CN107502310A - A kind of preparation method of magnesium sulfate/zeolite molecular sieve thermal energy storage material - Google Patents
A kind of preparation method of magnesium sulfate/zeolite molecular sieve thermal energy storage material Download PDFInfo
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Abstract
The invention belongs to a kind of preparation method of magnesium sulfate/zeolite molecular sieve thermal energy storage material of medium temperature heat accumulating preparing technical field.The magnesium sulfate/zeolite molecular sieve thermal energy storage material is pre-processed by distilled water to zeolite molecular sieve, open microporous molecular sieve, molecular sieve specific surface area is improved, is then prepared from the factor such as the Adlerika impregnated zeolite of different quality concentration, regulation and control dip time, drying temperature.Molecular sieve is pre-processed using distilled water, compared to corrosive solution, safety simple to operate and positive effects such as acid or alkali, reaction condition is gentle, and the raw material used are easy to get, safe and non-toxic, cheap, can be mass produced；The thermal energy storage material prepared simultaneously can recycle, and good economy performance, heat loss is few, be adapted to cross-season heat-storing, be a kind of preferably heat chemistry heat accumulating.
Description
Technical field
The invention belongs to medium temperature heat accumulating preparing technical field, more particularly to a kind of magnesium sulfate/zeolite molecular sieve is compound
The preparation method of heat accumulating.
Background technology
Solar energy, wind energy equal energy source are to use more renewable and clean energy resource, especially solar energy at present, very
It is multi-field to have obtained the development of comparative maturity.Photothermal complementary etc. is carried out using solar energy, can effectively reduce non-renewable energy resources
Consumption.And there is also periodicity, when summer, demand of the solar energy resources considerably beyond us for the utilization of solar energy；
Comparatively, it is insufficient for our living needs in temperature relatively low winter, solar energy resources.In order to solve solar cross
Seasonal periodicity utilizes, and is generally completed by energy storage technology.Conventional energy storage mode includes：Sensible heat energy storage, latent heat of phase change storage
Energy and heat chemistry energy storage, sensible heat heat accumulation are to improve own temperature by heat accumulating to carry out the storage of heat, heat storage
During, the rise of temperature will be limited by external condition, and storage density is small, and the space occupied is big, is not suitable for being used as across season
Save energy storage；Phase-change thermal storage technology, in current application than wide, research both at home and abroad in this respect at present is also compared more.Phase transformation
Heat-storage technology is that in phase transition temperature, possessed larger latent heat of phase change carries out the storage of heat using material, this method
Storage density is 5~10 times of sensible heat heat accumulation, but in actual applications, phase-change thermal storage can be by the shadow of material phase transformation temperature
Ring, there is certain limitation, the heat loss during phase-change thermal storage is also very important；Heat chemistry heat accumulation is that one kind is based on heat accumulation material
Material occurs chemical reaction and carries out the technology of energy stores release, wherein it is heat chemistry absorption/desorption reaction to have one kind, course of reaction
In, adsorbate directly contacts with adsorbent, requires no other media and transmits heat, storage density is high, and it is anti-that heat chemistry occurs
The temperature range scope answered is bigger, using low grade heat energy, suitable for cross-season heat-storing.Researcher has carried out correlation at present
Research, such as document Herbert Zondag, Benjamin Kikkert, Simon Smeding, Robert de Boer,
Marco Bakker.Prototype thermochemical heat storage with open reactor
In system.Applied Energy 109 (2013) 360-365, Energieonderazok Centrum Nederland is carried out to a large amount of hydration salt materials
Research and analyse, finally sum up MgSO4·7H2O、MgCl2·6H2O、CaCl2·2H2O、Al2(SO4)3·18H2Tetra- kinds of hydrations of O
Salt is more adapted to be used as heat chemistry heat accumulating；But when directly using hydrated salt as heat chemistry heat accumulating, due to hydration
Salt water imbibition is fabulous, easily forms compacted zone in hydrated salt surface moisture absorption deliquescence, prevents the salt of nexine from reacting, and then greatly
The thermal storage performance of material is influenceed, therefore from porous material as carrier, such as：The porous materials such as molecular sieve, vermiculite, silica gel and water
Close salt and be combined porous thermal energy storage material, i.e. heat chemistry energy storage material.Document Dong Ying is rich to wait [Dong Yingbo, vast stretch of wooded country, Liu Quan
Profit, chemical modification go to the influence of carbon, nitrogen pollutant in water removal, Sichuan University's journal (engineering science version) 5 (3) to zeolite
(2015):03-05] report, zeolite is modified using chemical method, by acetic acid, citric acid, sodium citrate, dodecane
6 kinds of base sodium sulfonate (SDS), sodium chloride, cetyl trimethylammonium bromide (HDTMA) differences it is inorganic organic chemistry modifying agent point
Do not mix with zeolite, by sodium hydrate regulator solution pH, mixed liquor is stirred using mixer, then it is dried
Processing, above-mentioned various inorganic/influences of the organic chemistry modifying agent to zeolite adsorption performance are studied, its preparation process is cumbersome, process
It is complicated.
