CN106582565A - Composite adsorbing material for comprehensively regulating environmental humiture and preparing method thereof - Google Patents
Composite adsorbing material for comprehensively regulating environmental humiture and preparing method thereof Download PDFInfo
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- CN106582565A CN106582565A CN201611039843.8A CN201611039843A CN106582565A CN 106582565 A CN106582565 A CN 106582565A CN 201611039843 A CN201611039843 A CN 201611039843A CN 106582565 A CN106582565 A CN 106582565A
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- adsorption material
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- humidity
- polyethylene glycol
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- 239000000463 material Substances 0.000 title claims abstract description 78
- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 230000001105 regulatory effect Effects 0.000 title claims abstract 5
- 230000007613 environmental effect Effects 0.000 title claims abstract 3
- 238000000034 method Methods 0.000 title claims description 15
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 68
- 238000001179 sorption measurement Methods 0.000 claims abstract description 50
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 44
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 44
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 11
- 239000011159 matrix material Substances 0.000 claims abstract description 10
- 239000011258 core-shell material Substances 0.000 claims abstract description 6
- 238000001694 spray drying Methods 0.000 claims abstract description 6
- 230000033228 biological regulation Effects 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- JNYAEWCLZODPBN-JGWLITMVSA-N (2r,3r,4s)-2-[(1r)-1,2-dihydroxyethyl]oxolane-3,4-diol Chemical compound OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O JNYAEWCLZODPBN-JGWLITMVSA-N 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 125000003827 glycol group Chemical group 0.000 claims description 2
- 229950008882 polysorbate Drugs 0.000 claims description 2
- 229920000136 polysorbate Polymers 0.000 claims description 2
- 230000001276 controlling effect Effects 0.000 claims 2
- 238000001035 drying Methods 0.000 claims 2
- 239000007970 homogeneous dispersion Substances 0.000 claims 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims 1
- 230000007928 solubilization Effects 0.000 claims 1
- 238000005063 solubilization Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 8
- 238000007791 dehumidification Methods 0.000 abstract description 6
- 239000002114 nanocomposite Substances 0.000 abstract description 6
- 238000000151 deposition Methods 0.000 abstract description 5
- 239000007791 liquid phase Substances 0.000 abstract description 5
- 238000003860 storage Methods 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 230000008021 deposition Effects 0.000 abstract 1
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 39
- 238000012360 testing method Methods 0.000 description 10
- 229920002594 Polyethylene Glycol 8000 Polymers 0.000 description 9
- 230000008859 change Effects 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000012071 phase Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- DTPCFIHYWYONMD-UHFFFAOYSA-N decaethylene glycol Chemical compound OCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO DTPCFIHYWYONMD-UHFFFAOYSA-N 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000012782 phase change material Substances 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000009825 accumulation Methods 0.000 description 4
- 230000002829 reductive effect Effects 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 229910052927 chalcanthite Inorganic materials 0.000 description 2
- UGWKCNDTYUOTQZ-UHFFFAOYSA-N copper;sulfuric acid Chemical compound [Cu].OS(O)(=O)=O UGWKCNDTYUOTQZ-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000003230 hygroscopic agent Substances 0.000 description 2
- 230000002977 hyperthermial effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 239000004113 Sepiolite Substances 0.000 description 1
- -1 Sodium alkyl benzene Chemical class 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000004500 asepsis Methods 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 239000004064 cosurfactant Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000001507 sample dispersion Methods 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000004781 supercooling Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0281—Sulfates of compounds other than those provided for in B01J20/045
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24F—AIR-CONDITIONING; AIR-HUMIDIFICATION; VENTILATION; USE OF AIR CURRENTS FOR SCREENING
- F24F3/00—Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems
- F24F3/12—Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems characterised by the treatment of the air otherwise than by heating and cooling
- F24F3/14—Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems characterised by the treatment of the air otherwise than by heating and cooling by humidification; by dehumidification
- F24F3/1411—Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems characterised by the treatment of the air otherwise than by heating and cooling by humidification; by dehumidification by absorbing or adsorbing water, e.g. using an hygroscopic desiccant
