CN107500591B - A kind of phase-change accumulation energy microballoon and preparation method thereof - Google Patents
A kind of phase-change accumulation energy microballoon and preparation method thereof Download PDFInfo
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- CN107500591B CN107500591B CN201710952207.2A CN201710952207A CN107500591B CN 107500591 B CN107500591 B CN 107500591B CN 201710952207 A CN201710952207 A CN 201710952207A CN 107500591 B CN107500591 B CN 107500591B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/12—Multiple coating or impregnating
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/0068—Ingredients with a function or property not provided for elsewhere in C04B2103/00
- C04B2103/0071—Phase-change materials, e.g. latent heat storage materials used in concrete compositions
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention discloses a kind of phase-change accumulation energy microballoons and preparation method thereof, using high-intensitive geopolymer tiny balloon as carrier, phase-change material is absorbed by the hollow interior of carrier microballoons using the method for vacuum suction, then the microballoon for carrying phase-change material is puddled with epoxy resin, epoxy resin is made to be coated in microsphere surface, powder dispersing agent is added, stirring, disperses microballoon, after epoxy resin solidification, extra powder dispersing agent is sieved, phase-change accumulation energy microballoon is obtained.The addition of the phase-change accumulation energy microballoon can significantly reduce hydrated cementitious exothermic temperature peak value, and influence on cement strength smaller.It is compared with existing phase-change accumulation energy method for preparing microsphere, this method preparation process is simple, is easy to industrial production.
Description
Technical field
The invention belongs to micro-sphere material technical fields, and in particular to a kind of phase-change accumulation energy microballoon and preparation method thereof.
Background technique
Due to subsea cryogenic hyperbaric environment, there are a large amount of gas hydrates in ocean deepwater shallow-layer.Hydrate is heated
It easily decomposes, is easy to cause well cementation accident, propose acid test for deep water cementing, it is serious or even submarine landslide can be caused etc.
Catastrophic failure.Require cement that there is low hydration heat characteristic when therefore cementing the well to hydrate layer, and it is currently used solid
Well cement system does not have low hydration heat characteristic.
It is that phase-change material is added in cement slurry that the exothermic method of hydrated cementitious commonly, which is effectively reduced, works as hydrated cementitious
When, material phase transformation heat absorption, and heat is stored, reduce hydrated cementitious heat release.Since common phase-change material is usually oil
Phase, layering can be detached from by being added directly into cement slurry, influence endothermic effect, and influence cement strength and packing performance.Therefore
Before applying in cement slurry, need to carry phase-change material using specific process.The C14 proposed such as CN104559981A
Paraffin, polyethylene glycol 400, six water ferric bromides and zeolite powder carry out being mixed to form phase-changing energy storage material according to mass ratio 3:1:1:4,
Wherein zeolite belongs to porous material, is used as carrier, but this kind of energy storage material influences Behavior of Hardened Cement Paste final strength performance；
The method using suspension polymerisation that CN105733519A is proposed, phase-change material is sealed up for safekeeping in methyl methacrylate microballoon, and
Using special dispersing agent, hydrophilic phase-change microcapsule is developed, such microcapsules are added in cement slurry, can obviously reduce
Hydrated cementitious heat release, and it is smaller on the influence of cement strength performance, but this kind of phase-change microcapsule preparation process is more complex, it is right
The performance requirement for preparing material is higher, using the material of different batches, may cause microcapsules preparation failure, it is difficult to realize industry
Change.
Summary of the invention
The purpose of the present invention is to overcome above-mentioned the deficiencies in the prior art, provide a kind of phase-change accumulation energy microballoon and its preparation side
Method.This method preparation process is simple, is easy to industrial production, the phase-change accumulation energy microballoon of this method preparation on cement strength influence compared with
It is small.
