CN110280192A - The preparation method of carbon nanotube-polyvinyl alcohol gel micro-ball - Google Patents
The preparation method of carbon nanotube-polyvinyl alcohol gel micro-ball Download PDFInfo
- Publication number
- CN110280192A CN110280192A CN201910621072.0A CN201910621072A CN110280192A CN 110280192 A CN110280192 A CN 110280192A CN 201910621072 A CN201910621072 A CN 201910621072A CN 110280192 A CN110280192 A CN 110280192A
- Authority
- CN
- China
- Prior art keywords
- carbon nanotube
- preparation
- polyvinyl alcohol
- dispersion liquid
- ball
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0056—Preparation of gels containing inorganic material and water
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Colloid Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of carbon nanotube-polyvinyl alcohol gel micro-ball.Carbon nanotube is first successively dispersed in the dispersed phase solution that carbon nanotube is formed in low concentration and the polyvinyl alcohol water solution of high concentration by the method, surfactant Span-80 is added in oily phase and prepares continuous phase solution, the solution formed using the mixed liquor that pure and mild amino alcohol is added in boron-containing compound is receiving liquid, using micro-fluidic method, the drop of formation drops onto receiving liquid naturally, and solidification obtains carbon nanotube-polyvinyl alcohol gel micro-ball.The present invention can make carbon nanotube be uniformly dispersed and stablize simultaneously in the structural intergrity for keeping carbon nanotube, and the microspherulite diameter being prepared is uniform, and form can keep complete smooth, and preparation process flow is simple.
Description
Technical field
The invention belongs to conductive material preparation technical fields, are related to a kind of system of carbon nanotube-polyvinyl alcohol gel micro-ball
Preparation Method.
Background technique
Carbon nanotube mechanical property with super strength, high aspect ratio and unique conductive characteristic, in electrode material, receive
The numerous areas such as rice electronic material, structural material show good application prospect.But due between carbon nanotube exist compared with
Strong Van der Waals force causes it to be easy to wind together or formed reunion, to restrict the application of carbon nanotube.To make carbon receive
Mitron better disperses, and the method for being often used some physics and chemistry is handled.Common physical method mainly has high energy ball
Mill, mechanical stirring, vibration of ultrasonic wave etc., and chemical method mainly uses strong acid and strong base activation, surfactant or covalent bond
The modified dispersion for promoting carbon nanotube.Time-consuming for physical method, and step is complicated, and high-intensitive mechanism will lead to carbon and receive
Mitron fragmentation greatly reduces its draw ratio, weakens the mechanical strength of carbon nanotube, the advantage of Young's modulus, and physics
The dispersion stability that method obtains is poor, can only continue very short time.Chemical method will lead to carbon nanometer due to Strong oxdiative processing
Pipe surface defect is excessive and reduces and even loses its excellent electric conductivity.
The method that carbon nanotube and high molecular material are used in combination at present is mainly mechanical stirring, high-energy ball milling etc..Such as
(Zhang Zhengzhong, Deng Chongqing, Li Jizhen wait carbon nanotube to AP/CMDB propellant burning property and mechanical property to Zhang Zhengzhong et al.
Influence [J] energetic material, 2018 (9): 744-748.) directly carbon nanotube is added in CMDB propellant, utilize machinery
The method of stirring and ultrasonic disperse is compound therewith by carbon nanotube；Chen Suhang et al. (Chen S, Tang Y, Yu H, et
al.Combustion enhancement of hydroxyl-terminated polybutadiene by doping
Multiwall carbon nanotubes [J] .Carbon, 2019,144:472-480.) utilize the method for high-energy ball milling by carbon
Nanotube is dispersed in HTPB.There are part agglomerations in CMDB propellant for the former carbon nanotube, although the latter can make
Carbon nanotube dispersion, but ball milling causes the rupture of carbon nanotube, so that the reduced performance of carbon nanotube.
Therefore, developing one kind dispersing Nano carbon tubes and can not generate secondary agglomeration, and can be with high molecular material
The simple and easy process being effectively used in combination seems particularly important.
