CN110746938A - Cellulose/polypyrrole supported composite phase change heat storage material and preparation method thereof - Google Patents
Cellulose/polypyrrole supported composite phase change heat storage material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a cellulose/polypyrrole-supported composite phase change heat storage material and a preparation method thereof. The invention can quickly convert electric energy into heat energy by utilizing the high conductivity of the polypyrrole, can raise the temperature to a higher temperature in a short time, has high heat storage efficiency, improves the thermal comfort and the energy utilization rate of heating, reduces the energy consumption loss, and has good market application prospect.
Description
Technical Field
The invention belongs to the field of phase-change materials, and particularly relates to a cellulose/polypyrrole supported composite phase-change heat storage material and a preparation method thereof.
Background
With the increase of a series of heat consumption projects such as heating area, the corresponding problems of environmental pollution and energy waste become more and more serious, for example, the energy conversion efficiency of a thermal power plant, and excessive heat energy is wasted due to the inconsistency of heating and power generation loads. Therefore, phase change heat storage materials like storage batteries that store heat and release energy when needed for maximum use of energy will be widely used. The electric-heat conversion phase-change heat storage material has good heating comfort, and can effectively reduce energy loss and shorten the time interval between energy demand and energy use due to the action of 'peak shifting and valley filling'. However, since the phase change material is easy to flow in a liquid state, leakage is easy to occur, and application is limited.
Disclosure of Invention
The invention aims to solve the technical problems of instability and poor heat storage efficiency of the phase-change material in the prior art by providing a cellulose/polypyrrole supported composite phase-change heat storage material and a preparation method thereof.
The invention provides a cellulose/polypyrrole-supported composite phase change heat storage material, which is obtained by growing polypyrrole on a cellulose porous material in situ and fixing the phase change heat storage material on the polypyrrole-modified cellulose porous material through capillary adsorption.
The phase-change heat storage material is one or more of tetradecanol, hexadecanol, stearic acid, palmitic acid, octadecane, eicosane, polyethylene glycol 2000, polyethylene glycol 4000 and polyethylene glycol 6000.
The invention provides a preparation method of a cellulose/polypyrrole supported composite phase change heat storage material, which comprises the following steps:
(1) adding a silane coupling agent into the cellulose nanowire suspension, and stirring and mixing uniformly; adding a branched polyethyleneimine aqueous solution into the suspension, stirring, freeze-drying, and baking to obtain a cellulose porous material;
(2) sequentially putting the cellulose porous material into ferric trichloride hexahydrate/5-sodium sulfosalicylate aqueous solution and pyrrole cyclohexane solution to be soaked in a refrigerator, wherein the complex formed by the ferric trichloride hexahydrate and the 5-sodium sulfosalicylate can slowly release Fe3+The pyrrole monomer is slowly subjected to oxidative polymerization to generate polypyrrole, so that the cellulose/polypyrrole porous material is obtained;
(3) and washing and drying the obtained cellulose/polypyrrole porous material, and then soaking the material in the phase-change heat storage material to obtain the cellulose/polypyrrole supported composite phase-change heat storage material.
The mass concentration of the cellulose nanowire suspension in the step (1) is 0.8-2.0 wt%; the mass ratio of the cellulose nanowires to the silane coupling agent is 1:0.5-1: 2; the mass ratio of the cellulose nanowires to the branched polyethyleneimine is 1:0.5-1: 2.
The silane coupling agent in the step (1) is KH 560.
The mass concentration of the branched polyethyleneimine aqueous solution in the step (1) is 10-60 wt%.
The stirring time after adding the silane coupling agent in the step (1) is 1-3h, and the stirring time after adding the branched polyethyleneimine water solution is 30-60 min.
The freeze drying time in the step (1) is 24-48 h; the baking temperature is 110-130 ℃, and the baking time is 10-30 min.
The concentrations of ferric trichloride hexahydrate and sodium 5-sulfosalicylate in the step (2) are both 0.18-0.72M; the concentration of pyrrole is 0.18-0.72M.
