CN109293982B - Preparation method of composite aerogel with high mechanical strength - Google Patents
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Abstract
The invention discloses a preparation method of a composite aerogel with high mechanical strength. The invention adopts one-dimensional nano-cellulose and two-dimensional graphene oxide to provide a skeleton structure, and improves the mechanical strength of the composite aerogel through the action of hydrogen bonds and gelatin molecules. The dialdehyde crosslinking agent is adopted to carry out chemical crosslinking with the nano-cellulose and the gelatin to respectively generate acetal and Schiff base to form a three-dimensional network structure, the mechanical strength of the composite aerogel is further improved, and the maximum specific compression modulus reaches 2.5MPa cm3(ii) in terms of/g. The used raw materials are non-toxic and harmless, are biodegradable, have simple preparation process, and meet the requirements of economy and environmental protection. The prepared composite aerogel has wide application in the aspects of heat insulation materials, energy-saving materials, sound insulation materials, adsorbents and the like.
Description
Technical Field
The invention belongs to the technical field of polymer composite materials, and particularly relates to a preparation method of a composite aerogel with high mechanical strength.
Background
Aerogel materials are nanoporous materials formed by the mutual coalescence of colloidal particles or polymer molecules, have a three-dimensional open-pore framework structure, and are mainly prepared by a sol-gel method and a special drying technology [ Boday D J, muritihi B, storver RJ, et al.j Non-crystals Solids, 2012, 358: 1575 1580; azevedo C, Cenedese P, Dubot P.J Mater Sci, 2011, 22: 1161-: 4243-; cui S, Cheng W, Shen X D, et al energy Environ Sci, 2011, 4 (6): 2070-2074]. However, since the general aerogel materials have the disadvantages of high brittleness, low strength and the like, the practical application of the aerogel materials is limited, and increasing the strength of the aerogel matrix becomes a key point of the current research. With the progress of nanotechnology, the improvement of mechanical properties of aerogel can be realized by compounding aerogel with nanomaterials [ feng jian, gao qingfu, feng army zong, etc.. the university of national defense science and technology, 2010, 32 (1): 40-44].
Gelatin is a linear polypeptide polymer containing eighteen different amino acids, has partial triple helix structure, and has-OH and-NH on molecular chain2and-COOH, etc. Gelatin, as a very traditional water-soluble natural polymer, has the advantages of no toxicity, biodegradability, low cost and the like, and is widely applied to the fields of food, medicine and photography. Gelatin is soluble in water at high temperatures and gels at low temperatures, and is an excellent base material for aerogel production [ Emo C, Patrizia C, Femandes E G, et al biomacromolecules, 2001, 2: 806-; elzoghby a o.j Control Release, 2013, 172: 1075-1091]。
Graphene can be regarded as a two-dimensional planar structure with a single atomic layer thickness constructed by hybridization of carbon atoms, and is a first true two-dimensional crystal material [ Geim a K, Novoselov K s.nat Mater, 2007, 6: 183-191]. The characteristic of the single-atom thickness of graphene enables atoms of the structure to be exposed, and the structure has ultrahigh specific surface area, and the excellent characteristics enable the graphene to show potential application prospects and wide application values in various fields [ Zhao J, Ren W, Cheng H-m.j Mater Chem, 2012, 22: 20197-20202].
Disclosure of Invention
The purpose of the invention is as follows: aiming at the defects in the prior art, the invention aims to provide the preparation method of the composite aerogel with high mechanical strength, and the prepared composite aerogel has high mechanical strength, the maximum yield strength of 42kPa and good practical application performance.
The technical scheme is as follows: in order to achieve the purpose of the invention, the invention adopts the technical scheme that:
a preparation method of composite aerogel with high mechanical strength comprises the steps of adding gelatin into a mixed solution of nano-cellulose and graphene, uniformly mixing and dispersing, adding a dialdehyde chemical cross-linking agent, and regulating and controlling an aerogel structure in a mode of forming acetal with the nano-cellulose and Schiff base with the gelatin to prepare the composite aerogel.
