CN106497521A - A kind of preparation method of ternary aliphatic acid silicon dioxide composite shape-stabilized phase phase-change material - Google Patents
A kind of preparation method of ternary aliphatic acid silicon dioxide composite shape-stabilized phase phase-change material Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000012782 phase change material Substances 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 23
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 19
- 125000001931 aliphatic group Chemical group 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002253 acid Substances 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 23
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 22
- 239000000194 fatty acid Substances 0.000 claims abstract description 22
- 229930195729 fatty acid Natural products 0.000 claims abstract description 22
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 18
- 230000009466 transformation Effects 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 238000002156 mixing Methods 0.000 claims description 31
- 230000005496 eutectics Effects 0.000 claims description 25
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 22
- 239000002904 solvent Substances 0.000 claims description 19
- 230000032683 aging Effects 0.000 claims description 18
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 15
- 238000002844 melting Methods 0.000 claims description 14
- 230000008018 melting Effects 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000006073 displacement reaction Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 230000004048 modification Effects 0.000 claims description 9
- 238000012986 modification Methods 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 150000004668 long chain fatty acids Chemical class 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000004567 concrete Substances 0.000 claims description 2
- 238000010348 incorporation Methods 0.000 claims description 2
- PPURVCXMNDMHBJ-UHFFFAOYSA-N CCCCCCCCCC(O)=O.CCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCC(O)=O Chemical compound CCCCCCCCCC(O)=O.CCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCC(O)=O PPURVCXMNDMHBJ-UHFFFAOYSA-N 0.000 claims 1
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 230000007704 transition Effects 0.000 abstract description 18
- 238000004146 energy storage Methods 0.000 abstract description 4
- 239000012567 medical material Substances 0.000 abstract 1
- 238000005191 phase separation Methods 0.000 abstract 1
- 238000011084 recovery Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 239000002918 waste heat Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 29
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 24
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 24
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 23
- 229910001868 water Inorganic materials 0.000 description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 16
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 description 12
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 12
- 239000005639 Lauric acid Substances 0.000 description 12
- 235000021360 Myristic acid Nutrition 0.000 description 12
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 description 12
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 12
- 230000008859 change Effects 0.000 description 10
- 239000000499 gel Substances 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000003756 stirring Methods 0.000 description 9
- 208000012826 adjustment disease Diseases 0.000 description 8
- 229910021529 ammonia Inorganic materials 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 230000001476 alcoholic effect Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 230000010355 oscillation Effects 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000003094 microcapsule Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004375 physisorption Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The present invention relates to a kind of ternary aliphatic acid silicon dioxide is combined the preparation method of qualitative phase-change material, with fatty acid as phase transformation core, and the species of the low fused matter fatty acid of ternary is selected according to Applicable temperature scope, constraint is packaged using the silicon dioxide with three-dimensional net structure to core for inorganic carrier, different so as to the obtain phase transition temperature and latent heat composite shape-setting phase-change material.The supporting role of carrier can ensure that the nonflowing character and machinability of phase-change material, can ensure which does not occur Seepage in phase transition process, therefore whole composite remains to keep the shape of its solid and performance, so as to ensure that the energy storage stability property of composite shape-setting phase-change material.The composite shape-setting phase-change material latent heat of the present invention is high and phase transition temperature is adjustable, without obvious phenomenon of phase separation, can be widely applied to the fields such as energy-saving building materialses, temperature-regulation garment, Solar use, medical material and waste heat recovery.
Description
Technical field
The present invention relates to phase-changing energy storage material and porous matrix material technology of preparing crossing domain, are related to a kind of ternary aliphatic
The preparation method of acid-silicon dioxide composite shape-stabilized phase phase-change material, and in particular to melting mixing prepares fatty acid with reference to sonic oscillation
Eutectic, and liquid state phase change material is dispersed in Si-O-Si inorganic network structures using sol-gel technology
One step prepares composite shape-setting phase-change material.
Background technology
Fatty acid is that nature has widest class solid-liquid phase change material, and which has, and latent heat of phase change is big, nontoxic and environmental protection
The advantages of can be recycled is so as to broader application.But the fusing point of single fat acid is often higher, can basis
Lowest total of the melting point is theoretical, two kinds or more of fatty acids is mixed according to a certain ratio, so as to obtain being more suitable for middle low temperature
The fatty acid eutectic in field, has widened its use range and has improve economic worth.But fatty acid is in phase transition process
Easily generation liquid phase substance seepage is loaded compound so as to prepare so as to reduce energy storage property, therefore using carrier material to which
Shaping phase-change material, had so both limited the flowing of liquid state phase change material while its mechanical property and stability are substantially changed
Kind.
