CN111082008A - Preparation method of nanocellulose/zinc oxide compound for electrochemical energy storage - Google Patents
Preparation method of nanocellulose/zinc oxide compound for electrochemical energy storage Download PDFInfo
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Abstract
The invention discloses a nano-cellulose/zinc oxide composite material for electrochemical energy storage, which comprises the following raw materials in parts by weight: the composition comprises the following raw materials in parts by weight: 10-20 parts of nano cellulose, 60-70 parts of zinc oxide, 5-10 parts of a template agent and 3-5 parts of a surfactant. In the invention, because the solution is alkaline in the synthesis process of the cellulose, the obtained cellulose is alkaline, when zinc oxide has a small amount of zinc ions and oxygen ions dissociated under an alkaline condition, the dissociated hetero ions enter the framework of the material to form a framework structure containing the hetero ions, the electrochemical energy storage capacity is favorably improved, and meanwhile, the triethylamine template agent is added, so that the nano cellulose/zinc oxide composite material can obtain an ordered pore channel structure in the subsequent crystallization process, the relative performance of the ordered pore channel structure material is stable, and the triethylamine template agent can play a more effective role in electrochemical energy storage.
Description
Technical Field
The invention belongs to the field of electrochemical energy storage electrode materials, and particularly relates to a preparation method of a nano-cellulose/zinc oxide compound for electrochemical energy storage.
Background
With the development of science and technology, the quality of life of people is continuously improved, and more electronic products become an indispensable part of life of people. On the other hand, problems of fossil fuel reserve consumption and environmental pollution are becoming more serious, and the popularization of electric vehicles is becoming a great trend. Under the premise, higher requirements are put on energy storage equipment such as lithium ion batteries, and the key point of the energy storage equipment is the electrode material, so that the design and development of the electrode material with excellent performance become problems which are urgently needed to be solved by researchers in various countries.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a preparation method of a nano-cellulose/zinc oxide compound for electrochemical energy storage.
The purpose of the invention can be realized by the following technical scheme:
a nano-cellulose/zinc oxide composite material for electrochemical energy storage comprises the following raw materials in parts by weight: 10-20 parts of nano cellulose, 60-70 parts of zinc oxide, 5-10 parts of a template agent and 3-5 parts of a thermal surfactant;
the preparation method of the nano-cellulose/zinc oxide composite material comprises the following steps:
s1 preparation method of cellulose is as follows:
taking wood pulp and deionized water according to a mass ratio of 1: 5, adding the mixture into a beaker, stirring the mixture until the mixture is uniformly dispersed to obtain a wood pulp dispersion liquid, adding sodium bromide of which the mass is one third of that of the wood pulp dispersion liquid, continuously stirring the mixture for 1 to 2 hours, adding sodium hydroxide in the stirring process, adjusting the pH value to be 8 to 9, and after the stirring is successfully completed, performing suction filtration, washing, drying and grinding the mixture into powder to obtain cellulose; the obtained cellulose is alkaline due to the fact that the solution in the cellulose synthesis process is alkaline, when the solution is in an alkaline condition and in the subsequent synthesis process of the nano-cellulose/zinc oxide composite material, a small part of zinc ions and oxygen ions are dissociated from zinc oxide, and the dissociated hybrid ions enter a material framework to form a framework structure containing the hybrid ions;
s2 preparation method of zinc oxide is as follows:
taking zinc oxide powder, roasting the zinc oxide powder in a muffle furnace at 400 ℃ for 4 hours, and cooling the zinc oxide powder to room temperature to obtain the zinc oxide required by the experiment; the purpose of roasting is to prevent the zinc oxide from absorbing moisture and influencing the subsequent experimental results;
s3 preparation method of the nano-cellulose/zinc oxide composite material is as follows:
putting nano-cellulose into a 250ml beaker, adding a certain amount of deionized water, stirring at normal temperature for 0.5-1 h, adding zinc oxide for 3 times, slowly dropwise adding a template agent by using a dropper, gradually enabling the solution to become more viscous, increasing the rotating speed of a stirring paddle, fixing the beaker by using iron, and stopping stirring after stirring for 1-2 h; the template agent is added to ensure that the nano-cellulose/zinc oxide composite material obtains an ordered pore channel structure in the subsequent crystallization process, the relative performance of the ordered pore channel structure material is stable, and the ordered pore channel structure material can play a more effective function when being applied to electrochemical energy storage;
taking a 250ml reaction kettle, pouring the stirred solution into the reaction kettle, adding a surfactant into the reaction kettle, sealing the reaction kettle, putting the reaction kettle into a 200 ℃ oven for crystallization for 48 hours, wearing a high-temperature-resistant glove, taking out, cooling to room temperature, opening, filtering, putting a filter cake into a 100 ℃ oven for drying, taking out, grinding into powder, putting into a tubular furnace, roasting at 350 ℃ for 6 hours under the nitrogen atmosphere, and cooling to room temperature to obtain the nano-cellulose/zinc oxide composite material; the synthesis of the nano-cellulose/zinc oxide composite material adopts a hydrothermal synthesis method, and aims to change the internal structure of the material in the complex reaction process of hydrothermal synthesis, artificially control the internal structure of the material by adding different chemical raw materials, and in turn enable experiments to verify the assumption of people again.