The preparation method of the composite aerogel with high mechanical strength comprises the following steps:
1) preparing nano-cellulose and graphene dispersion liquid, and uniformly mixing the nano-cellulose and graphene dispersion liquid through ultrasonic dispersion;
2) adding gelatin into the mixed dispersion liquid obtained in the step 1), and stirring and dispersing uniformly under a heating condition;
3) adding the dialdehyde crosslinking agent into the mixed solution obtained in the step 2), and uniformly stirring and dispersing;
4) pre-cooling the solution obtained in the step 3) to form hydrogel, then rapidly freezing the hydrogel by using liquid nitrogen, and freeze-drying the hydrogel in a freeze dryer to obtain a composite aerogel sample;
5) and curing the obtained composite aerogel in an oven.
In the step 1), the nanocellulose is one of cellulose nanofibrils, cellulose nanocrystals and bacterial cellulose.
In the step 1), the mixed dispersion liquid of the nano-cellulose and the graphene is stable and uniform, and the total mass percentage concentration of the nano-cellulose and the graphene is 0.5-2.0 wt%.
In the step 2), the heating and stirring temperature is 40-70 ℃.
In the step 2), the mass ratio of the nano-cellulose to the gelatin is 0.5: 99.5-10: 90, and the mass ratio of the graphene oxide to the nano-cellulose is 1: 5-1: 1.
In the step 3), the dialdehyde crosslinking agent is one of glyoxal, glutaraldehyde and dialdehyde starch.
In the step 3), the percentage of the dialdehyde crosslinking agent to the total mass of the nano-cellulose, the graphene and the gelatin is 3-30 wt%.
In the step 3), reacting for 2-6 h at 50-70 ℃ and pH of 5-6 to obtain a uniform and transparent solution.
In the step 4), the solution obtained in the step 3) is pre-cooled at 4 ℃ for 12h to form hydrogel, then the hydrogel is rapidly frozen by liquid nitrogen, and the hydrogel is freeze-dried in a freeze dryer at-91 ℃ for 3 days to obtain a composite aerogel sample.
In the step 5), the obtained composite aerogel is cured in an oven at 105-120 ℃ for 1-4 hours.
The composite aerogel obtained by the preparation method of the composite aerogel with high mechanical strength.
Has the advantages that: compared with the prior art, the invention has the following advantages:
1) the one-dimensional nano-cellulose and the two-dimensional graphene oxide are adopted to provide a skeleton structure, and the mechanical strength of the composite aerogel is improved through the action of hydrogen bonds and gelatin molecules.
2) The dialdehyde crosslinking agent is adopted to carry out chemical crosslinking with the nano-cellulose and the gelatin to respectively generate acetal and Schiff base to form a three-dimensional network structure, the mechanical strength of the composite aerogel is further improved, and the maximum specific compression modulus reaches 2.5MPa cm3/g。
3) The used raw materials are non-toxic and harmless, are biodegradable, have simple preparation process, and meet the requirements of economy and environmental protection.
4) The prepared composite aerogel has wide application prospect in the aspects of heat insulation materials, energy-saving materials, sound insulation materials, adsorbents and the like.
Drawings
Fig. 1 is a stress-strain curve diagram of a bacterial cellulose-graphene oxide-gelatin-dialdehyde starch composite aerogel, wherein the marks represent mass fraction ratios of gelatin, bacterial cellulose and graphene oxide;
fig. 2 is a photograph of an outline of cellulose nanofibril-graphene oxide-gelatin-glyoxal composite aerogel;
fig. 3 is a surface electron micrograph of cellulose nanofibril-graphene oxide-gelatin-glutaraldehyde composite aerogel;
fig. 4 is a graph of the equilibrium swelling degree of the bacterial cellulose-graphene oxide-gelatin-dialdehyde starch composite aerogel in a phosphate buffer solution with the pH value of 7.4, and the abscissa is the mass fraction ratio of gelatin, bacterial cellulose and graphene oxide.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
1. Preparation of cellulose nanofibril dispersion by TEMPO mediated oxidation
First, 10g of oven-dried fiber slurry was soaked in 500mL of deionized water, followed by the addition of TEMPO (0.16g) and NaBr (1.6g) sequentially and continuously mechanically stirred at room temperature to mix them uniformly. Then, 120mL of NaClO (7.6mmol/L) solution was added to start the oxidation reaction. The pH of the whole reaction system was kept between 10 and 10.5 during the reaction until the pH did not drop any more, and 50mL of ethanol was added to terminate the reaction. The reacted slurry is soaked in 0.1mol/L HCl for acidification and washing. Then, the washed slurry was quantified to 1.5 wt%, the pH was adjusted to 10, and treated with a probe-type ultrasonic cell disruptor (200W) for 20 minutes to obtain a uniform and transparent cellulose nanofibril dispersion.