The temperature of the refrigerator in the step (2) is 0-5 ℃.
The dipping time in the step (2) is 6-24 h.
The temperature for dipping the phase-change heat storage material in the step (3) is above the melting point of the corresponding phase-change material, and the dipping time is 10min-3 h.
Advantageous effects
The high-conductivity polypyrrole/phase-change material can quickly convert electric energy into heat energy, the heat energy is heated to a higher temperature in a short time, the heat storage efficiency is high, part of heat energy can be converted into phase-change energy by the phase-change material contained in the system for storage, the temperature of the material cannot be immediately reduced after power failure or when the power load is insufficient, the thermal comfort and the energy utilization rate of heating are improved, and the energy consumption loss is reduced; the whole preparation process is simple and economic, and the used raw materials and finished products have good biocompatibility and degradability, are green and environment-friendly, and have good market application prospect.
Drawings
FIG. 1 is a pictorial view of a cellulose porous material (a) and a cellulose/polypyrrole porous material (b) prepared in example 1;
FIG. 2 is a pictorial view of a cellulose/polypyrrole supported composite phase change heat storage material prepared in example 1;
FIG. 3 is a surface scanning electron microscope photograph of the cellulose/polypyrrole porous material prepared in example 2;
FIG. 4 is an electrical heating curve of the cellulose/polypyrrole porous material of example 2 at different voltages;
fig. 5 is an electrical heating curve of the cellulose/polypyrrole supported composite phase-change heat storage material of example 2 under different voltages.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
(1) Weighing 20g of cellulose nanowire suspension with the solid content of 1.2%, dropwise adding KH560 into the cellulose nanowire suspension, and magnetically stirring for 3 hours at room temperature to obtain uniform mixed suspension, wherein the mass ratio of the cellulose nanowires to the KH560 is 1: 1; preparing a branched polyethyleneimine water solution with the mass concentration of 25% by using deionized water, dropwise adding the branched polyethyleneimine water solution into the suspension, magnetically stirring for 40min at room temperature to obtain a uniform mixed suspension, wherein the mass ratio of the cellulose nanowires to the branched polyethyleneimine is 1:0.8, finally putting the mixed suspension into a freeze dryer for freeze drying, taking out the mixed suspension, putting the mixed suspension into an oven, and baking for 30min at the temperature of 110 ℃ to obtain the cellulose porous material.
(2) Preparation 1#Solution: 0.36M ferric chloride hexahydrate and 0.36M sodium 5-sulfosalicylate were weighed into 100mL deionized water, and magnetic stirring was carried out at normal temperature for 45min to obtain a uniform solution. Soaking the cellulose porous material in the step (1) in the prepared 1#In the solution, the cellulose porous material is completely soaked in the liquid, and is placed in a refrigerator (0-5 ℃) for standing for 12 hours.
(3) Preparation 2#Solution: 0.36M pyrrole solution is weighed and added into 100mL cyclohexane solution, and the solution is magnetically stirred for 20min under the condition of normal temperature, so that pyrrole liquid drops are uniformly dispersed in the cyclohexane solution. Taking out the cellulose porous material in the step (2) and putting the cellulose porous material into the prepared step 2#And (3) in the solution, ensuring that the cellulose porous material is completely soaked in the liquid, and placing the solution into a refrigerator for standing reaction for 24 hours. During the reaction, attention is paid to sealing work to prevent the volatilization of cyclohexane.
(4) And (3) after the reaction is finished, taking out the cellulose porous material, and soaking and cleaning the cellulose porous material by using water and ethanol in sequence until the washing liquor in the water and the ethanol is colorless. And then putting the porous material into a vacuum oven, and drying the porous material for 12 hours at the temperature of 60 ℃ to obtain the cellulose/polypyrrole porous material. Then, the phase-change material polyethylene glycol (PEG4000) is soaked for 3 hours at 70 ℃, and finally the cellulose/polypyrrole supported composite phase-change heat storage material is obtained. In the embodiment, the impregnation rate of the phase change material octadecane is 96 wt%, and the enthalpy value of the final composite heat storage material is 229.3J/g.
