CN107760279A - A kind of preparation method of magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material - Google Patents
A kind of preparation method of magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material Download PDFInfo
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- CN107760279A CN107760279A CN201710811334.0A CN201710811334A CN107760279A CN 107760279 A CN107760279 A CN 107760279A CN 201710811334 A CN201710811334 A CN 201710811334A CN 107760279 A CN107760279 A CN 107760279A
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- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/045—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing sulfur, e.g. sulfates, thiosulfates, gypsum
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- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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Abstract
The present invention provides the preparation method of a kind of magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material, comprises the following steps:13X zeolite molecular sieves are added in distilled water after standing 12 18h, taken out, dried, the zeolite molecular sieve pre-processed;Anhydrous magnesium sulfate is added in distilled water and mixed, magnesium trisilicate is added, the high-speed stirred at 30 50 DEG C, stands, filter, grinding, obtain magnesium trisilicate and magnesium sulfate mixed salt;Magnesium trisilicate and magnesium sulfate mixed salt are added to the water, stirring extremely forms stable suspension, add the zeolite molecular sieve of pretreatment, ultrasonic agitation, stand and place at room temperature, volatilize moisture, is placed in drying box and dries, is sealed to obtain magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material.Thermal energy storage material prepared by the present invention contains multi-stage pore structure, and hole permeability is good, and specific surface area is big, and adsorption capacity is big, and absorption strength is big, and heat loss is few, and can be recycled.
Description
Technical field
The invention belongs to zeolite molecular sieve thermal energy storage material field of material technology, and in particular to a kind of magnesium trisilicate and sulphur
The preparation method of sour magnesium mixed salt/zeolite molecular sieve thermal energy storage material.
Background technology
The in short supply and poor efficiency of the energy turns into the bottleneck for restricting Sustainable Socioeconomic Development, and energy storage technology is recognized
To be one of key technology for effectively improving comprehensive utilization rate of energy source, can be achieved energy resource supply and demand the time, space and
Matching regulation in intensity, store spring, summer, autumn sufficient solar thermal energy and be used for winter heating/hot water, be maximumlly to use
Solar energy is come the important way that improves building energy conservation benefit, realize emission reduction targets.
Thermal chemical reaction heat-storage technology is to carry out storing up/heat release using the reaction heat of heat accumulating reversible chemical reaction.Heat accumulation
Material absorbs heat, is decomposed into two kinds and material that the above is easily isolated, and memory phase is to be retained separately analyte, avoids phase
Mutual reactance causes energy loss, and the heat release stage is to be sufficiently mixed analyte, creates suitable condition and brings it about combination reaction, releases
Leave with the heat energy of storage.Heat chemistry heat-storage technology is segmented into heat chemistry absorption again, heat chemistry absorbs and thermal chemical reaction heat accumulation, its
In, it is different from thermal chemical reaction heat accumulation into heat chemistry absorption and heat chemistry absorption, thing does not occur during storage and release heat
The destruction and restructuring of matter molecular structure, heat accumulating are carried out catching fixed and discharged anti-by adsorbing or absorbing to specific gas
Answer heat.
Mainly there are silica gel, zeolite, sodium hydroxide solution, metal oxide, liquid suitable for the material of heat chemistry heat accumulation at present
Ammonia and hydrated salt etc..Zeolite is divided into natural zeolite and artificial zeolite, and the hydrophily of zeolite is good, can carry out physics suction to water vapour
Attached, physical absorption reduces the free degree of adsorption molecule, therefore can release heat of adsorption, and due to zeolite to water have it is very strong
Absorption property, therefore energy storage density is very high.
