CN104650816A - Low-temperature phase-change energy storage microcapsule and preparation method thereof - Google Patents
Low-temperature phase-change energy storage microcapsule and preparation method thereof Download PDFInfo
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- CN104650816A CN104650816A CN201510063676.XA CN201510063676A CN104650816A CN 104650816 A CN104650816 A CN 104650816A CN 201510063676 A CN201510063676 A CN 201510063676A CN 104650816 A CN104650816 A CN 104650816A
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Abstract
The invention discloses a low-temperature phase-change energy storage microcapsule and a preparation method thereof. According to the microcapsule, polymethyl methacrylate is used as a wall material and a binary organic phase-change material is used as a core material; the microcapsule is prepared by coating the binary organic phase-change material with polymethyl methacrylate by an emulsion polymerization method. The preparation method comprise the following steps: mixing deionized water, an emulsifier and a co-emulsifier by ultrasound to obtain a continuous-phase mixed solution needed in emulsion polymerization; orderly adding the binary organic phase-change material prepared according to a certain mass ratio and methyl methacrylate, carrying out shearing stirring to obtain an O/W emulsion; then adding a small amount of an initiator, filtrating, washing and drying to obtain a phase-change microcapsule material. The low-temperature phase-change energy storage microcapsule prepared according to the invention has the advantages of simple process, moderate reaction conditions, stable structure, high encapsulation rate, appropriate phase-change temperature and relatively high phase-change latent heat and therefore can be put into industrial production easily.
Description
Technical field
The invention belongs to technical field of phase-change energy storage, be specifically related to a kind of low temperature phase change accumulation energy microcapsule and preparation method thereof.
Background technology
Phase change material refers to and utilizes material heat absorption and release in phase transition process, carries out the storage of heat energy and the material of release, has control environment temperature and the object of carrying out heat storage.Traditional phase change material mostly existed cold, the defect such as be separated, and particularly for solid-liquid phase change material, there is easily flowing and leakage phenomenon in use procedure.At present, be that phase change material is carried out composite shape-setting mostly, by contrast, the microcapsule encapsulation technology of phase change material is good treatment process.
Microcapsule encapsulation technology is that phase change material carries out coatedly making its technology forming fine particle by a kind of high molecular polymer that utilizes.Encapsulated by microcapsule, can avoid revealing during phase change material phase-state change, and prevent phase change material to contact with the direct of external environment, expand the use range of phase change material.The phase-change microcapsule core reported at present has the tetradecane, octadecane, docosane etc., but has no report with n-dodecanol by the microcapsule that the binary organic phase change material that certain mass proportioning mixes is core with n-tetradecane.The wall material of the phase-change microcapsule reported at present has urea-formaldehyde resin, melamine urea-formaldehyde resin, melmac etc., but these wall materials in use can discharge the obnoxious flavoures such as formaldehyde.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, and low temperature energy storage phase-change microcapsule providing a kind of energy-storage property stable and preparation method thereof, this microencapsulation material with the polymethylmethacrylate of methyl methacrylate polymerization for wall material, this wall material can not discharge the obnoxious flavoures such as formaldehyde in life-time service process, safety and environmental protection, and polymerization process is simple, with n-tetradecane, n-dodecanol is core by the binary organic phase change material of certain mass ratio mixing, preparation process is simple, reaction conditions is gentle, Stability Analysis of Structures, encapsulation rate is high, and there is applicable transformation temperature and higher latent heat of phase change, be easy to suitability for industrialized production.
The technical scheme realizing the object of the invention is:
A kind of low temperature phase change accumulation energy microcapsule, is made up of core, wall material, emulsifying agent, initiator and deionized water; Described core is be the binary organic phase change material that the n-tetradecane of 8:2 and n-dodecanol are mixed by quality proportioning;
Described wall material is the polymethylmethacrylate (PMMA) be polymerized by methyl methacrylate (MMA);
Also comprise assistant for emulsifying agent;
The proportioning of the weight part of raw material is: binary organic phase change material 5-6.7 part, methyl methacrylate 3.3-5 part, emulsifying agent 0.5-1.5 part, assistant for emulsifying agent 0.2 part, initiator 0.2 part, deionized water 40 parts.