Further, the method comprises the following steps: the stirring speed in the step S3 is 200-250 r/min, and the rotating speed of the stirring paddle in the step S3 is increased to 250-300 r/min.
Further, the method comprises the following steps: the heating rates of the muffle furnace and the tube furnace are both 10 ℃/min.
Further, the method comprises the following steps: the interval time of adding zinc oxide 3 times in step S3 was 10min, and stirring was performed immediately after the addition of zinc oxide.
Further, the method comprises the following steps: the lining of the 250ml reaction kettle in the step S3 is made of polytetrafluoroethylene material.
Further, the method comprises the following steps: the preparation operation process of the nano-cellulose/zinc oxide composite material is completed in a fume hood, and the drying time of the 100 ℃ oven in the step S3 is 3-5 h.
Further, the method comprises the following steps: in step S3, the template agent is triethylamine, and the surfactant is dodecyl trimethyl ammonium bromide.
The invention has the beneficial effects that:
1. in the invention, because the solution is alkaline in the synthesis process of the cellulose, the obtained cellulose is also alkaline, when zinc oxide is in an alkaline condition, a small part of zinc ions and oxygen ions are dissociated, and the dissociated hetero ions enter a skeleton of the material to form a skeleton structure containing the hetero ions, thereby being beneficial to improving the electrochemical energy storage capacity.
2. According to the invention, after the triethylamine template agent is added, the nano-cellulose/zinc oxide composite material obtains an ordered pore channel structure in the subsequent crystallization process, the relative performance of the ordered pore channel structure material is relatively stable, and the material can play a more effective function when being applied to electrochemical energy storage.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
Example 1
The preparation method of the nano-cellulose/zinc oxide composite material comprises the following steps:
s1 preparation method of cellulose is as follows:
taking wood pulp and deionized water according to a mass ratio of 1: 5, adding the mixture into a beaker, stirring the mixture until the mixture is uniformly dispersed to obtain a wood pulp dispersion liquid, adding sodium bromide of which the mass is one third of that of the wood pulp dispersion liquid, continuously stirring the mixture for 1 to 2 hours, adding sodium hydroxide in the stirring process, adjusting the pH value to be 8 to 9, and after the stirring is successfully completed, performing suction filtration, washing, drying and grinding the mixture into powder to obtain cellulose;
s2 preparation method of zinc oxide is as follows:
taking zinc oxide powder, roasting the zinc oxide powder in a muffle furnace at 400 ℃ for 4 hours, and cooling the zinc oxide powder to room temperature to obtain the zinc oxide required by the experiment;
s3 preparation method of the nano-cellulose/zinc oxide composite material is as follows:
putting 10 parts of nano cellulose into a 250ml beaker, adding a certain amount of deionized water, stirring at normal temperature for 0.5-1 h, adding 60 parts of zinc oxide by 3 times, slowly dropwise adding 5 parts of template agent triethylamine by using a dropper, gradually enabling the solution to become more viscous, increasing the rotating speed of a stirring paddle, fixing the beaker by using iron, and stopping stirring after stirring for 1-2 h;
taking a 250ml reaction kettle, pouring the stirred solution into the reaction kettle, adding 3 parts of dodecyl trimethyl ammonium bromide serving as a surfactant into the reaction kettle, sealing the reaction kettle, putting the reaction kettle into a 200 ℃ oven for crystallization for 48 hours, wearing high-temperature-resistant gloves, taking out the reaction kettle, cooling the reaction kettle to room temperature, opening the reaction kettle, filtering the reaction kettle, putting a filter cake into a 100 ℃ oven for drying, taking out the filter cake, grinding the filter cake into powder, putting the powder into a tubular furnace, roasting the powder at 350 ℃ for 6 hours in a nitrogen atmosphere, and cooling the powder to room temperature to obtain the nano cellulose/zinc oxide composite material.
