CN107880852A - The preparation of paraffin/silicon rubber phase-change microcapsule - Google Patents

The preparation of paraffin/silicon rubber phase-change microcapsule Download PDF

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Publication number
CN107880852A
CN107880852A CN201711169824.1A CN201711169824A CN107880852A CN 107880852 A CN107880852 A CN 107880852A CN 201711169824 A CN201711169824 A CN 201711169824A CN 107880852 A CN107880852 A CN 107880852A
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China
Prior art keywords
paraffin
silicon rubber
change microcapsule
preparation
rubber phase
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CN201711169824.1A
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Chinese (zh)
Inventor
张佳星
谢忱
张鑫鑫
周敏
桑成功
冒海波
鲁天暄
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Nanjing Institute of Technology
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Nanjing Institute of Technology
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Priority to CN201711169824.1A priority Critical patent/CN107880852A/en
Publication of CN107880852A publication Critical patent/CN107880852A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/02Materials undergoing a change of physical state when used
    • C09K5/06Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
    • C09K5/063Materials absorbing or liberating heat during crystallisation; Heat storage materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

The invention discloses the preparation method and characterizing method of paraffin silicon rubber phase-change microcapsule, it is characterised in that:Including:Material is the core of paraffin, and silicon rubber is the composite of wall material composition.The present invention provides the preparation method and characterizing method of paraffin silicon rubber phase-change microcapsule, can realize the heat insulation function of material, and preparation cost is cheap, and technique is simple, preparation process green non-pollution;Have wide practical use in construction material and other insulation materials.

