CN113372612B - Preparation method of cellulose-based radiation temperature-regulating material - Google Patents
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Abstract
The invention belongs to the technical field of energy-saving materials, and particularly relates to a preparation method of a cellulose-based radiation temperature-regulating material, which comprises the following steps: uniformly dispersing a cellulose material in a solvent, and performing functional modification on the cellulose material to obtain a functional modified cellulose material cellulose dispersion liquid; chemically crosslinking the functionalized modified cellulose material dispersion liquid to obtain cellulose-based gel; and encapsulating the phase-change material in cellulose-based gel, and drying to obtain the cellulose-based radiation temperature-regulating material. The radiation temperature-regulating material is prepared on the basis of renewable cellulose, and can realize excellent radiation temperature-regulating effect under the synergistic effect of excellent heat storage and release capacity of the phase-change material and the radiation refrigeration characteristic of a cellulose matrix; the preparation method is simple in preparation process, low in cost, environment-friendly and nontoxic, and has wide application prospects in the fields of building energy conservation and the like.
Description
Technical Field
The invention belongs to the technical field of energy-saving materials, and particularly relates to a preparation method of a cellulose-based radiation temperature-regulating material.
Background
According to statistics, 30% of energy consumption worldwide comes from building energy consumption, wherein the energy consumption of indoor temperature adjusting means such as air conditioning and refrigeration accounts for the largest proportion, and accounts for about 2/3 of total building energy consumption. However, with the development of society, the rapid consumption of traditional energy and the environmental pollution problem caused by the traditional energy become huge challenges all over the world. Meanwhile, along with the aggravation of global warming and the higher and higher requirements of people on living quality, the development of a passive intelligent temperature regulating material with low energy consumption and environmental friendliness has great practical significance.
When the external environment temperature changes, the phase change material can realize reversible heat storage and release through the phase change of the phase change material, so that the aim of temperature regulation and control is fulfilled, and the phase change material has a great application prospect in the fields of intelligent buildings, intelligent temperature regulation textiles, solar heat utilization, biological medicines, military affairs, electronic device heat management and the like. Commonly used organic phase change materials include higher aliphatic hydrocarbons, alcohols, fatty acids or esters thereof, and the like. The materials have the advantages of high energy density, low price, easy obtainment, environmental friendliness, long cycle service life, adjustable phase-change temperature and the like, but the materials are usually solid-liquid phase-change materials, liquid is generated in the phase-change process, the shape of the materials is difficult to control, and the problems of leakage and the like are easy to occur; on the other hand, in the daytime, especially in hot summer, the phase change materials have limited energy storage capacity, and it is difficult to regulate the ambient temperature under the conditions of strong solar radiation and long duration, and these limitations limit their practical application.
Cellulose is one of natural polymer materials with the largest content and the widest distribution on the earth, is cheap and easily available, is green and renewable, has good biodegradability and compatibility, has a large number of reactive groups, and is beneficial to chemical modification. The method has wide application in the traditional fields of textile, building engineering, paper making, food and the like, and shows great research and application values in the field of advanced functional materials. Cellulose-based phase change materials (CN 102504186B and CN 110257010B) are prepared by adopting a method of grafting the cellulose to the phase change materials, but the method is usually low in grafting rate of the phase change materials and poor in phase change temperature regulation effect of the materials; cellulose-based phase change materials (CN 106675527B) are prepared by a method of constructing hydrogel, however, common organic phase change materials are difficult to dissolve in a water system, which limits the application of the materials; in addition, the cellulose and other high-thermal-conductivity materials are compounded to form the aerogel (CN 109517221B), such as graphene, on one hand, the cost is greatly increased, and on the other hand, the cellulose aerogel matrix loses the heat insulation effect, so that the application of the cellulose aerogel in the field of building heat insulation and temperature adjustment is not facilitated.