The content of the invention
It is an object of the invention to provide a kind of preparation method of magnesium sulfate/zeolite molecular sieve thermal energy storage material, its feature
It is, comprises the following steps that：
(1) distilled water and zeolite molecular sieve are weighed, is pre-processed with distillation water retting zeolite molecular sieve, after dipping
Molecular sieve is put into drying box and is dried, and is subsequently cooled to room temperature, and taking-up is sealed；
(2) distilled water is mixed with anhydrous slufuric acid magnesium dust, configures the Adlerika of different quality concentration；
(3) the pretreated zeolite molecular sieve of step (1) is placed in step (2) Adlerika and impregnated, dipping is completed
Place at room temperature afterwards, be then placed in drying box and be dried, be sealed in dry conditions, magnesium sulfate/zeolite is made
Molecular sieve thermal energy storage material.
Zeolite molecular sieve described in step (1), (3) is 13X zeolite molecular sieves.
The mass ratio (1.1~3) of distilled water and zeolite molecular sieve in step (1):1, in step (2) distilled water with it is anhydrous
The mass ratio of magnesium sulfate powder mixing is (20~25):(1~5).
Step (1) dip time is 12~18h, and drying temperature is 150~300 DEG C, and drying time is 6~10h.
Dip time is 12~18h in step (3), and room temperature places 2~4h, 120~300 DEG C of drying temperature, drying time 4
~6h.
Beneficial effects of the present invention are：
1st, the present invention is pre-processed using distilled water to molecular sieve, has been dredged molecular sieve channels, has been improved molecular sieve
Specific surface area, and then it is effectively compound to promote magnesium sulfate to be carried out with zeolite molecular sieve, improves the absorption property of thermal energy storage material；
2nd, preparation method of the present invention is prepared compared with being flowed back using conventional acid, alkali etc., distill chemical modification processing
Technique is simple, and reaction condition is gentle, environment-friendly and green, and repeatability is strong, and operation is controllable；
3rd, the raw material used in preparation method of the present invention is easy to get, safe and non-toxic, cheap, can be mass produced；
4th, temperature workable for thermal energy storage material prepared by the present invention can be achieved to recycle within 300 DEG C, economical
Property it is good, heat loss is few, is adapted to cross-season heat-storing, the building and heating being mainly used in cross-season heat-storing and indoor hot water heating
Deng.
Brief description of the drawings
Fig. 1 is the SEM results that 13x molecular sieves amplify 5000 times after distilling water pretreatment；
Fig. 2 is the SEM results without distilling 5000 times of the 13x molecular sieves amplification of water pretreatment；
Fig. 3 is X-ray diffraction (XRD) figure of magnesium sulfate/13x zeolite molecular sieve thermal energy storage materials prepared by embodiment 2.
Embodiment
The invention provides a kind of preparation method of magnesium sulfate/zeolite molecular sieve thermal energy storage material, below in conjunction with the accompanying drawings
The present invention is described further with embodiment.
Using ESEM (JSM6490LV) observation through distilling the 13x molecular sieves of water pretreatment and locating in advance without distilled water
The surface topography of the 13x molecular sieves of reason, as shown in figure accompanying drawing 1,2, contrast understands that the 13x molecular sieve surfaces by pretreatment can
It was observed that the undressed 13x molecular sieves of aperture ratio it is big, i.e., 13x molecular sieve pore passages are dredged.
The crystal structure of the magnesium sulfate/13x zeolite molecular sieve thermal energy storage materials prepared using XRD researchs, such as the institute of accompanying drawing 3
Show, XRD spectrum does not only have the diffraction maximum of 13x molecular sieves, has magnesium sulfate crystals diffraction maximum (20.5 °, 24.5 °) yet, shows sulfuric acid
Magnesium and 13x zeolite molecular sieves have excellent compatibility.
Magnesium sulfate prepared by the present invention/13x zeolite molecular sieve thermal energy storage materials, workable temperature within 300 DEG C,
Storage density in the temperature range substantially increases than 13x zeolite molecular sieves storage density；Under the same conditions, 13x boils
The monolayer adsorption amount of stone molecular sieve is up to 0.2 gram of (H2O)/gram (material), the sulfuric acid not prepared using distillation water pretreatment
The maximum monolayer adsorption amount of magnesium/13x zeolite molecular sieves is 0.288 gram of (H2O)/gram (material), and prepared through distilling water pretreatment
The monolayer adsorption amounts of magnesium sulfate/13x zeolite molecular sieve thermal energy storage materials reach as high as 0.356 gram of (H2O)/gram (material).