Description

The preparation of paraffin/silicon rubber phase-change microcapsule
Technical field
The present invention relates to a kind of paraffin silicon rubber phase-change microcapsule composite and preparation method thereof, more particularly to a kind of use In paraffin silicon rubber phase-change microcapsule composite of building heat preservation and preparation method thereof, belong to insulation material technical field.
Background technology
The most great threat of 21st century facing mankind is global warming, and architectural energy consumption accounts for global energy consumption 40% and with the discharge of greenhouse gases, very important effect is played in global warming.Therefore building field pair is improved The utilization rate of the energy, it is very helpful to slowing down energy crisis and solving environmental problem.Paraffin is as phase-changing energy storage material (phase change materials, PCM) has a higher latent heat of phase change, no supercooling and precipitation phenomenon and cheap extensive Using in construction material.But paraffin can not incite somebody to action when absorption outside energy is changed into liquid phase by solid phase because seepage can occur for flowing Energy stores, therefore paraffin need to be packaged.Phase-change material micro-capsule (Microencapsulated Phase Change Materials, MEPCM) microencapsulation technology is utilized, paraffin is coated to form molecule using inorganic or organic compound, When paraffin capsule-core is undergone phase transition, outer layer cyst wall remains solid-state, therefore is graininess before and after phase transformation, solves phase transition process The mobility of middle paraffin.But traditional cyst material without creep properties and wall thickness be micro/nano level it is other in the case of, it is impossible to support Volumetric expansion and contraction of the paraffin capsule-core in solid-liquid phase change, also due to cyst wall ruptures and seepage occurs.Therefore need to develop New microcapsule wall material, silicon rubber itself possess creep properties and to the clad ratio height of paraffin;, can be significantly compared with traditional material Improve microcapsules service life.
The content of the invention
The technical problems to be solved by the invention are to prepare a kind of physical property, and mechanical performance is preferable with chemical property, and And the heat-resisting preferable material of cold tolerance, and require the service life length of the material;Further, the present invention provides a kind of micro- The preparation method of capsule, method preparation cost is cheap, and technique is simple, preparation process green non-pollution, utilizes silicon rubber and paraffin The chemical stability and heat resistance of microballoon, using the paraffin microballoon of independent research as modifying agent, prepare with good heat insulating ability The material of energy;Further, the present invention provides a kind of preparation method of the paraffin microballoon of micro-meter scale, paraffin prepared by the method Microballoon adds the chemical stability of the microcapsules of the present invention, and utilizes the heat resistance of fluorosioloxane rubber, stability and mechanicalness Can, high a kind of service life is made, chemical stability is good, the high insulation material of mechanical bonding strength.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
Paraffin silicon rubber phase-change microcapsule composite, it is characterised in that:Including:Material is silicon rubber and paraffin microballoon group Into silicon rubber/paraffin microsphere compound.
The material of the silicon rubber includes model H1100 RTV fluorocarbon silicone rubbers.
The paraffin microballoon for micro-meter scale of the paraffin microballoon.
The preparation method of paraffin silicon rubber phase-change microcapsule composite, it is characterised in that:Comprise the following steps:
S01, paraffin microballoon is weighed in mass ratio and is placed in beaker, adds the appropriate aqueous solution, is adding surface thereto Activating agent is sufficiently stirred 5min;Described mass ratio is paraffin: surfactant=10: 2~3.
S02, silicon rubber is weighed in mass ratio, curing agent is added after stirring, then be sufficiently stirred 1~2min, Obtain mixed liquor;The mass ratio is silicon rubber: paraffin microballoon=10~5: 1~2;
S03, it will filter or centrifuge in the mixed liquor in step S02, the solid particle of gained is placed in surface plate, Treat its natural drying.
Curing agent is prepared for laboratory, generally the 1/10 of silicon rubber addition
The preparation method of the paraffin microballoon comprises the following steps:
Step 1, water and 3.75g Triton X-100 are added in three-neck flask, is put into 70 DEG C~80 DEG C perseverances 10~15min is heated in warm water bath, 2~3min is stirred with electric mixer;
Step 2, by the paraffin wax of solid-state, heating melting, form liquid paraffin;With the speed of per minute 3~5 drops, delay Slowly it is added drop-wise in three-neck flask, after constant temperature persistently stirs 2h, obtains paraffin wax emulsions;
Step 3, paraffin wax emulsions are poured into beaker, be aged 12h at room temperature;Upper strata accumulation of solids is pulled out, at room temperature certainly So dry, obtain paraffin microballoon.
Paraffin microballoon main body of the present invention, silicon rubber film is polymerize on its body structure surface, and enter one using silicon rubber microballoon Walk reinforcing material heat-insulating property.
Paraffin is 58~60 DEG C higher of paraffin wax of fusing point.
The present invention application method be:The paraffin silicon rubber phase-change microcapsule composite of the present invention is applied in wall Instead of yellow sand cement concrete or other insulation materials.
