CN115650215A - Preparation method of high-elasticity waterborne polyurethane/graphene aerogel - Google Patents
Preparation method of high-elasticity waterborne polyurethane/graphene aerogel Download PDFInfo
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Abstract
The invention relates to the technical field of graphene aerogel, in particular to a preparation method of high-elasticity aqueous polyurethane/graphene aerogel, which is characterized in that graphene oxide, aqueous polyurethane and ascorbic acid are mixed to prepare the graphene aerogel, the aqueous polyurethane is taken as a foaming agent to foam as a template, so that the three-dimensional structure of the graphene aerogel is more stable, the stability of the three-dimensional structure can be enhanced again in a compounding manner in the process, the aqueous polyurethane/graphene oxide foam can be placed in a large container without surface cracking, the later use requirement can be better met, the aqueous polyurethane/graphene aerogel has good biocompatibility and stability, secondary pollution to the environment can not be caused in use, and the preparation method has wide application prospects in some occasions such as water purification, pressure sensing and air purification.
Description
Technical Field
The invention relates to the technical field of graphene aerogel, in particular to a preparation method of high-elasticity waterborne polyurethane/graphene aerogel
Background
With the rapid development in recent years, the pollution of water resources is becoming serious day by day due to the leakage generated during oil exploitation and transportation, and the discharge of domestic sewage and industrial wastewater, which becomes a problem to be solved urgently. In recent years, graphene aerogel has been widely recognized worldwide as a carbon-based material with excellent oil-water separation. The graphene aerogel inherits the excellent characteristics of graphene, and has all the physical characteristics of the aerogel, such as high porosity, high elasticity, good heat insulation and the like. And the utilization of the high elasticity and the resilience cycle of the graphene aerogel has important significance in the recovery stage of oil-water treatment.
Moreover, the high elasticity and the resilience cyclicity of the graphene aerogel can also be applied to the piezoresistive strain sensor, and different from the traditional piezoresistive strain sensor, the density of the graphene aerogel is increased when the pore wall of the graphene aerogel is compressed, the nearby pore walls are contacted with each other to form a conductive path, the resistance is reduced, and therefore the graphene aerogel can also be widely applied to compressible sensing application. Particularly, due to strong pi-pi stacking and van der waals force among graphene sheets, the graphene sheets have a tendency of aggregation, and form a controllable structure through self-assembly, so that the graphene sheets stand out in a plurality of high-elasticity aerogel materials and become an ideal material for constructing a three-dimensional structure.
However, various preparation methods (a sol-gel method, a hydrothermal method and a chemical vapor deposition method) of the graphene aerogel at present have the defects of difficult industrialization, low rebound cycle frequency, poor elasticity and the like, and some preparation methods also use toxic reducing agents such as hydrazine hydrate and the like, so that secondary pollution is caused to the environment and human bodies in actual use. Therefore, the preparation of the green, efficient and stable graphene aerogel with high rebound cycle number is imperative.
Disclosure of Invention
The invention aims to provide the preparation method of the aqueous polyurethane/graphene aerogel, which is simple in process, low in cost, capable of being industrialized, green and free of secondary pollution, aiming at the problems that the graphene aerogel is easy to remove slag, the rebound cycle times are low, the elasticity is poor, the three-dimensional structure is easy to damage and the like in the conventional preparation method.
In order to achieve the purpose, the invention provides the following technical scheme: the preparation method of the high-elasticity aqueous polyurethane/graphene aerogel comprises the following steps:
s1: dispersing graphene oxide in deionized water, and performing ultrasonic treatment to uniformly disperse the graphene oxide in the deionized water to form graphene oxide aqueous dispersion;
s2: stirring the graphene oxide aqueous dispersion, the aqueous polyurethane liquid and the ascorbic acid to uniformly mix the graphene oxide aqueous dispersion, the aqueous polyurethane liquid and the ascorbic acid to obtain a mixed dispersion;
s3: stirring and foaming the mixed dispersion liquid to obtain waterborne polyurethane/graphene oxide foam;
s4: putting the waterborne polyurethane/graphene oxide foam into a specific mould, heating, reacting for a certain time, and taking out the waterborne polyurethane/graphene hydrogel;
s5: placing the waterborne polyurethane/graphene hydrogel in deionized water for dialysis soaking to remove reaction residues in the deionized water;
s6: freezing the dialyzed and soaked aqueous polyurethane/graphene hydrogel, then thawing, and washing with deionized water and absolute ethyl alcohol respectively after completely thawing;
s7: and (3) placing the washed waterborne polyurethane/graphene hydrogel in an oven for drying under normal pressure, and then carrying out annealing treatment to obtain the waterborne polyurethane/graphene hydrogel.
