CN112391149A - Preparation method of carbonized wood-based composite phase change energy storage material - Google Patents
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Abstract
The invention provides a preparation method of a carbonized wood-based composite phase change energy storage material, which takes a balsa wood block with part of lignin removed as a matrix and utilizes SiO2The aerogel is a reinforced phase supporting fiber matrix, and the phase change material is impregnated into the carbonized wood-SiO by a vacuum impregnation method2In an aerogel matrix. The method uses SiO2The aerogel reinforces the pore channel structure of the balsa, reduces the volume shrinkage of the balsa fiber matrix in the carbonization process, and maintains the original multistage pore structure of the wood; SiO 22The aerogel further enhances the specific surface area of the packaging base material and SiO when reinforcing the pore structure of the carbonized wood2The aerogel improves the holding capacity of the whole matrix to the phase-change material by a unique pore diameter and pore structure, and the encapsulation rate exceeds 90 percent. The problem of leakage of the phase change energy storage material in use is solved, the storage and discharge heat efficiency of the packaged phase change energy storage material is improved, and a new direction is developed for the research of a frame matrix of the phase change energy storage material.
Description
Technical Field
The invention relates to a preparation method of a high-carbonization wood-based composite phase-change energy storage material, belonging to the technical field of preparation of composite phase-change heat storage materials.
Background
The carbonized wood-based composite phase-change energy storage material is a novel biomass-based composite phase-change energy storage material formed by taking carbonized wood obtained by carbonizing a macroscopic wood entity as a base material and adsorbing the phase-change energy storage material through physical properties such as capillary tension, van der waals force and the like by utilizing a special three-dimensional network pore structure of the wood.
The carbonized wood-based composite phase change energy storage material has wide application prospect in the field of building energy conservation. At present, the volume of a carbonized wood frame substrate is reduced due to the reasons of large volume shrinkage of wood in the carbonization process, easy cracking and the like, the load capacity of a phase change energy storage material is too low, the application of the phase change energy storage material in production practice is restricted, and the effective accommodating volume of a composite phase change energy storage packaging substrate is strengthened so as to meet the requirements of efficient heat energy storage and utilization in the field of building energy conservation.
The components of wood are mainly cellulose, hemicellulose and lignin. Cellulose serves as a basic skeleton structure of wood, and hemicellulose and lignin serve as matrix substances filled in the cellulose skeleton to bond fibrils consisting of cellulose together. If a part of hemicellulose and lignin in wood is removed, a cellulose matrix having a three-dimensional porous structure can be obtained. The biomass carbon material formed after carbonization can improve the heat conduction performance. But the carbonized fiber skeleton is easy to shrink, and the load capacity of the energy storage material is reduced. The invention uses SiO2The aerogel fills and supports the cellulose matrix, and the large specific surface area of the aerogel is utilized to increase the adsorption of the phase change material. Improves the effective load rate of the carbonized wood-based phase-change heat storage material and solves the problem of using SiO2The problem of poor mechanical property of an aerogel packaging system.
