CN108102613A - A kind of anti-mildew organic composite shaping phase-change material and preparation method thereof - Google Patents
A kind of anti-mildew organic composite shaping phase-change material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of anti-mildew organic composite shaping phase-change materials and preparation method thereof, belong to new material technology field.A kind of anti-mildew organic composite shaping phase-change material, the material are made of coordination cross-linked network macromolecule, organic solid-liquid phase change material, antiseptic and preservative, wherein, by mass percentage, coordination cross-linked network macromolecule：1~50%, organic solid-liquid phase change material：44~98.8%, antiseptic 0.01~3%, mould inhibitor 0.01~3%, wherein, coordination cross-linked network macromolecule is complexed by high-molecular compound and metallic ion coordination.Synthesis technology of the present invention is simple, and using conveniently, the material phase transformation enthalpy is big, has excellent shaping effect, the liquid phenomenon of leakage will not occur during operation.The materials synthesis is simple for process, using conveniently, has broad application prospects in thermal energy storage and management domain.
Description
Technical field
The present invention relates to a kind of anti-mildew organic composite shaping phase-change materials and preparation method thereof, belong to new material technology
Field.
Background technology
Phase-change accumulation energy can by physics phase transition (solid-liquid, liquid-gas etc.) process, absorb or release amount of heat from
And realize energy stores and utilize that there is the advantages of energy storage density is big, and energy storage capacity is strong, it can effectively alleviate space in energy supply
With the time it is unbalance conflict, be one of the effective means for improving energy utilization efficiency.Wherein organic solid-liquid phase change material is due to it
Cheap cost, larger phase transformation enthalpy and smaller surfusion become the research hotspot in current phase transformation field.
But organic solid-liquid phase change material there is also it is notable the problem of, solid-liquid transformation in phase transition process exists serious
Leakage problem influence its application.And organic phase change material and backing material bio-toxicity are low, have gone mouldy.It is organic to solve
Solid-liquid phase change material there are the problem of, which introduces coordination cross-linked network macromolecule makes its setting as backing material, setting
Required backing material is few, enthalpy is influenced low；It introduces antiseptic and mould inhibitor realizes its anti-mildew performance.
The content of the invention
To solve problems of the prior art, the present invention provides a new class of anti-mildew organic composite fixed phase change material
Material and preparation method thereof.Anti-mildew organic composite shaping phase-change material anti-mildew prepared by the present invention can significantly improve same
When, also with larger phase transformation enthalpy and excellent shaping effect, the leakage of course of work no liquid.Such materials synthesis technique
Simply, available for practical application, have broad application prospects in thermal energy storage with the fields such as utilizing.
Technical scheme is as follows：
A kind of anti-mildew organic composite shaping phase-change material, the material is by coordination cross-linked network macromolecule, organic solid liquid phase
Become material, antiseptic and preservative to form, wherein, by mass percentage,
Coordination cross-linked network macromolecule：1~50%
Organic solid-liquid phase change material：44~98.8%
Antiseptic 0.01~3%
Mould inhibitor 0.01~3%,
Wherein, coordination cross-linked network macromolecule is complexed by high-molecular compound and metallic ion coordination.
In the above-mentioned technical solutions, the coordination cross-linked network macromolecule is by high-molecular compound and metallic ion coordination
It is complexed.
Preferably, the macromolecule is polyacrylic acid and its sodium, potassium or ammonium salt；Poly and its sodium, potassium or ammonium salt；Carboxylic
Methylcellulose and its sodium, potassium or ammonium salt；Sodium alginate, potassium or ammonium salt；Carboxymethyl starch and its sodium, potassium or ammonium salt；Polyethylene
Alcohol；Polyvinylpyrrolidone；Polyvinyl pyridine；Acid-co-maleic acid and its sodium, potassium or ammonium salt；Acrylic acid-methyl-prop
Olefin(e) acid copolymer and its sodium, potassium or ammonium salt；Methacrylic acid-maleic acid and its sodium, potassium or ammonium salt；It is above-mentioned high molecular
Molecular weight is 1000~9000000.
Above, by taking " polyacrylic acid and its sodium, potassium or ammonium salt " as an example, refer to high-molecular compound can be polyacrylic acid,
Sodium Polyacrylate, polyacrylic acid potassium or ammonium polyacrylate, other similar expression have identical meanings, repeat no more.
