CN110963483B - Aqueous carbon nanotube dispersion and preparation method thereof - Google Patents
Aqueous carbon nanotube dispersion and preparation method thereof Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
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- C01B2202/00—Structure or properties of carbon nanotubes
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Abstract
The invention relates to a water-based carbon nanotube dispersion liquid and a preparation method thereof, and the preparation method comprises the following steps: respectively weighing water, carbon nano tubes, a dispersing agent and a stabilizing agent for later use; the water content N for standby1Then the carbon nano tube is stirred and mixed with the carbon nano tube,obtaining a mixture A in which N1Is an integer of 2 or more; dividing the dispersant into N2Stirring and mixing with the mixture A to obtain a mixture B, wherein N is2Is an integer of 2 or more; and grinding the mixture B and the spare stabilizer to obtain the water-based carbon nanotube dispersion liquid. The carbon nano tube dispersion liquid prepared by the method can greatly reduce the viscosity of the dispersion liquid in the dispersion process and improve the preparation efficiency of the dispersion liquid, and the method has simple process, cleanness and environmental protection.
Description
Technical Field
The invention belongs to the technical field of carbon nanotube dispersion liquid, and particularly relates to a water-based carbon nanotube dispersion liquid and a preparation method thereof.
Background
Carbon nanotubes have unique structures, so that they have good physicochemical properties, electrical conductivity and mechanical properties, and thus are favored by scientists and enterprises, where the diameter of a carbon nanotube is only a few to tens of nanometers, and the length is on the order of a few micrometers to millimeters. Test results show that the carbon nano tube has excellent mechanical properties, the elastic modulus reaches 1Tpa (about 5 times of steel), the density is about 1/6 of the steel, and the elastic strain reaches 60 times of the steel; the carbon nano tube also has good conductivity, and when the carbon nano tube is added into a high polymer material, the resistance of the material can be reduced by more than three orders of magnitude, and the carbon nano tube is used for storing hydrogen, which is also a hot problem of research.
However, due to the nanometer size effect and the large aspect ratio, the van der waals force between the carbon nanotubes is very strong, so that the carbon nanotubes are extremely easy to agglomerate and wind in the dispersion process, and finally the exertion of the excellent performance of the carbon nanotubes is seriously hindered. The carbon nano tube aqueous dispersion liquid has long processing time, low preparation efficiency, high preparation cost and the like due to extremely high viscosity in the preparation process, and the wide application of the carbon nano tube aqueous dispersion liquid is seriously restricted.
Therefore, it is desired to fully utilize the excellent properties of the carbon nanotubes and to widely popularize and apply the carbon nanotubes, and it is important and critical to solve the problem of high viscosity during the dispersion process of the carbon nanotubes.
The present invention has been made in view of the above circumstances.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the water-based carbon nanotube dispersion and the preparation method thereof, the viscosity of the dispersion in the dispersion process can be greatly reduced, the preparation efficiency of the dispersion is improved, and the method is simple in process, clean and environment-friendly.
The first purpose of the invention is to provide a preparation method of an aqueous carbon nanotube dispersion, which comprises the following steps:
(1) respectively weighing water, carbon nano tubes, a dispersing agent and a stabilizing agent for later use;
(2) the water content N for standby1Stirring and mixing with the carbon nano tube to obtain a mixture A, wherein N is1Is an integer of 2 or more;
(3) dividing the dispersant into N2Stirring and mixing with the mixture A to obtain a mixture B, wherein N is2Is an integer of 2 or more;
(4) and grinding the mixture B and the spare stabilizer to obtain the water-based carbon nanotube dispersion liquid.
Further, the mass ratio of the water, the carbon nano tube, the dispersing agent and the stabilizing agent in the step (1) is 90-97:3-8:1-5: 1-5.
Further, step (2) Water N1The mass of each time the carbon nanotubes are mixed is the same or different.
Further, the first mixing is carried out by adding the carbon nano tube into water at the stirring speed of 300-500rpm within 1.5-2.5min, dispersing for 8-12min at the speed of 500-700rpm, adding water for the second time or more, and then stirring by adopting a dispersion disc at the stirring speed of 500-1500rpm for 8-12 min.
The inventor of the invention finds that the mixing of the water after the first water addition is not specially limited as long as the mixing purpose can be achieved, such as simple stirring, grinding and the like, and the water after the second water addition and above times needs to be stirred by a dispersion plate, the size of the dispersion plate is not less than 10% of the cross section of the container, the viscosity of the prepared mixture can be low at the stirring speed of the invention, the subsequent dispersant addition is facilitated, the viscosity of the dispersion liquid is reduced, and the preparation efficiency of the dispersion liquid is improved.