- F24F3/1423—Air-conditioning systems in which conditioned primary air is supplied from one or more central stations to distributing units in the rooms or spaces where it may receive secondary treatment; Apparatus specially designed for such systems characterised by the treatment of the air otherwise than by heating and cooling by humidification; by dehumidification by absorbing or adsorbing water, e.g. using an hygroscopic desiccant with a moving bed of solid desiccants, e.g. a rotary wheel supporting solid desiccants
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
本发明公开了一种综合调控环境温湿度的复合吸附材料及其制备方法。本发明结合喷雾干燥技术与原位液相沉积技术制得以聚乙二醇作为外壳包覆球形硫酸铜纳米基质的核壳结构纳米复合吸附材料。该材料能够实现环境温度与湿度的综合调控，相比现有技术中热湿材料，本发明提高了吸收速率，能够更快的达到吸附平衡，并且本发明复合吸附材料在保持原有除湿水平的基础上，提高了热储存容量。本发明合成途径简单，制得复合吸附材料环保无毒，并且结构稳定，在制作建筑围护结构以及除湿工程等领域具有巨大的潜力。此外，本发明纳米复合吸附材料能够利用低品位热能作为驱动力实现其商业运用，因此是一类节能、环保、高效的工程材料。
The invention discloses a composite adsorption material for comprehensively regulating the temperature and humidity of the environment and a preparation method thereof. The invention combines the spray drying technology and the in-situ liquid phase deposition technology to prepare the core-shell structure nano-composite adsorption material which uses polyethylene glycol as the outer shell to coat the spherical copper sulfate nano-matrix. The material can realize the comprehensive control of ambient temperature and humidity. Compared with the heat-humidity materials in the prior art, the present invention improves the absorption rate and can reach the adsorption balance faster, and the composite adsorption material of the present invention maintains the original dehumidification level. On the basis of this, the thermal storage capacity is improved. The synthesis method of the invention is simple, and the prepared composite adsorption material is environmentally friendly and non-toxic, and has a stable structure, and has great potential in the fields of making building enclosure structures, dehumidification engineering and the like. In addition, the nanocomposite adsorption material of the present invention can use low-grade thermal energy as a driving force to realize its commercial application, so it is a kind of energy-saving, environmental protection and high-efficiency engineering material.
Description
Technical field
The present invention relates to a kind of nano combined absorption with core shell structure for being capable of comprehensive regulation environment temperature and humidity
Material and preparation method thereof.
Background technology
As social economy constantly develops, people to living environment, working environment or even public building environment (waiting room,
Parking lot, subway etc.) requirement of control of temperature and humidity increasingly improves.In order to look for new regulation and control method, there is scholar to propose phase
Become temperature control material and prepare the technological approaches for forming new material with except wet stock is mutually combined.This composite material --- heat is wet compound
Material (endothermal-hygroscopic material) can realize that system is long using low-grade heat energy as driving force
Long Reversible Cycle.
However, at present also there is following subject matter in this composite material that can realize temperature and humidity control：Composite adsorption
Phase-change material inevitably reduces the contact area of hygroscopic agent and humid air in material, and this will cause hydrone in hygroscopic material
Mass transfer path in material is obstructed, and then reduces the rate of adsorption and quality of adsorption.For example, Fang Guiyin is by SiO2With diatomite conduct
Moisture absorption host material, is prepared for that the hot wet composite of temperature and humidity can be controlled using dissolving-gel method.And the composite wood
Material reached the time of equilibrium adsorption more than 48 hours.In addition, also scholar using sepiolite as host material, the heat of preparation
The wet composite only adsorbance with 1.2～2.1g/100g.In the prior art, usually through increase hygroscopic agent content with
The equilibrium adsorption capacity of compound adsorbent is improved, however, this method considerably reduces the storage density of hot wet composite.Example
Such as the composite only latent heat of phase change with 19J/g of Chen reports, the 10～15% of pure phase-change material latent heat are only accounted for, it is impossible to send out
Wave the accumulation of heat temperature control advantage of phase-change material.
The content of the invention
In view of mentioned above, the technical problem to be solved is to provide one kind can be to closing, semiclosed environment
Interior temperature and humidity carries out NEW TYPE OF COMPOSITE sorbing material of Comprehensive Control and preparation method thereof.Specifically, based on by except moist wood
The material theory so as to reach comprehensive regulation environment temperature and humidity compound with phase-change material, the present invention combine spray drying technology with
Liquid-phase deposition technique in situ is obtained using polyethylene glycol and is answered as the nuclear shell structure nano that shell coats spherical copper sulphate nanomatrix
Close sorbing material.For achieving the above object, the present invention is adopted the following technical scheme that：
One aspect of the present invention discloses a kind of composite adsorbing material of comprehensive regulation ambient temperature and humidity, the composite adsorbing material
It is the Core-shell structure material with spherical copper sulphate nanomatrix as kernel, with polyethylene glycol as shell.