Summary of the invention
In order to solve the problems, such as carbon nanotube bad dispersibility, easy secondary agglomeration and its exist with high molecular material compound tense,
The present invention provides a kind of preparation method of carbon nanotube-polyvinyl alcohol gel micro-ball.This method using polyvinyl alcohol as dispersing agent and
Carbon nanotube while keeping carbon nanotube evenly dispersed, and is fixed on poly- second using micro-fluidic method by microballoon binder
Microballoon is formed in enol, fixed carbon nanotube will not fall off, and prevent secondary agglomeration, and preservation that can be permanent.
Technical scheme is as follows:
The preparation method of carbon nanotube-polyvinyl alcohol gel micro-ball, the preparation of the dispersed phase solution including carbon nanotube connect
Preparation, the preparation of receiving liquid and the preparation of carbon nanotube-polyvinyl alcohol gel micro-ball of continuous phase, the specific steps are as follows:
(1) preparation of the dispersed phase solution of carbon nanotube
First carbon nanotube is added in dispersion liquid 1, is placed in ultrasonic disperse in water-bath, is then added in dispersion liquid 2, is stirred
The dispersed phase solution of carbon nanotube is formed, the dispersion liquid 1 and 2 is polyvinyl alcohol water solution, and wherein dispersion liquid 1 is 0.5
The concentration ratio of the polyvinyl alcohol water solution of~2.0wt.%, dispersion liquid 1 and dispersion liquid 2 is 1: 6~1: 10；
(2) preparation of continuous phase:
Surfactant Span-80 is added in oily phase, sonic oscillation is dissolved completely in surfactant in oily phase,
Form the continuous phase solution that surfactant volume fraction is 3~5%；
(3) preparation of receiving liquid
Boron-containing compound is added in proportion in the mixed liquor of pure and mild amino alcohol, magnetic agitation and heat make it dissolve, match
Receiving liquid is made；
(4) preparation of carbon nanotube-polyvinyl alcohol gel micro-ball
Using micro-fluidic method, the flow velocity for controlling the dispersed phase solution of carbon nanotube is 0.5~2mlh-1, continuous phase
The flow velocity of solution is 8~12mlh-1, the dispersed phase drop for shearing formation is dropped in receiving liquid, solidifies and carbon nanotube-is made
Polyvinyl alcohol gel microballoon.
Preferably, in step (1), the bath temperature is 80~90 DEG C.
Preferably, in step (2), the oil is mutually one of silicone oil, vegetable oil, salad oil and atoleine or two
Kind.
Preferably, in step (3), the boron-containing compound is one or both of borax and boric acid；The alcohol
For isoamyl alcohol, isooctanol and one or both of alcohol；Amino alcohol is one or both of triethanolamine and diethanol amine；
The volume ratio of the pure and mild amino alcohol is 2: 1, and concentration of the boron-containing compound in receiving liquid is 0.02~0.05gmL-1。
Preferably, in step (4), the curing time is 2~6h.
Compared with prior art, the invention has the following advantages that
1. dispersion liquid of the present invention using the poly-vinyl alcohol solution of micro- concentration as carbon nanotube, on the basis of ultrasonic disperse
On, carbon nanotube aggregate effectively and is thoroughly opened, the structural intergrity of carbon nanotube is maintained, avoids simultaneously
Introduce other chemical substances；
2. carbon nanotube is fixed in polyvinyl alcohol using micro-fluidic method and forms microballoon by the present invention, fixed carbon
Nanotube will not fall off, so that carbon nanotube will not generate secondary agglomeration, and preservation that can be permanent；
3. cross-linkable solidifying under method microballoon room temperature of the invention has dispersion effect good and stably dispersing, real under room temperature
Existing crosslinking curing, the microspherulite diameter being prepared is uniform, and form can keep complete smooth, and simple process preparation flow is short, environment
Pollute the advantages that small.
Detailed description of the invention
Fig. 1 is the dispersion effect figure of carbon nanotube of the invention.
Fig. 2 is the micro fluidic device figure that the present invention prepares carbon nanotube-polyvinyl alcohol gel micro-ball.
Fig. 3 is carbon nanotube-polyvinyl alcohol gelatin microspheres formula microscope figure prepared by the present invention.
Fig. 4 is that carbon nanotube is distributed SEM figure in carbon nanotube-polyvinyl alcohol gel micro-ball prepared by the present invention.