Further, dispersing agent N in step (3)2The mass of each time of mixing with the mixture A is the same or different.
Further, the dispersant is stirred and mixed with the mixture A for the first time and then is ground, the grinding speed is 800-1200rpm, the dispersant is added for the second time after the grinding times are 5-20 times, and then grinding is carried out, and the steps are repeated until the dispersant is completely added.
Further, the water is ultrapure water, and the resistivity of the ultrapure water at 25 ℃ is not less than 18M omega cm.
Further, the diameter of the carbon nano tube is 0.4-100nm, preferably, the diameter is 5-15nm, the length is 1-50 μm, preferably, the length is 10-20 μm.
The carbon nanotube used in the present invention is not particularly limited, and any carbon nanotube conventionally used in the art may be used. Carbon nanotubes of one or more of single-walled carbon nanotubes, double-walled carbon nanotubes, and multi-walled carbon nanotubes may be employed.
Further, the dispersant is one or more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, polyacrylamide, polysorbate, sorbitan fatty ester, sodium cellulose, 2,6, 6-tetramethylpiperidine oxide, polyethylene glycol, isotridecanol polyoxyethylene ether, a betaine type surfactant and a quaternary ammonium salt type cationic surfactant.
Further, the stabilizer is one or more of acacia, cellulose, carrageenan, xanthan gum and sodium alginate.
Further, the polishing speed in the step (4) is 800-1200rpm, and preferably, the polishing speed is 1000 rpm.
The second object of the present invention is to provide a carbon nanotube dispersion prepared by the method for preparing an aqueous carbon nanotube dispersion.
Compared with the prior art, the invention has the beneficial effects that:
(1) the carbon nano tube dispersion liquid prepared by the method can greatly reduce the viscosity of the dispersion liquid in the dispersion process and improve the preparation efficiency of the dispersion liquid, and the method has simple process, cleanness and environmental protection;
(2) the method of the invention can reduce the viscosity of the dispersion liquid by adding water and the dispersant for a plurality of times, and the inventor finds that after adding water for the second time and the above times, a dispersion disc is needed to be used for stirring, the size of the dispersion disc is not less than 10% of the sectional area of the container, and the viscosity of the prepared mixture can be low at the stirring speed of the invention, thereby being beneficial to adding the subsequent dispersant to reduce the viscosity of the dispersion liquid and improving the preparation efficiency of the dispersion liquid; the dispersant can keep the viscosity of the dispersion in a processable range stably by dividing the dispersant into a plurality of times.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Example 1
The preparation method of the aqueous carbon nanotube dispersion liquid of the embodiment includes the following steps:
(1) weighing the substances according to the mass ratio of 92:5:2:1 of water, carbon nano-tubes, a dispersing agent and a stabilizing agent, wherein the total mass is 2000g for later use, the ultrapure water has the resistivity of 18M omega cm at 25 ℃, the dispersing agent is isotridecanol polyoxyethylene ether (national group chemical reagent limited, analytically pure), the stabilizing agent is Arabic gum (DL-A-I brand from Dingli glue company Limited liability company), and the carbon nano-tubes (multi-walled carbon nano-tubes with the diameter of 9-11nm and the length of 10-15 mu M, NC7000 brand from Nanocyl company of Belgium);
(2) adding the standby water into the carbon nano tube according to the mass for 3 times, firstly, adding the water into an external stirrer for the first time, wherein the diameter of the stirrer is 25cm, the diameter of a dispersion disc is 5cm, then slowly adding the water at the speed of 400rpm at 25 ℃, adding the carbon nano tube for 2min, continuously dispersing the water at the speed of 600rpm for 10min at 25 ℃, adding one third of the water, dispersing the water at the speed of 600rpm for 10min at 25 ℃, adding the rest water into the stirrer, dispersing the water at the speed of 1000rpm for 10min at 25 ℃ to obtain a mixture A, and testing the viscosity of the mixture A to be 30000 cp;
(3) adding a third weight of dispersant into the mixture A, stirring for 5-10min, adding into a grinding machine (a cavity of the grinding machine is filled with 0.5mm zirconium balls which account for 6/10 of the volume of the cavity), grinding and mixing for 5 times at a grinding speed of 1000rpm at 30 ℃, adding the third weight of dispersant, continuing grinding for 5 times, adding the rest dispersant, continuing grinding for 20 times to obtain a mixture B, and testing the viscosity of the mixture B to be 2000 cp;
(4) adding a stabilizer into the cavity of the grinder and mixing with the mixture B for 20min at the grinding speed of 1000rpm and 30 ℃ to obtain the carbon nano tube dispersion liquid.
