tube suspension;
(7) step (6) carbon nano tube suspension is added in step (5) after taking out supernatant in remaining suspension, is carried out Decentralized processing obtains micro-nano size biomass fiber and carbon nanotube mixing suspension until carbon nanotube is evenly dispersed, Wherein mass fraction of the carbon nanotube in mixing suspension is 0.2%, and micro-nano size biomass fiber is in mixing suspension Mass fraction is 2%.
Through observing, the micro-nano size wood powder fiber and carbon nano tube suspension of embodiment preparation have good stability, room temperature Lower standing is still uniformly dispersed for 72 hours.

Claims (5)

1. a kind of micro-nano size biomass fiber and the suspension mixed preparation method of carbon nanotube, which is characterized in that step is such as Under:
(1) biomass fiber is mechanically pulverized, is sieved, obtains biomass fiber powder of the partial size less than 200 μm;
(2) step (1) biomass fiber powder is subjected to swelling treatment, biomass fiber powder mixed liquor is made;
(3) step (2) biomass fiber powder mixed liquor is placed into 10~40min at -3 DEG C~-12 DEG C;
(4) high speed shear processing will be carried out through the mixed liquor of step (3) freezing processing, will then carry out mixed liquor at grinding shearing Reason, obtains micro-nano biomass fiber suspension;
(5) aqueous solution of step (4) micro-nano biomass fiber suspension deionized water or low molecule alcohol compound is handled, Obtaining pH value is neutral suspension, is then allowed to stand, supernatant is taken out spare;
(6) carbon nanotube is added in step (5) supernatant, then carries out decentralized processing, until carbon nanotube is evenly dispersed Until, obtain finely dispersed carbon nano tube suspension;
(7) step (6) carbon nano tube suspension is added in step (5) after taking out supernatant in remaining suspension, is carried out Decentralized processing obtains micro-nano size biomass fiber and carbon nanotube mixing suspension until carbon nanotube is evenly dispersed, Wherein mass fraction of the carbon nanotube in mixing suspension is 0.01%~0.6%, and micro-nano size biomass fiber is outstanding in mixing Mass fraction in supernatant liquid is 0.1%~6%.
2. micro-nano size biomass fiber according to claim 1 and the suspension mixed preparation method of carbon nanotube, Be characterized in that: swelling treatment is to prepare the mixed aqueous solution of sodium hydroxide and urea, the mass fraction of sodium hydroxide in step (2) Mass fraction for 3%~12%, urea is 1.5%~7%;Then biomass fiber powder is added to sodium hydroxide and urea 30~60min is handled in mixed aqueous solution, biomass fiber powder mixed liquor is made, and the mass fraction of biomass fiber powder is 0.1%~6%.
3. micro-nano size biomass fiber according to claim 1 and the suspension mixed preparation method of carbon nanotube, Be characterized in that: high speed shear processing is to handle 3~5min in the case where high-speed shearing machine revolving speed is the r/min of 2000r/min~12000.
4. micro-nano size biomass fiber according to claim 1 and the suspension mixed preparation method of carbon nanotube, Be characterized in that: the aqueous solution of low molecule alcohol compound is methanol aqueous solution or ethanol water.
5. micro-nano size biomass fiber according to claim 1 and the suspension mixed preparation method of carbon nanotube, Be characterized in that: biomass fiber powder is wood powder, coffee shell powder, sisal hemp powder or ramie powder.
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CN116239385A (en) * 2023-02-10 2023-06-09 中国科学院金属研究所 3D printing silicon carbide slurry suitable for ink direct writing technology and preparation thereof

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CN112591736A (en) * 2020-12-16 2021-04-02 四川大学 Novel method for dispersing carbon nano-tubes with assistance of cellulose
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CN116239385A (en) * 2023-02-10 2023-06-09 中国科学院金属研究所 3D printing silicon carbide slurry suitable for ink direct writing technology and preparation thereof

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