A kind of mutually paraffin silicon rubber phase-change microcapsule composite and preparation method thereof provided by the invention, utilizes fluorine silicon rubber The heat resistance and cold resistance of glue, using the paraffin microballoon of independent research as core, prepare the material that can be incubated;This Invention is cheap using raw materials such as silicon rubber and paraffin, and preparation technology is simple, pollution-free;The material is mainly characterized by continuously growing Time uses, and simple to operate without regeneration treatment, easy to use, this method combines paraffin microballoon with fluorosioloxane rubber, no It is only capable of strengthening the service life of the material, moreover it is possible to the physical property, mechanical performance and chemical property of paraffin are strengthened, The development of construction industry in future can be advanced with substituting now architectural reinforced cement concrete used well.The present invention A kind of paraffin silicon rubber phase-change microcapsule composite provided and preparation method thereof, preparation cost is cheap, and technique is simple, prepares Process green non-pollution;Have wide practical use in field of heat insulating materials (such as construction material etc.).
Brief description of the drawings
Fig. 1 is the enlarged drawing of paraffin in the present invention/silicon rubber phase-change microcapsule;
Fig. 2 is the DSC curve figure of paraffin in the present invention/silicon rubber phase-change microcapsule;
Fig. 3 is the infrared spectrogram of paraffin in the present invention/silicon rubber phase-change microcapsule.
Embodiment
The present invention is further described below in conjunction with the accompanying drawings.
Embodiment 1:
As shown in Figures 1 to 3, paraffin silicon rubber phase-change microcapsule composite, it is characterised in that:Including:Material silicon rubber With silicon rubber/paraffin microsphere compound of paraffin microballoon composition.
The material of the silicon rubber includes model H1100 RTV fluorocarbon silicone rubbers (Shenzhen Guan Heng Co., Ltds).
The paraffin microballoon for micro-meter scale of the paraffin microballoon.
The preparation method of paraffin silicon rubber phase-change microcapsule composite, it is characterised in that:Comprise the following steps:
S01, paraffin microballoon is weighed in mass ratio and is placed in beaker, adds the appropriate aqueous solution, is adding surface thereto Activating agent is sufficiently stirred 5min;Described mass ratio is paraffin: surfactant=10: 2.
S02, weigh silicon rubber in mass ratio, added after stirring curing agent (curing agent: silicon rubber=1: 10), then 1~2min is sufficiently stirred, obtains mixed liquor;The mass ratio is silicon rubber: paraffin microballoon=5: 2;
S03, it will filter or centrifuge in the mixed liquor in step S02, the solid particle of gained is placed in surface plate, Treat its natural drying.
The preparation method of the paraffin microballoon comprises the following steps:
Step 1, add water in three-neck flask and a certain amount of Triton X-100 is (pungent according to polyethylene glycol Base phenyl ether: paraffin microballoon=4: 1 adds), 10~20min of heating in 70 DEG C~80 DEG C thermostat water baths is put into water-bath, 2~3min is stirred with electric mixer;
Step 2, by the paraffin wax of solid-state, heating melting, form liquid paraffin;With the speed of per minute 3~5 drops, delay Slowly it is added drop-wise in three-neck flask, after constant temperature persistently stirs 10~15min, obtains paraffin wax emulsions;
Step 3, paraffin wax emulsions are poured into beaker, be aged 12h at room temperature;Upper strata accumulation of solids is pulled out, at room temperature certainly So dry, obtain paraffin microballoon.
Embodiment 2:
As shown in Figures 1 to 3, paraffin silicon rubber phase-change microcapsule composite, it is characterised in that:Including:Material is silicon rubber Silicon rubber/paraffin microsphere compound of glue and paraffin microballoon composition.
The material of the silicon rubber includes model H1100 RTV fluorocarbon silicone rubbers (Shenzhen Guan Heng Co., Ltds).
The paraffin microballoon for micro-meter scale of the paraffin microballoon.
The preparation method of paraffin silicon rubber phase-change microcapsule composite, it is characterised in that:Comprise the following steps:
S01, paraffin microballoon is weighed in mass ratio and is placed in beaker, adds the appropriate aqueous solution, is adding surface thereto Activating agent is sufficiently stirred 5min;Described mass ratio is paraffin: surfactant=10: 3.
S02, weigh silicon rubber in mass ratio, added after stirring curing agent (curing agent: silicon rubber=1: 10), then 1~2min is sufficiently stirred, obtains mixed liquor;The mass ratio is silicon rubber: paraffin microballoon=5: 2;
S03, it will filter or centrifuge in the mixed liquor in step S02, the solid particle of gained is placed in surface plate, Treat its natural drying.
The preparation method of the paraffin microballoon comprises the following steps:
Step 1, water is added in three-neck flask and adds a certain proportion of curing agent and (presses curing agent: silicon rubber=1: 10 Add), be put into water-bath in 70 DEG C~80 DEG C thermostat water baths 10~15min of heating, with electric mixer stirring 2~ 3min;
Step 2, by the paraffin wax of solid-state, heating melting, form liquid paraffin;With the speed of per minute 3~5 drops, delay Slowly it is added drop-wise in three-neck flask, after constant temperature persistently stirs 10~15min, obtains paraffin wax emulsions;
Step 3, paraffin wax emulsions are poured into beaker, be aged 12h at room temperature;Upper strata accumulation of solids is pulled out, at room temperature certainly So dry, obtain paraffin microballoon.
Described above is only the preferred embodiment of the present invention, it should be pointed out that:For the ordinary skill people of the art For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should It is considered as protection scope of the present invention.