At present, how fatty acid is encapsulated the class that setting is which receives much concern as in phase-changing energy storage material research field
Topic, therefore select and fatty acid is effectively coated using suitable carrier and fixation be current R＆D work key.Common
Boarding techniques mainly include melting mixing and sonic oscillation combined techniqueses, microcapsule method, sol-gal process and chemical graft process etc..
Melting mixing and the process is simple of sonic oscillation combined techniqueses, but because only tying by simple physisorption between carrier and core
Close, its packaged stability is general.Microcapsule method particle diameter I increase overall heat dissipation area and machinability is strong, but complex process and
Encapsulation efficiencies are relatively low.Chemical graft process packaged stability is good but heat conductivility difference and is unfavorable for the quick response of accumulation of heat heat release.
Sol-gel process be at present using relatively broad and can room temperature realize function attachment a kind of wet chemical.
Content of the invention
The invention aims to overcoming the too high shortcoming with narrow application range of single fat acid phase transition temperature, and provide
A kind of preparation method of ternary aliphatic acid-silicon dioxide composite shape-stabilized phase phase-change material.
The technical scheme is that：A kind of ternary aliphatic acid-silicon dioxide is combined the preparation method of qualitative phase-change material,
Which comprises the following steps that：
(1) three kinds of long-chain fatty acid are weighed according to the ratio of calculating and added in container, it is placed in 50 after stoppering rubber stopper seal～
25-30min is heated in 60 DEG C of water-baths, and ultrasonic disperse after the complete melting mixing of thing to be mixed, so that obtain ternary eutectic thing fat
Fat acid, is then placed in standby in baking oven；
(2), after mixing in proportion presoma, dehydrated alcohol and deionized water, pH of mixed is adjusted to 3～4
Between, and stirred by magnetic stirrer；
(3) subsequently reaction system pH is adjusted to 6～8, the ternary eutectic thing fatty acid of molten state is mixed into, and water-bath
Ultrasonic disperse again after middle stirring；
(4) above-mentioned mixed solution is sealed respectively and be placed in aging 24-28h in dehydrated alcohol, temperature control is used at 48-50 DEG C
Normal hexane carries out solvent displacement to substitute residual fraction alcohol solvent；
(5) add modifying agent to the process of pluralgel modifying surface, then the gel is placed in baking oven and is dried to perseverance
Weight, finally gives ternary aliphatic acid-silicon dioxide composite phase-change material.
Long-chain fatty acid described in preferred steps (1) is ternary system, and concrete proportioning is as follows：Capric acid-lauric acid-lima bean
The mass ratio of cool acid is 1：(0.5-0.6)：(0.3-0.4), the mass ratio of capric acid-lauric acid-Palmic acid is 1：(0.5-0.6)：
(0.1-0.2), the mass ratio of capric acid-myristic acid-Palmic acid is 1：(0.3-0.4)：(0.2-0.25), lauric acid-Semen Myristicae
The mass ratio of acid-Palmic acid is 1：(0.6-0.7)：(0.3-0.4).
Presoma described in preferred steps (2) is tetraethyl orthosilicate；Presoma：Dehydrated alcohol：Deionized water according to
1:(4～6):The mass ratio mixing of (6～8)；Magnetic stirrer rotating speed is 350-400r/min, and mixing time is 28-
30min.
Bath temperature described in preferred steps (3) is 55-60 DEG C, and mixing time is 55-60min.
40-65% of the ternary aliphatic acid system volume for phase-change material quality in preferred steps (3).
Modification temperature described in preferred steps (5) is 48-50 DEG C, and modification time is 10-12h；Described oven temperature
For 55-60 DEG C.
It is preferred that stating modifying agent for the one kind in trim,ethylchlorosilane or normal hexane, modifying agent incorporation is pluralgel quality
10～15%.
