CN103045172B - Capric acid gel solid-solid phase change material and method thereof - Google Patents
Capric acid gel solid-solid phase change material and method thereof Download PDFInfo
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- CN103045172B CN103045172B CN201210570990.3A CN201210570990A CN103045172B CN 103045172 B CN103045172 B CN 103045172B CN 201210570990 A CN201210570990 A CN 201210570990A CN 103045172 B CN103045172 B CN 103045172B
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Abstract
The invention relates to a capric acid gel solid-solid phase change material and a method thereof, and in particular to a capric acid system which is doped with a multi-allyl acid esters radiation sensitizer by irradiation of high-energy electron beams generated by an electron accelerator. The molecules of the multi-allyl acid esters radiation sensitizer and the molecules of capric acid undergo grafting and cross-linking reaction to produce a hydrophobic capric acid gel material which has a solid-solid phase change property. The invention belongs to the technical field of radiation chemistry and polymer material processing.
Description
Technical field
The present invention relates to a kind of solid-solid phase change material and method thereof, particularly a kind of capric acid gel solid-solid phase change material and method thereof.
Background technology
Phase-changing energy storage material breaks through Conventional insulation (brick, cement etc.) single resistive properties, has potential heat value large, stores, the nearly quasi-isothermal feature of exothermic process, can prepare temp auto-controlled phase-change accumulation energy building thermal insulation material.Can phase-changing energy storage material be used for building trade, depends on the weather resistance of material, economy and application property.Normally 50 years working life of material of construction, this requirement is equally applicable to phase-changing energy storage material.But solid-liquid phase change material in use can from material of construction leak out (material surface frosting), greatly reduce the performance of phase-change accumulation energy building thermal insulation material.The advantages such as capric acid phase change material has wide material sources, with low cost, transformation temperature is 33 DEG C, can be used for preparing phase-change accumulation energy building thermal insulation material.One of its subject matter faced is the leakage phenomenon in phase transition process, if its phase transition property can be made to change solid-solid phase-change into by solid-liquid phase change by electron beam to irradiate crosslinked technology, then can overcome this problem,
Summary of the invention
An object of the present invention is to provide a kind of capric acid gel solid-solid phase change material.
Two of object of the present invention is the preparation method providing this phase change material a kind of, the high-power electron beam that the method adopts rumbatron to produce, irradiation is added with the capric acid system of many propenyl esters of gallic acid sensitizing agent, cause capric acid molecule and polymerization and crosslinking reaction occur, prepare hydrophobicity capric acid gelatinous material, make the phase transition property of capric acid change solid-solid phase-change into by solid-liquid phase change, overcome the leakage phenomenon of capric acid material in phase-change accumulation energy building thermal insulation material.
For achieving the above object, the present invention adopts following technical scheme:
A kind of capric acid gel solid-solid phase change material, it is characterized in that this material is by capric acid under the existence of radiosensitizer, cause crosslinking copolymerization through electron beam irradiation, form cancellated capric acid gel, wherein the quality of sensitizing agent is 3 ~ 5% of the quality of capric acid; Described radiosensitizer is many propenyl esters of gallic acid irradiation sensitizing agent.
Above-mentioned many propenyl esters of gallic acid irradiation sensitizing agent is trimethylolpropane trimethacrylate, 1,6 hexanediol diacrylate, Triethylene glycol dimethacrylate, triallyl cyanurate, propoxylation Viscoat 295 (PO-TMPTA) or propoxylation (2) neopentylglycol diacrylate (PO-NPGDA).
Prepare a method for above-mentioned capric acid gel solid-solid phase change material, it is characterized in that the concrete steps of the method are as follows:
A. heat capric acid all to dissolve to it;
B. joined in the capric acid solution of step a by irradiation sensitizing agent, obtain mixed solution, wherein the quality of irradiation sensitizing agent is 1%-9% of capric acid quality.