Further, the particle diameter of the copper sulphate nanomatrix is 50～500nm, and the polyethylene glycol forms the thickness of shell
Spend for 5～30nm.
Another aspect of the present invention discloses a kind of preparation method of the composite adsorbing material of comprehensive regulation ambient temperature and humidity, including
Following steps：
Step A：Compound concentration is the copper-bath of 0.05～0.3g/ml, and in the copper-bath surface is added
Activity is well mixed, and obtains mixed solution；The mixed solution is carried out into hyperthermic treatment, is then prepared by dried process spherical
Copper sulphate nanomatrix；
Step B：Polyethylene glycol is dissolved in ethanol solution homogeneous dispersing liquid is obtained, be then obtained step A
Spherical copper sulphate nanomatrix be dispersed in the homogeneous liquid, obtain suspension；The suspension is passed through into rotary distillation
The composite adsorbing material with spherical copper sulphate nanomatrix as kernel, with polyethylene glycol as shell is obtained.
Further, it is specific surface energy of the reduction copper-bath in dry run, helps copper sulphate to shrink globulate brilliant
Body, the mass fraction of surfactant is 0.1～5% in the mixed solution of step A of the present invention, and the surfactant is 12
Sodium alkyl benzene sulfonate, cetyl trimethylammonium bromide, fatty acid sorbitan and polysorbate.
Further, in order to increase surfactant solubility, to form more micellas evenly, step A of the present invention
Also include the temperature control of mixed solution in 30～60 DEG C.
Further, because spray drying treatment is simple to operate, nano material purity height, yield is obtained greatly and pattern can
Control, dried process is preferably spray drying treatment in step A of the present invention, and design parameter is as follows：Inlet temperature is 120～200 DEG C,
Feed rate is 100～1500ml/h.
Further, the environment temperature that homogeneous dispersing liquid is prepared in step B of the present invention is 50～80 DEG C.
Further, it is that so that obtained composite adsorbing material has suitable structure, a composition, step B of the present invention is hanged
Polyethylene glycol and copper sulphate mass ratio are polyethylene glycol: copper sulphate=1: 1～19 in turbid liquid.
Further, suspension carried out into rotary distillation in step B of the present invention so that ethanol evaporation, and then by poly- second two
Alcohol is deposited on spherical copper sulphate nanomatrix surface, it is preferable that the temperature of rotary evaporation is 80～110 DEG C.
The present invention is that copper sulphate is dissolved in water using surfactant purpose when copper-bath is dried
Form cupric sulfate pentahydrate (CuSO4·5H2O), cupric sulfate pentahydrate (CuSO4·5H2O) nanomatrix can be due in hot environment
Dehydration presents fairly obvious volume contraction, and the surface energy of sulfuric acid copper nanocrystallite is higher obtained from, easily causes copper sulphate
It is nanocrystalline diauxic growth occur, and use surfactant to reduce specific surface energy of the liquid in dry run, help sulphur
Sour copper shrinks globulate.During composite adsorbing material is prepared, the ethanol that can move freely, peg molecule play table
The role of face activating agent and cosurfactant.This has been greatly reduced the surface energy of sulfuric acid copper nanocrystallite, and then causes sulphur
The high-specific surface area of sour copper nanocrystallite is retained.Therefore, it is disclosed by the invention with spherical copper sulphate nanomatrix as kernel, with
Polyethylene glycol (PEG) is nuclear shell structure nano composite adsorbing material (the referred to as CuSO of shell4The nano combined adsorption materials of/PEG
Material) there is high inner boundary.These inner boundaries can be converted into temperature adjusting and humidity regulation this parameter to contradiction mutually
The parameter of optimization.According to embodiments of the present invention, for adsorption property, inner boundary changes polyethylene glycol (PEG) clad
Molecule so that the equilibrium adsorption capacity of PEG shells improves 40～200 times relative to pure PEG powders.So,
PEG shells can be formed " impoundment effect " so that copper sulphate quickly can obtain water from water enrichment area with the vapor in enriched air
Molecule further causes the compound adsorbent performance of the rate of adsorption or even adsorbance of composite adsorbing material of the present invention than having reported
It is excellent.