Preferably, the graphene oxide in the step S1 is powder or slurry, the sheet diameter of the graphene oxide is 5um to 200um, the ultrasonic time is 5min to 30min, and the ultrasonic power is 30W to 100W.
Preferably, in the step S2, the concentration of the graphene oxide aqueous dispersion is 3mg/ml to 20mg/ml, the curing amount of the aqueous polyurethane liquid is 30% to 60%, the purity of the ascorbic acid is 80% to 99.99%, and the mass ratio of the graphene oxide to the aqueous polyurethane liquid and the ascorbic acid is 1:1:1 to 1:6:5, the stirring speed is 200r/min to 500r/min, and the stirring time is 5min to 30min.
Preferably, the stirring speed of the mixed dispersion liquid in the step S3 is 700 r/min-2500 r/min, the stirring time is 5 min-30 min, and the foaming volume is 1.5-3 times of the volume of the original dispersion liquid.
Preferably, the heating in the step S4 is performed in a forced air drying oven, the heating temperature is 40 ℃ to 95 ℃, and the reaction time is 2h to 12h.
Preferably, the dialysis soaking time in the step S5 is 6 to 48 hours, and the dialysis soaking water changing times are 3 to 10 times.
Preferably, the freezing time in the step S6 is more than 6h, and the freezing temperature is-10 ℃ to-25 ℃.
Preferably, the drying temperature under normal pressure in the step S7 is 40 to 65 ℃, and the drying time is 6 to 72 hours.
Preferably, in the annealing in step S7, the annealing is performed in an atmosphere of an inert gas or a reducing gas, and the annealing temperature is 300 to 500 ℃ and the annealing time is 30min to 5h.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, graphene oxide, waterborne polyurethane and ascorbic acid are mixed to prepare graphene aerogel, waterborne polyurethane is taken as a foaming agent to foam as a template, so that the three-dimensional structure of the graphene aerogel can be more stable, the stability of the three-dimensional structure can be enhanced again in the process, the waterborne polyurethane/graphene oxide foam can be placed in a large container without surface cracking, the later use requirement can be better met, the waterborne polyurethane/graphene aerogel has good biocompatibility and stability, secondary pollution to the environment can not be caused during use, and the graphene aerogel has a wide application prospect in some occasions such as water purification, pressure sensing and air purification;
2. in the process of preparing the graphene aerogel, dense and stable bubbles can be generated by quickly stirring by using the special structure and characteristics of the waterborne polyurethane, so that the graphene oxide nanosheets can be attached to the bubbles and can be compounded with the waterborne polyurethane; then washing with ultrapure water and absolute ethyl alcohol can wash away the redundant stearic acid and ascorbic acid; the annealing treatment can remove the aqueous polyurethane therein, and only the graphene aerogel is left; finally, the waterborne polyurethane/graphene aerogel can be subjected to multiple cyclic elasticity tests without the occurrence of slag falling, three-dimensional structure damage and the like.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic flow chart of the preparation method of the present invention;
fig. 2 is an elastic modulus diagram of the aqueous polyurethane/graphene aerogel prepared in example two;
fig. 3 is an XRD pattern of the aqueous polyurethane/graphene aerogel prepared in example two.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution:
the preparation method of the high-elasticity waterborne polyurethane/graphene aerogel comprises the following steps:
s1: dispersing graphene oxide in deionized water, and performing ultrasonic treatment to uniformly disperse the graphene oxide in the deionized water to form a graphene oxide aqueous dispersion;
s2: stirring the graphene oxide aqueous dispersion, the aqueous polyurethane liquid and the ascorbic acid to uniformly mix the graphene oxide aqueous dispersion, the aqueous polyurethane liquid and the ascorbic acid to obtain a mixed dispersion;
s3: stirring and foaming the mixed dispersion liquid to obtain waterborne polyurethane/graphene oxide foam;
s4: putting the waterborne polyurethane/graphene oxide foam into a specific mould, heating, reacting for a certain time, and taking out the waterborne polyurethane/graphene hydrogel;
s5: placing the waterborne polyurethane/graphene hydrogel in deionized water for dialysis soaking to remove reaction residues in the deionized water;
s6: freezing the dialyzed and soaked waterborne polyurethane/graphene hydrogel, then thawing, and after completely thawing, respectively washing with deionized water and absolute ethyl alcohol;
s7: and (3) placing the washed waterborne polyurethane/graphene hydrogel in an oven for normal-pressure drying, and then carrying out annealing treatment to obtain the waterborne polyurethane/graphene hydrogel.
