CN113880876B - 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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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 liquid. The technical scheme adopted is as follows: 1) And (3) placing a certain amount of adenine in methanol, adding 3-glycidoxypropyl trimethoxy silane after ultrasonic stirring, uniformly stirring, reacting at 60 ℃ for 36 hours, and removing the methanol after the reaction. 2) And adding the reacted product into a HCOOH solution with a certain concentration, and stirring for 72 hours to obtain a dispersant DSiA solution. 3) Adding a certain mass of nano carbon material into a DSiA solution, preparing into different concentrations by using deionized water, performing water bath ultrasonic treatment for 5min for preliminary dispersion, and performing further ultrasonic dispersion for 30min by using an ultrasonic cell pulverizer to obtain a corresponding nano carbon material dispersion liquid.
Description
Technical Field
The invention relates to the field of dispersing agents and stabilizing agents, in particular to a self-crosslinking graphene dispersing agent, a preparation method and a nano carbon material dispersing liquid.
Background
The nano carbon material comprises Graphene (GR), carbon Nano Tube (CNT), reduced Graphene Oxide (RGO) and the like, has excellent properties of radiation resistance, chemical resistance, high thermal conductivity, high electrical conductivity, high specific surface area and the like, and has very wide application prospect in the fields of energy storage, sensors, photoelectricity and the like.
The nano carbon materials have very strong pi-pi conjugation effect, so aggregation is very easy to occur, the dispersibility of the nano carbon materials in water and organic solvents is very poor, and the application of the nano carbon materials in practical production and life is limited to a great extent. Therefore, it is 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 to graft different types of functional groups on the surface of the nano carbon material so as to improve the dispersion performance of the nano carbon material; the other is to better disperse the nanocarbon material through electrostatic action, steric hindrance action and the like of the dispersing agent. Existing dispersants mainly include two types: one class is traditional dispersants such as Sodium Dodecyl Benzene Sulfonate (SDBS), polyvinylpyrrolidone (PVP), acacia, and the like; the other is a novel complex organic molecule. The traditional dispersing agent has limited capability of dispersing the nano carbon material in water, generally has the problems of large dispersing agent dosage, low dispersing concentration and the like, and excessive dispersing agent molecules can have adverse effects on the application of the subsequent carbon material. Most of the novel dispersants reported in the literature generally have better dispersion performance on the nano carbon material, but also have the problems of complex synthesis, high cost, lack of functionality and the like, and cannot meet the needs of actual production and life.
Therefore, the novel and efficient graphene dispersing agent which has low raw material cost, simple synthesis method, small amount in actual use and higher reactivity is designed and synthesized, and has important significance. The nano carbon material dispersion prepared based on the method has great application potential in the fields of composite materials, energy sources, catalysis, environment and the like.
Disclosure of Invention
In view of the above, the present invention aims to provide a self-crosslinking graphene dispersing agent, a nanocarbon material dispersing 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 high-efficiency activity. In addition, the dispersant skeleton contains a plurality of N atoms, so that the carbon material can be further endowed with more excellent catalytic performance.
The invention provides a self-crosslinking graphene dispersing agent, which is DSiA with a structural formula shown as 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-glycidoxypropyl trimethoxy silane in a methanol reagent, stirring and reacting for a period of time at a certain temperature, and removing methanol by rotary evaporation after the reaction to obtain a dispersant precursor;
2) And adding a certain amount of dispersant precursor into a formic acid aqueous solution with a certain concentration, and stirring and reacting for a period of time at a certain temperature to obtain a DSiA solution.
Preferably, in the preparation method of the self-crosslinking graphene dispersing agent, in the step 1), the molar ratio of adenine to 3-glycidoxypropyl trimethoxysilane is 1:1.8-2.2.
Preferably, in the preparation method of the self-crosslinking graphene dispersing agent, in the step 1), the stirring reaction temperature is 65-75 ℃, the stirring reaction rotating speed is 150-200 rpm, and the stirring reaction time is 24-36 h.
Preferably, in the preparation method of the self-crosslinking graphene dispersing agent, in the step 1), the spin steaming temperature is 30-40 ℃, and the spin steaming pressure strength is less than 0.15Mpa.
Preferably, in the preparation method of the graphene dispersing agent, in the step 2), the stirring temperature is 20-60 ℃, and the stirring rotating speed is 100-150 rpm.
The nano carbon material dispersion liquid is characterized by comprising the following preparation method:
taking nano carbon material powder with certain mass, adding the self-crosslinking graphene dispersing agent, deionized water, performing water bath ultrasonic treatment,
further performing ultrasonic dispersion by using an ultrasonic cell grinder to obtain corresponding nano carbon material dispersion liquid.