Preferably, the metal ion for calcium ion, magnesium ion, ferrous ion, ferric ion, zinc ion, aluminium from
Son, bivalent cupric ion, barium ions, trivalent chromic ion, cobalt ions or silver ion.
Further, the metal ion is provided by metal ion compound, the metal ion compound for calcium ion,
Magnesium ion, ferrous ion, ferric ion, zinc ion, aluminium ion, bivalent cupric ion, barium ions, trivalent chromic ion, cobalt from
The chloride of son or silver ion, oxide, nitric acid compound, hydrosulphate, acetic acid compound.
Further, the mass ratio of the metal ion compound and high-molecular compound is 1:100~30:100.
In above-mentioned technical proposal, organic solid-liquid phase change material is paraffin, aliphatic acid, fatty alcohol, polyethylene glycol, fat
At least one of fat acid esters.
In the above-mentioned technical solutions, the paraffin is paraffin of the fusing point at 8~60 DEG C；The aliphatic acid is certain herbaceous plants with big flowers acid, ten
One kind in diacid, tetradecylic acid, pentadecanoic acid, palmitic acid, stearic acid, two or three；The fatty alcohol is lauryl alcohol, 14
One kind in alcohol, hexadecanol, octadecyl alcolol, two or three；The polyethylene glycol is the polyethylene glycol of molecular weight 200~20000；
The grease is erythritol tetrastearate, four palmitate of erythritol, six palmitate of galactitol, galactitol six
Stearic acid, glyceryl tristearate, tripalmitin, three myristins, butyl stearate, soybean oil, corn oil,
One kind in peanut oil, rapeseed oil, olive oil, castor oil, two or three.
In the above-mentioned technical solutions, the antiseptic is the nano silver that grain size is 5~300nm, penicillin, cynnematin,
Vancomycin, fluorine quinoline promise cave, Aminoglycoside, polymyxins, tetracycline, chloramphenicol, macrolide, clindamycin, Enoxacin,
One kind in Ofloxacin, Pefloxacin, Ciprofloxacin, Lomefloxacin, two or three.
In the above-mentioned technical solutions, the mould inhibitor for dimethyl fumarate, diethyl fumarate and dibutyl fumarate,
Fumaric acid, benzoic acid, sodium benzoate, parachloroxylenol, salicylanilide and tetra-chloro-phenol, pentachlorophenol, sorbic acid and its salt, chlorine
Acetic acid, halogenated phenoxy acetic acid, alkyl thiocyanic acid, halogenated salicylic acid, thiosalicylic acid, chloric acid and its salt, sodium chlorite, permanganic acid
One or both of potassium, iodide, boric acid and its salt, sulphite and pyrosulfite, sodium nitrite.
The present invention also provides the preparation methods of above-mentioned anti-mildew organic composite shaping phase-change material, include the following steps：
High-molecular compound and solvent are prepared by mixing into uniform solution (mass fraction is 1%~20%), it will be organic
Solid-liquid phase change material, antiseptic and mould inhibitor are added in above-mentioned Polymer Solution, and 1~10h is stirred at 20~80 DEG C, are added in
The metal ion compound solution of the metal ion is capable of providing, vacuum drying for 24 hours, obtains organic composite fixed phase change material
Material.
In the above-mentioned technical solutions, the metal ion compound is calcium ion, magnesium ion, ferrous ion, ferric iron
Ion, zinc ion, aluminium ion, bivalent cupric ion, barium ions, trivalent chromic ion, the chloride of cobalt ions or silver ion, oxidation
Object, nitric acid compound, hydrosulphate, acetic acid compound are 1 with high molecular mass ratio:100~30:100.
Preferably, the solvent is one kind in water, benzene, toluene, DMF, DMSO, tetrahydrofuran, methanol, ethyl alcohol, acetone
Or two kinds.
Preferably, the concentration of the metal ion compound solution is 0.05mol/L.
Beneficial effects of the present invention：It, should the present invention provides a kind of new anti-mildew organic composite shaping phase-change material
Material phase transformation enthalpy is big, has excellent shaping effect, the liquid phenomenon of leakage will not occur during operation.The materials synthesis technique
Simply, using conveniently, have broad application prospects in thermal energy storage and management domain.
Description of the drawings
Fig. 1 is the infrared spectrogram of anti-mildew organic composite shaping phase-change material in embodiment 1, wherein：A, polyethylene glycol,
B, anti-mildew organic composite shaping phase-change material.