Example 2
(1) Weighing 20g of cellulose nanowire suspension with the solid content of 1.0%, dropwise adding KH560 into the cellulose nanowire suspension, and magnetically stirring for 2 hours at room temperature to obtain uniform mixed suspension, wherein the mass ratio of the cellulose nanowires to the KH560 is 1: 1.2; preparing a branched polyethyleneimine aqueous solution with the mass concentration of 50% by using deionized water, dropwise adding the branched polyethyleneimine aqueous solution into the suspension, magnetically stirring for 50min at room temperature to obtain a uniform mixed suspension, wherein the mass ratio of the cellulose nanowires to the branched polyethyleneimine is 1:0.8, finally putting the mixed suspension into a freeze dryer for freeze drying, taking out the mixed suspension, putting the mixed suspension into an oven, and baking the mixed suspension for 20min at 120 ℃ to obtain the cellulose porous material.
(2) Preparing a No. 1 solution: 0.48M ferric chloride hexahydrate and 0.48M sodium 5-sulfosalicylate were weighed into 100mL deionized water, and magnetic stirring was carried out at normal temperature for 50min to obtain a uniform solution. Soaking the cellulose porous material in the step (1) in the prepared 1#And (3) in the solution, ensuring that the cellulose porous material is completely soaked in the liquid, and placing the solution into a refrigerator for standing for 10 hours.
(3) Preparing a No. 2 solution: 0.48M pyrrole solution is weighed and added into 100mL cyclohexane solution, and the solution is magnetically stirred for 30min under the condition of normal temperature, so that pyrrole liquid drops are uniformly dispersed in the cyclohexane solution. Taking out the cellulose porous material in the step (2) and putting the cellulose porous material into the prepared step 2#And in the solution, ensuring that the cellulose porous material is completely soaked in the liquid, and placing the solution into a refrigerator for standing reaction for 36 hours. During the reaction, attention is paid to sealing work to prevent the volatilization of cyclohexane.
(4) And (3) after the reaction is finished, taking out the cellulose porous material, and soaking and cleaning the cellulose porous material by using water and ethanol in sequence until the washing liquor in the water and the ethanol is colorless. And then putting the porous material into a vacuum oven, and drying the porous material for 10 hours at the temperature of 70 ℃ to obtain the cellulose/polypyrrole porous material. And then, soaking the phase-change material octadecane for 3 hours at the temperature of 50 ℃ to finally obtain the cellulose/polypyrrole supported composite phase-change heat storage material. In the embodiment, the impregnation rate of the phase change material polyethylene glycol is 94.60 wt%, and the enthalpy value of the final composite heat storage material is 169.7J/g.
The microstructure of the surface of the cellulose/polypyrrole porous material prepared in the above example is shown in fig. 3, and the surface of the fiber becomes rough and is covered with uniform polypyrrole particles. Because polypyrrole forms a good conductive pathway in the cellulose porous material, the cellulose/polypyrrole porous material can quickly convert electrical energy into thermal energy during power-on (fig. 4), and the higher the driving voltage, the higher the equilibrium temperature to which the porous material is raised.
Fig. 5 is an electrical heating curve of the cellulose/polypyrrole supported composite phase-change heat storage material under different voltages, the conductive porous material can rapidly convert electrical energy into heat energy during the power-on process, and unlike fig. 4, due to the existence of the phase-change material, when the temperature rises to the vicinity of the phase-change point of the phase-change material, the phase-change material can absorb the heat energy converted from the electrical energy; the stored heat energy can be slowly released under the condition of power failure, so that the heat can be maintained for a longer time, and a good heat preservation effect is achieved.