For composite adsorbing material phase transition performance of the present invention, according to the specific embodiment of the invention, in capillary work
With under, the crystallization temperature of PEG shells can freely be adjusted in the range of 9 DEG C, meanwhile, its melt temperature keeps constant.This means
The degree of supercooling of composite adsorbing material can be adjusted freely.
For the stability of composite adsorbing material, according to the specific embodiment of the invention, in the presence of PEG shells, energy
The Volume Changes of copper sulphate matrix are enough limited, and during adsorption/desorption is attached, presents stable micro-structural.
Compared to existing technology, the invention has the advantages that：
1st, composite adsorbing material disclosed by the invention can not only realize the comprehensive regulation of environment temperature and humidity, and solve
Having determined in absorption type accumulation of energy dehumidification system sorbing material cannot be while realizes the problem of accumulation of energy and dehumidifying matching, compared to existing technology
Middle hot wet stock, the present invention improves absorption rate, can faster reach adsorption equilibrium, and composite adsorbing material of the present invention
On the basis of original dehumidification level is kept, thermmal storage capacity is improve.
2nd, the composite adsorbing material that the present invention is provided can be using low-grade heats such as solar energy, waste heat of plant, vehicle exhausts
Can realize that it is commercially used as driving force, therefore be the potential engineering material of a class.
3rd, route of synthesis of the present invention is simple, and composite adsorbing material environment-protecting asepsis, and Stability Analysis of Structures is obtained, therefore is making
Energy-storing wall board material, gypsum material are applied to architectural exterior-protecting construction and are applied to dehumidification engineering field has huge potentiality.
Description of the drawings
Fig. 1 is CuSO prepared in the embodiment of the present invention 14The SEM spectrum of -1% copper sulphate nanomatrix.
Fig. 2 is the SEM spectrum of anhydrous cupric sulfate nanomatrix prepared in the embodiment of the present invention 2.
Fig. 3 is CuSO obtained in the embodiment of the present invention 34/ PEG8000-10%, CuSO4/ PEG8000-20% and CuSO4/
PEG8000-30% nano composite adsorption materials adsorb bent obtained by testing in the environment that temperature is 25 DEG C, relative humidity is 80%
Line.
Fig. 4 is that the embodiment of the present invention 4 prepares CuSO4/ PEG8000-10%, CuSO4/ PEG8000-20% and CuSO4/
The DSC curve of PEG8000-30% nano composite adsorption materials.
Fig. 5 is the stability experiment of composite adsorbing material of the present invention, wherein, Fig. 5 (a) and (a) ' be respectively to pure poly- second two
Alcohol (PEG8000) and CuSO4/ PEG-X% (X%=10,20 with 30) composite adsorbing material carry out OM before and after hyperthermic treatment into
As figure；Fig. 5 (b) and (b) ' be respectively to spontaneously dry cupric sulfate pentahydrate solution are obtained product (CSW), CuSO4/ SDBS1% and
CuSO4/ PEG 10% carries out carrying out micro-structural test result figure after adsorption treatment.
Specific embodiment
With reference to embodiments the present invention is described in detail with Figure of description, wherein CuSO in Figure of description4
It is abbreviated as CS：
Embodiment 1：
The present embodiment prepares copper sulphate nanomatrix, and concrete operations are as follows：
20g anhydrous slufuric acid copper powders are weighed, in being dissolved in the distilled water of 100ml, blueness copper sulfate solution is obtained；Xiang Rong
0.2g neopelexes (SDBS) are added in liquid, solution are heated to into 50 DEG C, and stirred using magnetic agitation instrument,
Obtain mixed solution；Above-mentioned mixed solution is carried out into spray drying treatment, spherical copper sulphate nanomatrix is obtained, will in the present invention
It is named as CuSO4- 1% nanomatrix.
Fig. 1 is that the present embodiment is obtained CuSO4The SEM spectrum of -1% nanomatrix, it can be seen from SEM spectrum, CuSO4- 1%
Sample is rendered as medicine ball of the particle diameter distribution at 0.5～2 μm, it can be seen from general knowledge as well known to those skilled in the art, above-mentioned test
As a result CuSO is shown4- 1% nanomatrix is very good adsorbing base.