Specifically, the graphene oxide in the step S1 is powder or slurry, the sheet diameter of the graphene oxide is 5um to 200um, the ultrasonic time is 5min to 30min, and the ultrasonic power is 30W to 100W.
Specifically, in the step S2, the concentration of the graphene oxide aqueous dispersion is 3mg/ml to 20mg/ml, the curing amount of the aqueous polyurethane liquid is 30% to 60%, the purity of the ascorbic acid is 80% to 99.99%, and the mass ratio of the graphene oxide to the aqueous polyurethane liquid to the ascorbic acid is 1:1:1 to 1:6:5, the stirring speed is 200r/min to 500r/min, and the stirring time is 5min to 30min.
Specifically, the stirring speed of the mixed dispersion liquid in the step S3 is 700 r/min-2500 r/min, the stirring time is 5 min-30 min, and the foaming volume is 1.5 times-3 times of the volume of the original dispersion liquid.
Specifically, the heating in the step S4 is carried out in a forced air drying oven, the heating temperature is 40-95 ℃, and the reaction time is 2-12 h.
Specifically, the dialysis soaking time in the step S5 is 6-48 h, and the dialysis soaking water changing times are 3-10 times.
Specifically, the freezing time in the step S6 is more than 6 hours, and the freezing temperature is-10 ℃ to-25 ℃.
Specifically, in the step S7, the drying temperature under normal pressure is 40-65 ℃, and the drying time is 6-72 h.
Specifically, during the annealing in step S7, the annealing is performed in an atmosphere of an inert gas or a reducing gas, and the annealing temperature is 300 to 500 ℃, and the annealing time is 30min to 5h.
Referring to fig. 1-2, a first embodiment of the present application is:
s1: dispersing graphene oxide with the sheet diameter of 200 mu m in deionized water, and performing ultrasonic treatment for 5min at the ultrasonic power of 30W to uniformly disperse the graphene oxide in the deionized water to form graphene oxide aqueous dispersion;
s2: uniformly mixing 3mg/ml graphene oxide aqueous dispersion with 60% aqueous polyurethane liquid and 99.99% ascorbic acid at a stirring speed of 200r/min for 30min to obtain a mixed dispersion, wherein the mass ratio of the graphene oxide to the aqueous polyurethane liquid to the ascorbic acid is 1:1:1;
s3: stirring the mixed dispersion liquid for 30 minutes at the rotating speed of 700r/min to ensure that the mixed dispersion liquid is foamed and expanded to be 1.5 times of the volume of the original dispersion liquid to obtain waterborne polyurethane/graphene oxide foam;
s4: putting the waterborne polyurethane/graphene oxide foam into a specific mould, and placing the mould in an air-blowing drying oven for heating, wherein the heating temperature is 40 ℃, and the reaction time is 12 hours, and then taking out the waterborne polyurethane/graphene hydrogel;
s5: placing the waterborne polyurethane/graphene hydrogel in deionized water for dialysis soaking for 48h, wherein the soaking water changing times are 3 times, and removing reaction residues in the water;
s6: freezing the dialyzed and soaked aqueous polyurethane/graphene hydrogel at-10 ℃ for more than 6 hours, thawing, and washing with deionized water and absolute ethyl alcohol respectively after complete thawing;
s7: and (3) placing the washed waterborne polyurethane/graphene hydrogel in an oven for drying at the normal pressure, wherein the drying temperature at the normal pressure is 40 ℃, the drying time is 2 hours, then carrying out annealing treatment, wherein the annealing temperature is 300 ℃, the annealing time is 5 hours, and the atmosphere is nitrogen, so as to obtain the waterborne polyurethane/graphene hydrogel.