Disclosure of Invention
The invention aims to provide a preparation method of a carbonized wood-based composite phase-change energy storage material, aiming at the defects of poor stability, low thermal conductivity and single function of the existing composite phase-change energy storage material. The preparation method has the advantages of simple and convenient process, easy control and low energy consumption, and improves the application potential of the biomass-based phase-change composite phase-change energy storage material. The technical scheme adopted by the invention is as follows: a preparation method of a carbonized wood-based composite phase change energy storage material comprises the specific steps of
The following were used:
(1) putting barktree fir wood block into deionized water, steaming at certain temperature for 2 hr, and transferring into 10% NaClO2Steaming at 80 deg.C for 2 hr until the wood block turns white. Go toRepeatedly soaking and washing in ionized water, and freeze-drying to obtain delignified balsawood blocks;
(2) adding Tetraethoxysilane (TEOS), methyltrimethoxysilane (MTMS), absolute ethyl alcohol and deionized water N, N-Dimethylformamide (DMF) into a beaker, dropwise adding hydrochloric acid until the pH value is 2-3 for hydrolysis, and magnetically stirring and uniformly mixing;
(3) adding 0.25mol/L ammonia water to pH 6-7, stirring, soaking blocky delignified balsawood into the solution, vacuum soaking for 40min, taking out, aging and standing for 12 h;
(4) uniformly mixing TEOS, MTMS and absolute ethyl alcohol according to the mass ratio of 0.8:0.2:6 to prepare an aging solution, and putting the aged gel into the aging solution for aging;
(5) placing the mixture in normal hexane for displacement treatment at 45 ℃ for 2 times;
(6) carrying out surface modification treatment by using a trimethylchlorosilane TMCS/n-hexane mixed solution until no oily matter is separated out, and replacing for 2 times by using n-hexane;
(7) drying by a sectional heating method to obtain the wood-SiO2An aerogel composite;
(8) wood-SiO2Carbonizing the aerogel composite material in a tubular furnace under the protection of argon;
(9) impregnating the evenly mixed paraffin into the prepared carbonized wood-SiO by adopting a vacuum impregnation method2And preparing the carbonized wood-based composite phase change energy storage material in the aerogel matrix.
Preferably, in step (1), the cooking temperature is 80 ℃, 10% NaClO2The pH of the solution was adjusted to 4 with acetic acid.
Preferably, in step (2), the amount ratio of TEOS to MTMS, absolute ethanol, deionized water, and DMF is 0.8:0.2:6:4:0.5, and the hydrolysis time is 3 hours.
Preferably, in the step (3), the vacuum degree is 0.08MPa, and the gel time is controlled to be 1-2 h.
Preferably, in the step (4), TEOS, MTMS and absolute ethyl alcohol are uniformly mixed according to the mass ratio of 0.8:0.2:6, and the aging time is 24 h.
Preferably, in step (5), n-hexane is replaced once for 6 h.
Preferably, in step (6), the volume ratio of the trimethylchlorosilane TMCS/n-hexane is 1: 9.
Preferably, in step (7), the sequence of stepwise drying is 30 ℃ for 2h, 50 ℃ for 2h, 80 ℃ for 4h, 100 ℃ for 2h, and 120 ℃ for 2 h.
Preferably, in step (8), the tube furnace temperature is set to: raising the temperature to 250 ℃ for 240min at room temperature, preserving the heat for 2h, raising the temperature to 450 ℃ for 100min, raising the temperature to 800 ℃ for 70min, and preserving the heat for 1h at 800 ℃.
Preferably, in the step (9), the molten paraffin phase-change material is mixed with the carbonized wood-SiO2The mass ratio of the aerogel is 5: 1-10: 1, the vacuum degree of the vacuum drying oven is 0.1MPa, the dipping temperature is 70 ℃, and the dipping time is 6-12 hours.
Compared with the prior art, the invention has the following advantages and effects:
1. compared with the carbonized wood-based composite phase change energy storage material, the carbonized wood-SiO2The aerogel-based composite phase-change heat storage material has strong controllability, high phase-change latent heat, good high-temperature stability and small environmental influence, and is favorable for popularization and utilization in the field of building energy conservation.