Beneficial effect：
Long-chain fatty acid make phase transformation core and have that low cost, nontoxic, heat stability be good, in phase transition process without supercool and phase
Segregation phenomenon, latent heat of phase change are high and wide material sources are easy to get, actually used in can select variety classes fatty acid according to not homogeneity
Amount ratio compounded so as to obtain phase transition temperature adjustable and more suitable for room temperature field application requirement ternary aliphatic acid mixing
Thing.In addition, the preparation process of ternary aliphatic acid eutectic simple, safely, saving time is easy to get.
(2) Schroeder's formula is for composition and ratio and relatively accurate (four in the present invention of hot physical property prediction of ternary phase change system
Deviation between the estimated value of group ternary aliphatic acid eutectic and DSC test numbers, latent heat of phase change ＜ 20J/g, phase transition temperature
5 DEG C of ＜), due to first having to select suitable phase transition temperature according to application, the therefore system in reality to fatty acid eutectic
Standby and application with certain reference role.
(3) silicon dioxide is used as specific surface area is big and mushy three dimensional structure carrier, can will be uniformly firm for phase transformation core
Ground interlocking its skeletal internal, effectively alleviates seepage of the solid-liquid phase change material in phase transition process.
(4) the silica gel structure that hydrophobic treatment is crossed has good hydrophobic function, it is ensured that the complete structure of carrier and
Which is for the firm constraint of core organic aliphatic acid.
(5) ternary aliphatic acid/silicon dioxide composite shape-stabilized phase phase-change material of the invention, latent heat of phase change is high and heat stability is good,
The composite wood of application conditions can be met by changing the species and quality proportioning of phase transformation core to regulate and control its phase transition temperature
Material.
Description of the drawings
Pictorial diagrams of the Fig. 1 for the LA-MA-PA/ silicon dioxide composite phase-change materials of the embodiment of the present invention 1；
SEM figures of the Fig. 2 for the LA-MA-PA/ silicon dioxide composite phase-change materials of the embodiment of the present invention 1；
DSC figures of the Fig. 3 for the LA-MA-PA/ silicon dioxide composite phase-change materials of the embodiment of the present invention 1.
Specific embodiment
The present invention is further illustrated below by embodiment.
Embodiment 1
First, lauric acid (LA), myristic acid (MA) and Palmic acid (PA) are weighed respectively according to 1 using electronic balance:
0.7:0.38 eutectic quality carries out proportioning, adds and covers in test tube after the complete melting mixing of rubber stopper seal thing to be mixed 60
25min and then ultrasonic disperse is heated in DEG C water-bath.Tetraethyl orthosilicate, dehydrated alcohol and deionized water are according to TEOS:H2O:
EtOH=1:5:After 7 ratio mixing, add hydrochloric acid pH value of solution to be adjusted to 3, and (rotating speed is 350r/ through magnetic stirrer
Min) uniform stirring 30min.Weak ammonia adjustment reaction system pH is added to 7, by the LA-MA-PA ternary eutectic things of molten state
Fatty acid is mixed into, and ultrasonic disperse again after 60 DEG C of stirred in water bath 58min.Mixed solution is sealed respectively and is placed in positive silicic acid
Each aging 24h in tetra-ethyl ester/dehydrated alcohol mixed liquor, aging temperature are 48 DEG C, carry out solvent displacement with normal hexane residual to substitute
Stay part alcohol solvent.Add account for the trim,ethylchlorosilane of pluralgel quality 10% to pluralgel modifying surface at
Reason, wherein modification temperature and time are respectively 50 DEG C and 10h.The gel is placed in 60 DEG C of baking ovens and is dried to constant weight, obtain phase transformation
30.0 DEG C of temperature and for latent heat for 99.3J/g LA-MA-PA/ silicon dioxide composite phase-change materials.
Embodiment 2
First, lauric acid (LA), myristic acid (MA) and Palmic acid (PA) are weighed respectively according to 1 using electronic balance:
0.64:0.35 eutectic quality carries out proportioning, add cover in test tube after the complete melting mixing of rubber stopper seal thing to be mixed
Heating 25min and then ultrasonic disperse in 60 DEG C of water-baths.Tetraethyl orthosilicate, dehydrated alcohol and deionized water are according to TEOS:H2O:
EtOH=1:5:After 7 ratio mixing, add hydrochloric acid pH value of solution to be adjusted to 3, and (rotating speed is 350r/ through magnetic stirrer
Min) uniform stirring 30min.Weak ammonia adjustment reaction system pH is added to 7, by the LA-MA-PA ternary eutectic things of molten state
Fatty acid is mixed into, and ultrasonic disperse again after 60 DEG C of stirred in water bath 58min.Mixed solution is sealed respectively and is placed in positive silicic acid
Each aging 24h in tetra-ethyl ester/dehydrated alcohol mixed liquor, aging temperature are 48 DEG C, carry out solvent displacement with normal hexane residual to substitute
Stay part alcohol solvent.The normal hexane for accounting for pluralgel quality 10% is added to process pluralgel modifying surface, wherein
Modification temperature and time are respectively 50 DEG C and 10h.The gel is placed in 60 DEG C of baking ovens and is dried to constant weight, obtain phase transition temperature 25.0
DEG C and for latent heat for 98.2J/g LA-MA-PA/ silicon dioxide composite phase-change materials.
