CN113880876A - Self-crosslinking graphene dispersing agent, preparation method thereof and nano carbon material dispersion liquid - Google Patents
Self-crosslinking graphene dispersing agent, preparation method thereof and nano carbon material dispersion liquid Download PDFInfo
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- CN113880876A CN113880876A CN202111325794.5A CN202111325794A CN113880876A CN 113880876 A CN113880876 A CN 113880876A CN 202111325794 A CN202111325794 A CN 202111325794A CN 113880876 A CN113880876 A CN 113880876A
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Abstract
The invention relates to the technical field of dispersing agents, and discloses a self-crosslinking graphene dispersing agent and a preparation method of a nano carbon material dispersing solution. The technical scheme is as follows: 1) putting a certain amount of adenine in methanol, ultrasonically stirring, adding 3-glycidyl ether oxypropyltrimethoxysilane, uniformly stirring, reacting at 60 ℃ for 36 hours, and removing the methanol after reaction. 2) And adding the reacted product into HCOOH solution with certain concentration, and stirring for 72h to obtain a dispersing agent DSiA solution. 3) Adding a certain mass of nano carbon material into DSiA solution, preparing into different concentrations by using deionized water, carrying out water bath ultrasound for 5min for preliminary dispersion, and further carrying out ultrasound dispersion for 30min by using an ultrasonic cell crusher to obtain corresponding nano carbon material dispersion liquid.
Description
Technical Field
The invention relates to the field of dispersing agents and stabilizing agents, and particularly relates to a self-crosslinking graphene dispersing agent, a preparation method of the self-crosslinking graphene dispersing agent and a nano carbon material dispersing solution.
Background
The nano carbon material comprises Graphene (GR), a Carbon Nano Tube (CNT), Reduced Graphene Oxide (RGO) and the like, has excellent performances of radiation resistance, chemical resistance, high thermal conductivity, high electrical conductivity, high specific surface area and the like, and has a very wide application prospect in the fields of energy storage, sensors, photoelectricity and the like.
The nano carbon materials are easy to aggregate due to strong pi-pi conjugation, so that the dispersibility of the nano carbon materials in water and organic solvents is poor, and the application of the nano carbon materials in actual production and life is limited to a great extent. Therefore, it is very important to solve the problem of dispersion of the nanocarbon material.
The existing methods for improving the dispersion performance of the nano carbon material mainly comprise two types, one is to directly modify the surface of the nano carbon material so as to graft different types of functional groups on the surface of the nano carbon material, thereby improving the dispersion performance of the nano carbon material; the other is to make the nano carbon material disperse better through the electrostatic action, steric hindrance action and the like of the dispersant. Existing dispersants mainly include two types: one is a conventional dispersant such as Sodium Dodecylbenzenesulfonate (SDBS), polyvinylpyrrolidone (PVP), gum arabic, etc.; another class is novel complex organic molecules. The traditional dispersing agent has limited capability of dispersing the nano carbon material in water, generally has the problems of large using amount of the dispersing agent, low dispersing concentration and the like, and excessive dispersing agent molecules can generate adverse effects on the application of the subsequent carbon material. Most of the novel dispersants reported in the literature generally have good dispersing performance on the nano carbon material, but have the problems of complex synthesis, high cost, lack of functionality and the like, and cannot meet the requirements of actual production and life.
Therefore, the design and synthesis of a novel and efficient graphene dispersing agent which is low in raw material cost, simple in synthesis method, small in dosage in practical use and high in reaction activity has important significance. The nano carbon material dispersion liquid prepared on the basis has great application potential in the fields of composite materials, energy, catalysis, environment and the like.
Disclosure of Invention
In view of the above, the present invention aims to provide a self-crosslinked graphene dispersant, a nano-carbon material dispersion liquid and a preparation method thereof. The dispersing agent can realize stable dispersion of the nano-carbon and can crosslink the nano-carbon into a film through self high-efficiency activity. In addition, the dispersant contains a plurality of N atoms in the skeleton, and can further impart more excellent catalytic performance to the carbon material.
