CN115649650A - Super-elastic intelligent packaging buffer material with pressure monitoring function and preparation method thereof - Google Patents
Super-elastic intelligent packaging buffer material with pressure monitoring function and preparation method thereof Download PDFInfo
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Images
Abstract
The invention discloses a super-elastic intelligent packaging buffer material with a pressure monitoring function and a preparation method thereof. Through crosslinking various two-dimensional materials with abundant functional groups on the surfaces or one-dimensional materials capable of forming sheets with a crosslinking agent, good and strong interaction is formed between the sheets, and a directional freeze drying method is adoptedObtaining the directional porous aerogel. The intelligent packaging buffer material has excellent mechanical property and sensing property: the high retention rate is more than 50 percent after more than 10000 times of fatigue test under the compression strain of more than 50 percent; the energy loss coefficient is more than 50%; the pressure response range is more than 20kPa, and the sensitivity is more than 1kPa ‑1 (ii) a The preparation process is simple, the cost is low, and the method is suitable for industrial mass production. The damping and buffering device can be used for damping, buffering and protecting valuables or fragile articles in the transportation process, and monitoring the impacted and pressed conditions in the transportation process. Has wide prospect in the field of intelligent buffer packaging.
Description
Technical Field
The invention belongs to the technical field of green intelligent buffer packaging, relates to the technical field of super-elastic aerogel pressure sensors, and particularly relates to a super-elastic intelligent packaging buffer material with a pressure monitoring function and a preparation method thereof. The shock absorption, buffering and protection device is mainly used for shock absorption, buffering and protection of precision instruments or more expensive fragile products (glass, ceramic products and the like) in the transportation process, impact in the transportation process, pressure condition monitoring and the like. Has very wide prospect in the field of intelligent buffer packaging.
Background
With the rapid development of the logistics industry, real-time continuous motion monitoring and protection of high-precision instruments in the transportation process are of great importance to intelligent packaging and modern logistics. The aerogel piezoresistive sensing material can protect goods from collision and monitor the compression borne by the goods in real time during transportation, but has not been reported yet. Commercial cushioning packaging materials such as polyethylene, polypropylene, polystyrene, and the like are non-renewable petroleum-based polymers and are susceptible to environmental pollution. In the field of green intelligent buffer packaging, the application range and the reuse rate of the intelligent buffer material can be improved by the characteristics of green degradability, super elasticity, fatigue resistance, wide stress response range, high pressure resistance sensitivity and the like, the strategy of green sustainable development is met, and the development trend of the intelligent buffer packaging material in the future is realized.
However, researchers have not been able to find intelligent cushioning packaging materials with respect to superelasticity, fatigue resistance, wide stress response range, and the like. Traditional aerogel takes place plastic deformation easily under big compressive strain, can not satisfy its structural stability's in practical application requirement. In addition, the conventional aerogel has a limited service life under high compressive strain, and is difficult to meet the requirement of the cushion packaging material for long-term use.
Chinese patent publication No. CN105566673B discloses a super-elastic and high-adsorbability MXene aerogel and its preparation method. The aerogel can only withstand 50% compressive strain with a maximum compressive strength of only 1.5kPa. In addition, the stress-strain curves of the aerogel under different compressive strains cannot be matched, and severe plastic deformation is shown.
Chinese patent publication No. CN105566673B discloses a preparation method of multifunctional cellulose elastic aerogel. The elastic aerogel has a height retention of only 85% after 1000 cycles of compression under 60% compressive strain.
Non-patent document 1 (Carbohydrate Polymers,2019,208, 232-240) describes an ultra-light, hydrophobic, anisotropic bamboo-derived cellulose nano-fibril aerogel having good shape recovery by freeze casting. The aerogel has a shape recovery of up to 92% after 100 cycles at 80% compression, but the aerogel has not been further investigated for fatigue resistance and has no pressure sensing properties.
The aerogel piezoresistive sensing material can protect goods from collision and monitor the compression condition borne by the aerogel piezoresistive sensing material in the transportation process in real time, but reports are not found yet, and how to realize that the aerogel intelligent buffering packaging material has both superelasticity and fatigue resistance under high compression strain still is a great challenge.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a super-elastic intelligent buffer material with a pressure monitoring function, and the aerogel has the characteristics of excellent mechanical strength, super-elasticity, fatigue resistance, wide stress response range and the like.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the preparation method of the superelastic intelligent packaging buffer material with the pressure monitoring function comprises the following steps of firstly crosslinking a two-dimensional material with rich functional groups on the surface or a one-dimensional material capable of forming a sheet shape by using a crosslinking agent, then preparing directional porous aerogel by adopting a directional freeze drying method, and then further improving the crosslinking degree by heating at high temperature to obtain the superelastic aerogel.