In recent years, the radiation refrigeration technology as a green and environment-friendly passive refrigeration mode has great application potential in the field of energy conservation, and the principle is that the radiation refrigeration technology can reflect a great deal of sunlight by regulating and controlling the radiation characteristic of materials, namely, the radiation refrigeration technology has high reflectivity in a sunlight wave band (0.3-2.5 mu m) and reduces the absorption of heat; meanwhile, the heat is spontaneously radiated to the outer space through the atmospheric window by self radiation, namely, the high-emissivity infrared radiation window has high emissivity in the waveband of the atmospheric infrared transmission window (8-13 mu m), so that the heat is exchanged with the outer space, and the purpose of reducing the temperature of the material is achieved. However, the manufacturing cost of radiation refrigeration materials such as much research meta-materials or photonic crystals is high, complex and expensive processing equipment is often required in the production process, and the radiation refrigeration materials are not beneficial to industrial application.
Recently, researchers have found that cellulosic materials possess excellent ability to reflect solar radiation and strong mid-infrared wavelength emission properties, exhibiting excellent radiation refrigeration characteristics. Therefore, use the cellulose material to construct the aerogel that has three-dimensional porous structure as the base member, network structure through the aerogel can show the load that promotes phase change material, on the other hand, three-dimensional confinement structure can effectively solve the easy defect of revealing of phase change material, in addition, the cellulose aerogel has lower heat conductivity, can play good thermal-insulated effect, more importantly, the inherent optical property of cellulose material can realize all-weather radiation refrigeration, through the complex with phase change material, can develop and have the novel high performance radiation temperature regulating material of phase change energy storage and radiation refrigeration difunctional characteristic concurrently, it has important meaning to energy saving and consumption reduction and renewable resources's development and utilization.
Disclosure of Invention
The invention aims to provide a preparation method of a cellulose-based radiation temperature-regulating material, which synthesizes a novel radiation temperature-regulating material with the characteristics of phase change energy storage and radiation refrigeration by a simple and low-cost method.
According to the technical scheme of the invention, the preparation method of the cellulose-based radiation temperature-regulating material comprises the following steps,
s1: uniformly dispersing a cellulose material in a solvent and performing functional modification on the cellulose material to obtain a functional modified cellulose material dispersion liquid; the method for functional modification is one or more of hydroformylation, carboxylation and amination.
S2: chemically crosslinking the functionalized modified cellulose material dispersion liquid to obtain cellulose-based gel;
s3: and encapsulating the phase-change material in cellulose-based gel, and drying to obtain the cellulose-based radiation temperature-regulating material.
According to the invention, a cheap cellulose material is used as a raw material, the aerogel packaging organic phase change energy storage material with a three-dimensional porous structure is constructed, the excellent solar radiation reflecting capacity and strong mid-infrared wavelength emission performance of the cellulose material are utilized to endow the material with good radiation refrigeration characteristics, and meanwhile, the porous gel confinement structure can effectively solve the problem of phase change material leakage, so that the novel high-performance radiation temperature regulating material integrating two temperature regulating means is obtained.
Further, the cellulose material is at least one of paper, filter paper, straw, cotton pulp, hemp, commercial microcrystalline cellulose, bacterial cellulose, cellulose nano-fiber and cellulose nano-crystal. The solvent may be water.
Further, the method for dispersing the cellulose material is one or more of an ultrasonic mechanical stirring method, a high-pressure homogenization method, an acid treatment method, a cellulase hydrolysis method, a mechanical ball milling method and the like.
Further, the concentration of the functionalized modified cellulose material dispersion is 0.5-30 wt.%.
Further, in step S1, the solvent is water or an organic solvent. Specifically, the organic solvent may be nitrogen-nitrogen dimethylformamide, acetone, or the like.
Further, in step S2, the chemical crosslinking is performed by a direct crosslinking reaction between the modified functional groups or a crosslinking reaction after adding a crosslinking agent.
Further, the cross-linking agent is one or more of an amino-terminated compound, an aldehyde-terminated compound, isocyanate and a silane coupling agent. Specifically, the amino-terminated compound can be melamine, the aldehyde-terminated compound can be glutaraldehyde, the isocyanate can be diphenylmethane diisocyanate, and the silane coupling agent can be N- (2-aminoethyl) -3-aminopropylmethyldimethoxysilane.
Further, in step S2, the cellulose-based gel is hydrogel or aerogel.
Further, the phase change material is an organic phase change material, such as polyethylene glycol, stearic acid, paraffin, octadecane, and the like.
Further, in step S3, the phase change material is encapsulated by pre-mixing, impregnation and solvent replacement.