Preferably, the ultrasonic power of the nano carbon material dispersion liquid is 350W, and the ultrasonic power is 3s for 3s and 0.5h for each ultrasonic wave.
Preferably, the mass ratio of the nanocarbon material, the dispersing agent and the water in the nanocarbon material dispersion liquid is 1 (0.3-2) (250-2000).
Preferably, the nanocarbon material dispersion liquid is one or more of graphene, multi-wall carbon nanotubes, redox graphene and carbon black.
The invention provides a preparation method of graphene dispersion liquid, which specifically comprises the following steps:
taking graphene powder with a certain mass, adding DSiA solution, performing water bath ultrasonic treatment for 5min, and performing further ultrasonic dispersion for 30min by using an ultrasonic cell pulverizer to obtain graphene dispersion liquid. The ultrasonic power is 350W, and the ultrasonic power is stopped for 3 seconds for 30 minutes every 3 seconds.
In the graphene dispersion liquid, the mass ratio of graphene to dispersing agent to water is 1 (0.3-2): (250-2000), and preferably the mass ratio of graphene to dispersing agent to water is 1:1:250.
The invention also provides a preparation method of the multiwall carbon nanotube dispersion liquid, which comprises the following steps:
adding carbon nano tube powder with certain mass into DSiA solution, performing water bath ultrasonic treatment for 5min, and performing ultrasonic treatment by using an ultrasonic cell pulverizer for 30min to obtain carbon nano tube dispersion liquid. The ultrasonic power is 350W, and the ultrasonic power is stopped for 3s every 3s for 30min.
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): (200-2000), and preferably the mass ratio of the carbon nanotubes to the dispersing agent to the water is 1:1:200.
The invention also provides a preparation method of the reduced graphene oxide dispersion liquid, which comprises the following steps:
adding a certain mass of reduced graphene oxide hydrogel into a DSiA solution, performing water bath ultrasonic treatment for 5min, and dispersing for 30min by using an ultrasonic cell pulverizer to obtain reduced graphene oxide dispersion liquid. The ultrasonic power is 350W, the ultrasonic power is stopped for 3s every 3s, and the ultrasonic power is 30min.
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 treatment at 80 ℃ for 12 hours, the excessive reducing agent is removed by washing with deionized water for several times, 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 dispersing agent to the water is 1 (0.3-2): 300-2000, and preferably the mass ratio of the reduced graphene oxide to the dispersing agent to the water is 1:1:300.
The invention has the following beneficial effects:
the N-containing dispersing agent prepared by adenine has the advantages that the conductivity of the carbon material is not changed, nitrogen can be directly introduced, and complicated experimental steps are avoided. The electron-deficient structure of the dispersant molecule is tightly combined with the electron-rich carbon material through pi-pi action, the hydroxyl groups drive the carbon material to disperse in water, long-term dispersion stability is realized by electrostatic mutual exclusion, and the terminal silicon hydroxyl groups can directly form a conductive film through self-crosslinking. The dispersing agent has rich nitrogen atoms, so that the dispersing agent has excellent catalytic performance. Compared with the traditional dispersing agent, the dispersing concentration of the graphene can reach 4mg/mL, which is higher than the dispersing value of most of the existing dispersing agents.
Drawings
FIG. 1 is a FT-IR spectrum of the starting adenine, GPTMS and product DSiA precursor.
FIG. 2 shows the starting adenine, GPTMS and product DSiA precursors 1 H NMR spectrum. Wherein a is GPTMS 1 H NMR chart, b is a DSiA precursor 1 H NMR chart, c is adenine 1 H NMR chart.
Fig. 3 is an SEM image of a graphene dispersion liquid after drying the surface of a silicon wafer and a TEM image of a graphene dispersion liquid after drying the surface of a copper mesh, respectively, wherein a is an SEM image of a graphene dispersion liquid after drying the surface of a silicon wafer, b is an SEM image of a graphene dispersion liquid after drying the surface of a silicon wafer, c is a TEM image of a graphene dispersion liquid after drying the surface of a copper mesh, which is enlarged by 10000 times, c is a TEM image of a graphene dispersion liquid after drying the surface of a copper mesh, which is enlarged by 25000 times, and d is a TEM image of a graphene dispersion liquid after drying the surface of a copper mesh.
Fig. 4 is an AFM image of a graphene dispersion after drying on a silicon wafer. Wherein a and c are the height distribution diagram of the few-layer graphene and the AFM diagram of the few-layer graphene, and b and d are the height distribution diagram of the single-layer graphene and the AFM diagram of the single-layer graphene.