The content of the carbon nanotube dispersion prepared in this example was 5%, the particle size of the carbon nanotube, D10, D50, and D90 were 247nm, 477nm, and the viscosity was 360 cp.
Example 2
The preparation method of the aqueous carbon nanotube dispersion liquid of the embodiment includes the following steps:
(1) weighing the substances according to the mass ratio of 90:3:5:2 of water, the carbon nano tube, the dispersing agent and the stabilizing agent, wherein the total mass is 2000g for later use, the ultrapure water has the resistivity of 18 MOmega-cm at 25 ℃, the dispersing agent is sodium dodecyl sulfate, the stabilizing agent is cellulose, and the carbon nano tube (the diameter is 0.4-1nm, the length is 5-7 mu M, and the multi-wall carbon nano tube) is adopted;
(2) adding the standby water into the carbon nano tube by 5 times according to the mass, firstly, adding 40 percent of water by weight into an external stirrer for the first time, wherein the diameter of the stirrer is 25cm, the diameter of a dispersion disc is 5cm, then slowly adding the water at 25 ℃ and 300rpm while stirring, adding the carbon nano tube for 2.5min, continuously dispersing at 25 ℃ and 500rpm for 12min after adding, adding 20 percent of water, dispersing at 25 ℃ and 500rpm for 12min, adding 20 percent of water into the stirrer, dispersing at 25 ℃ and 1000rpm for 12min, adding 10 percent of water into the stirrer, dispersing at 25 ℃ and 1200rpm for 12min, adding 10 percent of water into the stirrer, and dispersing at 25 ℃ and 500rpm for 10min to obtain a mixture A;
(3) adding 50% by weight of dispersant into the mixture A, stirring for 5-10min, adding into a grinder (a cavity of the grinder is filled with 0.5mm zirconium balls which account for 6/10 of the volume of the cavity), grinding and mixing for 10 times at the grinding speed of 30 ℃ and 800rpm, adding 20% by weight of dispersant, continuing grinding for 7 times, adding 10% by weight of dispersant, continuing grinding for 10 times, adding 10% by weight of dispersant, continuing grinding for 15 times, adding 10% by weight of dispersant, and continuing grinding for 20 times to obtain a mixture B;
(4) adding a stabilizer into the cavity of the grinder and mixing with the mixture B for 25min at the temperature of 30 ℃ and the grinding speed of 800rpm to obtain the carbon nano tube dispersion liquid.
The content of the carbon nanotube dispersion prepared in this example was 3%, the particle size D10 of the carbon nanotube was 242nm, the D50 was 463nm, the D90 was 974nm, and the viscosity was 312 cp.
Example 3
The preparation method of the aqueous carbon nanotube dispersion liquid of the embodiment includes the following steps:
(1) weighing the substances according to the mass ratio of 97:8:1:5 of water, the carbon nano tube, the dispersing agent and the stabilizing agent, wherein the total mass is 2000g for later use, the ultrapure water has the resistivity of 18 MOmega-cm at 25 ℃, the dispersing agent is a betaine type surfactant, the stabilizing agent is sodium alginate, and the carbon nano tube (the diameter is 4-10nm, the length is 8-12 mu M, and the single-walled carbon nano tube) is prepared;
(2) adding the standby water into the carbon nano tube for 6 times by mass, firstly, adding 20 percent of water by weight into an external stirrer for the first time, wherein the diameter of the stirrer is 25cm, the diameter of a dispersion disc is 5cm, then slowly adding the carbon nano tube at the temperature of 25 ℃ at the speed of 700rpm while stirring, finishing adding the carbon nano tube for 1.5min, continuing at the temperature of 25 ℃ after finishing adding, dispersing at 1500rpm for 8min, adding 20% water, cooling at 25 deg.C, dispersing at 1500rpm for 8min, adding 20% water into the stirrer, dispersing at 25 deg.C and 800rpm for 10min, adding 20% water into the stirrer, dispersing at 25 deg.C at 700rpm for 12min, adding 10% water into the stirrer, dispersing at 25 deg.C and 500rpm for 10min, adding 10% water into the stirrer, dispersing at 25 deg.C and 500rpm for 10min to obtain mixture A;
(3) adding 40% by weight of dispersing agent into the mixture A, stirring for 5-10min, adding into a grinding machine (a cavity of the grinding machine is filled with 0.5mm zirconium balls which account for 6/10 of the volume of the cavity), grinding and mixing for 15 times at the grinding speed of 30 ℃ and 1200rpm, adding 20% by weight of dispersing agent, continuing grinding for 14 times, adding 10% by weight of dispersing agent, continuing grinding for 10 times, adding 10% by weight of dispersing agent, continuing grinding for 18 times, adding 10% by weight of dispersing agent, continuing grinding for 15 times, adding 10% by weight of dispersing agent, and continuing grinding for 15 times to obtain a mixture B;
(4) adding a stabilizer into the cavity of the grinder and mixing with the mixture B for 15min at the grinding speed of 1200rpm and the temperature of 30 ℃ to obtain the carbon nano tube dispersion liquid.