Specific embodiment
Below with reference to specific embodiment and attached drawing, the invention will be further described.
Embodiment 1
(1) 0.5g PVA is added in the water of 49.5g, is warming up to 90 DEG C of heat preservation 1.5h, to its dissolution, forming concentration is
The polyvinyl alcohol water solution of 1.0wt.%.0.5g carbon nanotube ultrasonic disperse is added after cooling, forms dispersion liquid 1；By 3g PVA
It is added in the water of 47g, is warming up to 90 DEG C of heat preservation 2h, to its dissolution, form dispersion liquid 2, the concentration of dispersion liquid 1 and dispersion liquid 2
Than being 1: 6；Above two dispersion liquid is mixed, magnetic agitation 30min forms the disperse phase liquid of carbon nanotube.
(2) 1.5mL surfactant Sapn-80 is added in 48.5mL atoleine, sonic oscillation makes Span-80
It is dissolved completely in liquid to get the continuous phase liquid for being 3% to surfactant volume fraction.
(3) 1.5g borax is added in the mixture of 50mL isoamyl alcohol and 25mL triethanolamine, magnetic agitation is simultaneously slow
It is heated to 60 DEG C to make it dissolve, is configured to receiving liquid.
(4) above-mentioned dispersed phase solution and continuous phase solution are respectively charged into syringe, the flow velocity of dispersed phase is 0.5ml/
H, the flow velocity of continuous phase are 8ml/h, open microfluidic control device, and when the outflow of dispersed phase solution, the continuous phase of flowing is glued
Surface tension interaction between stagnant power and liquid causes dispersion fluid to be cut into drop at outflow port, and drop is certainly
So drop onto receiving liquid.The drop generated is collected in the culture dish equipped with receiving liquid, it is anti-to be slowly stirred down solidification at room temperature
4h is answered, drop can be solidified into carbon nanotube-polyvinyl alcohol gel micro-ball.
Embodiment 2
(1) 0.25g PVA is added in the water of 49.75g, is warming up to 80 DEG C of heat preservation 1h, to its dissolution, forming concentration is
The polyvinyl alcohol water solution of 0.5wt.%.0.4g carbon nanotube ultrasonic disperse is added after cooling, forms dispersion liquid 1；By 3.5g
PVA is added in the water of 71.5g, is warming up to 90 DEG C of heat preservation 2h, to its dissolution, forms dispersion liquid 2, dispersion liquid 1 and dispersion liquid 2
Concentration ratio is 1: 9.3；Above two dispersion liquid is mixed, magnetic agitation 30min forms the disperse phase liquid of carbon nanotube.
(2) 2mL surfactant Sapn-80 is added in 48mL silicone oil, sonic oscillation is completely dissolved Span-80
To get the continuous phase liquid for being 4% to surfactant volume fraction in liquid.
(3) 1.5g borax is added to 30mL in the mixture of alcohol and 15mL diethanol amine, magnetic agitation has simultaneously slowly added
Heat makes it dissolve to 60 DEG C, is configured to receiving liquid.
(4) above-mentioned dispersed phase solution and continuous phase solution are respectively charged into syringe, the flow velocity of dispersed phase is 0.8ml/
H, the flow velocity of continuous phase are 8ml/h, open microfluidic control device, prepare carbon nanotube-polyvinyl alcohol gel micro-ball drop, liquid
Drop nature drops onto receiving liquid.The drop generated is collected in the culture dish equipped with receiving liquid, is slowly stirred down solid at room temperature
Change reaction 2h, drop can be solidified into carbon nanotube-polyvinyl alcohol gel micro-ball.
Embodiment 3
(1) 1.0g PVA is added in the water of 49g, is warming up to 90 DEG C of heat preservation 2h, to its dissolution, forming concentration is
The polyvinyl alcohol water solution of 2.0wt.%.0.5g carbon nanotube ultrasonic disperse is added after cooling, forms dispersion liquid 1；By 6g PVA
It is added in the water of 44g, is warming up to 90 DEG C of heat preservation 2h, to its dissolution, form dispersion liquid 2, the concentration of dispersion liquid 1 and dispersion liquid 2
Than being 1: 6；Above two dispersion liquid is mixed, magnetic agitation 30min forms the disperse phase liquid of carbon nanotube.