Further, in step S3, the drying method is heating drying, freeze drying or supercritical carbon dioxide drying.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) the invention takes the natural high molecular material cellulose which has the most abundant reserves and the most extensive sources in the nature as the raw material, the raw material is cheap and easy to obtain, renewable, nontoxic, green and environment-friendly, and has good biodegradability and biocompatibility, thereby having important significance for the efficient utilization of biomass resources and the elimination of the dependence on petroleum-based products in human society;
(2) the cellulose-based aerogel material with the three-dimensional porous structure can effectively package the organic phase-change material, solves the defect that the organic phase-change material is easy to leak in the using process, is nontoxic and cheap, effectively reduces the construction cost of the temperature-regulating material, and can realize dynamic regulation and control of the temperature regulation temperature by changing the type of the phase-change material and the microstructure of aerogel;
(3) compared with the conventional phase-change temperature regulating material, the cellulose aerogel matrix constructed by the invention has good heat insulation performance, and the radiation refrigeration performance can be enhanced by regulating and controlling the structure of the aerogel, so that a more excellent all-weather temperature regulating effect is realized;
(4) the radiation temperature adjusting performance of the prepared material is greatly enhanced and the excellent temperature adjusting effect is realized by organically combining two means of radiation refrigeration and phase change temperature adjustment, and the novel zero-energy-consumption passive radiation temperature adjusting material can effectively reduce the temperature adjusting energy consumption and has important application value in the fields of building energy conservation and the like;
(5) the preparation process provided by the invention is simple, the prepared gel directly loads the phase-change material, complex post-treatment processes such as impurity removal and the like are not needed, the raw materials and the production cost are low, and the gel is safe and nontoxic and is suitable for large-scale production.
Drawings
FIG. 1 is a schematic representation of a cellulose-based radiant temperature regulating material of example 1 of the present invention;
FIG. 2 is a graph of the phase change energy storage performance of a cellulose-based radiant temperature regulating material of example 1 of the present invention;
FIG. 3 is a graph of the solar radiation reflecting performance of a cellulose-based radiation temperature regulating material of example 1 of the present invention;
FIG. 4 is a graph of the mid-infrared emission performance of the cellulose-based radiant temperature regulating material of example 1 of the present invention.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Example 1
Adding 1g of commercialized microcrystalline cellulose into 100mL of 64% sulfuric acid solution, reacting for 45 minutes at 45 ℃, washing the solution to be nearly neutral by suction filtration and centrifugation, preparing into cellulose nanocrystal dispersion liquid with the concentration of 1 wt.%, adding 1g of sodium periodate, reacting for 2 hours at normal temperature, removing impurities in the solution by suction filtration and centrifugation, preparing into aldehyde modified cellulose nanocrystal dispersion liquid with the concentration of 0.5 wt.%, adding organic phase change material polyethylene glycol, adding 0.1g of melamine and 0.1g of triaminobenzene as cross-linking agents, fully stirring and dissolving, adjusting the pH of the solution to be 2, obtaining cellulose nanocrystal/polyethylene glycol composite hydrogel, and freeze-drying to obtain the cellulose nanocrystal/polyethylene glycol composite material with the radiation temperature regulation function.
The physical diagram of the obtained cellulose nanocrystal/polyethylene glycol composite material is shown in figure 1; the phase change energy storage performance curve is shown in FIG. 2, and it can be seen that the phase change of the cellulose-based radiant temperature regulating material is about 30 ℃ and 50 ℃, and the enthalpy of phase change is about 140J/g and 146J/g; the curve of the performance of reflecting solar radiation is shown in fig. 3, and it can be seen that the solar radiation has a good reflection effect in the solar radiation band, the reflectivity of the visible light band can reach more than 90%, and the energy from the solar radiation is effectively reduced; the middle infrared emission performance curve is shown in fig. 4, and it can be seen that the cellulose-based radiation temperature-adjusting material has a high emissivity at an atmospheric infrared window band, which can reach more than 90%.