Further, the two-dimensional material with abundant functional groups on the surface or the one-dimensional material capable of forming a sheet shape refers to: one or more of graphene oxide, MXene, cellulose nanofiber, coarse fiber and the like.
Further, the crosslinking agent means: cationic type: cetyl trimethyl quaternary ammonium bromide, octadecyl dimethyl benzyl quaternary ammonium chloride; anionic type: stearic acid, sodium dodecylbenzene sulfonate; zwitterionic: lecithin, amino acid type, dodecyl dimethyl hydroxypropyl sulfobetaine, betaine type; non-ionic: glycerol esters of fatty acids, sorbitan (span) fatty acids, polysorbates; coupling agents used: gamma-Glycidoxypropyltrimethoxysilane (GPTMS), gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, gamma-mercaptopropyltriethoxysilane, gamma-mercaptopropyltrimethoxysilane, heptadecafluorodecyltrimethoxysilane, methyltrimethoxysilane (MTMS), tetrabutyltitanate.
Further, the addition amount of the cross-linking agent is 0.1-50% of the total mass, and the cross-linking condition is as follows: heating or reacting at room temperature for 10-300 min. The purpose of the cross-linking agent is to form strong interaction (such as covalent bond, ionic bond, hydrogen bond and coordination bond) between the components, have good continuity between internal channels and have good structural integrity of the whole material.
Further, the subsequent high-temperature heating temperature of the porous aerogel is 50-500 ℃, so as to further improve the crosslinking degree.
Further, the super-elastic aerogel is prepared by adopting a directional freeze-drying method and has an anisotropic three-dimensional porous structure.
Furthermore, the holes of the super-elastic aerogel are square holes, round holes and hexagonal holes.
Further, the density of the super elastic aerogel is 1-100mg/cm 3 。
Further, the hyperelastic aerogel is subjected to more than 10000 times of fatigue tests under the condition that the compressive strain is more than 50%, and the height retention rate is more than 50%; the energy loss coefficient is more than 50%.
The invention has the effects that the sensing performance of the obtained super-elastic aerogel is as follows: the working range is more than 20kPa, and the sensitivity is more than 1kPa -1 The glass fiber reinforced plastic has the service life of more than 10000 times under the strain of more than 50 percent, and can be used for shock absorption, buffering and protection of precision instruments or more expensive fragile glass and ceramic products in the transportation process, impact in the transportation process, pressure condition monitoring and the like.
Drawings
FIG. 1 is an SEM scanning electron micrograph of the superelastic smart packaging buffer material prepared in example 2.
FIG. 2 is a stress-strain plot of the superelastic smart package buffer material prepared in example 2.
Fig. 3 is a photograph of a compression experiment of the superelastic smart package buffer material prepared in example 2.
FIG. 4 is a stress-strain plot of cyclic compression-rebound at 80% strain for the superelastic smart package buffer prepared in example 2.
FIG. 5 is a graph of the height retention and change in ELC of the cyclic compression-rebound test at 80% strain for the superelastic smart package buffer prepared in example 2.
Fig. 6 is a graph of the sensitivity of the superlastic smart package cushioning material prepared in example 2.
Detailed description of the invention
Example 1:
(1) Weighing a certain mass of gamma-Glycidoxypropyltrimethoxysilane (GPTMS) to be dropwise added into a 15mg/mL MXene solution, and stirring for 10 minutes at 60 ℃ to hydrolyze and condense the GPTMS on the MXene, wherein the mass of the GPTMS is 0.1 percent of that of the MXene.
(2) And (2) pouring the solution obtained in the step (1) into an organic silicon mold, placing the organic silicon mold on liquid nitrogen or other freezing sources, waiting for the mixed solution to be completely frozen and crystallized, and freeze-drying the mixed solution for 36 hours by using a freeze dryer to obtain the porous aerogel.
(3) And (3) placing the porous aerogel obtained in the step (2) in a tube furnace, heating for 2 hours at the temperature of 200 ℃, and promoting MXene and GPTMS to be further crosslinked to finally obtain the super-elastic aerogel with the density of 1 mg/mL.