2. The preparation method has simple process, easy control and low energy consumption, takes the balsa wood fiber with partial hemicellulose and lignin removed as a matrix, and takes SiO as the matrix2Compounding aerogel and the composite material, carbonizing, and impregnating the phase change material into a balsa wood fiber matrix by using a vacuum impregnation method. The method is carried out by SiO2The aerogel reinforces the balsa frame, enlarges the pore structure of the carbonized wood, increases the specific surface area, improves the holding capacity of the carbonized wood to the phase-change material, and has good development prospect and further value of further extensive research.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The present invention will be described in detail with reference to specific examples below:
airless gel as support and specific surface area enhancement term for comparative example 1
(1) Putting 20 × 20 × 8mm Barbara fir wood blocks into deionized water, steaming at 80 deg.C for 2 hr, vacuumizing, and steaming for 1 hr when the wood blocks are at bottom;
(2) the thoroughly cooked wood pieces were transferred to 10% NaClO with pH 42Steaming at 80 deg.C for 2 hr. Soaking in deionized water repeatedly until the wood block turns white, and freeze drying to obtain delignified balsawood block;
(3) carbonizing delignified balsawood blocks in a tubular furnace under the protection of argon (room temperature 240min rising 250 ℃, heat preservation 2h, 100min rising 450 ℃, 70min rising 800 ℃, heat preservation 800 ℃ for 1 h);
(4) and (3) vacuum-impregnating the prepared carbonized wood at 60 ℃ with the evenly-mixed paraffin for 12 hours to complete saturated vacuum impregnation, and cooling the sample to room temperature to obtain the carbonized wood-based composite phase change energy storage material.
Example 1
(1) Putting 20 × 20 × 8mm Barbara fir wood blocks into deionized water, steaming at 80 deg.C for 2 hr, vacuumizing, and steaming for 1 hr when the wood blocks are at bottom;
(2) the thoroughly cooked wood pieces were transferred to 10% NaClO with pH 42Steaming at 80 deg.C for 2 hr, soaking in deionized water repeatedly until the wood block turns white, and freeze drying to obtain delignified balsa wood block;
(3) adding tetraethoxysilane, methyltrimethoxysilane, absolute ethyl alcohol and deionized water N, N-dimethylformamide into a beaker according to the mass ratio of 0.8:0.2:6:4:0.5, uniformly stirring and mixing by magnetic force, dropwise adding 0.1mol/L hydrochloric acid until the pH value is 2, hydrolyzing for 3 hours;
(4) adding 0.25mol/L ammonia water to pH 6, stirring, soaking the blocky delignified balsawood into the solution, vacuum soaking for 40min, taking out, aging and standing for 12h to enhance the skeleton structure;
(5) uniformly mixing TEOS, MTMS and absolute ethyl alcohol according to the mass ratio of 0.8:0.2:6 to prepare an aging solution, putting the aged gel into the aging solution to age for 24 hours, replacing the moisture in the wet gel and further enhancing the network framework structure of the wet gel;
(6) then placing the mixture in n-hexane for replacement treatment at 45 ℃, and replacing n-hexane once for 6 hours for 2 times;
(7) and then carrying out surface modification treatment by using TMCS/n-hexane mixed liquor with the volume ratio of 1:9 until no oil is precipitated and the modification is finished. Then n-hexane is used for replacement, and the n-hexane is replaced once for 6 hours and treated for 2 times;
(8) drying at 30 deg.C for 2 hr, at 50 deg.C for 2 hr, at 80 deg.C for 4 hr, at 100 deg.C for 2 hr, at 120 deg.C for 2 hr, and drying to obtain wood-SiO2An aerogel composite;
(9) wood-SiO2Carbonizing the aerogel composite material in a tube furnace under the protection of argon (the room temperature is 240min, the temperature is 250 ℃, the heat is preserved for 2h, the temperature is 100min, the temperature is 450 ℃, the temperature is 70min, the temperature is 800 ℃, and the heat is preserved for 1h at 800 ℃);
(10) prepared carbonized wood-SiO2And (3) carrying out vacuum impregnation on the uniformly mixed paraffin for 12h by using the aerogel at 70 ℃, completing saturated vacuum impregnation, and cooling the sample to room temperature to obtain the carbonized wood-based composite phase change energy storage material.
The results of example 1 and comparative example were tested and the results are shown in Table 1.