Referring to fig. 1-3, the second embodiment of the present application is:
s1: dispersing graphene oxide with the sheet diameter of 5 microns in deionized water, and performing ultrasonic treatment for 5min at the ultrasonic power of 30W to uniformly disperse the graphene oxide in the deionized water to form graphene oxide aqueous dispersion;
s2: uniformly mixing the graphene oxide aqueous dispersion with the concentration of 20mg/ml, the aqueous polyurethane liquid with the solidification amount of 30% and the ascorbic acid with the purity of 80% for 30min at a stirring speed of 500r/min to obtain a mixed dispersion, wherein the mass ratio of the graphene oxide to the aqueous polyurethane liquid to the ascorbic acid is 1:4:2;
s3: stirring the mixed dispersion liquid for 5 minutes at the rotating speed of 1500r/min to ensure that the mixed dispersion liquid is foamed and expanded to 2 times of the volume of the original dispersion liquid to obtain waterborne polyurethane/graphene oxide foam;
s4: putting the waterborne polyurethane/graphene oxide foam into a specific mould, and placing the mould in an air-blowing drying oven for heating, wherein the heating temperature is 75 ℃, and the reaction time is 12 hours, and then taking out the waterborne polyurethane/graphene hydrogel;
s5: placing the waterborne polyurethane/graphene hydrogel in deionized water for dialysis soaking for 24 hours, wherein the soaking water changing times are 3 times, and removing reaction residues in the water;
s6: freezing the dialyzed and soaked aqueous polyurethane/graphene hydrogel at-25 ℃ for more than 12 hours, thawing, and washing with deionized water and absolute ethyl alcohol respectively after complete thawing;
s7: and (3) placing the washed waterborne polyurethane/graphene hydrogel in an oven for drying at the normal pressure, wherein the drying temperature at the normal pressure is 65 ℃, the drying time is 2 hours, then carrying out annealing treatment, wherein the annealing temperature is 400 ℃, the annealing time is 5 hours, and the atmosphere is argon, so as to obtain the waterborne polyurethane/graphene hydrogel.
Referring to fig. 1, the third embodiment of the present application is:
s1: dispersing graphene oxide with the sheet diameter of 5-200 microns in deionized water, and performing ultrasonic treatment for 5-30 min at the ultrasonic power of 30-100W to uniformly disperse the graphene oxide in the deionized water to form graphene oxide aqueous dispersion;
s2: uniformly mixing 3-20 mg/ml graphene oxide water dispersion with 30-60% of curing amount of aqueous polyurethane liquid and 80-99.99% of ascorbic acid at a stirring speed of 200-500 r/min for 5-30 min to obtain a mixed dispersion, wherein the mass ratio of the graphene oxide to the aqueous polyurethane liquid to the ascorbic acid is 1:1:1 to 1:6:5;
s3: stirring the mixed dispersion liquid for 3-30 min at the rotating speed of 2500r/min to ensure that the mixed dispersion liquid is foamed and expanded to be 3 times of the volume of the original dispersion liquid to obtain waterborne polyurethane/graphene oxide foam;
s4: putting the waterborne polyurethane/graphene oxide foam into a specific mould, and placing the mould in an air-blowing drying oven for heating, wherein the heating temperature is 95 ℃, and the reaction time is 12 hours, and then taking out the waterborne polyurethane/graphene hydrogel;
s5: placing the waterborne polyurethane/graphene hydrogel in deionized water for dialysis soaking for 6 hours, wherein the soaking water changing times are 10 times, and removing reaction residues in the water;
s6: freezing the dialyzed and soaked waterborne polyurethane/graphene hydrogel at-25 ℃ for more than 12 hours, then thawing, and respectively washing with deionized water and absolute ethyl alcohol after completely thawing;
s7: and (3) placing the washed waterborne polyurethane/graphene hydrogel in an oven for drying at the normal pressure, wherein the drying temperature at the normal pressure is 65 ℃, the drying time is 6h, and then carrying out annealing treatment, wherein the annealing temperature is 500 ℃, the annealing time is 30min, and the atmosphere is argon, so that the waterborne polyurethane/graphene hydrogel is obtained.
In summary, the invention adopts a sol-gel method, takes bubbles and ice as templates, mixes the aqueous polyurethane and the graphene oxide solution, and adds a reducing agent to prepare the aqueous polyurethane/graphene aerogel. Different from the past research, the polyurethane block is used as a template, the waterborne polyurethane liquid is innovatively used as a foaming agent, and the waterborne polyurethane/graphene aerogel is prepared by a one-step method through simple mixing (as shown in figure 3, a characteristic peak of a waterborne polyurethane heavy chain at 24 degrees and a characteristic peak of the graphene aerogel at about 26 degrees can be seen).