The content of the carbon nanotube dispersion liquid prepared in this example was 7.2%, the particle size D10 of the carbon nanotube was 238nm, the particle size D50 was 456nm, the particle size D90 was 979nm, and the viscosity was 387 cp.
Comparative example 1
The carbon nanotube dispersion liquid of this example was prepared in the same manner as in example 1, except that water in step (2) was once mixed with the carbon nanotubes without separate mixing, and the viscosity of the prepared carbon nanotube dispersion liquid was determined to be 498 cp.
Comparative example 2
The carbon nanotube dispersion of this example was prepared by the same method as in example 1, except that the dispersant in step (3) was mixed with the mixture a at once, not separately, and the viscosity of the prepared carbon nanotube dispersion was measured to be 476 cp.
As can be seen from the viscosities of the carbon nanotube dispersions in comparative examples 1-2 and example 1, the viscosity of the carbon nanotube dispersion can be reduced by the method of the present invention.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. A preparation method of aqueous carbon nanotube dispersion is characterized by comprising the following steps:
(1) respectively weighing water, carbon nano tubes, a dispersing agent and a stabilizing agent for later use;
(2) the water content N for standby1Then stirring and mixing with the carbon nano tube to obtain a mixture A, wherein N is1Is an integer of 2 or more; moisture content N1The quality of each time is the same or different when the carbon nano tube is mixed with the carbon nano tube, the carbon nano tube is added into the water in the first mixing within 1.5-2.5min at the stirring speed of 300-500rpm, the dispersion is carried out for 8-12min at the speed of 700rpm, the water is added for the second time or more, the water is stirred by adopting a dispersion disc, the stirring speed is 500-1500rpm, and the stirring is carried out for 8-12 min;
(3) dividing the dispersant into N2Stirring and mixing with the mixture A to obtain a mixture B, wherein N is2Is an integer of 2 or more; dispersing agent is divided into N2The quality of each time is the same or different when the dispersant is mixed with the mixture A for the first time, the dispersant is stirred and mixed with the mixture A for the first time and then ground, the grinding speed is 800-1200rpm, the dispersant is added for the second time after the grinding times are 5-20 times, and then grinding is carried out again, and the steps are repeated until the dispersant is completely added;
(4) and grinding the mixture B and the spare stabilizer to obtain the water-based carbon nanotube dispersion liquid.
2. The method for preparing an aqueous carbon nanotube dispersion according to claim 1, wherein the mass ratio of water to the carbon nanotubes to the dispersant to the stabilizer in the step (1) is 90-97:3-8:1-5: 1-5.
3. The method according to claim 1, wherein the water is ultrapure water, and the ultrapure water has a resistivity of not less than 18M Ω ∙ cm at 25 ℃.
4. The method according to claim 1, wherein the carbon nanotubes have a diameter of 0.4 to 100nm and a length of 1 to 50 μm.
5. The method according to claim 4, wherein the carbon nanotubes have a diameter of 5-15nm and a length of 10-20 μm.
6. The method of claim 1, wherein the dispersant is one or more selected from the group consisting of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, polyacrylamide, polysorbate, sorbitan fatty ester, sodium cellulose, 2,6, 6-tetramethylpiperidine oxide, polyethylene glycol, isotridecanol polyoxyethylene ether, a betaine surfactant, and a quaternary ammonium salt cationic surfactant.
7. The method according to claim 1, wherein the stabilizer is one or more of acacia, cellulose, carrageenan, xanthan gum and sodium alginate.
8. The method as claimed in claim 1, wherein the grinding speed in step (4) is 800-1200 rpm.
9. The method for producing an aqueous carbon nanotube dispersion according to claim 8, wherein the grinding speed in the step (4) is 1000 rpm.
10. An aqueous carbon nanotube dispersion prepared by the method of any one of claims 1-9.
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