TABLE 1 test results of dimensional stability and paraffin loading performance of carbonized wood-based composite phase change energy storage material
| Categories | Original size | Size after carbonization | Paraffin loading rate | Phase transition temperature | Latent heat |
| Comparative example 1 | 20×20×8mm | 7.2×6.4×5.1mm | 72％ | 48.3℃ | 142J/g |
| Example 1 | 20×20×8mm | 15.4×16.9×6.8mm | 94％ | 51.6℃ | 193J/g |
Example 2
(1) Putting 20 × 20 × 8mm Barbara fir wood blocks into deionized water, steaming at 80 deg.C for 2 hr, vacuumizing, and steaming for 1 hr when the wood blocks are at bottom;
(2) the thoroughly cooked wood pieces were transferred to 10% NaClO with pH 42Steaming at 80 deg.C for 2 hr. Soaking in deionized water repeatedly until the wood block turns white, and freeze drying to obtain delignified balsawood block;
(3) adding tetraethoxysilane, methyltrimethoxysilane, absolute ethyl alcohol and deionized water N, N-dimethylformamide into a beaker according to the mass ratio of 0.8:0.2:6:4:0.5, uniformly stirring and mixing by magnetic force, dropwise adding 0.1mol/L hydrochloric acid until the pH value is 3, hydrolyzing for 3 hours;
(4) adding 0.25mol/L ammonia water to pH 7, stirring, soaking the blocky delignified balsawood into the solution, vacuum soaking for 40min, taking out, aging and standing for 12h to enhance the skeleton structure;
(5) uniformly mixing TEOS, MTMS and absolute ethyl alcohol according to the mass ratio of 0.8:0.2:6 to prepare an aging solution, putting the aged gel into the aging solution to age for 24 hours, replacing the moisture in the wet gel and further enhancing the network framework structure of the wet gel;
(6) then placing the mixture in n-hexane for replacement treatment at 45 ℃, replacing n-hexane once for 6 hours, and replacing for 2 times;
(7) and then carrying out surface modification treatment by using TMCS/n-hexane mixed liquor with the volume ratio of 1:9 until no oil is precipitated and the modification is finished. Then n-hexane is used for replacement, and the n-hexane is replaced once for 6 hours for 2 times;
(8) drying at 30 deg.C for 2 hr, at 50 deg.C for 2 hr, at 80 deg.C for 4 hr, at 100 deg.C for 2 hr, at 120 deg.C for 2 hr, and drying to obtain wood-SiO2An aerogel composite;
(9) wood-SiO2Carbonizing the aerogel composite material in a tube furnace under the protection of argon (the room temperature is 240min, the temperature is 250 ℃, the heat is preserved for 2h, the temperature is 100min, the temperature is 450 ℃, the temperature is 70min, the temperature is 800 ℃, and the heat is preserved for 1h at 800 ℃);
(10) prepared carbonized wood-SiO2And (3) carrying out vacuum impregnation on the uniformly mixed paraffin for 12h by using the aerogel at the temperature of 60 ℃, completing saturated vacuum impregnation, and cooling the sample to room temperature to obtain the carbonized wood-based composite phase change energy storage material.
The results of example 2 and comparative example were tested and are shown in table 2.