Example 2:
(1) Preparing 10mg/mL cellulose nano-fiber by oxidizing 2, 6-tetramethylpiperidine oxide (TEMPO), and mixing the cellulose nano-fiber and MXene (10 mg/mL) dispersion liquid in a mass ratio of 2:1, and mixing uniformly.
(2) And (2) dropwise adding a certain mass of GPTMS into the mixed solution obtained in the step (1), and stirring the mixture at room temperature for 2 hours to hydrolyze and condense the GPTMS on the cellulose nano-fiber and MXene, wherein the GPTMS accounts for 30% of the total mass of the cellulose nano-fiber and the MXene.
(3) And (3) pouring the solution obtained in the step (2) into an organic silicon mold, placing the organic silicon mold on liquid nitrogen or other freezing sources, waiting for the mixed solution to be completely frozen and crystallized, and freeze-drying the mixed solution for 36 hours by using a freeze dryer to obtain the porous aerogel.
(4) And (4) placing the porous aerogel obtained in the step (3) in a vacuum oven, and heating and curing for 30 minutes at the temperature of 100 ℃ to promote the GPTMS, the cellulose nanofiber and the MXene to be further crosslinked.
(5) Washing the aerogel obtained in the step (4) with deionized water, washing to remove unreacted GPTMS, placing the washed GPTMS in a freeze dryer for freeze drying for 36 hours again, and finally obtaining the aerogel with the density of 20mg/cm 3 The super-elastic aerogel of (1).
Example 3:
(1) Weighing a certain mass of GPTMS, dropwise adding the GPTMS into a 15mg/mL cellulose nanofiber mixed solution prepared by TEMPO oxidation, and stirring at room temperature for 2 hours to hydrolyze and condense the GPTMS on the cellulose nanofiber, wherein the GPTMS accounts for 10% of the mass of the cellulose nanofiber.
(2) Pouring the solution obtained in the step (1) into an organic silicon mold, placing the organic silicon mold on liquid nitrogen or other freezing sources, waiting for the mixed solution to be completely frozen and crystallized, and freeze-drying the mixed solution for 36 hours by using a freeze dryer to obtain the porous aerogel.
(3) Placing the porous aerogel obtained in the step (2) in a tubular furnace, heating for 6 hours at 500 ℃, promoting cellulose carbonization and further crosslinking with GPTMS, and finally obtaining the porous aerogel with the density of 40mg/cm 3 A super elastic aerogel of (a).
Example 4:
(1) Preparing 20mg/mL cellulose nano-fiber by TEMPO oxidation, and mixing the cellulose nano-fiber and MXene (40 mg/mL) dispersion in a mass ratio of 1:10 are mixed uniformly.
(2) And (2) dropwise adding certain mass of methyltrimethoxysilane (MTMS) into the mixed solution obtained in the step (1), and stirring at room temperature for 6 hours to hydrolyze and condense the MTMS on the cellulose nanofiber and MXene, wherein the MTMS is 50% of the total mass of the cellulose nanofiber and the MXene.
(3) And (3) pouring the solution obtained in the step (2) into an organic silicon mold, placing the organic silicon mold on liquid nitrogen or other freezing sources, waiting for the mixed solution to be completely frozen and crystallized, and freeze-drying the mixed solution for 36 hours by using a freeze dryer to obtain the porous aerogel.
(4) And (4) heating the porous aerogel obtained in the step (3) in a vacuum oven at 100 ℃ for 1 hour to promote further crosslinking of the MTMS, the cellulose nanofibers and MXene.
(5) Washing the aerogel obtained in the step (4) with deionized water, washing to remove unreacted MTMS, placing the washed aerogel in a freeze dryer, and freeze-drying the aerogel for 36 hours again to finally obtain the aerogel with the density of 100mg/cm 3 The super-elastic aerogel of (1).