Embodiment 1
Claim 300 grams of 13x zeolite molecular sieves, 450 grams of distilled water, placed using distillation water retting 13x molecular sieves after 12 hours
In drying box, dried 6 hours under conditions of 180 DEG C, take out and be cooled to room temperature, weighed quality and keep in case making
With；13.17 grams of anhydrous slufuric acid magnesium dust is weighed, 250 grams of distilled water, is configured to magnesium sulfate salt solution；Weigh pretreated 13x
200 grams of molecular sieve, is immersed in magnesium sulfate salt solution and outwells unnecessary liquid after 12 hours, is positioned over after standing 2 hours dry
In dry case, 150 DEG C of constant temperature 4 hours, it is brought rapidly up to 300 DEG C of constant temperature 2 hours, magnesium sulfate/compound storage of 13x zeolite molecular sieves is made
Hot material.
Weigh above-mentioned 20 grams of the thermal energy storage material for preparing to be placed in glassware, and be positioned in climatic chamber, set
The temperature of climatic chamber is 25 DEG C, relative humidity 80%RH, carries out monolayer adsorption experiment to material, ensures compound heat accumulation material
The adsorption time of material is 24 hours, and the quality of magnesium sulfate/13x zeolite molecular sieve thermal energy storage materials is weighed after taking-up, obtains sulphur
The adsorbance of sour magnesium/13x zeolite molecular sieve thermal energy storage materials is 0.226 gram of (H2O)/gram (material).
Embodiment 2
Claim 350 grams of 13x zeolite molecular sieves, 450 grams of distilled water, after distillation water retting 13x molecular sieves 16 hours, place
In drying box, taken out after being dried 8 hours under conditions of 150 DEG C and be cooled to room temperature, weighed quality and keep in case making
With；27.78 grams of anhydrous slufuric acid magnesium dust is weighed, 250 grams of distilled water, is configured to magnesium sulfate salt solution；Weigh pretreated 13x
150 grams of molecular sieve, is immersed in magnesium sulfate salt solution and outwells unnecessary liquid after 12 hours, is positioned over after standing 2 hours dry
In dry case, 150 DEG C of constant temperature 4 hours, it is brought rapidly up to 300 DEG C of constant temperature 2 hours, magnesium sulfate/compound storage of 13x zeolite molecular sieves is made
Hot material.
Weigh above-mentioned 20 grams of the thermal energy storage material for preparing to be placed in glassware, and be positioned in climatic chamber, set
The temperature of climatic chamber is 35 DEG C, relative humidity 60%RH, carries out monolayer adsorption experiment to material, ensures compound heat accumulation material
The adsorption time of material is 22 hours, and the quality of magnesium sulfate/13x zeolite molecular sieve thermal energy storage materials is weighed after taking-up, obtains sulphur
The adsorbance of sour magnesium/13x zeolite molecular sieve thermal energy storage materials is 0.252 gram of (H2O)/gram (material).
Embodiment 3
Claim 350 grams of 13x zeolite molecular sieves, 500 grams of distilled water, after distillation water retting 13x molecular sieves 12 hours, place
In drying box, taken out after being dried 6 hours under conditions of 200 DEG C and be cooled to room temperature, weighed quality and keep in case making
With；44.13 grams of anhydrous slufuric acid magnesium dust is weighed, 250 grams of distilled water, is configured to magnesium sulfate salt solution；Weigh pretreated 13x
100 grams of molecular sieve, is immersed in magnesium sulfate salt solution and outwells unnecessary liquid after 14 hours, is positioned over after standing 4 hours dry
In dry case, 150 DEG C of constant temperature 4 hours, it is brought rapidly up to 300 DEG C of constant temperature 1 hour, magnesium sulfate/compound storage of 13x zeolite molecular sieves is made
Hot material.
Weigh above-mentioned 30 grams of the thermal energy storage material for preparing to be placed in glassware, and be positioned in climatic chamber, set
The temperature of climatic chamber is 35 DEG C, relative humidity 70%RH, carries out monolayer adsorption experiment to material, ensures compound heat accumulation material
The adsorption time of material is 22 hours, and the quality of magnesium sulfate/13x zeolite molecular sieve thermal energy storage materials is weighed after taking-up, obtains sulphur
The adsorbance of sour magnesium/13x zeolite molecular sieve thermal energy storage materials is 0.273 gram of (H2O)/gram (material).
Embodiment 4
Claim 300 grams of 13x zeolite molecular sieves, 600 grams of distilled water, after distillation water retting 13x molecular sieves 18 hours, place
In drying box, taken out after being dried 8 hours under conditions of 200 DEG C and be cooled to room temperature, weighed quality and keep in case making
With；62.53 grams of anhydrous slufuric acid magnesium dust is weighed, 250 grams of distilled water, is configured to magnesium sulfate salt solution；Weigh pretreated 13x
100 grams of molecular sieve, is immersed in magnesium sulfate salt solution and outwells unnecessary liquid after 14 hours, is positioned over after standing 2 hours dry
In dry case, 120 DEG C of constant temperature 3 hours, it is brought rapidly up to 300 DEG C of constant temperature 3 hours, magnesium sulfate/compound storage of 13x zeolite molecular sieves is made
Hot material.