The invention provides a self-crosslinking graphene dispersing agent which is DSiA and has a structural formula shown in a formula (I),
the preparation method of the self-crosslinking graphene dispersing agent comprises the following steps:
1) taking a certain amount of adenine and 3-glycidyl ether oxypropyl trimethoxy silane in a methanol reagent, stirring and reacting for a period of time at a certain temperature, and performing rotary evaporation to remove methanol after reaction to obtain a dispersant precursor;
2) adding a certain amount of dispersant precursor into formic acid aqueous solution with a certain concentration, and stirring and reacting for a period of time at a certain temperature to obtain DSiA solution.
Preferably, in the preparation method of the self-crosslinking graphene dispersant, in step 1), the molar ratio of adenine to 3-glycidoxypropyltrimethoxysilane is 1: 1.8-2.2.
Preferably, in the preparation method of the self-crosslinking graphene dispersant, in the step 1), the stirring reaction temperature is 65-75 ℃, the stirring reaction speed is 150-200 rpm, and the stirring reaction time is 24-36 hours.
Preferably, in the preparation method of the self-crosslinking graphene dispersant, in the step 1), the rotary steaming temperature is 30-40 ℃, and the rotary steaming strength is less than 0.15 Mpa.
Preferably, in the preparation method of the graphene dispersant, in the step 2), the stirring temperature is 20-60 ℃, and the stirring speed is 100-150 rpm.
A nano carbon material dispersion liquid is characterized by comprising the following preparation methods:
taking carbon nanomaterial powder with a certain mass, adding the self-crosslinking graphene dispersing agent, deionized water, performing water bath ultrasound,
and further carrying out ultrasonic dispersion by using an ultrasonic cell crusher to obtain a corresponding nano carbon material dispersion liquid.
Preferably, the ultrasonic power of the nano carbon material dispersion liquid is 350W, the ultrasonic treatment is stopped for 3s every 3s, and the ultrasonic treatment is carried out for 0.5 h.
Preferably, the weight ratio of the nano carbon material, the dispersant and the water is 1 (0.3-2) to 250-2000.
Preferably, the nanocarbon material dispersion liquid is one or more of graphene, multi-walled carbon nanotubes, redox graphene and carbon black.
The invention provides a preparation method of a graphene dispersion liquid, which comprises the following steps:
taking certain mass of graphene powder, adding the DSiA solution, carrying out water bath ultrasound for 5min, and further carrying out ultrasonic dispersion for 30min by using an ultrasonic cell crusher to obtain a graphene dispersion liquid. The ultrasonic power is 350W, and the ultrasonic treatment is stopped for 3s for 30min every 3 s.
In the graphene dispersion liquid, the mass ratio of graphene to the dispersing agent to water is 1 (0.3-2) to (250-2000), and the mass ratio of graphene to the dispersing agent to water is preferably 1:1: 250.
The invention also provides a preparation method of the multi-walled carbon nanotube dispersion liquid, which comprises the following steps:
adding carbon nanotube powder with a certain mass into the DSiA solution, firstly carrying out water bath ultrasound for 5min, and then carrying out ultrasound for 30min by using an ultrasonic cell crusher to obtain a carbon nanotube dispersion liquid. The ultrasonic power is 350W, the ultrasonic is stopped for 3s every 3s, and the time is 30 min.
In the carbon nanotube dispersion liquid, the mass ratio of the carbon nanotubes to the dispersing agent to the water is 1 (0.25-1) to (200-2000), and the mass ratio of the carbon nanotubes to the dispersing agent to the water is preferably 1:1: 200.
The invention also provides a preparation method of the reduced graphene oxide dispersion liquid, which comprises the following steps:
and adding a certain mass of reduced graphene oxide hydrogel into the DSiA solution, performing water bath ultrasound for 5min, and dispersing for 30min by using an ultrasonic cell crusher to obtain a reduced graphene oxide dispersion liquid. The ultrasonic power is 350W, the ultrasonic is stopped for 3s every 3s, and the ultrasonic treatment is carried out for 30 min.
The reduced graphene oxide hydrogel is preferably prepared by a Hummers method, the mass ratio of graphene oxide to ascorbic acid is 1:2, the reduced graphene oxide hydrogel is obtained by hydrothermal for 12 hours at 80 ℃, the reduced graphene oxide hydrogel is washed by deionized water for several times to remove redundant reducing agents, and the hydrogel is primarily crushed by a glass rod.
In the reduced graphene oxide dispersion liquid, the mass ratio of the reduced graphene oxide to the dispersant to the water is 1 (0.3-2) to (300-2000), and the mass ratio of the reduced graphene oxide to the dispersant to the water is preferably 1:1: 300.