Described low temperature phase change accumulation energy microcapsule, is composited by the wall material of binary organic phase change material and coated phase-change material, and wherein the encapsulation rate of phase change material is 10%-65%.
Described emulsifying agent is Sodium dodecylbenzene sulfonate (DBSA).
Described assistant for emulsifying agent is n-hexadecane.
Described initiator is Diisopropyl azodicarboxylate (AIBN).
The transformation temperature of described binary organic phase change material is-20 DEG C ~ 0 DEG C, and phase transformation enthalpy is greater than 150 J/g.
The latent heat of phase change of described microcapsules of storing energy through phase change is 24.80 J/g ~ 132.397 J/g;
The preparation method of described low temperature phase change accumulation energy microcapsule material, comprises the following steps:
Step 1, takes each raw material by weight ratio, binary organic phase change material 5-6.7 part that the n-tetradecane of quality proportioning 8:2 and n-dodecanol are mixed, methyl methacrylate 3.3-5 part, emulsifying agent 0.5-1.5 part, assistant for emulsifying agent 0.2 part, initiator 0.2 part, deionized water 40 parts;
Step 2, joins in deionized water by emulsifying agent, assistant for emulsifying agent, is ultrasonicly mixed evenly;
Step 3, joins in the mixing solutions of step 2 by binary organic phase change material, stirs at ambient temperature, obtain O/W type emulsion with the rotating speed cutting of 1000 ~ 2000 rpm;
Step 4, is slowly added dropwise to methyl methacrylate in the type of O/W described in step 2 emulsion, stirs 1 h at ambient temperature with the rotating speed cutting of 1000-2000 rpm, obtains new O/W type emulsion;
Step 5, raised temperature 50 DEG C ~ 75 DEG C, slowly drips initiator, rotating speed is down to 100 ~ 200 rpm simultaneously, polyreaction 2-6 h, carry out breakdown of emulsion, filtration, washing and drying treatment successively afterwards, obtained low temperature phase change accumulation energy microcapsule.
Wherein, the breaking method described in step 5 is: in the emulsion after polyreaction, add saturated nacl aqueous solution, stratification.
Wherein, the drying treatment described in step 5 is: in temperature be under the condition of 40 DEG C vacuum-drying to constant weight.
The present invention compared with prior art has significant advantage: (1) Stability Analysis of Structures.The present invention adopts Microencapsulation techniques, prevents the leakage of phase change material when phase-state change and the contact with environment, thus the stable circulation performance of this material is stablized.(2) transformation temperature meets the requirement of low temperature energy, and has larger phase transformation enthalpy, and transformation temperature is constant.(3) preparation process is simple, and reaction conditions is gentle.(4) environment-protecting asepsis.The wall material used due to these microcapsule is the polymethylmethacrylate by methyl methacrylate polymerization, in use can not discharge obnoxious flavoures such as the formaldehyde of human body and bad environmental.(5) microcapsules of storing energy through phase change uniform particle sizes of the present invention, compact structure, temperature control is good, has larger use value.
Accompanying drawing explanation
Fig. 1 is the SEM photo of embodiment 1;
Fig. 2 is the DSC test result of embodiment 1;
Fig. 3 is the SEM photo of embodiment 2;
Fig. 4 is the DSC test result of embodiment 2;
Fig. 5 is the SEM photo of embodiment 3;
Fig. 6 is the DSC test result of embodiment 3.
Embodiment
Below in conjunction with embodiment and accompanying drawing, content of the present invention is further described, but is not limitation of the invention.
Embodiment 1
A preparation for low temperature phase change accumulation energy microcapsule, its step is as follows:
Step 1, joins in 40g deionized water by 0.5g emulsifying agent, 0.2g assistant for emulsifying agent respectively, is ultrasonicly mixed evenly;
Step 2, is that the binary organic phase change material that the n-tetradecane of 8:2 and n-dodecanol are mixed joins in the mixing solutions of step 1 by 5g mass ratio, stirs at ambient temperature, obtain O/W type emulsion with the rotating speed cutting of 1000-2000 rpm;
Step 3, is slowly added dropwise to 5g methyl methacrylate (MMA) in the type of O/W described in step 2 emulsion, stirs 1 h at ambient temperature with the rotating speed cutting of 1000-2000 rpm, obtains new O/W type emulsion;
Step 4, increases the temperature to 75 DEG C, slowly drips 0.2g initiator Diisopropyl azodicarboxylate (AIBN), rotating speed is down to 200 rpm, polyreaction 5-6 h simultaneously, carries out breakdown of emulsion, filtration, washing and drying treatment successively afterwards, obtain low temperature phase change accumulation energy microcapsule.