Example 2
The preparation method of the nano-cellulose/zinc oxide composite material comprises the following steps:
s1 preparation method of cellulose is as follows:
taking wood pulp and deionized water according to a mass ratio of 1: 5, adding the mixture into a beaker, stirring the mixture until the mixture is uniformly dispersed to obtain a wood pulp dispersion liquid, adding sodium bromide of which the mass is one third of that of the wood pulp dispersion liquid, continuously stirring the mixture for 1 to 2 hours, adding sodium hydroxide in the stirring process, adjusting the pH value to be 8 to 9, and after the stirring is successfully completed, performing suction filtration, washing, drying and grinding the mixture into powder to obtain cellulose;
s2 preparation method of zinc oxide is as follows:
taking zinc oxide powder, roasting the zinc oxide powder in a muffle furnace at 400 ℃ for 4 hours, and cooling the zinc oxide powder to room temperature to obtain the zinc oxide required by the experiment;
s3 preparation method of the nano-cellulose/zinc oxide composite material is as follows:
putting 20 parts of nano cellulose into a 250ml beaker, adding a certain amount of deionized water, stirring at normal temperature for 0.5-1 h, adding 70 parts of zinc oxide by 3 times, slowly dropwise adding 10 parts of template agent triethylamine by using a dropper, gradually enabling the solution to become more viscous, increasing the rotating speed of a stirring paddle, fixing the beaker by using iron, and stopping stirring after stirring for 1-2 h;
and (2) pouring the stirred solution into a 250ml reaction kettle, adding 5 parts of dodecyl trimethyl ammonium bromide serving as a surfactant into the reaction kettle, sealing the reaction kettle, putting the reaction kettle into a 200 ℃ oven for crystallization for 48 hours, wearing high-temperature-resistant gloves, taking out the reaction kettle, cooling the reaction kettle to room temperature, opening the reaction kettle, filtering the reaction kettle, putting a filter cake into a 100 ℃ oven for drying, taking out the filter cake, grinding the filter cake into powder, putting the powder into a tubular furnace, roasting the powder at 350 ℃ for 6 hours in a nitrogen atmosphere, and cooling the powder to room temperature to obtain the nano cellulose/zinc oxide composite material.
Example 3
The preparation method of the nano-cellulose/zinc oxide composite material comprises the following steps:
s1 preparation method of cellulose is as follows:
taking wood pulp and deionized water according to a mass ratio of 1: 5, adding the mixture into a beaker, stirring the mixture until the mixture is uniformly dispersed to obtain a wood pulp dispersion liquid, adding sodium bromide of which the mass is one third of that of the wood pulp dispersion liquid, continuously stirring the mixture for 1 to 2 hours, adding sodium hydroxide in the stirring process, adjusting the pH value to be 8 to 9, and after the stirring is successfully completed, performing suction filtration, washing, drying and grinding the mixture into powder to obtain cellulose;
s2 preparation method of zinc oxide is as follows:
taking zinc oxide powder, roasting the zinc oxide powder in a muffle furnace at 400 ℃ for 4 hours, and cooling the zinc oxide powder to room temperature to obtain the zinc oxide required by the experiment;
s3 preparation method of the nano-cellulose/zinc oxide composite material is as follows:
putting 15 parts of nano cellulose into a 250ml beaker, adding a certain amount of deionized water, stirring at normal temperature for 0.5-1 h, adding 65 parts of zinc oxide by 3 times, slowly dropwise adding 7 parts of template agent triethylamine by using a dropper, gradually enabling the solution to become more viscous, increasing the rotating speed of a stirring paddle, fixing the beaker by using iron, and stopping stirring after stirring for 1-2 h;
and (2) pouring the stirred solution into a 250ml reaction kettle, adding 4 parts of dodecyl trimethyl ammonium bromide serving as a surfactant into the reaction kettle, sealing the reaction kettle, putting the reaction kettle into a 200 ℃ oven for crystallization for 48 hours, wearing high-temperature-resistant gloves, taking out the reaction kettle, cooling the reaction kettle to room temperature, opening the reaction kettle, filtering the reaction kettle, putting a filter cake into a 100 ℃ oven for drying, taking out the filter cake, grinding the filter cake into powder, putting the powder into a tubular furnace, roasting the powder at 350 ℃ for 6 hours in a nitrogen atmosphere, and cooling the powder to room temperature to obtain the nano cellulose/zinc oxide composite material.
Example 4
The specific surface area and pore size distribution of the nanocellulose/zinc oxide composite materials prepared in examples 1 to 3 are shown in table 1.
TABLE 1 specific surface area and pore size distribution of the materials of examples 1-3
From the results of table 1, we can derive: the prepared nano-cellulose/zinc oxide composite material has a large specific surface area, and the average pore diameter of the nano-cellulose/zinc oxide composite material is within a mesoporous range, and through comparison between examples 1-3, it can be seen that different raw material composition ratios have some influence on the specific surface area and the average pore diameter of the nano-cellulose/zinc oxide composite material.