(2) 2.5mL surfactant Sapn-80 is added in 47.5mL atoleine, sonic oscillation makes Span-80
It is dissolved completely in liquid to get the continuous phase liquid for being 5% to surfactant volume fraction.
(3) 1.5g borax is added in the mixture of 20mL isooctanol and 10mL triethanolamine, magnetic agitation is simultaneously slow
It is heated to 60 DEG C to make it dissolve, is configured to receiving liquid.
(4) above-mentioned dispersed phase solution and continuous phase solution being respectively charged into syringe, the flow velocity of dispersed phase is 2ml/h,
The flow velocity of continuous phase is 12ml/h, opens microfluidic control device, prepares carbon nanotube-polyvinyl alcohol gel micro-ball drop, liquid
Drop nature drops onto receiving liquid.The drop generated is collected in the culture dish equipped with receiving liquid, is slowly stirred down solid at room temperature
Change reaction 6h, drop can be solidified into carbon nanotube-polyvinyl alcohol gel micro-ball.
Embodiment 4
(1) 1g PVA is added in the water of 64g, is warming up to 90 DEG C of heat preservation 2h, to its dissolution, forming concentration is
The polyvinyl alcohol water solution of 1.54wt.%.0.5g carbon nanotube ultrasonic disperse is added after cooling, forms dispersion liquid 1；By 5.5g
PVA is added in the water of 44.5g, is warming up to 90 DEG C of heat preservation 2h, to its dissolution, forms dispersion liquid 2, dispersion liquid 1 and dispersion liquid 2
Concentration ratio is 1: 7.15；Above two dispersion liquid is mixed, magnetic agitation 30min forms the disperse phase liquid of carbon nanotube.
(2) 1.5mL surfactant Sapn-80 is added in 48.5mL salad oil, sonic oscillation keeps Span-80 complete
Fully dissolved is in liquid to get the continuous phase liquid for being 3% to surfactant volume fraction.
(3) 2g borax is added in the mixture of 30mL isoamyl alcohol and 15mL triethanolamine, magnetic agitation simultaneously slowly adds
Heat makes it dissolve to 60 DEG C, is configured to receiving liquid.
(4) above-mentioned dispersed phase solution and continuous phase solution being respectively charged into syringe, the flow velocity of dispersed phase is 1ml/h,
The flow velocity of continuous phase is 8ml/h, opens microfluidic control device, prepares carbon nanotube-polyvinyl alcohol gel micro-ball drop, drop
Naturally it drops onto receiving liquid.The drop generated is collected in the culture dish equipped with receiving liquid, is slowly stirred down and solidifies at room temperature
4h is reacted, drop can be solidified into carbon nanotube-polyvinyl alcohol gel micro-ball.
Embodiment 5
(1) 0.5g PVA is added in the water of 49.5g, is warming up to 90 DEG C of heat preservation 2h, to its dissolution, forming concentration is
The polyvinyl alcohol water solution of 1.0wt.%.0.6g carbon nanotube ultrasonic disperse is added after cooling, forms dispersion liquid 1；By 5g PVA
It is added in the water of 45g, is warming up to 80 DEG C of heat preservation 1.5h, to its dissolution, form dispersion liquid 2, dispersion liquid 1 is dense with dispersion liquid 2
Degree is than being 1: 10；Above two dispersion liquid is mixed, magnetic agitation 30min forms the disperse phase liquid of carbon nanotube.
(2) 2mL surfactant Sapn-80 is added in 48mL vegetable oil, sonic oscillation keeps Span-80 completely molten
Solution is in liquid to get the continuous phase liquid for being 4% to surfactant volume fraction.
(3) 2.5g borax is added in the mixture of 40mL isoamyl alcohol and 20mL diethanol amine, magnetic agitation is simultaneously slow
It is heated to 60 DEG C to make it dissolve, is configured to receiving liquid.
(4) above-mentioned dispersed phase solution and continuous phase solution are respectively charged into syringe, the flow velocity of dispersed phase is 1.5ml/
H, the flow velocity of continuous phase are 10ml/h, open microfluidic control device, prepare carbon nanotube-polyvinyl alcohol gel micro-ball drop,
Drop drops onto receiving liquid naturally.The drop generated is collected in the culture dish equipped with receiving liquid, is slowly stirred down at room temperature
Curing reaction 3h, drop can be solidified into carbon nanotube-polyvinyl alcohol gel micro-ball.