TABLE 2 test results of dimensional stability and paraffin loading performance of carbonized wood-based composite phase change energy storage material
| Categories | Original size | Size after carbonization | Paraffin loading rate | Phase transition temperature | Latent heat |
| Comparative example 1 | 20×20×8mm | 7.2×6.4×5.1mm | 72％ | 48.3℃ | 142J/g |
| Example 2 | 20×20×8mm | 14.8×16.6×6.2mm | 92％ | 52.9℃ | 185J/g |
As can be seen from comparison between the examples and comparative examples summarized in tables 1 and 2, the carbonized wood-based composite phase change energy storage material obtained by the method of the invention has greatly improved effective volume of the phase change material.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The preparation method of the carbonized wood-based composite phase change energy storage material is characterized by comprising the following steps:
(1) putting barktree fir wood blocks into deionized water, cooking for 2h at a certain temperature, and transferring into 10% NaClO2Steaming at 80 deg.C for 2 hr until the wood block turns white, repeatedly soaking in deionized water, and freeze drying to obtain delignified balsa wood block;
(2) adding Tetraethoxysilane (TEOS), methyltrimethoxysilane (MTMS), absolute ethyl alcohol and deionized water N, N-Dimethylformamide (DMF) into a beaker, dropwise adding hydrochloric acid until the pH value is 2-3 for hydrolysis, and magnetically stirring and uniformly mixing;
(3) adding 0.25mol/L ammonia water to pH 6-7, stirring, soaking blocky delignified balsawood into the solution, vacuum soaking for 40min, taking out, aging and standing for 12 h;
(4) uniformly mixing TEOS, MTMS and absolute ethyl alcohol according to the mass ratio of 0.8:0.2:6 to prepare an aging solution, and putting the aged gel into the aging solution for aging;
(5) placing the mixture in normal hexane for displacement treatment at 45 ℃ for 2 times;
(6) carrying out surface modification treatment by using a Trimethylchlorosilane (TMCS)/n-hexane mixed solution until no oily matter is separated out, and replacing for 2 times by using n-hexane;
(7) drying by a sectional heating method to obtain the wood-SiO2An aerogel composite;
(8) wood-SiO2Carbonizing the aerogel composite material in a tubular furnace under the protection of argon;
(9) the phase change energy storage material is encapsulated in the prepared carbonized wood-SiO by a vacuum impregnation mode2And preparing the carbonized wood-based composite phase change energy storage material in the aerogel matrix.
2. The method according to claim 1, wherein in the step (1), the cooking temperature is 80 ℃ and 10% NaClO is used2The pH of the solution was adjusted to 4 with acetic acid.
3. The preparation method according to claim 1, wherein in the step (2), the mass ratio of TEOS to MTMS, absolute ethanol, deionized water and DMF is 0.8:0.2:6:4:0.5, and the hydrolysis time is 3 hours.
4. The preparation method according to claim 1, wherein in the step (3), the vacuum degree is 0.08MPa, and the gel time is controlled to be 1-2 h.
5. The preparation method according to claim 1, wherein in the step (4), TEOS, MTMS and absolute ethyl alcohol are uniformly mixed according to the mass ratio of 0.8:0.2:6, and the aging time is 24 h.
6. The method according to claim 1, wherein in the step (5), n-hexane is replaced once for 6 hours.
7. The preparation method according to claim 1, wherein in the step (6), the volume ratio of the trimethylchlorosilane TMCS/n-hexane is 1: 9.
8. The method according to claim 1, wherein in the step (7), the stepwise drying sequence is 30 ℃ for 2 hours, 50 ℃ for 2 hours, 80 ℃ for 4 hours, 100 ℃ for 2 hours, and 120 ℃ for 2 hours.
9. The method according to claim 1, wherein in the step (8), the tube furnace temperature is set to: raising the temperature to 250 ℃ for 240min at room temperature, preserving the heat for 2h, raising the temperature to 450 ℃ for 100min, raising the temperature to 800 ℃ for 70min, and preserving the heat for 1h at 800 ℃.
10. The preparation method according to claim 1, wherein in the step (9), the phase change energy storage material can be one of paraffin emulsion, polyethylene glycol, stearic acid, polybasic fatty acid, and the like; phase change material and carbonized wood-SiO2The mass ratio of the aerogel is 5: 1-10: 1, the vacuum degree of a vacuum drying oven is 0.1MPa, the dipping temperature is 70 ℃, and the dipping time is 6-12 h。
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| CN114106782A (en) * | 2021-12-08 | 2022-03-01 | 华中科技大学 | Fast-growing wood matrix composite sensible heat-thermochemical heat storage material and preparation method thereof |
| CN114106782B (en) * | 2021-12-08 | 2022-12-09 | 华中科技大学 | Fast-growing wood matrix composite sensible heat-thermochemical heat storage material and preparation method thereof |
| CN114196381A (en) * | 2021-12-28 | 2022-03-18 | 浙江海洋大学 | High-energy-storage-density phase-change material and preparation method thereof |
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