Embodiment 3
First, capric acid (CA), lauric acid (LA) and myristic acid (MA) are weighed respectively according to 1 using electronic balance:0.60:
0.33 eutectic quality carries out proportioning, adds and covers in test tube after the complete melting mixing of rubber stopper seal thing to be mixed in 55 DEG C of water
Heating 28min and then ultrasonic disperse in bath.Tetraethyl orthosilicate, dehydrated alcohol and deionized water are according to TEOS:H2O:EtOH=
1:6:After 7 ratio mixing, hydrochloric acid is added to adjust pH value of solution to 4, and uniform through magnetic stirrer (rotating speed is 380r/min)
Stirring 30min.Add weak ammonia adjustment reaction system pH to 6, the LA-MA-PA ternary eutectic thing fatty acids of molten state are mixed
Enter, and ultrasonic disperse again after 55 DEG C of stirred in water bath 58min.Mixed solution is sealed respectively be placed in tetraethyl orthosilicate/
Each aging 27h in dehydrated alcohol mixed liquor, aging temperature are 50 DEG C, carry out solvent displacement to substitute residual fraction second with normal hexane
Alcoholic solvent.Add the trim,ethylchlorosilane for accounting for pluralgel quality 12% to the process of pluralgel modifying surface, wherein change
Property temperature and time be respectively 48 DEG C and 11h.The gel is placed in 58 DEG C of baking ovens and is dried to constant weight, phase transition temperature is obtained for 14.5
DEG C and latent heat for 75.2J/g CA-LA-MA/ silicon dioxide composite phase-change materials.
Embodiment 4
First, capric acid (CA), lauric acid (LA) and myristic acid (MA) are weighed respectively according to 1 using electronic balance:0.55:
0.36 eutectic quality carries out proportioning, adds and covers in test tube after the complete melting mixing of rubber stopper seal thing to be mixed in 55 DEG C of water
Heating 28min and then ultrasonic disperse in bath.Tetraethyl orthosilicate, dehydrated alcohol and deionized water are according to TEOS:H2O:EtOH=
1:6:After 7 ratio mixing, hydrochloric acid is added to adjust pH value of solution to 4, and uniform through magnetic stirrer (rotating speed is 380r/min)
Stirring 30min.Add weak ammonia adjustment reaction system pH to 6, the LA-MA-PA ternary eutectic thing fatty acids of molten state are mixed
Enter, and ultrasonic disperse again after 55 DEG C of stirred in water bath 58min.Mixed solution is sealed respectively be placed in tetraethyl orthosilicate/
Each aging 27h in dehydrated alcohol mixed liquor, aging temperature are 50 DEG C, carry out solvent displacement to substitute residual fraction second with normal hexane
Alcoholic solvent.The normal hexane for accounting for pluralgel quality 12% is added to the process of pluralgel modifying surface, wherein modification temperature
48 DEG C and 11h are respectively with the time.The gel is placed in 58 DEG C of baking ovens and is dried to constant weight, obtain phase transition temperature for 13.5 DEG C and latent
CA-LA-MA/ silicon dioxide composite phase-change material of the heat for 76.1J/g.