2. The preparation method of the cellulose nanofibril-graphene oxide-gelatin-dialdehyde starch composite aerogel comprises the following steps:
1) blending the cellulose nanofibril dispersion liquid and the graphene oxide dispersion liquid (sold in the market), and treating and dispersing for 15 minutes by using a probe type ultrasonic cell disruption instrument (200W) to obtain uniform mixed dispersion liquid, wherein the mass fractions of the cellulose nanofibril and the graphene oxide are 0.8 wt% and 0.4 wt%, respectively;
2) and adding gelatin particles into the dispersion liquid of the cellulose nanofibrils and the graphene oxide, and rapidly and mechanically stirring for 2 hours at the temperature of 60 ℃ to uniformly disperse the gelatin particles. The absolute dry mass ratio of the gelatin to the cellulose nanofibrils to the graphene oxide is 8.5: 1: 0.5;
3) gelatinizing dialdehyde starch at 95 ℃ for 30min, adding 10 wt% of gelatinized glutaraldehyde (relative to the total mass of gelatin, cellulose nanofibrils and graphene oxide) into a uniformly mixed solution of cellulose nanofibrils, graphene oxide and gelatin, adding a proper amount of water, and controlling the total solid content in the aqueous solution to be 1.5 wt%; reacting for 3 hours at the temperature of 60 ℃ and the pH value of 5.5 to obtain a uniform and transparent solution;
4) precooling the uniform and transparent solution obtained in the step 3) for 12 hours at 4 ℃ to form hydrogel, then quickly freezing the hydrogel by using liquid nitrogen, and freeze-drying the hydrogel in a freeze-dryer at-91 ℃ for 3 days to obtain a composite aerogel sample;
5) curing the obtained composite aerogel in an oven at 110 ℃ for 2 h;
6) taking composite aerogel with the diameter of 10mm and the height of 20mm, and testing the stress-strain curve of the composite aerogel on an universal mechanical testing machine under the following test conditions: the loading rate was 2mm/min and the strain was 70%. As a result, as shown in FIG. 1, the maximum yield strength was 42kPa, and the elastic modulus was 72 kPa.
The figure of the cellulose nanofibril-graphene oxide-gelatin-glyoxal composite aerogel is shown in fig. 1; the surface electron micrograph of the cellulose nanofibril-graphene oxide-gelatin-glutaraldehyde composite aerogel is shown in fig. 2, and the aerogel has a microscopic three-dimensional network structure and is beneficial to improving the mechanical strength of the aerogel.
Example 2
The preparation method of the bacterial cellulose-graphene oxide-gelatin-dialdehyde starch composite aerogel comprises the following steps:
1) and (2) blending the bacterial cellulose dispersion liquid (sold in the market) and the graphene oxide dispersion liquid (sold in the market), and treating and dispersing for 15 minutes by using a probe type ultrasonic cell disruptor (200W) to obtain uniform mixed dispersion liquid, wherein the mass fractions of the bacterial cellulose and the graphene oxide are 0.6 wt% and 0.6 wt%, respectively.