Weigh above-mentioned 25 grams of the thermal energy storage material for preparing to be placed in glassware, and be positioned in climatic chamber, set
The temperature of climatic chamber is 30 DEG C, relative humidity 75%RH, carries out monolayer adsorption experiment to material, ensures compound heat accumulation material
The adsorption time of material is 20 hours, and the quality of magnesium sulfate/13x zeolite molecular sieve thermal energy storage materials is weighed after taking-up, obtains sulphur
The adsorbance of sour magnesium/13x zeolite molecular sieve thermal energy storage materials is 0.356 gram of (H2O)/gram (material).
Claims (5)
1. the preparation method of a kind of magnesium sulfate/zeolite molecular sieve thermal energy storage material, it is characterised in that comprise the following steps that：
(1) distilled water and zeolite molecular sieve are weighed, is pre-processed with distillation water retting zeolite molecular sieve, by the molecule after dipping
Sieve, which is put into drying box, to be dried, and is subsequently cooled to room temperature, taking-up is sealed；
(2) distilled water is mixed with anhydrous slufuric acid magnesium dust, configures the Adlerika of different quality concentration；
(3) the pretreated zeolite molecular sieve of step (1) is placed in step (2) Adlerika and impregnated, after the completion of dipping
Place at room temperature, be then placed in drying box and be dried, be sealed in dry conditions, magnesium sulfate/zeolite molecules are made
Sieve thermal energy storage material.
2. the preparation method of magnesium sulfate according to claim 1/zeolite molecular sieve thermal energy storage material, it is characterised in that
Zeolite molecular sieve described in step (1), (3) is 13X zeolite molecular sieves.
3. the preparation method of magnesium sulfate according to claim 1/zeolite molecular sieve thermal energy storage material, it is characterised in that
The mass ratio (1.1~3) of distilled water and zeolite molecular sieve in step (1):1, distilled water and anhydrous slufuric acid magnesium powder in step (2)
The mass ratio of end mixing is (20~25):(1~5).
4. the preparation method of magnesium sulfate according to claim 1/zeolite molecular sieve thermal energy storage material, it is characterised in that
Step (1) dip time is 12~18h, and drying temperature is 150~300 DEG C, and drying time is 6~10h.
5. the preparation method of magnesium sulfate according to claim 1/zeolite molecular sieve thermal energy storage material, it is characterised in that
Dip time is 12~18h in step (3), and room temperature places 2~4h, 120~300 DEG C of drying temperature, 4~6h of drying time.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110079280A (en) * | 2019-05-29 | 2019-08-02 | 上海理工大学 | A kind of thermal energy storage material of binary hydrated salt |
| CN110743490A (en) * | 2019-11-25 | 2020-02-04 | 南京金合能源材料有限公司 | Composite chemical adsorption material based on porous clay and preparation method thereof |
| CN113652206A (en) * | 2021-08-20 | 2021-11-16 | 郑州轻工业大学 | Calcium-magnesium-based thermochemical adsorption heat storage material and preparation method thereof |
| CN115710717A (en) * | 2022-11-25 | 2023-02-24 | 华北电力大学 | Method for synthesizing Na-A zeolite molecular sieve by using microplasma |
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| CN102351213A (en) * | 2011-07-21 | 2012-02-15 | 中国地质大学（武汉） | Method for preparing 3A type zeolite molecular sieve |
| CN104130752A (en) * | 2014-06-26 | 2014-11-05 | 北京化工大学 | Magnesium sulfate ammonium complex salt/ porous zeolite composite material and preparation method and application thereof |
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| CN102351213A (en) * | 2011-07-21 | 2012-02-15 | 中国地质大学（武汉） | Method for preparing 3A type zeolite molecular sieve |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079280A (en) * | 2019-05-29 | 2019-08-02 | 上海理工大学 | A kind of thermal energy storage material of binary hydrated salt |
| CN110743490A (en) * | 2019-11-25 | 2020-02-04 | 南京金合能源材料有限公司 | Composite chemical adsorption material based on porous clay and preparation method thereof |
| CN113652206A (en) * | 2021-08-20 | 2021-11-16 | 郑州轻工业大学 | Calcium-magnesium-based thermochemical adsorption heat storage material and preparation method thereof |
| CN115710717A (en) * | 2022-11-25 | 2023-02-24 | 华北电力大学 | Method for synthesizing Na-A zeolite molecular sieve by using microplasma |
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