The performance of carbon nanotube-polyvinyl alcohol gel micro-ball and pattern made from Examples 1 to 5 are close.Fig. 1 is the present invention
Carbon nanotube dispersion effect figure.It will be seen from figure 1 that carbon nanotube is dispersed in polyvinyl alcohol water solution, when long
Between place will not occur settle and do not generate secondary agglomeration.Fig. 2 is that the present invention prepares carbon nanotube-polyvinyl alcohol gel micro-ball
Micro fluidic device figure.Fig. 3 is carbon nanotube-polyvinyl alcohol gelatin microspheres formula microscope figure prepared by the present invention.It can be with from Fig. 3
Find out, carbon nanotube-polyvinyl alcohol gel micro-ball uniform particle diameter, form keeps complete smooth.Fig. 4 is that carbon prepared by the present invention is received
Carbon nanotube distribution SEM figure in mitron-polyvinyl alcohol gel microballoon.From fig. 4, it can be seen that carbon nanotube effectively and thoroughly by
It is dispersed in polyvinyl alcohol microparticles after opening, fixed carbon nanotube will not fall off, and will not generate secondary agglomeration.
Comparative example 1
This comparative example is substantially the same manner as Example 1, unique the difference is that the concentration of polyvinyl alcohol water solution is in dispersion liquid 1
0.4wt.%.Under this condition, carbon nanotube easily precipitates after distribution since the concentration of dispersion liquid 1 is too low, can not keep for a long time
Evenly dispersed characteristic.
Comparative example 2
This comparative example is substantially the same manner as Example 3, unique the difference is that the concentration of polyvinyl alcohol water solution is in dispersion liquid 1
3.0wt.%.Under this condition, carbon nanotube can not effectively be opened due to the excessive concentration of dispersion liquid 1, dispersion is uneven, easily
It causes to reunite.
Comparative example 3
This comparative example is substantially the same manner as Example 2, unique the difference is that the concentration ratio of dispersion liquid 1 and dispersion liquid 2 is 1: 4.
Under this condition, the dispersed phase solution of carbon nanotube can not form microballoon drop in micro fluidic device, and drop onto receiving liquid
It easily scatters, cannot keep spherical shape.
Comparative example 4
This comparative example is substantially the same manner as Example 1, unique the difference is that the concentration ratio of dispersion liquid 1 and dispersion liquid 2 is 1: 12.
Under this condition, the dispersed phase solution of carbon nanotube due to excessive concentration, easily causes the stifled of pipeline and connector in micro fluidic device
Plug.
Comparative example 5
This comparative example is substantially the same manner as Example 3, unique the difference is that dispersed phase flow velocity is 0.3mlh-1.Under this condition,
Since dispersed phase solution flow velocity is excessively slow, it is cut into slowing for drop at outflow port, causes the too fast outflow of continuous phase
Loss.
Comparative example 6
This comparative example is substantially the same manner as Example 4, unique the difference is that dispersed phase flow velocity is 3mlh-1.Under this condition, by
It is too fast in dispersed phase solution flow velocity, it is cut into strip drop at outflow port, spherical shape can not be formed.
Claims (9)
1. the preparation method of carbon nanotube-polyvinyl alcohol gel micro-ball, which is characterized in that specific step is as follows:
(1) preparation of the dispersed phase solution of carbon nanotube
First carbon nanotube is added in dispersion liquid 1, is placed in ultrasonic disperse in water-bath, is then added in dispersion liquid 2, stirring is formed
The dispersed phase solution of carbon nanotube, the dispersion liquid 1 and 2 is polyvinyl alcohol water solution, wherein dispersion liquid 1 be 0.5~
The concentration ratio of the polyvinyl alcohol water solution of 2.0wt.%, dispersion liquid 1 and dispersion liquid 2 is 1: 6~1: 10；
(2) preparation of continuous phase:
Surfactant Span-80 is added in oily phase, sonic oscillation is dissolved completely in surfactant in oily phase, is formed
The continuous phase solution that surfactant volume fraction is 3~5%；
(3) preparation of receiving liquid
Boron-containing compound is added in proportion in the mixed liquor of pure and mild amino alcohol, magnetic agitation and heat make it dissolve, be configured to
Receiving liquid；
(4) preparation of carbon nanotube-polyvinyl alcohol gel micro-ball
Using micro-fluidic method, the flow velocity for controlling the dispersed phase solution of carbon nanotube is 0.5~2mlh-1, continuous phase solution
Flow velocity be 8~12mlh-1, the dispersed phase drop for shearing formation is dropped in receiving liquid, solidifies and the poly- second of carbon nanotube-is made
Enol gel micro-ball.