Fig. 2 is the DSC curve of anti-mildew organic composite shaping phase-change material in embodiment 1.
Fig. 3 is the shaping effect photo of anti-mildew organic composite shaping phase-change material in embodiment 1.
Specific embodiment
Following non-limiting examples can make those of ordinary skill in the art be more fully understood the present invention, but not with
Any mode limits the present invention.Test method described in following embodiments is conventional method unless otherwise specified；The examination
Agent and material unless otherwise specified, commercially obtain.
Embodiment 1
(1) 0.8889g sodium alginates are taken in three-necked flask, 80mL water is added in, stirs 30min at 70 DEG C, obtain seaweed
Acid sodium solution；
(2) adding the PEG-600 of 8g, (sodium alginate and polyethylene glycol mass ratio are 10:90), 0.05g is (in the material
Mass fraction 0.5%) tetracycline and 0.03g (mass fraction 0.3% in the material) dimethyl fumarate, continue to stir 30min,
Calcium chloride solution (0.05mol/L) is added dropwise to gel is formed, obtains compound calcium alginate gel；
(3) 40 DEG C of vacuum drying for 24 hours, obtain anti-mildew organic composite shaping phase-change material.
Anti-mildew organic composite shaping phase-change material prepared by embodiment 1 and it is not added with the organic of mould inhibitor and antiseptic
Composite shape-setting phase-change material is placed on simultaneously in 37 DEG C of environment, and blank control group is gone mouldy after 3 months, and prepared by embodiment 1
Anti-mildew organic composite shaping phase-change material without mildew phenomena.
Fig. 1 is the infrared spectrogram of anti-mildew organic composite shaping phase-change material in embodiment 1, wherein：A, polyethylene glycol
600, b, anti-mildew organic composite shaping phase-change material.In Fig. 1 as can be seen that infrared peak of composite material and polyethylene glycol ratio
Compared in 1026cm-1The C-O peaks of appearance belong to sodium alginate and the C-O-Ca-O-C structures formed after the crosslinking of Ca ion coordinations,
Demonstrate the coordination of sodium alginate and calcium ion.(Fig. 2) can be obtained from DSC curve, polyethylene glycol phase transformation enthalpy 161.3J/
G, anti-mildew organic composite shaping phase-change material phase transformation enthalpy are 115.0J/g, and 12.6 DEG C of phase transition temperature has larger phase transformation
Enthalpy.Anti-mildew composite shape-setting phase-change material and Macrogol 600 are placed on warm table, at 30 DEG C, polyethylene glycol has been
Start to melt, 45 DEG C of whens become liquid completely, and anti-mildew composite shape-setting phase-change material appearance is without significant change, Neng Goubao
Dimensionally stable is held, without the phenomenon of leakage (Fig. 3).Illustrate that there is the anti-mildew composite shape-setting phase-change material prepared good setting to imitate
Fruit.
Embodiment 2-4
The mass ratio of sodium alginate and polyethylene glycol (Mn=600) is changed to 50 respectively:50,25:75,5:95, obtain phase
The organic composite shaping phase-change material answered, other conditions are consistent with embodiment 1.Measurement result shows that is be prepared is anti-mildew
Organic composite shaping phase-change material has good shaping effect.
Embodiment 5-9
Using Sodium Polyacrylate, poly potassium, polyvinyl pyridine, carboxymethyl cellulose, polyvinyl alcohol as needing to be coordinated
High molecular material, obtain corresponding anti-mildew organic composite shaping phase-change material, other conditions are consistent with embodiment 1.
Embodiment 10-18
Magnesium chloride, frerrous chloride, iron chloride, zinc sulfate, aluminum nitrate, copper sulphate, barium chloride, silver nitrate, chromic acetate are made
For coordination of metal ion, corresponding anti-mildew organic composite shaping phase-change material is obtained, other conditions are consistent with embodiment 1.It surveys
Determine the results show that the anti-mildew organic composite shaping phase-change material being prepared has good shaping effect.
Embodiment 19-21
Using lauric acid/dodecanoic acid, palmitic acid, stearic acid as organic solid-liquid phase change material, obtain corresponding anti-mildew organic multiple
Shaping phase-change material is closed, other conditions are consistent with embodiment 1.Measurement result shows that the anti-mildew organic composite being prepared is determined
Shape phase-change material has good shaping effect.