Claims (7)

1. paraffin silicon rubber phase-change microcapsule composite, it is characterised in that:Including:Described main body is paraffin silicon rubber phase transformation Microcapsules.
2. paraffin silicon rubber phase-change microcapsule composite according to claim 1, it is characterised in that:The material of the paraffin Matter includes the paraffin wax that molecular weight is [8002-74-2].
3. paraffin silicon rubber phase-change microcapsule composite according to claim 1, it is characterised in that:The silicon rubber Material includes model H1100 vulcanization fluorosioloxane rubber.
4. paraffin silicon rubber phase-change microcapsule composite according to claim 1, it is characterised in that:The paraffin microballoon For the paraffin microballoon of micro-meter scale.
5. the preparation method of the paraffin silicon rubber phase-change microcapsule composite according to any one of Claims 1 to 4, it is special Sign is:Comprise the following steps:
S01, paraffin microballoon is weighed in mass ratio and is placed in beaker, adds the appropriate aqueous solution, is adding surface-active thereto Agent is sufficiently stirred 5min;Described mass ratio is paraffin: surfactant=10: 2~3.
S02, silicon rubber is weighed in mass ratio, curing agent is added after stirring, then be sufficiently stirred 1~2min, obtain mixed Close liquid;The mass ratio is silicon rubber: paraffin microballoon=10~5: 1;
S03, it will filter or centrifuge in the mixed liquor in step S02, the solid particle of gained is placed in surface plate, treats it Natural drying.
6. the preparation method of paraffin silicon rubber phase-change microcapsule composite according to claim 5, it is characterised in that:Institute The preparation method for stating paraffin microballoon comprises the following steps:
Step 1, water and surfactant are added in three-neck flask: paraffin=4: 1 surfactant, places into 70~80 10~15min is heated in DEG C thermostat water bath, 2~3min is stirred with electric mixer;
Step 2, by the paraffin wax of solid-state, heating melting, form liquid paraffin;With the speed of per minute 3~5 drops, slowly drip It is added in the three-neck flask of step 1, after constant temperature persistently stirs 2~2.5h, obtains paraffin wax emulsions;
Step 3, paraffin wax emulsions are poured into beaker, be aged at least 12h at room temperature;Upper strata accumulation of solids is pulled out, at room temperature certainly So dry, obtain paraffin microballoon.
7. the preparation method of paraffin silicon rubber phase-change microcapsule composite according to claim 6, it is characterised in that:Institute Stating surfactant includes Triton X-100.
CN201711169824.1A 2017-11-16 2017-11-16 The preparation of paraffin/silicon rubber phase-change microcapsule Pending CN107880852A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113414869A (en) * 2021-06-07 2021-09-21 中建材创新科技研究院有限公司 Phase-change building material product with temperature control performance and preparation method thereof
CN115322599A (en) * 2022-08-31 2022-11-11 上海大学 Temperature-control coating, preparation method and application thereof
CN117603621A (en) * 2023-12-01 2024-02-27 胜利油田金岛实业有限责任公司 Anti-scale and anti-corrosion coating for oil pipe and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103933907A (en) * 2014-05-15 2014-07-23 中国工程物理研究院激光聚变研究中心 Preparation method of elastic phase change microcapsules
CN105080185A (en) * 2015-08-14 2015-11-25 南京工程学院 Interpenetrating network type porous polymer with adjustable and controllable surface performance and preparation method of interpenetrating network type porous polymer

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103933907A (en) * 2014-05-15 2014-07-23 中国工程物理研究院激光聚变研究中心 Preparation method of elastic phase change microcapsules
CN105080185A (en) * 2015-08-14 2015-11-25 南京工程学院 Interpenetrating network type porous polymer with adjustable and controllable surface performance and preparation method of interpenetrating network type porous polymer

Non-Patent Citations (1)

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Title
于强强: ""石蜡类相变材料微胶囊的制备与表征"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113414869A (en) * 2021-06-07 2021-09-21 中建材创新科技研究院有限公司 Phase-change building material product with temperature control performance and preparation method thereof
CN115322599A (en) * 2022-08-31 2022-11-11 上海大学 Temperature-control coating, preparation method and application thereof
CN117603621A (en) * 2023-12-01 2024-02-27 胜利油田金岛实业有限责任公司 Anti-scale and anti-corrosion coating for oil pipe and preparation method thereof
CN117603621B (en) * 2023-12-01 2024-04-23 胜利油田金岛实业有限责任公司 Anti-scale and anti-corrosion coating for oil pipe and preparation method thereof

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Application publication date: 20180406