2. preparation method according to claim 1, which is characterized in that in step (1), the bath temperature is 80~90
℃。
3. preparation method according to claim 1, which is characterized in that in step (2), the oil is mutually silicone oil, plant
One or both of oil, salad oil and atoleine.
4. preparation method according to claim 1, which is characterized in that in step (3), the boron-containing compound is borax
One or both of with boric acid.
5. preparation method according to claim 1, which is characterized in that in step (3), the alcohol is isoamyl alcohol, different pungent
Pure and mild one or both of alcohol.
6. preparation method according to claim 1, which is characterized in that in step (3), amino alcohol is triethanolamine and diethyl
One or both of hydramine.
7. preparation method according to claim 1, which is characterized in that in step (3), the volume of the pure and mild amino alcohol
Than being 2: 1.
8. preparation method according to claim 1, which is characterized in that in step (3), boron-containing compound is in receiving liquid
Concentration is 0.02~0.05gmL-1。
9. preparation method according to claim 1, which is characterized in that in step (4), the curing time is 2~6h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910621072.0A CN110280192B (en) | 2019-07-10 | 2019-07-10 | Preparation method of carbon nano tube-polyvinyl alcohol gel microspheres |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910621072.0A CN110280192B (en) | 2019-07-10 | 2019-07-10 | Preparation method of carbon nano tube-polyvinyl alcohol gel microspheres |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110280192A true CN110280192A (en) | 2019-09-27 |
| CN110280192B CN110280192B (en) | 2022-05-20 |
Family
ID=68021212
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910621072.0A Active CN110280192B (en) | 2019-07-10 | 2019-07-10 | Preparation method of carbon nano tube-polyvinyl alcohol gel microspheres |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110280192B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111039326A (en) * | 2020-01-13 | 2020-04-21 | 清华大学 | Method for preparing uranium dioxide microspheres at normal temperature |
| CN112973589A (en) * | 2021-02-05 | 2021-06-18 | 中国工程物理研究院激光聚变研究中心 | Preparation method of sulfonated RF aerogel microspheres |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000281433A (en) * | 1999-03-31 | 2000-10-10 | Japan Atom Energy Res Inst | Production of lithium titanate minute sintered particle |
| CN102895927A (en) * | 2012-10-23 | 2013-01-30 | 中国科学技术大学 | Grain size controllable monodisperse polyvinyl alcohol gel microsphere, preparation method thereof and applied device |
| CN104692357A (en) * | 2015-02-15 | 2015-06-10 | 清华大学 | Carbon nano-tube/carbon multilevel pore spherical composite and preparation method thereof |
| CN105060268A (en) * | 2015-07-09 | 2015-11-18 | 河海大学 | Preparation method of CNT (carbon nanotube) microspheres |
| CN105771762A (en) * | 2016-03-11 | 2016-07-20 | 北京工业大学 | Physical dispersion method of carbon nanotubes |
| CN106267164A (en) * | 2016-09-12 | 2017-01-04 | 蚌埠医学院 | Single dispersing insulin/chitosan gel rubber microsphere of size tunable and preparation method thereof |
| CN107552020A (en) * | 2017-09-18 | 2018-01-09 | 同济大学 | The method of the polyvinyl alcohol of synthesizing blender carbon nanomaterial/sodium alginate gel ball adsorbent |
-
2019
- 2019-07-10 CN CN201910621072.0A patent/CN110280192B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000281433A (en) * | 1999-03-31 | 2000-10-10 | Japan Atom Energy Res Inst | Production of lithium titanate minute sintered particle |
| CN102895927A (en) * | 2012-10-23 | 2013-01-30 | 中国科学技术大学 | Grain size controllable monodisperse polyvinyl alcohol gel microsphere, preparation method thereof and applied device |
| CN104692357A (en) * | 2015-02-15 | 2015-06-10 | 清华大学 | Carbon nano-tube/carbon multilevel pore spherical composite and preparation method thereof |