Embodiment 22-25
Using lauryl alcohol, tetradecyl alchohol, hexadecanol, octadecyl alcolol as organic solid-liquid phase change material, the mixing of second alcohol and water is made
For solvent, the Polymer Solution mass fraction of preparation is 1%, obtains corresponding anti-mildew organic composite shaping phase-change material,
His condition is consistent with embodiment 1.Measurement result shows that the anti-mildew organic composite shaping phase-change material being prepared has good
Shaping effect.
Embodiment 26-31
By erythritol tetrastearate, six palmitate of galactitol, glyceryl tristearate, three palmitic acids
Ester, soybean oil, olive oil are respectively as organic solid-liquid phase change material, and DMF and water mixing are as solvent, the Polymer Solution of preparation
Mass fraction is 2%, obtains corresponding anti-mildew organic composite shaping phase-change material, and other conditions are consistent with embodiment 1.It measures
The results show that the anti-mildew organic composite shaping phase-change material being prepared has good shaping effect.
Embodiment 32-46
By grain size be 5~300nm nano silver, penicillin, cynnematin, vancomycin, fluorine quinoline promise cave, Aminoglycoside,
Polymyxins, chloramphenicol, macrolide, clindamycin, Enoxacin, Ofloxacin, Pefloxacin, Ciprofloxacin, Lome are husky
Star obtains corresponding anti-mildew organic composite shaping phase-change material, other conditions are consistent with embodiment 1 respectively as antiseptic.
Measurement result shows that the anti-mildew organic composite shaping phase-change material being prepared has good shaping effect.
Embodiment 47-61
By diethyl fumarate, fumaric acid, benzoic acid, sodium benzoate, parachloroxylenol, salicylanilide, pentachlorophenol,
Potassium sorbate, monoxone, chloro phenoxy acetic acid, sodium chlorite, potassium permanganate, potassium iodide, boric acid, sodium nitrite are respectively as anti-
Mould dose, corresponding anti-mildew organic composite shaping phase-change material is obtained, other conditions are consistent with embodiment 1.Measurement result shows,
The anti-mildew organic composite shaping phase-change material being prepared has good shaping effect.
Embodiment 62-64
The mass fraction of antibiotic is changed to 0.01%, 1%, 2% respectively, obtains corresponding anti-mildew organic composite setting
Phase-change material, other conditions are consistent with embodiment 1.Measurement result shows, the anti-mildew organic composite fixed phase change being prepared
Material has good shaping effect.
Embodiment 65-68
The mass fraction of mould inhibitor is changed to 0.03%, 0.5%, 1%, 2% respectively, is obtained corresponding anti-mildew organic multiple
Shaping phase-change material is closed, other conditions are consistent with embodiment 1.Measurement result shows that the anti-mildew organic composite being prepared is determined
Shape phase-change material has good shaping effect.
Claims (10)
1. a kind of anti-mildew organic composite shaping phase-change material, it is characterised in that：Composite shape-setting phase-change material is by coordination cross-linked net
Network macromolecule, organic solid-liquid phase change material, antiseptic and preservative form, wherein, by mass percentage,
Coordination cross-linked network macromolecule：1~50%
Organic solid-liquid phase change material：44~98.8%
Antiseptic 0.01~3%
Mould inhibitor 0.01~3%,
Wherein, coordination cross-linked network macromolecule is complexed by high-molecular compound and metallic ion coordination.
2. anti-mildew organic composite shaping phase-change material according to claim 1, it is characterised in that：The macromolecule is chemical combination
Object polyacrylic acid and its sodium, potassium or ammonium salt；Poly and its sodium, potassium or ammonium salt；Carboxymethyl cellulose and its sodium, potassium or ammonium
Salt；Sodium alginate, potassium or ammonium salt；Carboxymethyl starch and its sodium, potassium or ammonium salt；Polyvinyl alcohol；Polyvinylpyrrolidone；Polyethylene
Pyridine；Acid-co-maleic acid and its sodium, potassium or ammonium salt；Acrylic acid-methacrylic acid copolymer and its sodium, potassium or ammonium
Salt；Methacrylic acid-maleic acid and its sodium, potassium or ammonium salt；The molecular weight of above-mentioned high-molecular compound for 1000~
9000000。
3. anti-mildew organic composite shaping phase-change material according to claim 1, it is characterised in that：The metal ion is calcium
Ion, magnesium ion, ferrous ion, ferric ion, zinc ion, aluminium ion, bivalent cupric ion, barium ions, trivalent chromic ion,
Cobalt ions or silver ion.