Embodiment 5
First, capric acid (CA), lauric acid (LA) and Palmic acid (PA) are weighed respectively according to 1 using electronic balance:0.60:
0.15 eutectic quality carries out proportioning, adds and covers in test tube after the complete melting mixing of rubber stopper seal thing to be mixed in 55 DEG C of water
Heating 30min and then ultrasonic disperse in bath.Tetraethyl orthosilicate, dehydrated alcohol and deionized water are according to TEOS:H2O:EtOH=
1:5:After 8 ratio mixing, hydrochloric acid is added to adjust pH value of solution to 4, and uniform through magnetic stirrer (rotating speed is 400r/min)
Stirring 30min.Add weak ammonia adjustment reaction system pH to 6, the LA-MA-PA ternary eutectic thing fatty acids of molten state are mixed
Enter, and ultrasonic disperse again after 59 DEG C of stirred in water bath 60min.Mixed solution is sealed respectively be placed in tetraethyl orthosilicate/
Each aging 28h in dehydrated alcohol mixed liquor, aging temperature are 48 DEG C, carry out solvent displacement to substitute residual fraction second with normal hexane
Alcoholic solvent.Add the trim,ethylchlorosilane for accounting for pluralgel quality 15% to the process of pluralgel modifying surface, wherein change
Property temperature and time be respectively 49 DEG C and 12h.The gel is placed in 60 DEG C of baking ovens and is dried to constant weight, phase transition temperature is obtained for 16.3
DEG C and latent heat for 69.3J/g CA-LA-PA/ silicon dioxide composite phase-change materials.
Embodiment 6
First, capric acid (CA), lauric acid (LA) and Palmic acid (PA) are weighed respectively according to 1 using electronic balance:0.55:
0.2 eutectic quality carries out proportioning, adds and covers in test tube after the complete melting mixing of rubber stopper seal thing to be mixed in 55 DEG C of water
Heating 30min and then ultrasonic disperse in bath.Tetraethyl orthosilicate, dehydrated alcohol and deionized water are according to TEOS:H2O:EtOH=
1:5:After 8 ratio mixing, hydrochloric acid is added to adjust pH value of solution to 4, and uniform through magnetic stirrer (rotating speed is 400r/min)
Stirring 30min.Add weak ammonia adjustment reaction system pH to 6, the LA-MA-PA ternary eutectic thing fatty acids of molten state are mixed
Enter, and ultrasonic disperse again after 59 DEG C of stirred in water bath 60min.Mixed solution is sealed respectively be placed in tetraethyl orthosilicate/
Each aging 28h in dehydrated alcohol mixed liquor, aging temperature are 48 DEG C, carry out solvent displacement to substitute residual fraction second with normal hexane
Alcoholic solvent.The normal hexane for accounting for pluralgel quality 15% is added to the process of pluralgel modifying surface, wherein modification temperature
49 DEG C and 12h are respectively with the time.The gel is placed in 60 DEG C of baking ovens and is dried to constant weight, obtain phase transition temperature for 15.7 DEG C and latent
CA-LA-PA/ silicon dioxide composite phase-change material of the heat for 70.2J/g.
Embodiment 7
First, capric acid (CA), myristic acid (MA) and Palmic acid (PA) are weighed respectively according to 1 using electronic balance:0.32:
0.25 eutectic quality carries out proportioning, adds and covers in test tube after the complete melting mixing of rubber stopper seal thing to be mixed in 60 DEG C of water
Heating 30min and then ultrasonic disperse in bath.Tetraethyl orthosilicate, dehydrated alcohol and deionized water are according to TEOS:H2O:EtOH=
1:4:After 8 ratio mixing, hydrochloric acid is added to adjust pH value of solution to 3, and uniform through magnetic stirrer (rotating speed is 380r/min)
Stirring 30min.Add weak ammonia adjustment reaction system pH to 7, the LA-MA-PA ternary eutectic thing fatty acids of molten state are mixed
Enter, and ultrasonic disperse again after 55 DEG C of stirred in water bath 60min.Mixed solution is sealed respectively be placed in tetraethyl orthosilicate/
Each aging 24h in dehydrated alcohol mixed liquor, aging temperature are 50 DEG C, carry out solvent displacement to substitute residual fraction second with normal hexane
Alcoholic solvent.Add the trim,ethylchlorosilane for accounting for pluralgel quality 15% to the process of pluralgel modifying surface, wherein change
Property temperature and time be respectively 49 DEG C and 12h.The gel is placed in 60 DEG C of baking ovens and is dried to constant weight, phase transition temperature is obtained for 18.2
The CA-MA-PA/ silicon dioxide composite phase-change materials of DEG C latent heat for 58.0J/g.