The aqueous polyurethane/graphene aerogel has the advantages of good elasticity (90%), high resilience times (10 times) (as shown in figure 2), adjustable shape, biocompatibility, strong experimental repeatability and the like, so that the aqueous polyurethane/graphene aerogel has great competitiveness in the existing fields of high elasticity and adsorption and high commercial value.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (9)
1. The preparation method of the high-elasticity waterborne polyurethane/graphene aerogel is characterized by comprising the following steps: the preparation method comprises the following steps:
s1: dispersing graphene oxide in deionized water, and performing ultrasonic treatment to uniformly disperse the graphene oxide in the deionized water to form graphene oxide aqueous dispersion;
s2: stirring the graphene oxide aqueous dispersion, the aqueous polyurethane liquid and the ascorbic acid to uniformly mix the graphene oxide aqueous dispersion, the aqueous polyurethane liquid and the ascorbic acid to obtain a mixed dispersion;
s3: stirring and foaming the mixed dispersion liquid to obtain waterborne polyurethane/graphene oxide foam;
s4: putting the waterborne polyurethane/graphene oxide foam into a specific mould, heating, reacting for a certain time, and taking out the waterborne polyurethane/graphene hydrogel;
s5: placing the waterborne polyurethane/graphene hydrogel in deionized water for dialysis soaking to remove reaction residues in the deionized water;
s6: freezing the dialyzed and soaked aqueous polyurethane/graphene hydrogel, then thawing, and washing with deionized water and absolute ethyl alcohol respectively after completely thawing;
s7: and (3) placing the washed waterborne polyurethane/graphene hydrogel in an oven for drying under normal pressure, and then carrying out annealing treatment to obtain the waterborne polyurethane/graphene hydrogel.
2. The preparation method of the high-elasticity aqueous polyurethane/graphene aerogel according to claim 1, wherein the preparation method comprises the following steps: the graphene oxide in the step S1 is powder or slurry, the sheet diameter of the graphene oxide is 5-200 um, the ultrasonic time is 5-30 min, and the ultrasonic power is 30-100W.
3. The preparation method of the high-elasticity aqueous polyurethane/graphene aerogel according to claim 1, wherein the preparation method comprises the following steps: in the step S2, the concentration of the graphene oxide aqueous dispersion is 3 mg/ml-20 mg/ml, the curing amount of the aqueous polyurethane liquid is 30% -60%, the purity of the ascorbic acid is 80% -99.99%, and the mass ratio of the graphene oxide to the aqueous polyurethane liquid to the ascorbic acid is 1:1:1 to 1:6:5, the stirring speed is 200r/min to 500r/min, and the stirring time is 5min to 30min.
4. The preparation method of the high-elasticity aqueous polyurethane/graphene aerogel according to claim 1, characterized by comprising the following steps: the stirring speed of the mixed dispersion liquid in the step S3 is 700 r/min-2500 r/min, the stirring time is 5 min-30 min, and the foaming volume is 1.5 times-3 times of the volume of the original dispersion liquid.
5. The preparation method of the high-elasticity aqueous polyurethane/graphene aerogel according to claim 1, characterized by comprising the following steps: and the heating in the step S4 is carried out in a forced air drying oven, the heating temperature is 40-95 ℃, and the reaction time is 2-12 h.
6. The preparation method of the high-elasticity aqueous polyurethane/graphene aerogel according to claim 1, wherein the preparation method comprises the following steps: the dialysis soaking time in the step S5 is 6-48 h, and the dialysis soaking water changing times is 3-10 times.
7. The preparation method of the high-elasticity aqueous polyurethane/graphene aerogel according to claim 1, characterized by comprising the following steps: the freezing time in the step S6 is more than 6h, and the freezing temperature is-10 ℃ to-25 ℃.
8. The preparation method of the high-elasticity aqueous polyurethane/graphene aerogel according to claim 1, wherein the preparation method comprises the following steps: the drying temperature under normal pressure in the step S7 is 40-65 ℃, and the drying time is 6-72 h.
9. The preparation method of the high-elasticity aqueous polyurethane/graphene aerogel according to claim 1, wherein the preparation method comprises the following steps: and in the annealing in the step S7, annealing is carried out in the atmosphere of inert gas or reducing gas, the annealing temperature is 300-500 ℃, and the annealing time is 30 min-5 h.
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