Example 3
(1) Weighing 20g of cellulose nanowire suspension with the solid content of 1.6%, dropwise adding KH560 into the cellulose nanowire suspension, and magnetically stirring for 2h at room temperature to obtain uniform mixed suspension, wherein the mass ratio of the cellulose nanowires to the KH560 is 1: 0.8; preparing a branched polyethyleneimine water solution with the mass concentration of 50% by using deionized water, dropwise adding the branched polyethyleneimine water solution into the mixed suspension, and magnetically stirring for 50min at room temperature to obtain a uniform mixed suspension, wherein the mass ratio of the cellulose nanowires to the branched polyethyleneimine is 1:1. And finally, putting the mixed suspension into a freeze dryer for freeze drying, taking out and putting into a drying oven, and baking for 10min at the temperature of 130 ℃ to obtain the cellulose porous material.
(2) Preparing a No. 1 solution: 0.60M ferric chloride hexahydrate and 0.60M sodium 5-sulfosalicylate are weighed and added into 100mL deionized water, and the mixture is magnetically stirred for 45min under the condition of normal temperature to obtain a uniform solution. Soaking the cellulose porous material in the step (1) in the prepared 1#And (3) in the solution, ensuring that the cellulose porous material is completely soaked in the liquid, and placing the solution into a refrigerator for standing for 12 hours.
(3) Preparing a No. 2 solution: 0.60M pyrrole solution is weighed and added into 100mL cyclohexane solution, and the pyrrole liquid drops are uniformly dispersed in the cyclohexane solution by magnetic stirring for 40min under the condition of normal temperature. And (3) taking out the porous cellulose material in the step (2), putting the porous cellulose material into the prepared No. 2 solution to ensure that the porous cellulose material is completely soaked in the liquid, and putting the porous cellulose material into a refrigerator for standing reaction for 48 hours. During the reaction, attention is paid to sealing work to prevent the volatilization of cyclohexane.
(4) And (3) after the reaction is finished, taking out the cellulose porous material, and soaking and cleaning the cellulose porous material by using water and ethanol in sequence until the washing liquor in the water and the ethanol is colorless. And then putting the porous material into a vacuum oven, and drying the porous material for 8 hours at the temperature of 80 ℃ to obtain the cellulose/polypyrrole porous material. And then, the phase-change material cetyl alcohol is soaked for 1h at the temperature of 60 ℃, and finally the cellulose/polypyrrole supported composite phase-change heat storage material is obtained. In the embodiment, the impregnation rate of the phase change material hexadecanol is 92.10 wt%, and the enthalpy value of the final composite heat storage material is 152.1J/g.
Example 4
(1) Weighing 20g of cellulose nanowire suspension with the solid content of 2.0 wt%, dropwise adding KH560 into the cellulose nanowire suspension, and magnetically stirring for 3 hours at room temperature to obtain uniform mixed suspension, wherein the mass ratio of the cellulose nanowires to the KH560 is 1: 1; preparing a branched polyethyleneimine water solution with the mass concentration of 60 wt% by using deionized water, dropwise adding the branched polyethyleneimine water solution into the mixed suspension, and magnetically stirring for 60min at room temperature to obtain a uniform mixed suspension, wherein the mass ratio of the cellulose nanowires to the branched polyethyleneimine is 1: 1.2. And finally, putting the mixed suspension into a freeze dryer for freeze drying, taking out and putting into a drying oven, and baking for 30min at the temperature of 110 ℃ to obtain the cellulose porous material.
(2) Preparing a No. 1 solution: 0.36M ferric chloride hexahydrate and 0.36M sodium 5-sulfosalicylate were weighed into 100mL deionized water, and magnetic stirring was carried out at normal temperature for 45min to obtain a uniform solution. Soaking the cellulose porous material in the step (1) in the prepared 1#And (3) in the solution, ensuring that the cellulose porous material is completely soaked in the liquid, and placing the solution into a refrigerator for standing for 16 hours.