A kind of ammonium magnesium sulfate double salt/porous zeolite composite and its preparation side disclosed in Chinese patent CN104130752B
Method and application, halloysite nanotubes, sodium hydroxide, silica and alundum (Al2O3) mixed grinding are calcined, ageing,
It is transferred in the stainless steel reactor with polytetrafluoroethylliner liner and reacts, washing drying obtains zeolite, by epsom salt and sulphur
Sour ammonium, which is dissolved in deionized water, coordinates mixed solution, heating stirring, then frozen water crystallisation by cooling, dries, obtains six hydrated sulfuric acids
Magnesium-ammonium mixed salt, by six hydrated sulfuric acid magnesium-ammonium mixed salts formation solution soluble in water, zeolite is added, is ultrasonically treated, moisture evaporation, obtains
Ammonium magnesium sulfate/Zeolite composite materials.Chinese document (characterization of adsorption and thermal storage performance of magnesium chloride/Zeolite composite materials, Xu Jiaxing
Deng, Journal of Chemical Industry and Engineering, the 67th S2 phases phase, 2016.12) magnesium chloride/Zeolite composite materials disclosed in, by Magnesium dichloride hexahydrate crystal
Add in 80 DEG C of distilled water and form solution, 13X zeolitic molecular sieve particles are immersed, stand 96h to bubble-free generation, mistake
Filter, the surface salting liquid of residual is taken out using distilled water Rapid Cleaning surface, it is multiple that 200 DEG C of drying and dewaterings obtain magnesium chloride/zeolite
Condensation material.From above-mentioned prior art, by being porous matrix material by zeolite molecular sieve, answered with other hydrated salts such as magnesium
Close, the composite being prepared has high salinity, high adsorption capacity, high heat storage performance.But the hole of zeolite molecular sieve is more
Unprocessed, molecular sieve channels are not opened completely, are unfavorable for the effective compound of water and salt and zeolite molecular sieve.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of magnesium trisilicate and magnesium sulfate mixed salt/compound storage of zeolite molecular sieve
The preparation method of hot material, using the zeolite molecular sieve for distilling water pretreatment as perforated substrate, magnesium sulfate and magnesium trisilicate are answered
Conjunction forms micro/nano level double salt, then double salt is adsorbed in zeolite molecular sieve hole, forms thermal energy storage material.It is prepared by the present invention
Thermal energy storage material contain multi-stage pore structure, hole permeability is good, and specific surface area is big, and adsorption capacity is big, absorption strength it is big,
Heat loss is few, and can be recycled.
In order to solve the above technical problems, the technical scheme is that:
A kind of preparation method of magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material, it is characterised in that
The magnesium trisilicate includes zeolite molecular sieve and magnesium trisilicate and sulfuric acid with magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material
The particle diameter of magnesium mixed salt, the magnesium trisilicate and magnesium sulfate mixed salt is micro/nano level, and the zeolite molecular sieve is through distilling water pretreatment.
Specific preparation method, comprises the following steps:
(1) 13X zeolite molecular sieves are added to after standing 12-18h in distilled water, take out, dry, the boiling pre-processed
Stone molecular sieve;
(2) anhydrous magnesium sulfate is added in distilled water and mixed, add magnesium trisilicate, the high-speed stirred at 30-50 DEG C is quiet
Put, filter, grinding, obtain magnesium trisilicate and magnesium sulfate mixed salt;
(3) magnesium trisilicate prepared by step (2) is added to the water with magnesium sulfate mixed salt, stirring to the suspension for forming stabilization
Liquid, the zeolite molecular sieve of pretreatment prepared by step (1) is added, ultrasonic agitation, stands place at room temperature, volatilize moisture, puts
Dried in drying box, be sealed to obtain magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material.
As the preferred of above-mentioned technical proposal, in the step (1), the mass ratio of zeolite molecular sieve and distilled water is 1:
1.1-3。
As the preferred of above-mentioned technical proposal, in the step (1), dry temperature is 150-300 DEG C, time 6-
10h。
As the preferred of above-mentioned technical proposal, in the step (2), the mass ratio of anhydrous magnesium sulfate and distilled water is 1-5:
20-25。
As the preferred of above-mentioned technical proposal, in the step (2), the mass ratio of anhydrous magnesium sulfate and magnesium trisilicate is 1-
3:1。
As the preferred of above-mentioned technical proposal, in the step (2), the rotating speed of high-speed stirred is 1800-2000r/min,
Time is 30-60min.
As the preferred of above-mentioned technical proposal, in the step (2), the particle diameter of magnesium trisilicate and magnesium sulfate mixed salt is micro-nano
Meter level.
As the preferred of above-mentioned technical proposal, in the step (3), the time of standing is 12-24h.