C. step b gained mixed solution sonic oscillation 10 ~ 15 minutes at the temperature of 70 DEG C ~ 80 DEG C, make capric acid and irradiation sensitizing agent fully miscible;
D. again step c gained solution in an inert atmosphere, at 70 DEG C of temperature, with electron beam irradiation, irradiation dose is 5kGy ~ 200kGy; Namely capric acid gel solid-solid phase change material is obtained.
At normal temperatures and pressures, by high-energy electron beam irradiation polyenoid propyl group acid esters capric acid solution, make capric acid molecule polymerization occur and be cross-linked, form lipophilicity capric acid gel, its technical process is simple, with short production cycle in the present invention.After capric acid molecule generation gelation reaction, the change of its phase transition performance generation essence, changes solid-solid phase-change (capric acid gelatinous material) into by the solid-liquid phase change before molecule crosslinked.The phase transition performance change of this phase change material, has very large impact to the application of phase transformation building thermal insulation material.For solid-liquid phase change material, when heating materials is to temperature of fusion, material just produces from solid-state to the phase transformation of liquid state, and in the process of fusing, phase change material absorbs and stores a large amount of latent heat; When phase change material cools, the heat of storage will be dispersed in environment and go in certain temperature range, carries out from liquid state to solid-state reverse transformation.In these two kinds of phase transition process, energy that is stored or release is called latent heat of phase change.When physical condition changes, the temperature of material self almost remains unchanged before phase transformation completes, and forms a wide temperature platform, although temperature-resistant, absorb or the latent heat of release quite large.This performance of phase change material can be applied to building heat preservation field, but there is a problem, Gu often there is a careless omission phenomenon in the phase-change energy-storing thermal insulation material that-liquid phase change material is made, namely when phase change material becomes liquid phase, due to capillary effect, liquid phase change material can infiltrate (material surface frosting) between caking agent-concrete finedraw gap.How to prevent the careless omission phenomenon of liquid phase change material from being the gordian technique ensureing high quality phase-change energy-storing thermal insulation material.Radiotechnology makes the phase transition property of capric acid change solid-solid phase-change into by solid-liquid phase change, and just say, capric acid gelatinous material does not exist the state of liquid phase in its phase transition process, avoids the leakage phenomenon of capric acid material in phase-change accumulation energy building thermal insulation material yet.
Accompanying drawing explanation
fig. 1 is pure capric acid and adds 5%TMPTMA and irradiation dose is the infared spectrum of the capric acid gel solid-solid phase change material of 150kGy.
Embodiment
Technical essential of the present invention is set forth further below in conjunction with specific embodiment.These examples have further described and demonstrated the embodiment in the scope of the invention.The embodiment provided only for illustration of object, do not form any restriction to the present invention, can carry out various change to its concentration under the condition not deviating from spirit and scope of the invention, all concentration listed in embodiment are concentration expressed in percentage by weight.
After now specific embodiments of the invention being described in.
embodiment 1:technological process in the present embodiment and step as follows:
Weighing a certain amount of capric acid puts in a reservoir, this container is put into 70 DEG C of water-baths and heats, capric acid is all dissolved; Joined by irradiation sensitizing agent trimethylolpropane trimethacrylate (TMPTMA) in the capric acid solution dissolved, wherein the content of trimethylolpropane trimethacrylate is 5% of capric acid amount.This container is put into the ultrasonic cleaner that water temperature is 70 DEG C-80 DEG C, sonic oscillation 15 minutes, make capric acid and trimethylolpropane trimethacrylate two kinds of liquid fully miscible, obtain the capric acid solution of trimethylolpropane trimethacrylate; Continue to make trimethylolpropane trimethacrylate capric acid system be in liquid state (temperature of 70 DEG C), rush nitrogen 15 minutes to the liquid in container, the oxygen in container is discharged, sealed vessel.Under room temperature condition of normal pressure, the trimethylolpropane trimethacrylate capric acid in the electron beam irradiation step d produced with rumbatron, irradiation dose is 5kGy 10kGy, 60kGy, 90kGy, 120kGy, 150Gy, 200kGy;
Trimethylolpropane trimethacrylate capric acid sample after irradiation being put into temperature is 70 DEG C of baking oven insulations 1 hour, observe sample, find to present except transparent liquid except the blank sample of non-irradiation, other irradiation sample all adularescent solid exists, and illustrates that capric acid molecule and trimethylolpropane trimethacrylate there occurs polymerization and crosslinking reaction.To add the capric acid system of 5% irradiation sensitizing agent, irradiation dose is the sample of 150 kGy is example, and the sample after irradiation is through Soxhlet extractor extracting, and the gel content calculating sample is 21.5%.