Embodiment 2：
The present embodiment prepares three kinds of different anhydrous cupric sulfate nanomatrixes using different technologies means：
Weigh the embodiment of the present invention 1 and CuSO is obtained4- 1% sample 30g, and it is divided into three equal parts, it is respectively designated as CuSO4-
1%A samples, CuSO4- 1%B samples and CuSO4- 1%C samples；By CuSO4- 1%A samples are directly placed at 110 DEG C of high temperature rings
It is dried in border, products obtained therefrom is named as CuSO4-A；By CuSO4- 1%B sample dispersions are steamed in 30ml absolute ethyl alcohols using rotation
Method is evaporated, is dried between 80～110 DEG C, products obtained therefrom is named as CuSO4-B；1.11gPEG8000 polymer is added
In 30ml absolute ethyl alcohols, and it is heated to 60 DEG C, treats that PEG8000 polymer is completely dissolved, then by CuSO4- 1%C samples are added in
In above-mentioned solution, using rotary distillation method, it is dried between 80～110 DEG C, products obtained therefrom is named as CuSO4/
PEG8000-C, CuSO in the present embodiment4The preparation of/PEG8000-C samples is to adopt liquid-phase deposition technique.
Fig. 2 is the SEM spectrum of three kinds of anhydrous cupric sulfate nanomatrixes prepared by this enforcement, it can be seen from SEM test results,
CuSO4It is 0.5～5 μm of hollow ball that-A is rendered as particle diameter, and the copper sulphate primary particle for constituting these hollow balls occurs substantially
Reunite.Thus speculate, copper sulphate is placed in alcoholic solution, the structure of micron ball can be kept.But, constitute the one of hollow ball
There is crystal growing process in secondary particle.This is decreased obviously the specific surface area for causing it.CuSO4- B samples be by it is substantial amounts of once
Particle aggregation is formed, and the particle diameter of these nano-particles is between 50～200nm.By contrast, CuSO4/ PEG8000-C samples have
There is outstanding microscopic appearance, it had both remained the structure (particle diameter is 0.5～2 μm) of copper sulphate matrix solid micron ball, retained again
The structure of copper sulphate primary particle (particle diameter is 5～50nm).Therefore, CuSO4/ PEG8000-C samples have boundary in greatly
Face, it is ensured that it has excellent accumulation of heat wet-out property.
Embodiment 3：
With reference to described in the present embodiment 2, the composite sample with core shell structure is prepared using liquid-phase deposition technique.Composite sample
In, CuSO4- 1% is respectively 9 with the mass ratio of PEG8000：1、8：2 and 7：3, and it is respectively designated as CuSO4/PEG8000-
10%th, CuSO4/ PEG8000-20% and CuSO4/ PEG8000-30%；Then three kinds of composite samples are placed in 25 DEG C of environment
Adsorption and dehumidification is carried out, adsorption curve as shown in Figure 3 is obtained, wherein it is gained test under 80% environment that figure (a) is relative humidity
Curve, it is gained test curve under 50% environment that figure (b) is relative humidity.
It can be seen from test result, when the relative humidity of environment is 80%, CuSO4- 1%, CuSO4/PEG8000-
10%th, CuSO4/ PEG8000-20% and CuSO4The equilibrium adsorption capacity of/PEG8000-30% is respectively 39.8g/100g, 38.5g/
100g, 37.5g/100g and 35.6g/100g；According to following prediction equation：
Wherein, FTAnd FCSRespectively composite sample and pure CuSO4Equilibrium adsorption capacity of -1% sample under equivalent environment, it is single
Position is g/100g；β is the quality ratio of copper sulphate matrix in composite sample.
According to reckoning, PEG 8000 (PEG8000) shell take part in adsorption process in the present embodiment, its adsorbance
(with FPEGRepresent) 27g/100g is reached, improve 44 times compared to pure polyethylene glycol.
In the same manner, PEG8000 shells equilibrium adsorption capacity when relative humidity is 50% is in the present embodiment composite sample
15.8g/100g, compared to pure PEG polymer 188 times are improve.
It can be seen from result above, the absorption property of polyethylene glycol (PEG) shell is substantially optimised.In adsorption process,
Polyethylene glycol (PEG) shell can with the vapor in enriched air, formed " impoundment effect " so that copper sulphate matrix can quickly from
Water enrichment area obtains hydrone, and then causes CuSO of the present invention4The rate of adsorption of/PEG nano composite adsorption materials is optimised.Root
Understand according to adsorption curve shown in Fig. 3, pure CuSO4- 1% sample reaches flat under the conditions of relative humidity is respectively 80% and 50%
The time of weighing apparatus absorption is respectively 9 hours and 15 hours.And under equivalent environment, CuSO of the present invention4The nano combined adsorption materials of/PEG
Expect that the time for being up to equilibrium adsorption has shortened to 4 hours and 5 hours.