To achieve the above object, the present invention adopts the following technical solutions:
A kind of preparation method of phase-change accumulation energy microballoon, using high-intensitive geopolymer tiny balloon as carrier, using true
Phase-change material is absorbed into the hollow interior of carrier microballoons, then the microballoon and asphalt mixtures modified by epoxy resin that will carry phase-change material by the method that empty pump is inhaled
Rouge is puddled, and epoxy resin is made to be coated in microsphere surface, and powder dispersing agent is added, and stirring disperses microballoon, to epoxy
After hardening of resin, extra powder dispersing agent is sieved, phase-change accumulation energy microballoon is obtained.
Preferably, the phase-change material is solid paraffin C18-30.
Preferably, the phase-change material dosage is the 10%~20% of geopolymer tiny balloon quality, and epoxy resin adds
Amount is the 5%~15% of geopolymer tiny balloon quality.
It is further preferred that the phase-change material dosage is the 10%~18% of geopolymer tiny balloon quality, epoxy
Resin dosage is the 8%~15% of geopolymer tiny balloon quality.
Preferably, the epoxy resin is aqueous or oiliness room temperature curing type epoxy resin.
Preferably, the ingredient of the powder dispersing agent is calcium carbonate superfine powder, silicon powder, metakaolin, graphite powder and ultra-fine mine
One or more of slag.
Preferably, the partial size of the powder dispersing agent is 1000~2000 mesh.
It is further preferred that the partial size of the powder dispersing agent is 1200~1500 mesh.
Preferably, the mixing speed that the microballoon is dispersed in powder dispersing agent is 100~500r/min, when stirring
Between be 0.5~2 hour.
It is further preferred that the mixing speed that the microballoon is dispersed in powder dispersing agent is 100~300r/min,
Mixing time is 0.5~1.5 hour.
The present invention also provides the phase-change accumulation energy microballoons by above-mentioned phase-change accumulation energy method for preparing microsphere preparation.
The high intensity geopolymer tiny balloon the preparation method comprises the following steps: by sodium hydroxide (NaOH), sodium metasilicate
(Na2SiO3·9H2O) and balling-up auxiliary agent is dissolved in the water to form solution A, and reactive powder is added in solution A and is uniformly mixed
Slurry B is formed afterwards, and slurry B is added in oily phase and is dispersed with stirring balling-up, after stirring, geopolymer microballoon is obtained by filtration, by microballoon
After cleaning, high-intensitive ground polymeric hollow microsphere is obtained after carrying out high-temperature calcination；Wherein, described NaOH, Na2SiO3·9H2O and at
The mass percent of ball auxiliary agent is (10~40%): (20~60%): (20~60%), the water and reactive powder mass ratio are
1:2~1, the slurry B account for the 5%~50% of the oily phase decentralized medium volume；The high-temperature calcination temperature is 800~1500
DEG C, calcination time is 1~8 hour.
The vacuum suction method particularly includes: the phase-change material of ground polymeric hollow microsphere and molten condition is placed in one
In open-top receptacle, open-top receptacle is placed in vacuum chamber, vacuum room temperature is higher than the fusing point of phase-change material, presses in -0.1MPa
Under power, 30~80min is vacuumized, microballoon, which is moved to refrigeration to phase-change material under 4 DEG C of environment from vacuum chamber, becomes solid, phase transformation material
Material is stored in the center portion of tiny balloon in solid form, obtains the microballoon for carrying phase-change material.
Beneficial effects of the present invention:
The preparation of a kind of preparation method of phase-change accumulation energy microballoon provided by the invention and current existing phase-change accumulation energy microballoon
Method is compared, and has simple process, the prices of raw materials are cheap, and from a wealth of sources, production cost is low, and what can be mass produced is excellent
Point.Phase-change accumulation energy microballoon provided by the invention can significantly reduce hydrated cementitious exothermic temperature peak value, and to the intensity of Behavior of Hardened Cement Paste
It influences smaller.
Detailed description of the invention
Above-mentioned and/or additional aspect of the invention and advantage will become from the description of the embodiment in conjunction with the following figures
Obviously and it is readily appreciated that, in which:
Fig. 1 is the micrograph of geopolymer tiny balloon；
Fig. 2 is micrograph of the present invention using the phase-change accumulation energy microballoon after calcium carbonate powder dispersion.
Fig. 3 is the micrograph for the paraffin being absorbed into geopolymer tiny balloon.
Specific embodiment
The present invention will be further elaborated with reference to the accompanying drawings and examples, it should which explanation, following the description is only
It is not to be defined to its content to explain the present invention.
High-intensitive geopolymer tiny balloon preparation method (referenced patent: 201710473085.9): sodium hydroxide
(NaOH) 1.5g, sodium metasilicate (Na2SiO3·9H2O) 5g and sodium chloride (NaCl) 3g are dissolved in 10g water and form solution A, by 10g
Slurry B is formed after being uniformly mixed in metakaolin addition solution A, slurry B is added in corn oil, slurry B accounts for corn oil
The 10% of volume, stirring make slurry B disperse balling-up, and mixing speed 550r/min stirs 2h, corn oil temperature 60 C, filtering
Geopolymer microballoon I is obtained, after microballoon is cleaned, obtains high intensity, porous ground polymeric hollow microsphere after 900 DEG C of high-temperature calcination 2h
(Fig. 1), gained high-intensitive ground polymerizing microballoons average grain diameter is 200 μm, 20-30 μm of microballoon wall thickness.
Embodiment 1
Using high-intensitive geopolymer tiny balloon as carrier, using the method for vacuum suction by phase-change material paraffin
C18-30 is absorbed into the hollow interior of carrier microballoons.The vasoliniment of ground polymerizing microballoons and molten condition is placed in an open-top receptacle
It is interior, open-top receptacle is placed in vacuum chamber, under -0.1MPa pressure, vacuumizes 60min, microballoon is moved into 4 DEG C of ice from vacuum chamber
Refrigeration to paraffin becomes solid to get to the microballoon (paraffin-ground polymerizing microballoons) for carrying phase-change material in case.Quality of Paraffin Waxes is
Paraffin-ground polymerizing microballoons and water-based room temperature solidified type epoxy resin are puddled, make asphalt mixtures modified by epoxy resin by the 15% of tiny balloon quality
Rouge is coated in microsphere surface, and epoxy resin quality is the 10% of tiny balloon quality, and it is 1200 mesh calcium carbonate that partial size, which is then added,
Powder dispersing agent, 100r/min stirs 0.5h, microballoon is dispersed, and after hardening of resin, extra powder dispersing agent is sieved
Point, obtain phase-change accumulation energy microsphere sample 1.
Embodiment 2
Using high-intensitive geopolymer tiny balloon as carrier, using the method for vacuum suction by phase-change material (C18-
30) it is absorbed into the hollow interior of carrier microballoons.The vasoliniment of ground polymerizing microballoons and molten condition is placed in an open-top receptacle,
Open-top receptacle is placed in vacuum chamber, under -0.1MPa pressure, vacuumizes 30min, microballoon is moved into 4 DEG C of refrigerators from vacuum chamber
Interior refrigeration to paraffin becomes solid to get to the microballoon (paraffin-ground polymerizing microballoons) for carrying phase-change material.Quality of Paraffin Waxes is sky
Paraffin-ground polymerizing microballoons and oiliness room temperature curing type epoxy resin are puddled, make epoxy resin by the 10% of heart microspheres quality
Coated in microsphere surface, epoxy resin quality is the 8% of tiny balloon quality, partial size is added then as 1500 mesh powdered graphites point
Powder, 150r/min stirs 1h, microballoon is dispersed, and after hardening of resin, extra powder dispersing agent is sieved, phase transformation is obtained
Storing-energy microspheres sample 2.
Embodiment 3
Using high-intensitive geopolymer tiny balloon as carrier, using the method for vacuum suction by phase-change material (C18-
30) it is absorbed into the hollow interior of carrier microballoons.The vasoliniment of ground polymerizing microballoons and molten condition is placed in an open-top receptacle,
Open-top receptacle is placed in vacuum chamber, under -0.1MPa pressure, vacuumizes 40min, microballoon is moved into 4 DEG C of refrigerators from vacuum chamber
Interior refrigeration to paraffin becomes solid to get to the microballoon (paraffin-ground polymerizing microballoons) for carrying phase-change material.Quality of Paraffin Waxes is sky
Paraffin-ground polymerizing microballoons and water-based room temperature solidified type epoxy resin are puddled, make epoxy resin by the 12% of heart microspheres quality
Coated in microsphere surface, epoxy resin quality is the 12% of tiny balloon quality, and it is 1500 mesh silica fume powders that partial size, which is then added,
Dispersing agent, 150r/min stirs 0.5h, microballoon is dispersed, and after hardening of resin, extra powder dispersing agent is sieved, is obtained
Phase-change accumulation energy microsphere sample 3.
Embodiment 4
Using high-intensitive geopolymer tiny balloon as carrier, using the method for vacuum suction by phase-change material (C18-
30) it is absorbed into the hollow interior of carrier microballoons.The vasoliniment of ground polymerizing microballoons and molten condition is placed in an open-top receptacle,
Open-top receptacle is placed in vacuum chamber, under -0.1MPa pressure, vacuumizes 80min, microballoon is moved into 4 DEG C of refrigerators from vacuum chamber
Interior refrigeration to paraffin becomes solid to get to the microballoon (paraffin-ground polymerizing microballoons) for carrying phase-change material.Quality of Paraffin Waxes is sky
Paraffin-ground polymerizing microballoons and oiliness room temperature curing type epoxy resin are puddled, make epoxy resin by the 18% of heart microspheres quality
Coated in microsphere surface, epoxy resin quality is the 15% of tiny balloon quality, and it is 1500 mesh ultrafine slags that partial size, which is then added,
Powder dispersing agent, 300r/min stirs 1.5h, microballoon is dispersed, and after hardening of resin, extra powder dispersing agent is sieved
Point, obtain phase-change accumulation energy microsphere sample 4.
Fig. 2 is the micrograph of phase-change accumulation energy microsphere sample 1, it can be seen that microsphere surface uniform fold has epoxy resin, and
After the dispersion of calcium carbonate powder dispersing agent, microballoon dispersion effect is good, without agglomeration；Choose phase-change accumulation energy microsphere sample 1
The microballoon of middle rupture carries out microexamination, as shown in Figure 3, it can be seen that paraffin is successfully absorbed into geopolymer tiny balloon
It is interior.
Above-mentioned difference phase-change accumulation energy microsphere sample comments the hydration heat temperature of cement slurry and the impact effect of compression strength
Valence is as shown in table 1.
Influence result of the 1 phase-change accumulation energy microsphere sample of table to cement slurry property
Evaluation result shows that the addition of phase-change accumulation energy microballoon significantly reduces hydrated cementitious exothermic temperature peak value, and to cement
Stone intensity effect is smaller.
Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not protects model to the present invention
The limitation enclosed, based on the technical solutions of the present invention, those skilled in the art are not needed to make the creative labor and can be done
Various modifications or changes out are still within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of phase-change accumulation energy microballoon, which is characterized in that using high-intensitive geopolymer tiny balloon as load
Phase-change material is absorbed into the hollow interior of carrier microballoons using the method for vacuum suction, then will carry the micro- of phase-change material by body
Ball is puddled with epoxy resin, and epoxy resin is made to be coated in microsphere surface, and powder dispersing agent is added, and stirring carries out microballoon
Extra powder dispersing agent is sieved after epoxy resin solidification, obtains phase-change accumulation energy microballoon by dispersion；
The high intensity geopolymer tiny balloon the preparation method comprises the following steps: sodium hydroxide, sodium metasilicate and balling-up auxiliary agent are dissolved in
Solution A is formed in water, reactive powder is added in solution A after being uniformly mixed and is formed slurry B, slurry B is added in oily phase
It is dispersed with stirring balling-up, after stirring, geopolymer microballoon is obtained by filtration, after microballoon is cleaned, is obtained after progress high-temperature calcination high-strength
Degree ground polymeric hollow microsphere；Wherein, described NaOH, Na2SiO3·9H2The mass percent of O and balling-up auxiliary agent be (10~
40%): (20~60%): (20~60%), the water and reactive powder mass ratio are 1:2~1, and the slurry B accounts for the oil
The 5%~50% of phase decentralized medium volume；The high-temperature calcination temperature is 800~1500 DEG C, and calcination time is 1~8 hour；Institute
Stating balling-up auxiliary agent is sodium chloride.