Example 5
The composite materials prepared in examples 1 to 3 were subjected to a test of electrochemical energy storage performance under a condition of a current density of 5A/g, and subjected to 100-cycle comparison, and the life effect of the composite materials in the aspect of electrochemical energy storage was tested, with test data of 30, 60, and 100 times, respectively, and the test results are shown in tables 2 and 3.
Table 2 electrochemical energy storage Performance test results for the materials of examples 1-3
TABLE 3 electrochemical energy storage Life Effect test results for the materials of examples 1-3
As can be seen from tables 2 and 3, the prepared nanocellulose/zinc oxide composite material has excellent performance when applied to the field of electrochemical energy storage, because in the preparation process of the material, cellulose is alkaline, when zinc oxide has a small amount of zinc ions and oxygen ions to dissociate under an alkaline condition, the dissociated hetero ions enter the framework of the material to form a framework structure containing hetero ions, and the stability of the hetero atom framework is better, and through the hydrothermal synthesis method, the internal pore diameter of the material reaches a mesoporous state, and the internal microstructure of the material in the mesoporous state is better linked and has better stability.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. A nano-cellulose/zinc oxide composite material for electrochemical energy storage comprises the following raw materials in parts by weight: 10-20 parts of nano cellulose, 60-70 parts of zinc oxide, 5-10 parts of a template agent and 3-5 parts of a surfactant;
the preparation method of the nano-cellulose/zinc oxide composite material comprises the following steps:
s1: the preparation method of the cellulose comprises the following steps:
taking wood pulp and deionized water according to a mass ratio of 1: 5, adding the mixture into a beaker, stirring the mixture until the mixture is uniformly dispersed to obtain a wood pulp dispersion liquid, adding sodium bromide of which the mass is one third of that of the wood pulp dispersion liquid, continuously stirring the mixture for 1 to 2 hours, adding sodium hydroxide in the stirring process, adjusting the pH value to be 8 to 9, and after the stirring is successfully completed, performing suction filtration, washing, drying and grinding the mixture into powder to obtain cellulose;
s2: the preparation method of the zinc oxide comprises the following steps:
taking zinc oxide powder, roasting the zinc oxide powder in a muffle furnace at 400 ℃ for 4 hours, and cooling the zinc oxide powder to room temperature to obtain the zinc oxide required by the experiment;
s3: the preparation method of the nano-cellulose/zinc oxide composite material comprises the following steps:
putting nano-cellulose into a 250ml beaker, adding a certain amount of deionized water, stirring at normal temperature for 0.5-1 h, adding zinc oxide for 3 times, slowly dropwise adding a template agent by using a dropper, gradually enabling the solution to become more viscous, increasing the rotating speed of a stirring paddle, fixing the beaker by using iron, and stopping stirring after stirring for 1-2 h;
and (2) taking a 250ml reaction kettle, pouring the stirred solution into the reaction kettle, adding a surfactant into the reaction kettle, sealing the reaction kettle, putting the reaction kettle into a 200 ℃ oven for crystallization for 48 hours, wearing a high-temperature-resistant glove, taking out, cooling to room temperature, opening, filtering, washing, putting a filter cake into a 100 ℃ oven for drying, taking out, grinding into powder, putting into a tubular furnace, roasting at 350 ℃ for 6 hours under the nitrogen atmosphere, and cooling to room temperature to obtain the nano-cellulose/zinc oxide composite material.
2. The nano-cellulose/zinc oxide composite material for electrochemical energy storage as claimed in claim 1, wherein the stirring speed in step S3 is 200-250 r/min, and the stirring paddle speed in step S3 is increased to 250-300 r/min.
3. The nanocellulose/zinc oxide composite material for electrochemical energy storage according to claim 1, wherein the heating rate of the muffle furnace and the tube furnace is 10 ℃/min.
4. The nano-cellulose/zinc oxide composite material for electrochemical energy storage as claimed in claim 1, wherein the interval between 3 times of adding zinc oxide in step S3 is 10min, and stirring is performed immediately after adding zinc oxide.
5. The nanocellulose/zinc oxide composite material for electrochemical energy storage as claimed in claim 1, wherein in step S3, the lining of the 250ml reaction kettle is made of polytetrafluoroethylene material.
6. The nanocellulose/zinc oxide composite material for electrochemical energy storage as claimed in claim 1, wherein the preparation process of the nanocellulose/zinc oxide composite material is completed in a fume hood, and the drying time of the 100 ℃ oven in step S3 is 3-5 h.
7. The nanocellulose/zinc oxide composite material for electrochemical energy storage as claimed in claim 1, wherein said template agent is triethylamine and surfactant is dodecyl trimethyl ammonium bromide in step S3.
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