As the preferred of above-mentioned technical proposal, in the step (3), dry temperature is 120-300 DEG C, time 5-
10h。
Compared with prior art, the invention has the advantages that:
(1) magnesium trisilicate prepared by the present invention and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material, are boiled with 13X
Stone molecular sieve is main porous matrix, and 13X zeolite molecular sieves are a kind of porous materials of high adsorption capacity, and specific surface area is about
621-747m2/g, total pore volume 0.344-0.394cm2/g, by 13X zeolite molecular sieves after distilling water pretreatment, hole it
Between connectedness it is more preferable, specific surface area and total pore volume all further improve, and further promote magnesium trisilicate and magnesium sulfate mixed salt
With effective compound, the raising adsorbance of zeolite molecular sieve.
(2) magnesium trisilicate prepared by the present invention in magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material with containing three silicon
Sour magnesium and magnesium sulfate, magnesium sulfate are a kind of water and salt, and water and magnesium sulfate can complete most of dehydration at 150 DEG C, and heat accumulation is close
Degree reaches 2.2GJ/m3, is 9 times of researching of sensible heat storage material, but the influence such as the heat storage capacity of Magnesium sulfate heptahydrate is stressed, temperature
It is larger, and water and magnesium sulfate easily liquefy in desorption process, cause particle porosity to decline, and dehydration is incomplete, because
Magnesium trisilicate is combined to form mixed salt by this present invention with magnesium sulfate, and magnesium trisilicate is the indefinite hydrous magnesium silicate of composition, is had
It is linked to be the lightweight magnesium silicate containing Shuifu County of shape structure, there is larger specific surface area, good absorption property and rheological property can
It is scattered to be adsorbed water and magnesium sulfate using the absorption property of itself, be advantageous to the water suction and dehydration of Magnesium sulfate heptahydrate, improve storage
Heat density, finally the magnesium trisilicate of micro/nano level is promoted to adsorb and disperse again with magnesium sulfate mixed salt with 13X zeolite molecular sieves
Magnesium sulfate, magnesium sulfate is realized complete dehydration at 150 DEG C, and adsorbed by bilayer, excellent thermal insulation performance, heat loss is small, follows
Ring utilization rate improves.
(3) preparation method of the invention is simple, wide without using the complex process technique such as soda acid, low in raw material price, source
General, product cost is low, green safe, and adsorbance is big, and strong adsorption force, excellent thermal insulation performance, heat loss is small, recycles stability
It is good, the excellent combination property in terms of heat accumulation field.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1:
(1) it is 1 according to mass ratio:1.1,13X zeolite molecular sieves are added to after standing 12h in distilled water, taken out,
6h, the zeolite molecular sieve pre-processed are dried at 150 DEG C.
(2) by weight, 1 part of anhydrous magnesium sulfate is added in 20 parts of distilled water and mixed, according to anhydrous magnesium sulfate
Mass ratio with magnesium trisilicate is 1:1, magnesium trisilicate is added, at 30 DEG C, with 1800r/min speed high-speed stirred 30min,
6h is stood, is filtered, grinding, obtains micro/nano level magnesium trisilicate and magnesium sulfate mixed salt.
(3) magnesium trisilicate and magnesium sulfate mixed salt are added to the water, stirring adds pretreatment to stable suspension is formed
Zeolite molecular sieve, ultrasonic agitation, stand place 12h at room temperature, volatilize moisture, is placed in 120 DEG C of drying box and dries 5h, close
Envelope preservation obtains magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material.
Embodiment 2:
(1) it is 1 according to mass ratio:3,13X zeolite molecular sieves are added to after standing 18h in distilled water, taken out, 300
10h, the zeolite molecular sieve pre-processed are dried at DEG C.
(2) by weight, 5 parts of anhydrous magnesium sulfate is added in 25 parts of distilled water and mixed, according to anhydrous magnesium sulfate
Mass ratio with magnesium trisilicate is 3:1, magnesium trisilicate is added, at 50 DEG C, with 2000r/min speed high-speed stirred 60min,
8h is stood, is filtered, grinding, obtains micro/nano level magnesium trisilicate and magnesium sulfate mixed salt.
(3) magnesium trisilicate and magnesium sulfate mixed salt are added to the water, stirring adds pretreatment to stable suspension is formed
Zeolite molecular sieve, ultrasonic agitation, stand place 24h at room temperature, volatilize moisture, is placed in 300 DEG C of drying box and dries 10h,
It is sealed to obtain magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material.