The invention has the following beneficial effects:
the N-containing dispersant with non-covalent bond function prepared by adenine does not change the conductivity of the carbon material, and can directly introduce nitrogen, thereby avoiding fussy experimental steps. The electron-deficient structure of the dispersant molecule is tightly combined with the carbon material rich in electrons through pi-pi action, hydroxyl drives the carbon material to disperse in water, long-term dispersion stability is realized through electrostatic mutual exclusion, and silicon hydroxyl at the tail end can directly form a conductive film through self-crosslinking. The dispersant has excellent catalytic performance due to the abundant nitrogen atoms. Compared with the traditional dispersing agent, the graphene dispersing concentration can reach 4mg/mL, which is higher than the dispersing value of most of the existing dispersing agents.
Drawings
FIG. 1 shows FT-IR spectra of adenine, GPTMS and DSiA precursor.
FIG. 2 shows the precursors of adenine, GPTMS and DSiA1H NMR spectrum. Wherein a is GPTMS1H NMR chart, b for DSiA precursor1H NMR chart, c for adenine1H NMR chart.
Fig. 3 is an SEM image of the graphene dispersion after drying on the surface of the silicon wafer and a TEM image of the graphene dispersion after drying on the surface of the copper mesh, in which a is an SEM image of the graphene dispersion after drying on the surface of the silicon wafer at 600 times, b is an SEM image of the graphene dispersion after drying on the surface of the silicon wafer at 10000 times, c is a TEM image of the graphene dispersion after drying on the surface of the copper mesh at 25000 times, and d is a TEM image of the graphene dispersion after drying on the surface of the copper mesh at 25000 times, respectively.
Fig. 4 is an AFM image of the graphene dispersion after drying on a silicon wafer. Wherein a and c are a height distribution diagram of the few-layer graphene and an AFM diagram of the few-layer graphene, and b and d are a height distribution diagram of the single-layer graphene and an AFM diagram of the single-layer graphene.
FIG. 5 is SEM images of a CNT without DSiA and DSiA: CNT ratios of 1:1,1:2,1:3,1:4,1:5, respectively, wherein a is an SEM image of a CNT without DSiA at 7000 times and 15000 times magnification, b is an SEM image of a CNT mass ratio of 1:1 at 7000 times and 15000 times magnification, c is an SEM image of a CNT at 1:2 at 7000 times and 15000 times magnification, d is an SEM image of a DSiA: CNT at 1:3 at 7000 times and 15000 times magnification, e is an SEM image of a DSiA: CNT at 1:4 at 7000 times and 15000 times magnification, and f is an SEM image of a CNT at 1:5 at 7000 times and 15000 times magnification.
Fig. 6 is an SEM image of the reduced graphene oxide dispersion after drying on the surface of the silicon wafer.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the present invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the present invention and is not intended to limit the scope of the claims which follow.
The following are examples of specific applications of the present invention.
Example 1
The invention discloses a graphene dispersant, which has the following structure:
the preparation method of the graphene dispersing agent comprises the following specific steps:
1) adding 1g of adenine and 3.5g of 3-glycidoxypropyltrimethoxysilane into 50ml of anhydrous methanol reagent, placing the mixture into a flask, stirring and reacting at 65 ℃ for 36h, taking out a product after the reaction, cooling to room temperature, transferring the cooled solution into a rotary evaporation bottle, and removing methanol by rotary evaporation at 40 ℃ in a vacuum state to obtain a dispersant precursor.
2) Adding 2g of dispersant precursor into 40ml of 0.1mol/L formic acid aqueous solution, carrying out water bath ultrasound on the mixed solution for 5min to uniformly mix the solution, transferring the mixed solution into a flask, and carrying out stirring reaction for 72h at 25 ℃ to obtain the DSiA solution. The DSiA solution obtained from the reaction was prepared at 10mg/mL with deionized water and transferred to a reagent bottle for further use.
FIG. 1 shows FT-IR spectra of adenine, GPTMS and DSiA precursor. The FT-IR spectrum showed 908cm in DSiA (C) compared to GPTMS-1The disappearance of the peak indicates the occurrence of the ring-opening reaction. And 1650cm-1The C is equal to N and the vibration peak is 3196cm-1The C-H stretching vibration peak on the imidazole ring proves the successful synthesis of DSiA (C).