2. a kind of preparation method of phase-change accumulation energy microballoon according to claim 1, which is characterized in that the phase-change material is
Solid paraffin C18-30.
3. a kind of preparation method of phase-change accumulation energy microballoon according to claim 1, which is characterized in that the phase-change material adds
Amount is the 10%~20% of geopolymer tiny balloon quality, and epoxy resin dosage is the 5% of geopolymer tiny balloon quality
~15%.
4. a kind of preparation method of phase-change accumulation energy microballoon according to claim 1, which is characterized in that the epoxy resin is
Aqueous or oiliness room temperature curing type epoxy resin.
5. a kind of preparation method of phase-change accumulation energy microballoon according to claim 1, which is characterized in that the powder dispersing agent
Ingredient is one or more of calcium carbonate superfine powder, silicon powder, metakaolin, graphite powder and ultrafine slag.
6. a kind of preparation method of phase-change accumulation energy microballoon according to claim 1, which is characterized in that the powder dispersing agent
Partial size be 1000~2000 mesh.
7. a kind of preparation method of phase-change accumulation energy microballoon according to claim 1, which is characterized in that the microballoon is in powder
The mixing speed dispersed in dispersing agent is 100~500r/min, and mixing time is 0.5~2 hour.
8. the phase-change accumulation energy microballoon of the preparation of preparation method described in claim 1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710952207.2A CN107500591B (en) | 2017-10-13 | 2017-10-13 | A kind of phase-change accumulation energy microballoon and preparation method thereof |
| US16/485,450 US11685683B2 (en) | 2017-06-21 | 2018-05-25 | High-strength geopolymer hollow microsphere, preparation method thereof and phase change energy storage microsphere |
| PCT/CN2018/088411 WO2018233449A1 (en) | 2017-06-21 | 2018-05-25 | High-strength polymer hollow microsphere, preparation method therefor, and phase transition energy storage microsphere |
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| CN201710952207.2A CN107500591B (en) | 2017-10-13 | 2017-10-13 | A kind of phase-change accumulation energy microballoon and preparation method thereof |
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| WO2018233449A1 (en) * | 2017-06-21 | 2018-12-27 | 中国石油大学(华东) | High-strength polymer hollow microsphere, preparation method therefor, and phase transition energy storage microsphere |
| CN112442337A (en) * | 2019-08-29 | 2021-03-05 | 张立强 | Resin type phase change energy storage material and preparation method thereof |
| CN112898956A (en) * | 2021-01-27 | 2021-06-04 | 西安工程大学 | Temperature-responsive well cementation cement slurry and preparation method thereof |
| CN114790089B (en) * | 2022-06-15 | 2023-08-25 | 中国石油大学(华东) | Preparation method and device of wide-range temperature-regulating heat storage microcapsule |
| CN116119955A (en) * | 2023-02-08 | 2023-05-16 | 哈尔滨工业大学 | Preparation method of phase-change energy-storage microspheres for building |
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| CN101555401B (en) * | 2008-04-10 | 2011-12-21 | 中国科学院化学研究所 | Microcapsule of organic phase change energy storage material and preparation method thereof |
| CN104496544A (en) * | 2014-12-30 | 2015-04-08 | 深圳大学 | Phase change energy storage ceramsite and preparation method thereof |
| CN106215854A (en) * | 2016-09-30 | 2016-12-14 | 东莞深圳清华大学研究院创新中心 | A kind of coal ash for manufacturing is for the method for ceramic adsorbent articles |
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