FIG. 5 shows a DSiA-free CNT and a DSiA: CNT ratio of 1:1,1:2,1:3,1:4,1:5, respectively, wherein a is a DSiA-free CNT at 7000 times and 15000 times magnification, b is a DSiA: CNT mass ratio of 1:1 at 7000 times and 15000 times magnification, c is a DSiA: CNT mass ratio of 1:2 at 7000 times and 15000 times magnification, d is a DSiA: CNT mass ratio of 1:3 at 7000 times and 15000 times magnification, e is a DSiA: CNT mass ratio of 1:4 at 7000 times and 15000 times magnification, and f is a DSiA: CNT mass ratio of 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 present invention, preferred embodiments of the invention are described below in conjunction with the examples, but it should be understood that these descriptions are merely intended to illustrate further features and advantages of the invention, and are not limiting of the claims of the invention.
The following are examples of specific applications of the invention.
Example 1
The invention discloses a graphene dispersing agent, which has the structure as follows:
the preparation method of the graphene dispersing agent comprises the following specific steps:
1) 1g of adenine and 3.5g of 3-glycidoxypropyl trimethoxysilane are added into 50ml of anhydrous methanol reagent, the mixture is placed into a flask, stirred and reacted for 36 hours at 65 ℃, the product is taken out after the reaction and cooled to room temperature, and then the cooled solution is transferred into a rotary evaporation bottle, methanol is removed by rotary evaporation at 40 ℃ under vacuum, so that a dispersant precursor is obtained.
2) 2g of dispersant precursor is taken and added into 40ml of 0.1mol/L formic acid aqueous solution, the mixed solution is firstly subjected to water bath ultrasonic treatment for 5min to be uniformly mixed, then the mixture is transferred into a flask, and stirring reaction is carried out for 72h at 25 ℃, thus obtaining DSiA solution. The DSiA solution obtained by the reaction was prepared to 10mg/mL with deionized water and transferred to a reagent bottle for use.
FIG. 1 is a FT-IR spectrum of the starting adenine, GPTMS and product DSiA precursor. FT-IR spectrum showed 908cm in DSiA (C) compared to GPTMS -1 The peak at the position disappeared, indicating that the ring-opening reaction occurred. 1650cm -1 C=N stretching vibration peak appears at the position of 3196cm -1 The C-H stretching vibration peak on imidazole ring shows that DSiA (C) is successfully synthesized.
FIG. 2 shows the starting adenine, GPTMS and product DSiA precursors 1 H NMR spectrum. Wherein a in GPTMS 1 、a 2 The peak disappeared and the chemical shift changed obviously, which indicates the occurrence of ring-opening reaction, and the successful synthesis of the product can be proved.
Example 2
A preparation method of graphene dispersion liquid, using the dispersing agent described in example 1, comprises the following specific preparation method:
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 deionized water, performing water bath ultrasonic treatment for 5min for preliminary dispersion, and performing ultrasonic dispersion for 30min by using an ultrasonic cell grinder to obtain corresponding graphene dispersion liquid. The ultrasonic power is 350W during ultrasonic treatment, and the ultrasonic treatment is stopped for 3 seconds for 30 minutes every 3 seconds.
A series of 0.5mg/mL GR dispersions were prepared at 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 a dispersion with a very uniform appearance. When the dispersion concentration of GR is increased to 5mg/mL under the condition that the ratio of DSiA to GR is 1:1, no obvious particle aggregation phenomenon appears in appearance. Fig. 3 is an SEM image of a graphene dispersion after drying the surface of a silicon wafer and a TEM image of a graphene dispersion after drying the surface of a copper mesh, respectively. Fig. 4 is an AFM image of graphene dispersion after drying on a silicon wafer, by which the presence of a monolayer GR can be demonstrated.
Example 3
A method for preparing a carbon nanotube dispersion, using the dispersant described in example 1, comprising the following steps:
taking 5mg of multi-wall carbon nano tube powder, respectively adding the powder into 0, 0.5mL, 0.25mL, 0.17mL, 0.13mL and 0.1mL of DSiA solution, adding deionized water to 10mL to prepare a dispersion liquid of 0.5mg/mL, performing water bath ultrasonic treatment on the prepared dispersion liquid for 5min, and performing ultrasonic treatment on the obtained dispersion liquid by using an ultrasonic cell grinder for 30min to completely disperse the obtained dispersion liquid, thus obtaining the corresponding multi-wall carbon nano tube dispersion liquid. The power of the ultrasonic is 350W, and the ultrasonic is stopped for 3s for 30min every 3 s.