| CN105060268A (en) * | 2015-07-09 | 2015-11-18 | 河海大学 | Preparation method of CNT (carbon nanotube) microspheres |
| CN105771762A (en) * | 2016-03-11 | 2016-07-20 | 北京工业大学 | Physical dispersion method of carbon nanotubes |
| CN106267164A (en) * | 2016-09-12 | 2017-01-04 | 蚌埠医学院 | Single dispersing insulin/chitosan gel rubber microsphere of size tunable and preparation method thereof |
| CN107552020A (en) * | 2017-09-18 | 2018-01-09 | 同济大学 | The method of the polyvinyl alcohol of synthesizing blender carbon nanomaterial/sodium alginate gel ball adsorbent |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111039326A (en) * | 2020-01-13 | 2020-04-21 | 清华大学 | Method for preparing uranium dioxide microspheres at normal temperature |
| CN111039326B (en) * | 2020-01-13 | 2020-12-01 | 清华大学 | Method for preparing uranium dioxide microspheres at normal temperature |
| CN112973589A (en) * | 2021-02-05 | 2021-06-18 | 中国工程物理研究院激光聚变研究中心 | Preparation method of sulfonated RF aerogel microspheres |
| CN112973589B (en) * | 2021-02-05 | 2022-04-29 | 中国工程物理研究院激光聚变研究中心 | Preparation method of sulfonated RF aerogel microspheres |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110280192B (en) | 2022-05-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104449590B (en) | A kind of Nano capsule of phase-changing energy storage material and preparation method thereof | |
| CN101670256B (en) | Preparation method of phase change material microcapsule | |
| CN110280192A (en) | The preparation method of carbon nanotube-polyvinyl alcohol gel micro-ball | |
| CN109364835B (en) | Phase-change microcapsule and preparation method and application thereof | |
| CN103464203B (en) | Preparation method of thermosensitive microgel asymmetric supported nano silver catalyst | |
| CN101269827B (en) | Method for preparing high-dispersion magnesium hydroxide combustion inhibitor with one-step hydrothermal method | |
| CN102600776B (en) | Preparation method for magnetic microcapsule | |
| CN103435820B (en) | Pre-treatment method of asphalt and spherical graphite negative electrode material coated by using asphalt | |
| CN109243748A (en) | A kind of pair of dispersion magnetorheological fluid and preparation method thereof | |
| CN211303056U (en) | Dispersion reactor | |
| CN108774499A (en) | A kind of graphene-silica compound wall materials phase transformation Nano capsule and preparation method | |
| CN104559327A (en) | Surface modified nano calcium carbonate with core-shell structure and preparation method thereof | |
| CN103342991A (en) | Composite nanocapsule phase-change material and preparation method thereof | |
| CN101599335A (en) | A kind of oxidation resistant dimethyl silicon oil based magnetic fluid and preparation method thereof | |
| CN103737018A (en) | Method for continuous and rapid preparation of nano nickel by microfluidics technology | |
| Rao et al. | Preparation and thermal properties of microencapsulated phase change material for enhancing fluid flow heat transfer | |
| CN113637513A (en) | Use of inorganic sub-nanowires in organic solvent curing, transport and storage | |
| CN104962242A (en) | Low super-cooling degree phase-change material microcapsule and preparation method thereof | |
| CN104072656A (en) | Method for preparing ferroferric oxide-macromolecule magnetic composite microspheres | |
| CN100573756C (en) | A kind of method for preparing hollow magnetic ball | |
| CN102344517B (en) | Polymer microballoons and preparation method thereof | |
| CN103113853A (en) | Suspension stabilized phase change energy storage fluid and preparation method thereof | |
| CN113321219B (en) | Preparation method of spherical silicon micropowder | |
| CN107365571B (en) | Preparation process of carbon tube nano fluid and microchannel heat transfer working medium | |
| CN111567517A (en) | Novel aqueous pesticide suspending agent and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |