CN101284986A - Preparation method of macrocapsule of wax shaping phase-change material - Google Patents
Preparation method of macrocapsule of wax shaping phase-change material Download PDFInfo
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Abstract
The invention relates to a method for making paraffinic figuration phase change material macro-capsules. The method comprises the following: 1. a step of making paraffinic figuration phase change material particles; 2. a step of carrying out surface modification treatment to the phase change material particles, which is to carry out surface modification treatment to the phase change material particles obtained in the step 1 with chromic acid modification liquid for 2 to 3 hours, filter, wash for 3 to 5 times and dry the particles naturally for standby application; 3. a step of making macro-capsules, during which, the particles obtained in the step 2 is put into a coating pot; ultrafine powder is added in as additive; capsule wall liquid is spray to the particles; after the surfaces of the particles are covered by a layer of capsule wall liquid, spraying is stopped, and the capsule wall liquid is dried with hot blast; then curing liquid is sprayed to the particles, and after the surfaces of the particles are covered by a layer of curing liquid, spraying is stopped, and the curing liquid is dried with hot blast; the spraying steps are repeated, i.e. the capsule wall liquid and the curing liquid are alternately sprayed, and the layers of liquid are sprayed and dried one by one until the capsule wall liquid and the curing liquid with the designed volume are alternately sprayed over; after the last layer of curing liquid is dried, 100+-1 ml of auxiliary curing liquid per kilogram of the particles is sprayed, and then cold blast is provided; the particles are taken out after 30 to 60 minutes and dried at the temperature less than or equal to 40 DEG C, and then the macro-capsules can be obtained.
Description
Technical field
The present invention relates to the functional materials manufacturing technology, be specially a kind of preparation method of macrocapsule of wax shaping phase-change material, international Patent classificating number intends being Int.Cl.C09K5/02 (2006.01) I.
Background technology
Phase transformation (energy storage) material is a kind of rapidly environmental protection and energy saving material of development in recent years, and is in field widespread uses such as Heating,Ventilating and Air Conditioning (HVAC), building, sun power utilization, clothes, significant.Phase change material (PCM) mainly contains solid-solid phase transition material and solid-liquid phase change material by its work phase.Wherein solid-solid phase transition material can remain its fixed profile in storing thermal process, the convenient application, but the available material category of solid-solid phase transition material is few, and majority costs an arm and a leg, and application is very limited.Solid-liquid PCM because of mobile liquid generation is arranged, has caused inconvenience to use in storing thermal process, but its source is abundant, cheap, is still the more phase change material of present application.
Solid-liquid phase change material commonly used comprises mineral-type solid-liquid phase change material (hydrated inorganic salt, melting salt etc.) and organic class solid-liquid phase change material (alkane, lipid acid, ester, superpolymer etc.).Mineral-type solid-liquid phase change material heat accumulation value height, good heat conductivity, but corrodibility is big, poor heat stability; Organic class solid-liquid phase change material Heat stability is good, corrodibility is little, toxicity is little, cheap, but heat conductivility is poor.Therefore there is the investigator to study preparation and has shaping phase-change material fixing outward appearance, that integrate inorganic, organic materials superiority (referring to Inaba etc., a kind of thermophysics performance evaluation of the paraffin solid-liquid phase change material that formalizes, caloic is transmitted magazine: Inaba H, Tu P.Evaluation of thermophysical characteristicson shape-stabilized paraffin as a solid-liquid phase change material.Heat andMass Transfer, 1997,32:307-312.); People such as Ye Hong are (referring to Ye Hong etc., the preparation of polyethylene-paraffin composite shape-setting solid-liquid phase change material, solar energy materials and solar cell magazine: Preparation ofpolyethylene-paraffin compound as a form-stable solid-liquid phase changematerial, Solar Energy Materials and Solar Cells, 2000, (9): 37-44.) studied the shaping phase-change material that high density polyethylene(HDPE) and paraffin prepare, the massfraction of storage mass paraffin can reach 0.74～0.75; People such as Xiao Min are (referring to Xiao Min etc., good heat conduction, shape keep the preparation and the performance of phase change heat storage material, solar energy journal, 2001, (4): 427-430.) studied the composite phase-change material that paraffin and SBS Thermoplastic Elastomer are formed, and add graphite therein, and improving its heat-conductive characteristic, the massfraction that adds paraffin is in 0.20～0.80 scope; People such as Xavier Py are (referring to Xavier Py etc., a kind of high stable thermal energy storage material---paraffin/porous graphite based composites, international caloic is transmitted magazine: Paraffin/porous-graphite-matrix composite as a high and constant power thermalstorage material, International Journal of Heat and Mass Transfer, 2001,44 (14): 2727-2737.) adopt the method for porous graphite absorption paraffin to prepare shaping phase-change material, wherein the shared massfraction of storage mass paraffin can reach 0.65～0.95, and the thermal conductivity of composite phase-change material improves a lot with respect to the thermal conductivity of paraffin refined wax class.The method preparation that above-mentioned these technology mainly adopt twin-roll mixing or twin screw to extrude, composite shape-setting phase-change material can be made tabular or particulate state, does not need special packaging container.
But in use, the paraffin in the above-mentioned shaping phase-change material can be gradually to surface transport and loss.Do not ooze processing if do not take the surface to support, behind experience several times phase transition process, the mass loss of this phase change material can reach more than 20% (referring to Zhang Dong etc., granule type phase-change energy-storage composite material, matrix material journal, 2004,21 (5): 103-109).
Chinese patent CN 1546596A has announced title of people such as Yang Rui " is prevented blending the method for fire-retardant finish " to the shaping phase-change material surface patent of invention.The reaction solution that this patent employing polar monomer and solvent are made into obtains the shaping phase-change material of surface grafting polar monomer by the uviolizing surface grafting.This method can be received polar monomer the surface of shaping phase-change material, make the surface of paraffin ooze out phenomenon be improved significantly, this material has also possessed certain flame retardant properties simultaneously.But preparation method's operation is loaded down with trivial details, and the cost height is unfavorable for scale production.
Chinese patent CN 1657587A has announced that names such as Wang Shujun are called the application for a patent for invention of " a kind of preparation method of phase transformation material for microcapsult packing and forming ".This patent adopts situ aggregation method to use cyanurotriamide modified urea resin that the paraffin shaping phase-change material is carried out the microcapsule encapsulation, and preparation contains the microcapsule figuration composite phase-changing material of arbitrary specification paraffin from 1% to 70%.This preparation method's deficiency is that microcapsule wall material contains formaldehyde, is unfavorable for environmental protection, and encapsulates after shaping phase-change material need being broken into micron particles again, and preparation section is more.
In the scope of applicant's retrieval, yet there are no report in the research aspect the following macrocapsule of wax shaping phase-change material of the present invention.
Summary of the invention
At the deficiencies in the prior art, the technical problem to be solved in the present invention is, designs a kind of preparation method of macrocapsule of wax shaping phase-change material, and this preparation method's technology is simple, and processing ease is with low cost, is suitable for industrializing implementation; Prepared large capsule steady quality, performance improves, and is cheap, helps actual applying.
The technical scheme that the present invention solves described preparation method's technical problem is: design a kind of preparation method of macrocapsule of wax shaping phase-change material, it comprises following step:
(1) preparation paraffin class shaping phase-change material particle;
(2) phase change material particulate surface modification treatment: the phase change material particle that step (1) is obtained joins in the chromic acid modification liquid, heating in water bath to 40～60 ℃, and surface modification treatment 2～3 hours is filtered, washing 3～5 times, and seasoning is standby; Described chromic acid modification liquid is according to K
2Cr
2O
7: dense H
2SO
4: H
2O=5: 100: 8 part by weight preparation;
(3) preparation large capsule: the particle that step (2) obtains is put in the coating pan, open coating pan, and set 20～50 rev/mins of its rotating speeds, be preheating to 40～45 ℃ with warm air, add the additive ultrafine powder, to described particle spray coating cyst wall liquid, after particle surface covers one deck cyst wall liquid, stop spraying, use hot blast drying; Control particulate temperature again to the particle spray coating solid solution, after particle surface covers one deck solid solution, stops spraying at 40～45 ℃, uses hot blast drying; Repeat according to this then, alternately spray cyst wall liquid and solid solution, be coated with one deck, dry one deck is till the cyst wall liquid of design flow and solid solution have alternately sprayed; After last one deck solid solution drying, spray the auxiliary solid solution of 100 ± 1ml/ per kilogram particulate again, change then and blow a cold wind over, after 30～60 minutes; Take out encapsulated particle, place≤40 ℃ of temperature under, be drying to obtain;
Described additive is titanium dioxide or talcum powder, and median size is between 500nm～3 μ m, and consumption is 1/5～1/15 of a paraffin class shaping phase-change material particle weight;
Described cyst wall liquid is the sodium silicate aqueous solution that contains softening agent, and its pH value is 8～9.5, and the weight concentration of water glass is 10～20%, and dioxide-containing silica is controlled at 10～40% in the gel that obtains; Described softening agent is a glycerine, and weight concentration is 5～20% of the silicon-dioxide aqueous solution; The spraying design flow of cyst wall liquid is 500 ± 50ml/ per kilogram particle;
Described solid solution is any one in sulfuric acid, nitric acid, hydrochloric acid, acetic acid and the phosphoric acid, and its weight concentration is 10～20%; The spraying design flow of solid solution is 500 ± 50ml/ per kilogram particle;
Described auxiliary solid solution is that weight concentration is 2～5% calcium chloride water.
It is that cyst wall, paraffin class/polyethylene shaping phase-change material are the millimeter level large capsule of the capsule heart with silica gel that the present invention adopts the situ aggregation method preparation.Compared with prior art, macrocapsule of wax shaping phase-change material of the present invention has following obvious advantage:
(1) function improves.Millimeter level large capsule improves with respect to the phase change material content in its unit weight of microcapsule on the one hand, therefore can guarantee making full use of of thermal efficiency effectively; On the other hand, the wetting ability by the shaping phase-change material behind the silica gel packing can significantly improve, and helps the blend with material of construction, improves the stability of its heat transfer efficiency and goods;
(2) cost reduces.Because the shaping phase-change material that uses the twin screw extrusion by melting to obtain can directly carry out packing, need not further pulverizing, thereby has shortened production process; The wall material of packing adopts cheap water glass inorganic salt simultaneously, thereby can further save production cost, and helps spreading the new technique;
(3) large capsule of the present invention has overcome the not shortcoming of the easy seepage of shaping phase-change material paraffin of packing, and for example, 10 thermocycling experiments detect
The stopping property of cylindrical Octadecane/polyethylene composite shape-setting phase-change material (paraffin seepage), the rate of weight loss of material of the present invention is 0.56%, and similarity condition not the rate of weight loss of coating material be 4.53% (referring to embodiment 2), and have flame retardant properties preferably.
Macrocapsule of wax shaping phase-change material of the present invention is particularly useful for solar heat-preservation system and building heat preservation body of wall, has the energy-saving and emission-reduction meaning.
Embodiment
Further narrate the present invention below in conjunction with embodiment:
The preparation method (abbreviation preparation method) of the macrocapsule of wax shaping phase-change material of the present invention's design, it comprises following step:
(1) preparation paraffin class shaping phase-change material particle.The present invention prepares paraffin class shaping phase-change material particle and adopts prior art, is about to paraffin and olefin polymer blend, again through dual-screw-stem machine extruding pelletization (referring to Yang Rui etc., a kind of preparation method of shaping phase-change material, Chinese invention patent CN1369537A).The weight percent of paraffin class shaping phase-change material of the present invention is 20～80%, embodiment preferred mass per-cent is 50～80% paraffin class phase change material with mass percent is that 50～20% high density polyethylene(HDPE) mixes, mixture can obtain paraffin class shaping phase-change material particle through twin screw extruder blend granulation; Described paraffin class phase change material comprises commercial wax, the purified straight-chain paraffin after purifying, at least a as in the materials such as n-dodecane, n-tetradecane, n-hexadecane, Octadecane, NSC 62789.
(2) phase change material particulate surface modification treatment.The phase change material particle that step (1) is obtained joins in the chromic acid modification liquid, heating in water bath to 40～60 ℃, and surface modification treatment 2～3 hours is filtered, washing 3～5 times, and seasoning is standby; Described chromic acid modification liquid is according to K
2Cr
2O
7: dense H
2SO
4: H
2O=5: 100: 8 part by weight preparation, consumption require submergence paraffin class shaping phase-change material particle.
Preparation method of the present invention utilizes chromic acid modification liquid to handle paraffin class shaping phase-change material particle, can make its surface oxidized, produces hydroxyl, carbonyl and carboxylic group, to improve the hydrophilicity of material surface, improves the sticking power of its surface and cyst wall silica gel.
(3) preparation large capsule: the particle that step (2) obtains is put in the coating pan, open coating pan, and setting dressing machine rotating speed is 20～50 rev/mins, be preheating to 40～45 ℃ with warm air, add the additive ultrafine powder, to particle spray coating cyst wall liquid, after particle surface covers one deck cyst wall liquid, stop spraying, use hot blast drying; Control particulate temperature again to the particle spray coating solid solution, after particle surface covers one deck solid solution, stops spraying at 40～45 ℃, uses hot blast drying; Repeat according to this then, alternately spray cyst wall liquid and solid solution, and be coated with one deck, dry one deck is till the cyst wall liquid of design flow and solid solution have alternately sprayed; After last one deck solid solution drying, spray the auxiliary solid solution of 100 ± 1ml/ per kilogram particulate again, change then and blow a cold wind over, after 30～60 minutes (are standard with the large capsule surface-brightening), take out, place≤40 ℃ of temperature under, be drying to obtain;
Described additive is titanium dioxide or talcum powder, and median size is between 500nm～3 μ m, and consumption is 1/5～1/15 of a paraffin class shaping phase-change material particle weight; Embodiment selects talcum powder for use.
Described cyst wall liquid is the sodium silicate aqueous solution that contains softening agent, and its pH value is 8～9.5, and the weight concentration of water glass is preferred 10～20%, and dioxide-containing silica is controlled at 10～40% in the gel that obtains; Described softening agent is a glycerine, and weight concentration is 5～20% of the silicon-dioxide aqueous solution; The spraying design flow of cyst wall liquid is 500 ± 50ml spray coating liquor/per kilogram particle.
Described solid solution is that any one can provide H
+Common acid, comprise sulfuric acid, nitric acid, hydrochloric acid, acetic acid and phosphoric acid, its weight concentration is 10～20%.Because hydrochloric acid has characteristics such as volatile, the preferred hydrochloric acid of the embodiment of the invention is as solidifying agent.The spraying design flow of solid solution is 500 ± 50ml spray coating liquor/per kilogram particle;
Described auxiliary solid solution is that weight concentration is 2～5% calcium chloride water.
Described spraying should guarantee that each particle surface is fully wetting and wetting evenly, and it is too many or irregular also will to avoid spraying, and makes between the particle inter-adhesive.
The principle of design of preparation method's exemplary embodiments of the present invention is: select for use sodium silicate aqueous solution to make cyst wall liquid, select for use hydrochloric acid to do solid solution, both reactions at first generate orthosilicic acid, and the orthosilicic acid part is water insoluble, can form colloid, and its reaction formula is:
Na
2SiO
3+2HCl→2NaCl+H
4SiO
4 (1)
Because the strong adsorption on the paraffin class shaping phase-change material surface after the modification, it can be deposited on the particle surface of shaping phase-change material, and the acid-basicity of regulation system can make most of colloid at the shaping phase-change material surface deposition.At a certain temperature, the orthosilicic acid dehydration of being heated just forms the silica gel thin film of macromolecule network, and shaping phase-change material is encapsulated in the silica gel large capsule (abbreviation large capsule).Its reaction formula is:
nH
4SiO
4-(2n-1)H
2O→nSiO
2·H
2O (2)
The calcium chloride water of auxiliary solidifying agent 2～5% weight of spraying can make the incomplete orthosilicic acid of gel generate Calucium Silicate powder, and cyst wall is further solidified.Its reaction is:
H
2SiO
3+CaCl
2→2HCl+CaSiO
3 (3)
The large capsule of preparation method's gained of the present invention can adopt the thermocycling experiment method to check its sealing property.Concrete grammar is: load weighted large capsule sample is wrapped with filter paper, placed 50 ℃ thermostatic drying chamber to keep 1 hour, take out postcooling to room temperature; Be placed on interior the maintenance after 30 minutes of refrigerating chamber of refrigerator again, taking-up is weighed, and calculates the weight loss of large capsule.This is a thermocycling experiment, so repeats 10 times and gets final product.
The present invention does not address part and is applicable to prior art.
Provide specific embodiments of the invention below, but it does not constitute the restriction to claim of the present invention.
Embodiment 1
The exemplary embodiments of large capsule preparation:
Get the Octadecane phase change material of 50 parts of weight, add the high density polyethylene(HDPE) of 50 parts of weight, mix,, obtain through twin screw extruder blend granulation
Cylindrical Octadecane/polyethylene composite shape-setting phase-change material particle.The gained particle is joined in the chromic acid modification liquid, heating in water bath to 55 ℃, surface modification treatment 2.5 hours is filtered, washing 5 times, seasoning.Getting this particle of 100g joins in the coating pan, open coating pan, and set 50 rev/mins of coating pan rotating speeds, be preheating to 40 ℃ with warm air, add 10g talcum powder ultrafine powder, to the sodium silicate solution (glycerine that wherein contains 15% weight) of particle spray coating 10% weight, after particle surface covers one deck cyst wall liquid, stop spraying, use hot blast drying; Control particulate temperature to the hydrochloric acid soln of particle spray coating 10% weight, after particle surface covers one deck solid solution, stops spraying at 40 ℃, uses hot blast drying; By this repetitive operation, till 50ml sodium silicate solution and 50ml hydrochloric acid soln sprays, during the wettability of continuous detection particle surface, prevent the mutual adhesion of capsule-core particle, be coated with one deck, dry one deck; After last one deck cyst wall liquid and the solid solution drying, spray the auxiliary solidifying agent of 10ml 5% weight again, change then and blow a cold wind over, after 50 minutes, the large capsule surface-brightening takes out, and places under 40 ℃ the temperature to be drying to obtain.
Adopt the stopping property of thermocycling experiment method check large capsule, through 10 thermocycling experiments, the rate of weight loss of gained large capsule is 0.48%; Similarity condition detects packing not
Cylindrical Octadecane/polyethylene composite shape-setting phase-change material particulate rate of weight loss is 3.13%.
Embodiment 2
Get the NSC 62789 phase change material heat fused of 80 parts of weight, add the high density polyethylene(HDPE) of 20 parts of weight, be stirred to dissolving fully,, obtain through twin screw extruder blend granulation
Cylindrical NSC 62789/polyethylene composite shape-setting phase-change material particle.Following steps are undertaken by embodiment 1.
The rate of weight loss that records 10 thermocycling experiments of large capsule is 0.56%, and similarity condition records packing not
Cylindrical Octadecane/polyethylene composite shape-setting phase-change material particulate rate of weight loss is 4.53%.
Embodiment 3
Get the industrial paraffin phase change material of 70 parts of weight, add the high density polyethylene(HDPE) of 30 parts of weight, mix,, obtain through twin screw extruder blend granulation
Cylindrical paraffin/polyethylene composite shape-setting phase-change material particle.The gained particle is joined in its chromic acid modification liquid of submergence, heating in water bath to 60 ℃, surface modification treatment 3 hours is filtered, washing 3 times, seasoning.Getting this particle of 100g joins in the coating pan, open coating pan and set 30 rev/mins of coating pan rotating speeds, be preheating to 45 ℃ with warm air, add 7g talcum powder ultrafine powder, sodium silicate solution (glycerine that wherein contains 11% weight) to particle spray coating 15% weight, after particle surface covers one deck cyst wall liquid, stop spraying, use hot blast drying; Control particulate temperature to the hydrochloric acid soln of particle spray coating 15% weight, after particle surface covers one deck solid solution, stops spraying at 45 ℃, uses hot blast drying; By this repetitive operation, till 50ml sodium silicate solution and 50ml hydrochloric acid soln sprays, during the wettability of continuous detection particle surface, prevent the mutual adhesion of capsule-core particle, be coated with one deck, dry one deck; After last one deck cyst wall liquid and the solid solution drying, spray the auxiliary solidifying agent of 10ml 3% weight again, change then and blow a cold wind over, after 40 minutes, the large capsule surface-brightening takes out, and places under 40 ℃, is drying to obtain.
Adopt the stopping property of thermocycling experiment method check large capsule, through 10 thermocycling experiments, the rate of weight loss of gained large capsule is 0.35%; Similarity condition detects packing not
Cylindrical Octadecane/polyethylene composite shape-setting phase-change material particulate rate of weight loss is 3.87%.
Embodiment 4
Get the n-tetradecane phase change material of 75 parts of weight, add the high density polyethylene(HDPE) of 25 parts of weight, mix,, obtain through twin screw extruder blend granulation
Cylindrical n-tetradecane/polyethylene composite shape-setting phase-change material particle.The gained particle is joined in the chromic acid modification liquid, heating in water bath to 40 ℃, surface modification treatment 2 hours is filtered, washing 3 times, seasoning.Getting this particle of 100g joins in the coating pan, open coating pan and set 30 rev/mins of coating pan rotating speeds, be preheating to 40 ℃ with warm air, add 20g talcum powder ultrafine powder, sodium silicate solution (glycerine that wherein contains 20% weight) to particle spray coating 20% weight, after particle surface covers one deck cyst wall liquid, stop spraying, use hot blast drying; Control particulate temperature to the hydrochloric acid soln of particle spray coating 20% weight, after particle surface covers one deck solid solution, stops spraying at 40 ℃, uses hot blast drying; By this repetitive operation, till 50ml sodium silicate solution and 50ml hydrochloric acid soln sprays, during the wettability of continuous detection particle surface, prevent the mutual adhesion of capsule-core particle, be coated with one deck, dry one deck; After last one deck cyst wall liquid and the solid solution drying, spray the auxiliary solidifying agent of 10ml 5% weight again, change then and blow a cold wind over, after 30 minutes, the large capsule surface-brightening takes out, and places under 35 ℃ the temperature, is drying to obtain.
Adopt the stopping property of thermocycling experiment method check large capsule.Through 10 thermocycling experiments, the rate of weight loss of gained large capsule is 0.42%; Similarity condition detects packing not
Cylindrical Octadecane/polyethylene composite shape-setting phase-change material particulate rate of weight loss is 4.63%.
Embodiment 5
Investigate the influence of softening agent to the large capsule sealing property:
Prepare according to embodiment 1 method
Cylindrical Octadecane/polyethylene composite shape-setting phase-change material particle, but in cyst wall liquid, do not add softening agent glycerine, all the other conditions and step are with embodiment 1.Detect the sealing property of this large capsule, the rate of weight loss of 10 thermocycling experiments is 1.87%.
Embodiment 6
Investigate of the influence of chromic acid modification liquid to the large capsule sealing property:
Method preparation according to embodiment 1
Cylindrical Octadecane/polyethylene composite shape-setting phase-change material large capsule, but in technological process, particle is handled without described chromic acid modification liquid, directly carries out packing, and is surplus with embodiment 1.Detect the sealing property of this large capsule, the rate of weight loss of 10 thermocycling experiments is 0.83%.
Embodiment 7
Investigate of the influence of auxiliary solidifying agent to the large capsule sealing property:
Except not spraying auxiliary solidifying agent, other processing methodes are all identical with embodiment 1 in the present embodiment.Detect the sealing property of this large capsule, the rate of weight loss of 10 thermocycling experiments is 1: 36%.
By embodiment 5-7 as can be seen, chromic acid modification liquid of the present invention is less relatively to the influence of large capsule sealing property, and described softening agent is relatively large to the influence of large capsule sealing property.
Claims (2)
1. the preparation method of a macrocapsule of wax shaping phase-change material, it comprises following step:
(1) preparation paraffin class shaping phase-change material particle;
(2) phase change material particulate surface modification treatment: the phase change material particle that step (1) is obtained joins in the chromic acid modification liquid, and heating in water bath is to 40-60 ℃, and surface modification treatment 2-3 hour, to filter, washing 3-5 time, seasoning is standby; Described chromic acid modification liquid is according to K
2Cr
2O
7: dense H
2SO
4: H
2O=5: 100: 8 part by weight preparation;
(3) preparation large capsule: the particle that step (2) obtains is put in the coating pan, open coating pan, and set 20-50 rev/min of its rotating speed, be preheating to 40-45 ℃ with warm air, add the additive ultrafine powder, to described particle spray coating cyst wall liquid, after particle surface covers one deck cyst wall liquid, stop spraying, use hot blast drying; Control particulate temperature again to the particle spray coating solid solution, after particle surface covers one deck solid solution, stops spraying at 40-45 ℃, uses hot blast drying; Repeat according to this then, alternately spray cyst wall liquid and solid solution, be coated with one deck, dry one deck is till the cyst wall liquid of design flow and solid solution have alternately sprayed; After last one deck solid solution drying, spray the auxiliary solid solution of 100 ± 1ml/ per kilogram particulate again, change then and blow a cold wind over, after 30-60 minute; Take out encapsulated particle, place≤40 ℃ of temperature under, be drying to obtain;
Described additive is titanium dioxide or talcum powder, and median size is between 500nm-3 μ m, and consumption is the 1/5-1/15 of paraffin class shaping phase-change material particle weight;
Described cyst wall liquid is the sodium silicate aqueous solution that contains softening agent, and its pH value is 8-9.5, and the weight concentration of water glass is 10-20%, and dioxide-containing silica is controlled at 10-40% in the gel that obtains; Described softening agent is a glycerine, and weight concentration is the 5-20% of the silicon-dioxide aqueous solution; The spraying design flow of cyst wall liquid is 500 ± 50ml/ per kilogram particle;
Described solid solution is any one in sulfuric acid, nitric acid, hydrochloric acid, acetic acid and the phosphoric acid, and its weight concentration is 10-20%; The spraying design flow of solid solution is 500 ± 50ml/ per kilogram particle;
Described auxiliary solid solution is that weight concentration is the calcium chloride water of 2-5%.
2. the preparation method of macrocapsule of wax shaping phase-change material according to claim 1 is characterized in that described solid solution is a hydrochloric acid; Described additive is a talcum powder.
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| CN101838520A (en) * | 2010-04-28 | 2010-09-22 | 清华大学深圳研究生院 | Preparation method of composition containing phase-change and energy-storage micro-capsules |
| CN102127395A (en) * | 2010-12-10 | 2011-07-20 | 东南大学 | Paraffin wax phase change energy storage material and preparation method thereof |
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| CN101671547B (en) * | 2009-09-30 | 2012-06-27 | 林光舜 | Phase-change thermal-storage material taking waste engine oil as main material |
| CN101838520A (en) * | 2010-04-28 | 2010-09-22 | 清华大学深圳研究生院 | Preparation method of composition containing phase-change and energy-storage micro-capsules |
| CN101838520B (en) * | 2010-04-28 | 2012-10-17 | 清华大学深圳研究生院 | Preparation method of composition containing phase-change and energy-storage micro-capsules |
| CN102127395A (en) * | 2010-12-10 | 2011-07-20 | 东南大学 | Paraffin wax phase change energy storage material and preparation method thereof |
| WO2012075747A1 (en) * | 2010-12-10 | 2012-06-14 | 东南大学 | Paraffin phase change energy storage materials and preparation method thereof |
| CN102127395B (en) * | 2010-12-10 | 2012-12-19 | 东南大学 | Paraffin wax phase change energy storage material and preparation method thereof |
| CN103468223A (en) * | 2013-09-30 | 2013-12-25 | 天津工业大学 | Phase change energy storage material macro-capsule and method for preparing same |
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| CN105112020A (en) * | 2015-06-11 | 2015-12-02 | 宁波绿凯节能科技有限公司 | Flame-retardant microcapsule phase-change material |
| CN109370539A (en) * | 2018-12-11 | 2019-02-22 | 安徽绿元素建材科技有限公司 | A kind of phase-change accumulation energy microballoon and preparation method thereof |
| CN109370539B (en) * | 2018-12-11 | 2021-04-20 | 安徽纳微技术研发中心有限公司 | Phase-change energy-storage microsphere and preparation method thereof |
| CN113429937A (en) * | 2021-05-17 | 2021-09-24 | 中国地质大学（武汉） | Energy-saving temperature-control phase-change microcapsule for wall and preparation method thereof |
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