Example 2
1g of paper is dispersed into 20ml of aqueous solution by a high-pressure homogenization method, impurities in the solution are removed by suction filtration and centrifugation to prepare cellulose dispersion liquid with the concentration of 1 wt.%, 5g of ammonium persulfate is added, the mixture is reacted at 70 ℃ for 10 hours, and then the impurities in the solution are removed by suction filtration and centrifugation to prepare carboxylated cellulose dispersion liquid with the concentration of 1 wt.%. 1g of adipic acid dihydrazide was added to prepare an aminated modified cellulose, and impurities in the solution were removed by suction filtration centrifugation to prepare an aminated modified cellulose dispersion having a concentration of 10 wt.%. Dispersing 1g of filter paper into 20ml of aqueous solution by a high-pressure homogenization method, removing impurities in the solution by suction filtration and centrifugation to prepare cellulose dispersion liquid with the concentration of 1 wt.%, adding 1g of sodium periodate, reacting for 2 hours at normal temperature, removing impurities in the solution by suction filtration and centrifugation to prepare aldehyde modified cellulose dispersion liquid with the concentration of 10 wt.%. Performing mixing on an amination modified cellulose dispersion liquid and an aldehyde modified cellulose dispersion liquid according to the weight ratio of 1: 1, fully stirring, adjusting the pH value of the solution to 6 to obtain cellulose hydrogel, and performing supercritical drying to obtain the cellulose aerogel. And soaking the cellulose aerogel into the molten phase-change material stearic acid to obtain the cellulose/stearic acid composite material with the radiation temperature-regulating function.
Example 3
2g of straws and 20g of deionized water are added into a ball mill to be ball-milled for 10 hours at 300 revolutions per minute, and then the solution is washed to remove impurities by suction filtration and centrifugation and is prepared into cellulose dispersion liquid with the concentration of 1 wt.%. Preparing a carboxylated modified cellulose dispersion liquid by using a TEMPO oxidation system, adding 1g of adipic acid dihydrazide to synthesize aminated modified cellulose, removing impurities in the solution through suction filtration and centrifugation, and preparing the aminated modified cellulose dispersion liquid with the concentration of 5 wt.%. Adding 1mL of 50% glutaraldehyde solution, fully stirring and dissolving, adjusting the pH value of the solution to 5 to obtain cellulose hydrogel, and freeze-drying to obtain the cellulose aerogel. And soaking the cellulose aerogel into the molten phase-change material paraffin to obtain the cellulose/paraffin composite material with the radiation temperature-regulating function.
Example 4
Adding 2mL of endoglucanase into 100mL of 1 wt.% cotton pulp dispersion, reacting at 50 ℃ for 120 minutes, washing the solution by suction filtration and centrifugation to remove impurities, preparing cellulose dispersion with the concentration of 1 wt.%, adding 1g of sodium periodate, reacting at normal temperature for 2 hours, and removing the impurities in the solution by suction filtration and centrifugation to prepare aldehyde modified cellulose dispersion with the concentration of 10 wt.%. Adding organic phase change material polyethylene glycol, adding 0.2g of melamine, fully stirring and dissolving, then adjusting the pH value of the solution to 3 to obtain cellulose hydrogel, and freeze-drying to obtain the cellulose/polyethylene glycol composite material with the radiation temperature-adjusting function.
Example 5
Uniformly dispersing 1g of cellulose nanofibers into an aqueous solution by an ultrasonic mechanical stirring method, and preparing a cellulose nanofiber dispersion solution with a concentration of 30 wt.% in a ratio of 1: 1, adding sodium periodate, reacting for 2 hours at normal temperature, removing impurities in the solution through suction filtration and centrifugation to prepare an aldehyde modified cellulose dispersion solution with the concentration of 10 wt.%, adding 0.5g of hexamethylenediamine, fully stirring and dissolving, then adjusting the pH of the solution to weak acidity to obtain a cellulose hydrogel, obtaining a cellulose aerogel under the supercritical drying condition, and soaking the cellulose aerogel into a molten phase-change material octadecane to obtain the cellulose/octadecane composite material with the radiation temperature adjusting function.