Embodiment 3:
(1) it is 1 according to mass ratio:1.5,13X zeolite molecular sieves are added to after standing 12-18h in distilled water, taken out,
8h, the zeolite molecular sieve pre-processed are dried at 160 DEG C.
(2) by weight, 2 parts of anhydrous magnesium sulfate is added in 23 parts of distilled water and mixed, according to anhydrous magnesium sulfate
Mass ratio with magnesium trisilicate is 2:1, magnesium trisilicate is added, at 45 DEG C, with 1900r/min speed high-speed stirred 45min,
7h is stood, is filtered, grinding, obtains micro/nano level magnesium trisilicate and magnesium sulfate mixed salt.
(3) magnesium trisilicate and magnesium sulfate mixed salt are added to the water, stirring adds pretreatment to stable suspension is formed
Zeolite molecular sieve, ultrasonic agitation, stand place 16h at room temperature, volatilize moisture, is placed in 150 DEG C of drying box and dries 6h, close
Envelope preservation obtains magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material.
Embodiment 4:
(1) it is 1 according to mass ratio:2,13X zeolite molecular sieves are added to after standing 16h in distilled water, taken out, 200
8h, the zeolite molecular sieve pre-processed are dried at DEG C.
(2) by weight, 2 parts of anhydrous magnesium sulfate is added in 23 parts of distilled water and mixed, according to anhydrous magnesium sulfate
Mass ratio with magnesium trisilicate is 2:1, magnesium trisilicate is added, at 45 DEG C, with 2000r/min speed high-speed stirred 35min,
6.5h is stood, is filtered, grinding, obtains micro/nano level magnesium trisilicate and magnesium sulfate mixed salt.
(3) magnesium trisilicate and magnesium sulfate mixed salt are added to the water, stirring adds pretreatment to stable suspension is formed
Zeolite molecular sieve, ultrasonic agitation, stand place 18h at room temperature, volatilize moisture, is placed in 200 DEG C of drying box and dries 8h, close
Envelope preservation obtains magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material.
Embodiment 5:
(1) it is 1 according to mass ratio:2.5,13X zeolite molecular sieves are added to after standing 14h in distilled water, taken out,
7h, the zeolite molecular sieve pre-processed are dried at 250 DEG C.
(2) by weight, 4 parts of anhydrous magnesium sulfate is added in 23 parts of distilled water and mixed, according to anhydrous magnesium sulfate
Mass ratio with magnesium trisilicate is 1.5:1, magnesium trisilicate is added, at 45 DEG C, with 1800r/min speed high-speed stirred
40min, 8h is stood, filtered, grinding, obtain micro/nano level magnesium trisilicate and magnesium sulfate mixed salt.
(3) magnesium trisilicate and magnesium sulfate mixed salt are added to the water, stirring adds pretreatment to stable suspension is formed
Zeolite molecular sieve, ultrasonic agitation, stand place 20h at room temperature, volatilize moisture, is placed in 250 DEG C of drying box and dries 7h, close
Envelope preservation obtains magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material.
Embodiment 6:
(1) it is 1 according to mass ratio:3,13X zeolite molecular sieves are added to after standing 12h in distilled water, taken out, 300
6h, the zeolite molecular sieve pre-processed are dried at DEG C.
(2) by weight, 5 parts of anhydrous magnesium sulfate is added in 20 parts of distilled water and mixed, according to anhydrous magnesium sulfate
Mass ratio with magnesium trisilicate is 3:1, magnesium trisilicate is added, at 30 DEG C, with 2000r/min speed high-speed stirred 30min,
8h is stood, is filtered, grinding, obtains micro/nano level magnesium trisilicate and magnesium sulfate mixed salt.
(3) magnesium trisilicate and magnesium sulfate mixed salt are added to the water, stirring adds pretreatment to stable suspension is formed
Zeolite molecular sieve, ultrasonic agitation, stand place 12h at room temperature, volatilize moisture, is placed in 300 DEG C of drying box and dries 5h, close
Envelope preservation obtains magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material.
Comparative example 1:
(1) by weight, 1 part of anhydrous magnesium sulfate is added in 20 parts of distilled water and mixed, according to anhydrous magnesium sulfate
Mass ratio with magnesium trisilicate is 1:1, magnesium trisilicate is added, at 30 DEG C, with 1800r/min speed high-speed stirred 30min,
6h is stood, is filtered, grinding, obtains micro/nano level magnesium trisilicate and magnesium sulfate mixed salt.