According to the invention, various two-dimensional materials with abundant functional groups on the surfaces or one-dimensional materials capable of forming sheets are crosslinked with the crosslinking agent, so that good and strong interaction is formed between the sheets, and the oriented porous aerogel obtained by adopting an oriented freeze drying method has excellent mechanical property, compression resilience, fatigue resistance and wide pressure response range. For example, a square-pore superelastic aerogel was obtained based on example 2, as shown in the SEM electron micrograph of fig. 1. The super-elasticity shows that the material can be completely recovered under different compressive strains, and the maximum compressive strain can reach 90%, as shown in the stress-strain curve of fig. 2. The fatigue resistance is shown under 80% compressive strain, and after cyclic compression of 100000 times, the strain can still reach 14.5kPa, the height retention rate is 90.3%, and the energy loss coefficient is 70.5%, as shown in figures 3-5. And the superelastic aerogel showed a broad working range of 0-52.8kPa, as shown in fig. 6. Based on the above properties, the prior art can not achieve the above properties.
The above embodiments are merely illustrative of the present invention and should not be limited to the disclosure of the embodiments. The specific substances in the product components disclosed in the technical scheme of the invention can be implemented by the invention, and the technical effects are the same as those obtained in the examples, and the examples are not separately illustrated. Therefore, it is intended that all equivalents and modifications which do not depart from the spirit of the invention disclosed herein are deemed to be within the scope of the invention.
Claims (10)
1. A preparation method of a superelastic intelligent packaging buffer material with a pressure monitoring function is characterized by comprising the following steps of firstly crosslinking a two-dimensional material with rich functional groups on the surface or a one-dimensional material capable of forming a sheet shape by using a crosslinking agent, then preparing an oriented porous aerogel by adopting an oriented freeze drying method, and then further improving the crosslinking degree by heating at high temperature to obtain the superelastic aerogel.
2. The method for preparing the superelastic intelligent packaging buffer material with the pressure monitoring function according to claim 1, wherein the two-dimensional material with rich functional groups on the surface or the one-dimensional material capable of forming a sheet shape is as follows: one or more of graphene oxide, MXene, cellulose nanofiber, coarse fiber and the like.
3. The preparation method of the superelastic intelligent packaging buffer material with the pressure monitoring function according to claim 1, wherein the crosslinking agent is: cationic type: cetyl trimethyl quaternary ammonium bromide, octadecyl dimethyl benzyl quaternary ammonium chloride; anionic type: stearic acid, sodium dodecylbenzenesulfonate; zwitterionic: lecithin, amino acid type, dodecyl dimethyl hydroxypropyl sulfobetaine, betaine type; non-ionic: glycerol esters of fatty acids, sorbitan (span) fatty acids, polysorbates; coupling agents used: gamma-Glycidoxypropyltrimethoxysilane (GPTMS), gamma-aminopropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, gamma-mercaptopropyltriethoxysilane, gamma-mercaptopropyltrimethoxysilane, heptadecafluorodecyltrimethoxysilane, methyltrimethoxysilane (MTMS), tetrabutyltitanate.
4. The preparation method of the superelastic intelligent packaging buffer material with the pressure monitoring function as claimed in claim 1, wherein the amount of the added crosslinking agent is 0.1-50% of the total mass, and the crosslinking conditions are as follows: heating or reacting at room temperature for 10-300 min.
5. The superelastic intelligent packaging buffer material with pressure monitoring function and the method for preparing the same according to claim 1, wherein the porous aerogel is subsequently heated at 50-500 ℃ in order to further increase the degree of crosslinking.
6. The method for preparing the superelastic intelligent packaging buffer material with the pressure monitoring function according to claim 1, wherein the superelastic aerogel is prepared by a directional freeze-drying method, and the aerogel has an anisotropic three-dimensional porous structure.
7. The method for preparing the superelastic intelligent packaging buffer material with the pressure monitoring function according to claim 1 or 6, wherein the holes of the superelastic aerogel are square holes, round holes or hexagonal holes.
8. The method for preparing the superelastic intelligent packaging buffer material with the pressure monitoring function according to claim 1, wherein the density of the superelastic aerogel is 1-100mg/cm 3 。
9. The superelastic intelligent packaging buffer material with the pressure monitoring function is characterized by being prepared by the method of any one of claims 1-8, wherein the height retention rate of the obtained superelastic aerogel is more than 50%; the energy loss coefficient is more than 50%, the working range is more than 20kPa, and the sensitivity is more than 1kPa -1 And the service life is more than 10000 times under the strain of more than 50 percent.
10. The application of the superlastic intelligent packaging buffer material with the pressure monitoring function in the aspects of shock absorption, buffering and protection in the transportation process and monitoring of impacted and pressed conditions in the transportation process of the superelastic intelligent packaging buffer material with the pressure monitoring function in claim 9.
Priority Applications (1)
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