Example 6
Uniformly dispersing 0.5g of bacterial cellulose into 50mL of aqueous solution, adding 10g of ammonium persulfate, treating at 80 ℃ for 12h to obtain carboxylated modified cellulose, washing, carrying out suction filtration to remove impurities, uniformly dispersing into 20mL of nitrogen-nitrogen dimethyl formamide solution, and mixing the cellulose and isocyanate 1: 1, adding diphenylmethane diisocyanate, fully stirring, adding a small amount of triethylamine serving as a catalyst, continuously stirring for 12 hours at 90 ℃ to form gel, sequentially soaking the gel in acetone and an aqueous solution to obtain cellulose hydrogel, directly soaking the gel in a glass beaker filled with molten polyethylene glycol, obtaining cellulose/polyethylene glycol composite gel through solvent replacement between water and polyethylene glycol melt, and heating and drying to obtain the cellulose/polyethylene glycol composite material with the radiation temperature-regulating function.
Example 7
2g of hemp was added to 100mL of a 64% sulfuric acid solution, reacted at 45 ℃ for 45 minutes, the solution was washed to near neutrality by suction filtration centrifugation and prepared as a cellulose nanocrystal dispersion with a concentration of 5 wt.% according to the following formula for cellulose and sodium periodate 1: 4, adding sodium periodate into the mixture according to the proportion, reacting for 2 hours at room temperature, carrying out suction filtration and centrifugation to remove impurities, preparing into aldehyde with the concentration of 10 wt.% to carry out modification to obtain cellulose dispersion liquid, adjusting the pH of the solution to be subacidity by using acetic acid, slowly adding 5 wt.% of N- (2-aminoethyl) -3-aminopropylmethyldimethoxysilane into the solution, reacting for 1 hour at room temperature to form gel, and carrying out freeze drying to obtain the cellulose aerogel. And soaking the cellulose aerogel into the molten phase-change material polyethylene glycol to obtain the cellulose/polyethylene glycol composite material with the radiation temperature-regulating function.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (10)
1. A preparation method of a cellulose-based radiation temperature-regulating material is characterized by comprising the following steps,
s1: uniformly dispersing a cellulose material in a solvent and carrying out functional modification on the cellulose material to obtain a functional modified cellulose material dispersion liquid; the method for functional modification is one or more of hydroformylation, carboxylation and amination;
s2: chemically crosslinking the cellulose material dispersion to obtain a cellulose-based gel, wherein the cellulose-based gel is in a three-dimensional porous structure;
s3: and encapsulating a phase change material in the cellulose-based gel, and drying to obtain the cellulose-based radiation temperature regulating material, wherein the phase change material is selected from polyethylene glycol, stearic acid, paraffin or octadecane.
2. The method of preparing a cellulose-based radiation temperature regulating material according to claim 1, wherein the cellulose material is one or more of paper, straw, cotton pulp, hemp, commercial microcrystalline cellulose, bacterial cellulose, cellulose nanofibers, and cellulose nanocrystals.
3. The method for preparing a cellulose-based radiant temperature regulating material as claimed in claim 1, wherein the cellulose-based material is dispersed by one or more of ultrasonic mechanical stirring, high pressure homogenization, acid treatment, cellulose hydrolysis, and mechanical ball milling in step S1.
4. The method of preparing a cellulose-based radiation thermoregulating material according to claim 1, wherein the dispersion of the functionalized modified cellulose material has a concentration of 0.5-30wt. -%.
5. The method of preparing a cellulose-based radiation temperature regulating material according to claim 1, wherein the solvent is water or an organic solvent in the step S1.
6. The method for preparing a cellulose-based radiation temperature regulating material according to claim 1, wherein the chemical crosslinking is performed by a direct crosslinking reaction between the modified functional groups or a crosslinking reaction after adding a crosslinking agent in step S2.
7. The method of preparing a cellulose-based radiation temperature regulating material according to claim 6, wherein the cross-linking agent is one or more of an amino-terminated compound, an aldehyde-terminated compound, an isocyanate, and a silane coupling agent.
8. The method for preparing a cellulose-based radiation temperature regulating material according to claim 1, wherein the cellulose-based gel is hydrogel or aerogel in the step S2.
9. The method of preparing a cellulose-based radiant temperature regulating material as claimed in claim 1, wherein the phase change material is encapsulated by pre-mixing, impregnation or solvent replacement in step S3.
10. The method for preparing a cellulose-based radiant temperature regulating material as claimed in claim 1, wherein the drying manner is heat drying, freeze drying or supercritical carbon dioxide drying in the step S3.
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