(2) magnesium trisilicate and magnesium sulfate mixed salt are added to the water, stirring adds zeolite molecules to stable suspension is formed
Sieve, ultrasonic agitation, stand place 12h at room temperature, volatilize moisture, is placed in 120 DEG C of drying box and dries 5h, is sealed
To zeolite molecular sieve thermal energy storage material.
Comparative example 2:
By weight, 1 part of anhydrous magnesium sulfate is added in 20 parts of distilled water and mixed, add zeolite molecular sieve, surpassed
Sound stirs, and stands place 12h at room temperature, and volatilize moisture, is placed in 120 DEG C of drying box and dries 5h, is sealed and is boiled
Stone molecular sieve thermal energy storage material.
After testing, magnesium trisilicate and the magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material that prepared by embodiment 1-6 and
The maximum monolayer adsorption amount of zeolite molecular sieve thermal energy storage material prepared by comparative example 1-2, storage density, the knot of cyclical stability
Fruit is as follows:
As seen from the above table, the magnesium trisilicate that prepared by the present invention is inhaled with magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material
Attached amount is high, and energy storage density is high, good cycling stability.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
- A kind of 1. preparation method of magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material, it is characterised in that:Institute Stating magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material includes zeolite molecular sieve and magnesium trisilicate and magnesium sulfate The particle diameter of mixed salt, the magnesium trisilicate and magnesium sulfate mixed salt is micro/nano level, and the zeolite molecular sieve is through distilling water pretreatment.
- 2. the system of a kind of magnesium trisilicate according to claim 1 and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material Preparation Method, it is characterised in that comprise the following steps:(1) 13X zeolite molecular sieves are added to after standing 12-18h in distilled water, take out, dry, the zeolite pre-processed point Son sieve;(2) anhydrous magnesium sulfate is added in distilled water and mixed, added magnesium trisilicate, the high-speed stirred at 30-50 DEG C, stand, mistake Filter, grinding, obtains magnesium trisilicate and magnesium sulfate mixed salt;(3) magnesium trisilicate prepared by step (2) is added to the water with magnesium sulfate mixed salt, stirring adds to stable suspension is formed Enter the zeolite molecular sieve of the pretreatment of step (1) preparation, ultrasonic agitation, stand place at room temperature, volatilize moisture, is placed in drying Dried in case, be sealed to obtain magnesium trisilicate and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material.
- 3. the system of a kind of magnesium trisilicate according to claim 2 and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material Preparation Method, it is characterised in that:In the step (1), the mass ratio of zeolite molecular sieve and distilled water is 1:1.1-3.
- 4. the system of a kind of magnesium trisilicate according to claim 2 and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material Preparation Method, it is characterised in that:In the step (1), dry temperature is 150-300 DEG C, time 6-10h.
- 5. the system of a kind of magnesium trisilicate according to claim 2 and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material Preparation Method, it is characterised in that:In the step (2), the mass ratio of anhydrous magnesium sulfate and distilled water is 1-5:20-25.
- 6. the system of a kind of magnesium trisilicate according to claim 2 and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material Preparation Method, it is characterised in that:In the step (2), the mass ratio of anhydrous magnesium sulfate and magnesium trisilicate is 1-3:1.
- 7. the system of a kind of magnesium trisilicate according to claim 2 and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material Preparation Method, it is characterised in that:In the step (2), the rotating speed of high-speed stirred is 1800-2000r/min, time 30- 60min。
- 8. the system of a kind of magnesium trisilicate according to claim 2 and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material Preparation Method, it is characterised in that:In the step (2), the particle diameter of magnesium trisilicate and magnesium sulfate mixed salt is micro/nano level.
- 9. the system of a kind of magnesium trisilicate according to claim 2 and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material Preparation Method, it is characterised in that:In the step (3), the time of standing is 12-24h.
- 10. the system of a kind of magnesium trisilicate according to claim 2 and magnesium sulfate mixed salt/zeolite molecular sieve thermal energy storage material Preparation Method, it is characterised in that:In the step (3), dry temperature is 120-300 DEG C, time 5-10h.
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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 |
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