(3) Preparing a No. 2 solution: 0.36M pyrrole solution is weighed and added into 100mL cyclohexane solution, and the solution is magnetically stirred for 20min under the condition of normal temperature, so that pyrrole liquid drops are uniformly dispersed in the cyclohexane solution. Taking out the cellulose porous material in the step (2) and putting the cellulose porous material into the prepared step 2#In the solution, ensuring the porous cellulose material to be completely soaked in the liquid, and placing the porous cellulose material into a refrigerator for standingThe reaction is carried out for 48 hours. During the reaction, attention is paid to sealing work to prevent the volatilization of cyclohexane.
(4) And (3) after the reaction is finished, taking out the cellulose porous material, and soaking and cleaning the cellulose porous material by using water and ethanol in sequence until the washing liquor in the water and the ethanol is colorless. And then putting the porous material into a vacuum oven, and drying the porous material for 12 hours at the temperature of 60 ℃ to obtain the cellulose/polypyrrole porous material. And then, soaking the phase-change material stearic acid for 1h at the temperature of 85 ℃ to finally obtain the cellulose/polypyrrole supported composite phase-change heat storage material. In the embodiment, the impregnation rate of the phase change material stearic acid is 92.40 wt%, and the enthalpy value of the final composite heat storage material is 210J/g.
Claims (10)
1. The composite phase change heat storage material supported by cellulose/polypyrrole is characterized in that: the phase change heat storage material is obtained by growing polypyrrole on a cellulose porous material in situ and fixing the phase change heat storage material on the cellulose porous material modified by the polypyrrole through capillary adsorption.
2. The composite phase change heat storage material of claim 1, wherein: the phase-change heat storage material is one or more of tetradecanol, hexadecanol, stearic acid, palmitic acid, octadecane, eicosane, polyethylene glycol 2000, polyethylene glycol 4000 and polyethylene glycol 6000.
3. A preparation method of a cellulose/polypyrrole supported composite phase change heat storage material comprises the following steps:
(1) adding a silane coupling agent into the cellulose nanowire suspension, and stirring and mixing uniformly; adding a branched polyethyleneimine aqueous solution into the suspension, stirring, freeze-drying, and baking to obtain a cellulose porous material;
(2) sequentially putting the cellulose porous material into ferric trichloride hexahydrate/5-sodium sulfosalicylate aqueous solution and pyrrole cyclohexane solution, and dipping in a refrigerator to obtain a cellulose/polypyrrole porous material;
(3) and washing and drying the obtained cellulose/polypyrrole porous material, and then soaking the material in the phase-change heat storage material to obtain the cellulose/polypyrrole supported composite phase-change heat storage material.
4. The production method according to claim 3, characterized in that: the mass concentration of the cellulose nanowire suspension in the step (1) is 0.8-2.0 wt%; the mass ratio of the cellulose nanowires to the silane coupling agent is 1:0.5-1: 2; the mass ratio of the cellulose nanowires to the branched polyethyleneimine is 1:0.5-1: 2.
5. The production method according to claim 3, characterized in that: the mass concentration of the branched polyethyleneimine aqueous solution in the step (1) is 10-60 wt%.
6. The production method according to claim 3, characterized in that: the freeze drying time in the step (1) is 24-48 h; the baking temperature is 110-130 ℃, and the baking time is 10-30 min.
7. The production method according to claim 3, characterized in that: the concentrations of ferric trichloride hexahydrate and sodium 5-sulfosalicylate in the step (2) are both 0.18-0.72M; the concentration of pyrrole is 0.18-0.72M.
8. The production method according to claim 3, characterized in that: the temperature of the refrigerator in the step (2) is 0-5 ℃.
9. The production method according to claim 3, characterized in that: the dipping time in the step (2) is 6-24 h.
10. The production method according to claim 3, characterized in that: the temperature for dipping the phase-change heat storage material in the step (3) is above the melting point of the corresponding phase-change material, and the dipping time is 10min-3 h.
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