Embodiment 4：
The present embodiment is obtained CuSO with reference to described in the present embodiment 2 using liquid-phase deposition technique4/ PEG-5% samples, CuSO4/
PEG-10% samples, CuSO4/ PEG-17.5% samples, CuSO4/ PEG-20% samples and CuSO4/ PEG-30% samples, then
Using the phase transition temperature and latent heat of the prepared composite adsorbing material of differential scanning calorimetric analysis (DSC) the technical testing present invention.
According to Fig. 4 test results, such as shown in figure (a), the latent heat of composite adsorbing material of the present invention is then with polyethylene glycol
(PEG) shell content increases and is stepped up.As shown in figure (b), the melting temperature of polyethylene glycol (PEG) shell is without substantially change
Change, this represents the change of its crystal structure and functional group for its endothermic process has not significant impact, meanwhile, according to figure (c)
Shown, the crystallization temperature of polyethylene glycol (PEG) shell can fluctuate in 37.2～46.3 DEG C of scopes.This shows present invention preparation
The phase transition temperature of composite adsorbing material has Modulatory character.
Embodiment 5：
The present embodiment is to PEG8000, CuSO4/ PEG-10%, CuSO4/ PEG-20% and CuSO4/ PEG-30% samples exist
Temperature is contrasted for optical microphotograph collection of illustrative plates is respectively adopted before and after heating under the conditions of 75 DEG C, is illustrated in figure 5 this embodiment institute
Result figure is obtained, according to Fig. 5 (a) and Fig. 5 (a) ' contrasts as can be seen that before heating PEG8000 is rendered as gill shape, after the heating
Due to it is capillary effect be reduced into it is spherical；And by these three materials of CS/PEG-10%, CS/PEG-20% and CS/PEG-30%
Material is exposed in hot environment, and their structure is without substantially change.This means that polyethylene glycol can be limited by matrix, from
And resist the alteration of form of surface tension induction.Therefore, CS/PEG composites are sizing phase-change material.
In order to further verify the stability of composite adsorbing material of the present invention, the present embodiment is by cupric sulfate pentahydrate (CuSO4·
5H2O) solution is directly slow in atmosphere is dried prepared products C SW and CuSO4/ SDBS 1% and CuSO4/ PEG-10% samples
Temperature is placed in for 25 DEG C, relative humidity be 60% environment in carry out within 12 hours adsorption experiment, and before above-mentioned adsorption treatment
Test the morphosis of each sample respectively afterwards as a comparison, this embodiment acquired results figure is illustrated in figure 5, according to Fig. 5 (b)
(b) ' contrast is as can be seen that CSW presents obvious volumetric expansion, CSW after rough estimate adsorption treatment after adsorption treatment
Volumetric expansion exceeded 20%；CuSO4The volumetric expansions after adsorption treatment of/SDBS 1% are reduced to 10%, and stromal surface
It is coated with the composite adsorbing material of PEG shells, i.e. CuSO4Volume Changes of/the PEG-10% after adsorption treatment are less than 2%；
According to above-mentioned experimental result, core shell structure composite adsorbing material presents extremely stable microstructure.
Embodiment 6：
Table 1 below is the solidification temperature of the hot wet composite and embodiment of the present invention composite adsorbing material reported at present
Degree, latent heat and water absorption these three performance parameters contrasts：
With reference to above example as can be seen that as the content of PEG8000 in composite adsorbing material of the present invention increases from 0%
To 30%, the water absorption of composite adsorbing material is only reduced to 35.6g/100g from 39.8g/100g, and original moisture absorption is kept substantially
Level；However, the energy storage density of the latent heat of phase change of composite adsorbing material is rapidly increased to 48.3J/g from 0J/g.
As it can be seen from table 1 the equilibrium adsorption capacity of existing hot wet composite is less than 10g/100g, the balance of this level
Adsorbance is low, by contrast, the CuSO that the present invention is provided4/ PEG composite adsorbing materials illustrate more excellent comprehensive
Energy.
The principle and its effect of above-described embodiment only illustrative present invention, it is of the invention not for limiting.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and the scope without prejudice to the present invention to above-described embodiment.Cause
This, such as those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
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| CN110280225A (en) * | 2019-05-05 | 2019-09-27 | 天津大学 | A kind of resin sorbent and its preparation method and application wrapping up phase-change energy storage capsule |
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