FIG. 2 shows the precursors of adenine, GPTMS and DSiA1H NMR spectrum. Wherein a in GPTMS1、a2The peak disappears and the chemical shift changes significantly, indicating the occurrence of a ring opening reaction, which can prove the successful synthesis of the product.
Example 2
A preparation method of a graphene dispersion liquid, which uses the dispersant described in example 1, specifically comprises the following steps:
taking 5mg of graphene powder, respectively adding 1mL, 0.5mL, 0.25mL, 0.17mL and 0.13mL of 10mg/mL DSiA solution, preparing 0.5mg/mL graphene dispersion liquid by using deionized water, carrying out water bath ultrasound for 5min for preliminary dispersion, and further carrying out ultrasound dispersion for 30min by using an ultrasonic cell crusher to obtain the corresponding graphene dispersion liquid. The ultrasonic power is 350W during ultrasonic treatment, and ultrasonic treatment is stopped for 3s for 30min every 3 s.
GR dispersions of 0.5mg/mL were prepared in a DSiA/GR mass ratio of 2:1, 1:1,1:2,1:3 and 1:4 and dispersed by an ultrasonic cell disruptor to give dispersions of very uniform appearance. Under the condition that the ratio of DSiA to GR is 1:1, the GR dispersion concentration is increased to 5mg/mL, and no obvious particle aggregation phenomenon appears in appearance. Fig. 3 is an SEM image of the graphene dispersion after drying on the surface of the silicon wafer and a TEM image of the graphene dispersion after drying on the surface of the copper mesh, respectively. Fig. 4 is an AFM image of the graphene dispersion after being dried on a silicon wafer, and the existence of the monolayer GR can be proved by a map.
Example 3
A method for preparing a carbon nanotube dispersion, using the dispersant described in example 1, specifically comprises the following steps:
taking 5mg of multi-walled carbon nanotube powder, respectively adding the powder into 0mL, 0.5mL, 0.25mL, 0.17mL, 0.13mL and 0.1mL of DSiA solution, then adding deionized water to 10mL to prepare 0.5mg/mL of dispersion liquid, carrying out water bath ultrasound on the prepared dispersion liquid for 5min, and then carrying out ultrasound on the dispersion liquid for 30min by using an ultrasonic cell crusher to completely disperse the dispersion liquid, thus obtaining the corresponding multi-walled carbon nanotube dispersion liquid. The power of the ultrasonic wave is 350W, the ultrasonic wave stops for 3s every 3s, and the time is 30 min.
CNT dispersions having a CNT concentration of 0.5mol/L and having a DSiA/CNT ratio of 0:1, 1:1,1:2,1:3,1:4, and 1:5, respectively, were prepared. The newly prepared dispersion was still uniformly dispersed in appearance at a DSiA to CNT ratio of 1:5, while the dispersion without DSiA was allowed to stand for several minutes before aggregation and sedimentation occurred at the bottom of the dispersion. The dispersion was centrifuged at 5000rpm for 30min using a high speed centrifuge, with little settling at the bottom of the dispersion with a DSiA to CNT ratio of 1:5, and no settling occurred with the other dispersant amounts of the dispersion. Meanwhile, a natural standing mode is adopted for judging the dispersion stability, and the bottom of each proportion of dispersion liquid is not settled after standing for 1 month, so that the graphene dispersing agent disclosed by the invention is good in dispersibility. FIG. 5 is SEM images of DSiA-free CNTs and DSiA/CNT ratios of 1:1,1:2,1:3,1:4, and 1:5, respectively, and it can be seen that CNTs not added with DSiA are entangled with each other and are seriously aggregated, but that the dispersion effect of carbon nanotubes in each ratio of fields is good after DSiA is added.
Example 4
A preparation method of a reduced graphene oxide dispersion liquid, which uses the dispersant described in example 1, specifically comprises the following steps:
preparing graphene oxide dispersion liquid by a Hummers method, carrying out hydrothermal reaction on 1g of graphene oxide and 2g of ascorbic acid at 80 ℃ for 12 hours to obtain reduced graphene oxide hydrogel, washing the reduced graphene oxide hydrogel with deionized water for several times to remove redundant reducing agents, and primarily crushing the hydrogel with a glass rod.