CNT dispersions having a CNT concentration of 0.5mol/L were prepared with DSiA: CNT ratios of 0:1,1:1,1:2,1:3,1:4,1:5, respectively. When the DSiA/CNT ratio of the newly prepared dispersion liquid is 1:5, the dispersion liquid is still uniformly dispersed in appearance, and the bottom of the dispersion liquid is aggregated and settled after the dispersion liquid without adding the DSiA is left to stand for a plurality of minutes. The dispersion was centrifuged at 5000rpm for 30min using a high-speed centrifuge, with only a small sedimentation at the bottom of the dispersion with a DSiA: CNT ratio of 1:5, and no sedimentation of the dispersion with other dispersant amounts. Meanwhile, a natural standing mode is adopted for judging the dispersion stability, and no sedimentation occurs at the bottom of the dispersion liquid in each proportion after standing for 1 month, so that the dispersibility of the graphene dispersing agent is proved to be better. FIG. 5 is a SEM image of DSiA-free CNTs and DSiA to CNT ratios of 1:1,1:2,1:3,1:4, and 1:5, respectively, and it can be seen from the image that CNTs without DSiA are entangled with each other to form severe agglomerates, but after DSiA is added, the dispersion effect of carbon nanotubes in each ratio field is good.
Example 4
A preparation method of a reduced graphene oxide dispersion liquid, using the dispersing agent described in example 1, comprises the following specific preparation method:
and (3) preparing graphene oxide dispersion liquid by adopting a Hummers method, carrying out hydrothermal treatment on 1g of graphene oxide and 2g of ascorbic acid at 80 ℃ for 12 hours to obtain reduced graphene oxide hydrogel, washing with deionized water for several times to remove redundant reducing agent, and carrying out preliminary crushing on the hydrogel by using a glass rod.
Taking 5mg of reduced graphene oxide hydrogel, respectively adding 1mL, 0.5mL, 0.25mL and 0.17mL of DSiA solution, adding deionized water to prepare a dispersion liquid of 0.5mg/mL, performing ultrasonic treatment for 5min by using a water bath to perform primary dispersion, and performing dispersion for 30min by using an ultrasonic cell pulverizer to completely disperse the reduced graphene oxide, thereby obtaining a corresponding reduced graphene oxide dispersion liquid. The power is set to be 350W during ultrasonic treatment, 3s is stopped for 3s every ultrasonic treatment, and the ultrasonic treatment lasts for 30min.
A dispersion with a low concentration was prepared, the fixed RGO was 0.5mg/mL, and dispersion was carried out at a DSiA to RGO ratio of 2:1,1:1,1:2, and 1:3, respectively, and found to be good in appearance. The mass ratio of DSiA to RGO is kept to be 1:1, the dispersion concentration is improved to 3mg/mL, and the dispersion state can still be kept. Fig. 6 is an SEM image of reduced graphene oxide dispersion after drying on the silicon wafer surface, from which it can be seen that DSiA also has good dispersing ability for RGO.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
2. the method for preparing the self-crosslinking graphene dispersing agent as claimed in claim 1, which is characterized by comprising the following steps:
1) Taking a certain amount of adenine and 3-glycidoxypropyl trimethoxy silane in a methanol reagent, stirring and reacting for a period of time at a certain temperature, and removing methanol by rotary evaporation after the reaction to obtain a dispersant precursor;
2) And adding a certain amount of dispersant precursor into a formic acid aqueous solution with a certain concentration, and stirring and reacting for a period of time at a certain temperature to obtain a DSiA solution.
3. The method for preparing a self-crosslinking graphene dispersing agent according to claim 2, wherein in the step 1), the molar ratio of adenine to 3-glycidoxypropyl trimethoxysilane is 1:1.8-2.2.
4. The method for preparing a self-crosslinking graphene dispersing agent 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 method for preparing a self-crosslinking graphene dispersing agent according to claim 4, wherein in the step 1), the spin steaming temperature is 30-40 ℃, and the spin steaming pressure strength is less than 0.15Mpa.
6. The method for preparing a graphene dispersing agent according to claim 5, wherein in the step 2), the stirring temperature is 20-60 ℃, and the stirring speed is 100-150 rpm.
7. The nano carbon material dispersion liquid is characterized by comprising the following preparation method:
taking a certain mass of nano carbon material powder, adding the self-crosslinking graphene dispersing agent described in claim 1, deionized water, performing water bath ultrasonic treatment, and further performing ultrasonic dispersion by using an ultrasonic cell pulverizer to obtain a corresponding nano carbon material dispersion liquid.
8. The nanocarbon material dispersion of claim 7, wherein the ultrasonic power is 350W, 3s at 3s per ultrasonic wave, and 0.5h of ultrasonic wave.
9. The nanocarbon material dispersion of claim 8, wherein the mass ratio of the nanocarbon material, the dispersant and the water is 1 (0.3 to 2): 250 to 2000.
10. The nanocarbon material dispersion of claim 9, wherein the nanocarbon material is one or more of graphene, multi-walled carbon nanotubes, redox graphene, and carbon black.
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