2) And adding gelatin particles into the dispersion liquid of the bacterial cellulose and the graphene oxide, and rapidly and mechanically stirring for 2 hours at the temperature of 60 ℃ to uniformly disperse the gelatin particles. The oven dry mass ratio of the gelatin, the bacterial cellulose and the graphene oxide is 9: 0.5;
3) gelatinizing dialdehyde starch at 95 ℃ for 30min, adding 20 wt% of gelatinized dialdehyde starch (relative to the total mass of gelatin, bacterial cellulose and graphene oxide) into a uniformly mixed solution of bacterial cellulose, graphene oxide and gelatin, adding a proper amount of water, and controlling the total solid content in the aqueous solution to be 2 wt%; reacting for 3 hours at the temperature of 60 ℃ and the pH value of 5.5 to obtain a uniform and transparent solution;
4) precooling the uniform and transparent solution obtained in the step 3) for 12 hours at 4 ℃ to form hydrogel, then quickly freezing the hydrogel by using liquid nitrogen, and freeze-drying the hydrogel in a freeze-dryer at-91 ℃ for 3 days to obtain a composite aerogel sample;
5) curing the obtained composite aerogel in an oven at 105 ℃ for 2.5 h;
6) taking composite aerogel with the diameter of 10mm and the height of 20mm, and testing the stress-strain curve of the composite aerogel on an universal mechanical testing machine under the following test conditions: the loading rate was 2mm/min and the strain was 70%. The yield strength was measured to be 27kPa, and the elastic modulus was measured to be 62 kPa.
The equilibrium swelling degree of the bacterial cellulose-graphene oxide-gelatin-dialdehyde starch composite aerogel in a phosphate buffer solution with the pH value of 7.4 is shown in figure 3, and the abscissa represents the mass fraction ratio of gelatin, bacterial cellulose and graphene oxide. The obtained aerogel has good water absorption swelling performance, and the integrity of the aerogel in a water phase is ensured by the cross-linked structure.
The stress-strain curves of the bacterial cellulose-graphene oxide-gelatin-dialdehyde starch composite aerogel with different content ratios are shown in fig. 1, and the marks in the graph indicate the mass fraction ratio of gelatin, bacterial cellulose and graphene oxide.
Example 3
1. Preparation of cellulose nanofibril dispersion by TEMPO mediated oxidation
First, 10g of oven-dried fiber slurry was soaked in 500mL of deionized water, followed by the addition of TEMPO (0.16g) and NaBr (1.6g) sequentially and continuously mechanically stirred at room temperature to mix them uniformly. Then, a solution of 120mL NaClO (7.6mmol/L) was added to start the oxidation reaction. The pH of the whole reaction system was kept between 10 and 10.5 during the reaction until the pH did not drop any more, and 50mL of ethanol was added to terminate the reaction. The reacted slurry is soaked in 0.1mol/L HCl for acidification and washing. Then, the washed slurry was quantified to 1.5 wt%, the pH was adjusted to 10, and treated with a probe-type ultrasonic cell disruptor (200W) for 20 minutes to obtain a uniform and transparent cellulose nanofibril dispersion.
2. The preparation method of the cellulose nanofibril-gelatin-dialdehyde starch composite aerogel comprises the following steps:
1) and adding gelatin particles into the cellulose nanofibril dispersion liquid, and rapidly and mechanically stirring for 2 hours at the temperature of 60 ℃ to uniformly disperse the gelatin particles. The oven dry mass ratio of the gelatin to the cellulose nanofibrils is 8.5: 1.5;
2) gelatinizing dialdehyde starch at 95 ℃ for 30min, adding 10 wt% of gelatinized glutaraldehyde (relative to the total mass of gelatin and cellulose nanofibrils) into the uniformly mixed solution of cellulose nanofibrils and gelatin, adding a proper amount of water, and controlling the total solid content in the aqueous solution to be 1.5 wt%; reacting for 3 hours at the temperature of 60 ℃ and the pH value of 5.5 to obtain a uniform and transparent solution;
3) precooling the uniform and transparent solution obtained in the step 2) for 12 hours at 4 ℃ to form hydrogel, then quickly freezing the hydrogel by using liquid nitrogen, and freeze-drying the hydrogel in a freeze-dryer at-91 ℃ for 3 days to obtain a composite aerogel sample;
4) curing the obtained composite aerogel in an oven at 110 ℃ for 2 h;
5) taking composite aerogel with the diameter of 10mm and the height of 20mm, and testing the stress-strain curve of the composite aerogel on an universal mechanical testing machine under the following test conditions: the loading rate was 2mm/min and the strain was 70%. The maximum yield strength was measured at 15kPa, and the elastic modulus was measured at 30 kPa. Therefore, the mechanical strength of the composite aerogel without the added graphene oxide is obviously reduced compared with that of the composite aerogel with the added graphene oxide.