Embodiment 8
First, capric acid (CA), myristic acid (MA) and Palmic acid (PA) are weighed respectively according to 1 using electronic balance:0.4:
0.2 eutectic quality carries out proportioning, adds and covers in test tube after the complete melting mixing of rubber stopper seal thing to be mixed in 60 DEG C of water
Heating 30min and then ultrasonic disperse in bath.Tetraethyl orthosilicate, dehydrated alcohol and deionized water are according to TEOS:H2O:EtOH=
1:4:After 8 ratio mixing, hydrochloric acid is added to adjust pH value of solution to 3, and uniform through magnetic stirrer (rotating speed is 380r/min)
Stirring 28min.Add weak ammonia adjustment reaction system pH to 7, the LA-MA-PA ternary eutectic thing fatty acids of molten state are mixed
Enter, and ultrasonic disperse again after 55 DEG C of stirred in water bath 60min.Mixed solution is sealed respectively be placed in tetraethyl orthosilicate/
Each aging 24h in dehydrated alcohol mixed liquor, aging temperature are 50 DEG C, carry out solvent displacement to substitute residual fraction second with normal hexane
Alcoholic solvent.The normal hexane for accounting for pluralgel quality 15% is added to the process of pluralgel modifying surface, wherein modification temperature
49 DEG C and 12h are respectively with the time.The gel is placed in 60 DEG C of baking ovens and is dried to constant weight, phase transition temperature is obtained for 18.0 DEG C of latent heat
CA-MA-PA/ silicon dioxide composite phase-change materials for 60.0J/g.
Relevant parameter and test result are as shown in table 1.
Claims (7)
1. a kind of ternary aliphatic acid-silicon dioxide is combined the preparation method of qualitative phase-change material, and which comprises the following steps that：
(1) three kinds of long-chain fatty acid are weighed according to the ratio of calculating and added in container, after stoppering rubber stopper seal, be placed in 50～60 DEG C
Heat 25-30min in water-bath, ultrasonic disperse after the complete melting mixing of thing to be mixed, so as to obtain ternary eutectic thing fatty acid,
It is then placed in standby in baking oven；
(2), after mixing in proportion presoma, dehydrated alcohol and deionized water, pH of mixed is adjusted between 3～4,
And stirred by magnetic stirrer；
(3) subsequently reaction system pH is adjusted to 6～8, the ternary eutectic thing fatty acid of molten state is mixed into, and is stirred in water-bath
Ultrasonic disperse again after mixing；
(4) above-mentioned mixed solution is sealed respectively and is placed in aging 24-28h in dehydrated alcohol, temperature control at 48-50 DEG C, with just oneself
Alkane carries out solvent displacement；
(5) add modifying agent to the process of pluralgel modifying surface, then the gel is placed in baking oven and is dried to constant weight, most
Ternary aliphatic acid-silicon dioxide composite phase-change material is obtained eventually.
2. preparation method according to claim 1, it is characterised in that the long-chain fatty acid described in step (1) is triplet
System, concrete proportioning are as follows：The mass ratio of capric acid-lauric acid-myristic acid is 1：(0.5-0.6)：(0.3-0.4), capric acid-Laurel
The mass ratio of acid-Palmic acid is 1：(0.5-0.6)：(0.1-0.2), the mass ratio of capric acid-myristic acid-Palmic acid is 1：
(0.3-0.4)：(0.2-0.25), the mass ratio of lauric acid-myristic acid-Palmic acid is 1：(0.6-0.7)：(0.3-0.4).
3. preparation method according to claim 1, it is characterised in that the presoma described in step (2) is positive silicic acid tetrem
Ester；Presoma：Dehydrated alcohol：Deionized water is according to 1:(4～6):The mass ratio mixing of (6～8)；Magnetic stirrer rotating speed is
350-400r/min, mixing time are 28-30min.
4. preparation method according to claim 1, it is characterised in that the bath temperature described in step (3) is 55-60 DEG C,
Mixing time is 55-60min.
5. preparation method according to claim 1, it is characterised in that ternary aliphatic acid system volume is phase transformation in step (3)
The 40-65% of quality of materials.
6. preparation method according to claim 1, it is characterised in that the modification temperature described in step (5) is 48-50 DEG C,
Modification time is 10-12h；Described oven temperature is 55-60 DEG C.
7. preparation method according to claim 1, it is characterised in that the modifying agent is trim,ethylchlorosilane or normal hexane
In one kind, modifying agent incorporation for pluralgel quality 10～15%.
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