4. anti-mildew organic composite shaping phase-change material according to claim 3, it is characterised in that：The metal ion is by gold
Belong to ionic compound provide, the metal ion compound for calcium ion, magnesium ion, ferrous ion, ferric ion, zinc from
Son, aluminium ion, bivalent cupric ion, barium ions, trivalent chromic ion, the chloride of cobalt ions or silver ion, oxide, nitrification
The mass ratio of object, hydrosulphate, acetic acid compound, the metal ion compound and high-molecular compound is 1:100~30:100.
5. anti-mildew organic composite shaping phase-change material according to claim 1, it is characterised in that：Organic solid-liquid phase change
Material is at least one of paraffin, aliphatic acid, fatty alcohol, polyethylene glycol, aliphatic ester.
6. anti-mildew organic composite shaping phase-change material according to claim 5, it is characterised in that：The paraffin exists for fusing point
8~60 DEG C of paraffin；The aliphatic acid is certain herbaceous plants with big flowers acid, lauric acid/dodecanoic acid, tetradecylic acid, pentadecanoic acid, palmitic acid, one kind in stearic acid, two
Kind or three kinds；The fatty alcohol for lauryl alcohol, tetradecyl alchohol, hexadecanol, one kind in octadecyl alcolol, two or three；The poly- second
Glycol is the polyethylene glycol of molecular weight 200~20000；The grease is erythritol tetrastearate, four palm of erythritol
Acid esters, six palmitate of galactitol, six stearic acid of galactitol, glyceryl tristearate, tripalmitin, three cardamoms
One kind in acid glyceride, butyl stearate, soybean oil, corn oil, peanut oil, rapeseed oil, olive oil, castor oil, two kinds or
Three kinds.
7. anti-mildew organic composite shaping phase-change material according to claim 1, which is characterized in that the antiseptic is：
Grain size be 5~300nm nano silver, penicillin, cynnematin, vancomycin, fluorine quinoline promise cave Aminoglycoside, polymyxins, four
In ring element, chloramphenicol, macrolide, clindamycin, Enoxacin, Ofloxacin, Pefloxacin, Ciprofloxacin, Lomefloxacin
One kind, two or three.
8. anti-mildew organic composite shaping phase-change material according to claim 1, which is characterized in that the mould inhibitor is：
Dimethyl fumarate, diethyl fumarate and dibutyl fumarate, fumaric acid, benzoic acid, sodium benzoate, parachloroxylenol,
Salicylanilide and tetra-chloro-phenol, pentachlorophenol, sorbic acid and its salt, monoxone, halogenated phenoxy acetic acid, alkyl thiocyanic acid, halogenated water
Poplar acid, thiosalicylic acid, chloric acid and its salt, sodium chlorite, potassium permanganate, iodide, boric acid and its salt, sulphite and Jiao Ya
One or both of sulfate, sodium nitrite.
9. the preparation method of the anti-mildew organic composite shaping phase-change material of claim 1~8 any one of them, feature exist
In：It the described method comprises the following steps：
High-molecular compound and solvent are prepared by mixing into uniform solution, mass fraction 1%-20%；By organic solid-liquid
Phase-change material, antiseptic and mould inhibitor are added in above-mentioned Polymer Solution, 1~10h are stirred at 20~80 DEG C, addition can
The metal ion compound solution of the metal ion is provided, vacuum drying for 24 hours, obtains organic composite shaping phase-change material.
10. the preparation method of anti-mildew organic composite shaping phase-change material according to claim 9, it is characterised in that described
Metal ion compound is the chloride of metal ion, oxide, nitric acid compound, hydrosulphate, acetic acid described in claim 4
Object.
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Cited By (3)
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| CN111269698A (en) * | 2020-03-02 | 2020-06-12 | 南通大学 | Acrylic polymer/fatty acid crosslinked solid-solid phase change material and preparation method thereof |
| CN111423857A (en) * | 2020-03-02 | 2020-07-17 | 南通大学 | Maleic anhydride copolymer/fatty acid crosslinked solid-solid phase change material and preparation method thereof |
| CN114940889A (en) * | 2022-05-25 | 2022-08-26 | 大连理工大学 | Composite phase change energy storage material with temperature-sensitive conductive characteristic and preparation method and application thereof |
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