Embodiment
2
Change following condition, other condition is with embodiment 1.
Joined by irradiation sensitizing agent Triethylene glycol dimethacrylate (TMPTMA) in the capric acid solution dissolved, wherein the content of Triethylene glycol dimethacrylate is 1%-9% of capric acid amount, and irradiation dose is 120kGy.
Sample after irradiation being put into temperature is 70 DEG C of baking oven insulations 1 hour, and observe sample, find except the sample not putting irradiation sensitizing agent presents transparent liquid, other irradiation sample all adularescent solid exists.To add the capric acid system of 3% irradiation sensitizing agent, irradiation dose is the sample of 120 kGy is example, and the sample after irradiation is through Soxhlet extractor extracting, and the gel content calculating sample is 7.9%.
The present invention adopts electronic beam irradiation technology, by adding irradiation sensitizing agent, makes the capric acid molecule containing long chain hydrocarbon take out hydrogen effect, produces free radical, and then polymerization and crosslinking reaction occur, and prepares the capric acid gelatinous material with solid-solid phase change performance.Can find out from the infrared spectrum of Fig. 1,1710 cm-1 places are that the stretching vibration of C=O causes, and 1258 cm-1 places are the symmetrical stretching vibration peaks of C-O in carboxyl.For TMPTMA, at 1722 cm-1 places, and there is the symmetric curvature vibration absorption peak of CH3 in ester group charateristic avsorption band at 1380 cm-1 places, 1170 cm-1 places are the symmetrical stretching vibration peaks of the C-O in ester group simultaneously.Obtain the infrared spectrum of product from TMPTMA and oleic acid copolymerization, we are clear that 3007 cm-1 places are disappeared by the C-H stretching vibration absorption peak on unsaturated carbon, and the symmetrical stretching vibration peak of the C-O in ester group is there is at 1158cm-1 place, having there is the symmetrical stretching vibration peak of C-O in carboxyl in 1249cm-1 place, it can be said that bright capric acid and TMPTMA really there occurs copolymerization under irradiation.
Claims (3)
1. a capric acid gel solid-solid phase change material, is characterized in that this material is by capric acid under the existence of radiosensitizer, and cause crosslinking copolymerization through electron beam irradiation, form cancellated capric acid gel, wherein the quality of sensitizing agent is 3 ~ 5% of the quality of capric acid; Described radiosensitizer is many propenyl esters of gallic acid irradiation sensitizing agent.
2. capric acid gel solid-solid phase change material according to claim 1, it is characterized in that described many propenyl esters of gallic acid irradiation sensitizing agent is trimethylolpropane trimethacrylate, 1,6 hexanediol diacrylate, Triethylene glycol dimethacrylate, triallyl cyanurate, propoxylation Viscoat 295 (PO-TMPTA) or propoxylation (2) neopentylglycol diacrylate (PO-NPGDA).
3. prepare a method for capric acid gel solid-solid phase change material according to claim 1 and 2, it is characterized in that the concrete steps of the method are as follows:
A. heat capric acid all to dissolve to it;
B. joined in the capric acid solution of step a by irradiation sensitizing agent, obtain mixed solution, wherein the quality of irradiation sensitizing agent is 3 ~ 5% of capric acid quality
C. step b gained mixed solution sonic oscillation 10 ~ 15 minutes at the temperature of 70 DEG C ~ 80 DEG C, make capric acid and irradiation sensitizing agent fully miscible;
D. again step c gained solution in an inert atmosphere, at 70 DEG C of temperature, with electron beam irradiation, irradiation dose is 5kGy ~ 200kGy; Namely capric acid gel solid-solid phase change material is obtained.
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