The SEM photo of this embodiment and DSC test result are respectively as shown in Figure 1 and Figure 2.
The transformation temperature of gained low temperature phase change accumulation energy microcapsule material is-6.711 DEG C, and latent heat of phase change value is 24.82 J/g.
Embodiment 2
A preparation for low temperature phase change accumulation energy microcapsule, its step is as follows:
Step 1, joins in 40g deionized water by 1.0g emulsifying agent, 0.2g assistant for emulsifying agent respectively, is ultrasonicly mixed evenly;
Step 2, joins in the mixing solutions of step 1 by the binary organic phase change material that the n-tetradecane of 5g mass ratio 8:2 and n-dodecanol are mixed, and stirs at ambient temperature, obtain O/W type emulsion with the rotating speed cutting of 1000-2000 rpm;
Step 3, is slowly added dropwise to 5g methyl methacrylate (MMA) in the type of O/W described in step 2 emulsion, stirs 1 h at ambient temperature with the rotating speed cutting of 1000-2000 rpm, obtains new O/W type emulsion;
Step 4, increases the temperature to 75 DEG C, slowly drips 0.2g initiator Diisopropyl azodicarboxylate (AIBN), rotating speed is down to 200 rpm, polyreaction 5-6 h simultaneously, carries out breakdown of emulsion, filtration, washing and drying treatment successively afterwards, obtain low temperature phase change accumulation energy microcapsule.
The SEM photo of this embodiment and DSC test result are respectively as shown in Figure 3, Figure 4.
The transformation temperature of gained low temperature phase change accumulation energy microcapsule material is-6.136 DEG C, and latent heat of phase change value is 82.522 J/g.
Embodiment 3
A preparation for low temperature phase change accumulation energy microcapsule, its step is as follows:
Step 1, joins in 40g deionized water by 1.0g emulsifying agent, 0.2g assistant for emulsifying agent respectively, is ultrasonicly mixed evenly;
Step 2, joins in the mixing solutions of step 1 by the binary organic phase change material that the n-tetradecane of 6g quality proportioning 8:2 and n-dodecanol are mixed, and stirs at ambient temperature, obtain O/W type emulsion with the rotating speed cutting of 1000-2000 rpm;
Step 3, is slowly added dropwise to 4g methyl methacrylate (MMA) in the type of O/W described in step 2 emulsion, stirs 1 h at ambient temperature with the rotating speed cutting of 1000-2000 rpm, obtains new O/W type emulsion;
Step 4, increases the temperature to 75 DEG C, slowly drips 0.2g initiator Diisopropyl azodicarboxylate (AIBN), rotating speed is down to 200 rpm simultaneously, polyreaction 5-6 h, carries out breakdown of emulsion, filtration, washing and drying treatment afterwards successively, obtains low temperature phase change accumulation energy microcapsule.
The SEM photo of this embodiment and DSC test result are respectively as shown in Figure 5, Figure 6.
The transformation temperature of gained low temperature phase change accumulation energy microcapsule material is-5.474 DEG C, and latent heat of phase change value is 132.397 J/g.
The foregoing is only preferred embodiment of the present invention, be not used for limiting practical range of the present invention, so the equivalent change of all feature raw materials according to scope of the present invention, characterization step and improvement, all should be included within claim of the present invention.
Claims (9)
1. a low temperature phase change accumulation energy microcapsule, be made up of core, wall material, emulsifying agent, initiator and deionized water, it is characterized in that:
Described core is be the binary organic phase change material that the n-tetradecane of 8:2 and n-dodecanol are mixed by quality proportioning;
Described wall material is by the polymethylmethacrylate of methyl methacrylate polymerization;
Also comprise assistant for emulsifying agent;
The proportioning of the weight part of raw material is: binary organic phase change material 5-6.7 part, methyl methacrylate 3.3-5 part, emulsifying agent 0.5-1.5 part, assistant for emulsifying agent 0.2 part, initiator 0.2 part, deionized water 40 parts.
2. low temperature phase change accumulation energy microcapsule according to claim 1, is characterized in that: described emulsifying agent is Sodium dodecylbenzene sulfonate.
3. low temperature phase change accumulation energy microcapsule according to claim 1, is characterized in that: described assistant for emulsifying agent is n-hexadecane.
4. low temperature phase change accumulation energy microcapsule according to claim 1, is characterized in that: described initiator is Diisopropyl azodicarboxylate.
5. low temperature phase change accumulation energy microcapsule according to claim 1, is characterized in that: the transformation temperature of described binary organic phase change material is-20 DEG C ~ 0 DEG C, and phase transformation enthalpy is greater than 150 J/g.
6. low temperature phase change accumulation energy microcapsule according to claim 1, is characterized in that: the latent heat of phase change of described low temperature phase change accumulation energy microcapsule is 24.80 J/g ~ 132.397 J/g.
7. the preparation method of the low temperature phase change accumulation energy microcapsule according to claim 1,2,3,4, is characterized in that comprising the following steps:
Step 1, takes each raw material by weight ratio, and quality proportioning is binary organic phase change material 5-6.7 part that the n-tetradecane of 8:2 and n-dodecanol are mixed, methyl methacrylate 3.3-5 part, emulsifying agent 0.5-1.5 part, assistant for emulsifying agent 0.2 part, initiator 0.2 part, deionized water 40 parts;
Step 2, joins in deionized water by emulsifying agent, assistant for emulsifying agent, is ultrasonicly mixed evenly;
Step 3, joins in the mixing solutions of step 2 by binary organic phase change material, stirs at ambient temperature, obtain O/W type emulsion with the rotating speed cutting of 1000 ~ 2000 rpm;
Step 4, is slowly added dropwise to methyl methacrylate in the type of O/W described in step 3 emulsion, stirs 1 h at ambient temperature with the rotating speed cutting of 1000-2000 rpm, obtains new O/W type emulsion;
Step 5, raised temperature 50 DEG C ~ 75 DEG C, slowly drips initiator, rotating speed is down to 100 ~ 200 rpm simultaneously, polyreaction 2-6 h, carry out breakdown of emulsion, filtration, washing and drying treatment successively afterwards, obtained low temperature phase change accumulation energy microcapsule.
8. preparation method according to claim 7, is characterized in that: the breaking method described in step 5 is: in the emulsion after polyreaction, add excessive saturated nacl aqueous solution, stratification.
9. preparation method according to claim 7, is characterized in that: the drying treatment described in step 5 is: in temperature be under the condition of 40 DEG C vacuum-drying to constant weight.
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| CN105647481A (en) * | 2016-01-18 | 2016-06-08 | 北京理工大学 | Medium-low temperature phase change cold storage material and preparation method thereof |
| CN106085368A (en) * | 2016-06-22 | 2016-11-09 | 桂林电子科技大学 | Composite phase-change energy storage material for microcapsule that a kind of nano heat-conductive strengthens and preparation method thereof |
| CN106567253A (en) * | 2016-10-25 | 2017-04-19 | 浙江理工大学 | Thermoregulation thermal-storage bamboo fiber and preparation method thereof |
| CN107903876A (en) * | 2017-11-09 | 2018-04-13 | 中国皮革和制鞋工业研究院 | A kind of phase-change microcapsule and its preparation method and application |
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| CN114316920A (en) * | 2021-12-29 | 2022-04-12 | 中铁大桥局集团有限公司 | High-thermal-conductivity phase-change microcapsule and preparation method and application thereof |
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| CN114381238A (en) * | 2022-01-10 | 2022-04-22 | 无锡万斯家居科技股份有限公司 | Phase-change material microcapsule, preparation process thereof and pillow containing phase-change material microcapsule |
| CN117821025A (en) * | 2024-03-06 | 2024-04-05 | 成都理工大学 | Phase-change microcapsule and preparation method thereof |
| CN117821025B (en) * | 2024-03-06 | 2024-05-10 | 成都理工大学 | Phase-change microcapsule and preparation method thereof |
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Application publication date: 20150527 |