Example 4
The preparation method of the bacterial cellulose-graphene oxide-gelatin composite aerogel comprises the following steps:
1) and (2) blending the bacterial cellulose dispersion liquid (sold in the market) and the graphene oxide dispersion liquid (sold in the market), and treating and dispersing for 15 minutes by using a probe type ultrasonic cell disruptor (200W) to obtain uniform mixed dispersion liquid, wherein the mass fractions of the bacterial cellulose and the graphene oxide are 0.6 wt% and 0.6 wt%, respectively.
2) And adding gelatin particles into the dispersion liquid of the bacterial cellulose and the graphene oxide, and rapidly and mechanically stirring for 2 hours at the temperature of 60 ℃ to uniformly disperse the gelatin particles. The oven dry mass ratio of the gelatin, the bacterial cellulose and the graphene oxide is 9: 0.5;
3) precooling the uniform and transparent solution obtained in the step 2) for 12 hours at 4 ℃ to form hydrogel, then quickly freezing the hydrogel by using liquid nitrogen, and freeze-drying the hydrogel in a freeze-dryer at-91 ℃ for 3 days to obtain a composite aerogel sample;
4) taking composite aerogel with the diameter of 10mm and the height of 20mm, and testing the stress-strain curve of the composite aerogel on an universal mechanical testing machine under the following test conditions: the loading rate was 2mm/min and the strain was 70%. The yield strength was measured at 22kPa, and the elastic modulus was measured at 40 kPa. The composite aerogel which is not crosslinked by dialdehyde starch can not keep complete shape after swelling in water, and the structure of the composite aerogel is gradually disintegrated along with the time.
Claims (4)
1. A preparation method of composite aerogel with high mechanical strength is characterized in that gelatin is added into a mixed solution of nano-cellulose and graphene, the mixture is uniformly mixed and dispersed, a dialdehyde chemical cross-linking agent is added, and the aerogel structure is regulated and controlled in a mode of forming an acetal and Schiff base structure to prepare the composite aerogel; the method comprises the following steps:
1) preparing nano-cellulose and graphene dispersion liquid, and uniformly mixing the nano-cellulose and graphene dispersion liquid through ultrasonic dispersion; the mixed dispersion liquid of the nano-cellulose and the graphene is stable and uniform, and the total mass percentage concentration of the nano-cellulose and the graphene is 0.5-2.0 wt%;
2) adding gelatin into the mixed dispersion liquid obtained in the step 1), and stirring and dispersing uniformly under a heating condition; heating and stirring at the temperature of 40-70 ℃, wherein the mass ratio of the nanocellulose to the gelatin is 0.5: 99.5-10: 90, and the mass ratio of the graphene to the nanocellulose is 1: 5-1: 1;
3) adding a dialdehyde crosslinking agent into the mixed solution obtained in the step 2), and reacting for 2-6 h at 50-70 ℃ and pH of 5-6 to obtain a uniform and transparent solution; the dialdehyde crosslinking agent is one of glyoxal, glutaraldehyde and dialdehyde starch, and accounts for 3-30 wt% of the total mass of the nano-cellulose, the graphene and the gelatin;
4) pre-cooling the solution obtained in the step 3) to form hydrogel, then rapidly freezing the hydrogel by using liquid nitrogen, and freeze-drying the hydrogel in a freeze dryer to obtain a composite aerogel sample;
5) curing the obtained composite aerogel in an oven at 105-120 ℃ for 1-4 h.
2. The method for preparing a composite aerogel having high mechanical strength according to claim 1, wherein in step 1), the nanocellulose is one of cellulose nanofibrils, cellulose nanocrystals and bacterial cellulose.
3. The method for preparing a composite aerogel having high mechanical strength according to claim 1, wherein in the step 4), the solution obtained in the step 3) is pre-cooled at 4 ℃ for 12h to form hydrogel, then is rapidly frozen by using liquid nitrogen, and is freeze-dried in a freeze-dryer at-91 ℃ for 3 days to obtain a composite aerogel sample.
4. A composite aerogel obtained by the method for producing a composite aerogel having high mechanical strength according to any one of claims 1 to 3.
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