Taking 5mg reduced graphene oxide hydrogel, respectively adding 1mL, 0.5mL, 0.25mL and 0.17mL of DSiA solution, adding deionized water to prepare 0.5mg/mL of dispersion liquid, firstly performing ultrasonic treatment in a water bath for 5min to preliminarily disperse the dispersion liquid, and then dispersing the dispersion liquid in an ultrasonic cell crusher for 30min to completely disperse the reduced graphene oxide to obtain corresponding reduced graphene oxide dispersion liquid. The power is set to 350W during ultrasonic treatment, the ultrasonic treatment is stopped for 3s every 3s, and the ultrasonic treatment is carried out for 30 min.
A dispersion having a lower concentration was prepared, and the dispersion was carried out while fixing RGO at 0.5mg/mL and having DSiA to RGO ratios of 2:1, 1:1,1:2, and 1:3, respectively, and was found to be good in appearance. The mass ratio of DSiA to RGO is kept at 1:1, the dispersion concentration is increased to 3mg/mL, and the dispersion state can be maintained. FIG. 6 is an SEM image of the reduced graphene oxide dispersion after drying on the surface of a silicon wafer, and it can be seen that DSiA has good dispersibility for RGO.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A self-crosslinking graphene dispersant is characterized in that the self-crosslinking graphene dispersant is DSiA, the structural formula is shown as a formula (I),
2. the preparation method of the self-crosslinking graphene dispersant of claim 1, characterized by comprising the following steps:
1) taking a certain amount of adenine and 3-glycidyl ether oxypropyl trimethoxy silane in a methanol reagent, stirring and reacting for a period of time at a certain temperature, and performing rotary evaporation to remove methanol after reaction to obtain a dispersant precursor;
2) adding a certain amount of dispersant precursor into formic acid aqueous solution with a certain concentration, and stirring and reacting for a period of time at a certain temperature to obtain DSiA solution.
3. The method for preparing the self-crosslinking graphene dispersant according to claim 2, wherein in the step 1), the molar ratio of adenine to 3-glycidoxypropyltrimethoxysilane is 1: 1.8-2.2.
4. The preparation method of the self-crosslinking graphene dispersant according to claim 3, wherein in the step 1), the stirring reaction temperature is 65-75 ℃, the stirring reaction speed is 150-200 rpm, and the stirring reaction time is 24-36 h.
5. The preparation method of the self-crosslinking graphene dispersant according to claim 4, wherein in the step 1), the rotary steaming temperature is 30-40 ℃, and the rotary steaming strength is less than 0.15 Mpa.
6. The preparation method of the graphene dispersant according to claim 5, wherein in the step 2), the stirring temperature is 20-60 ℃, and the stirring speed is 100-150 rpm.
7. A nano carbon material dispersion liquid is characterized by comprising the following preparation methods:
adding the self-crosslinking graphene dispersing agent of claim 1 into nano carbon material powder with a certain mass, deionized water, performing ultrasonic treatment in a water bath, and further performing ultrasonic dispersion by using an ultrasonic cell crusher to obtain a corresponding nano carbon material dispersion liquid.
8. The nanocarbon material dispersion liquid according to claim 7, wherein the ultrasonic power is 350W, 3s is stopped for each 3s ultrasonic, and the ultrasonic time is 0.5 h.
9. The nanocarbon material dispersion liquid as claimed in claim 8, wherein the mass ratio of the nanocarbon material to the dispersant to water is 1 (0.3-2) to (250-2000).
10. The nanocarbon material dispersion liquid according to claim 9, wherein the nanocarbon material is one or more of graphene, multiwalled carbon nanotube, redox graphene, and carbon black.
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| CN115124562A (en) * | 2022-07-05 | 2022-09-30 | 辽宁大学 | Naphthyl high-reactivity graphene dispersing agent and preparation method and application thereof |
| CN115215897A (en) * | 2022-07-28 | 2022-10-21 | 辽宁大学 | Purine molecule-based high-reactivity nano carbon material dispersant and preparation method thereof |
| CN115322214A (en) * | 2022-07-25 | 2022-11-11 | 辽宁大学 | Self-crosslinkable thienyl graphene dispersing agent and preparation method and application thereof |
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| CN115215897B (en) * | 2022-07-28 | 2024-04-12 | 辽宁大学 | High-reactivity nano carbon material dispersing agent based on purine molecules and preparation method thereof |
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