CN104774593A - Cool temperature controlled microcapsule and preparation method thereof - Google Patents
Cool temperature controlled microcapsule and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cool temperature controlled microcapsule and a preparation method thereof. The cool temperature control microcapsule uses polymethyl methacrylate as a wall material and an organic phase change material as a core material, wherein the weight ratio of the wall material to the core material is 1:1-2. The preparation method is as below: first stirring the organic phase change material, an emulsifier, an auxiliary emulsifier, an initiator and distilled water to form an emulsion system; then dropwise adding methyl methacrylate in the system, heating up to 65 DEG C, carrying out prepolymerization reaction under the protection of nitrogen for 1 h, then heating to 80 DEG C, carrying out a polymerization reaction for 5-7 h, standing the reaction liquid obtained from the polymerization reaction, and conducting suction filtration, washing and drying to obtain the environment-friendly, non-toxic cool temperature controlled microcapsule with high mechanical strength and good heat resistance. The microcapsule can be added to the fabric, so that the clothing has a phase change function to adjust the balance of the internal temperature of the clothing, achieve instant and lasting cooling sense in the clothing and to maintain constant body temperature.
Description
Technical field
What the present invention relates to is a kind of cool feeling temperature control microcapsule and preparation method thereof, and these cool feeling temperature control microcapsule specifically one have temp regulating function, blocks the heat trnasfer between human body and external environment, keeps the microcapsule of normal temps in human body clothes.
Background technology
Phase-change material micro-capsule (MEPCMs), small " container " that comprise phase change material in Nang core, it is as a kind of matrix material, volume change and leakage problem when solving solid-liquid phase change material phase transformation, achieve being permanently fixed of phase change material, core material and external environment are completely cut off, the effect of oxygen, light etc. can be resisted, efficiently solve the leakage of phase change material, be separated and the problem such as corrodibility, improve the application performance of phase change material, improve the efficiency that phase change material uses, make the use of phase change material, storage and transport convenient.Phase-change material micro-capsule provides large heat transfer area improvement heat transfer simultaneously, thus extends the use range of phase change material.Therefore, the encapsulated concern being more and more subject to researchist of phase change material, the preparations and applicatio of microencapsulated phase change material has become one of the focus and difficult point problem of research field.The standard of living of modern people achieves larger raising, people are also become clear day by day to the pursuit of improving the quality of living, hot summer, high temperature of going out is hard to bear, and people have urgent demand to cool feeling textiles, and on market, various cool feeling textiles emerges in an endless stream, and many cool feeling textiless only possess unidirectional temperature adjustment function, namely can only improve heat insulation effect, or reduce temperature in clothes to a certain extent, but environmentally temperature variation can not automatically regulate inner temperature.
And cool feeling temperature control weaving microcapsule can in envrionment temperature by lower than to the heat in absorbing environmental during transformation temperature higher than phase change material, solid-liquid phase occurs to be changed, and core heat enthalpy value is high, can keep the balance of inner temperature in a long time.
The reaction monomers that current emulsion polymerization prepares organic phase change material microcapsule mainly contains methacrylic acid, methyl methacrylate, hydroxyethyl methylacrylate, vinylbenzene etc., wherein polymethylmethacrylate is due to advantages such as environment-protecting asepsis, physical strength are high, good heat resistances, is the preferred wall material preparing organic phase change material microcapsule.
Summary of the invention
An object of the present invention is the unidirectional temperature adjustment function in order to solve above-mentioned textile fabric, namely heat insulation effect can only be improved, or reduce temperature in clothes to a certain extent, but can not environmentally temperature variation automatically regulate the technical problems such as inner temperature and a kind of cool feeling temperature control microcapsule are provided, these cool feeling temperature control microcapsule can in envrionment temperature by lower than to the heat in absorbing environmental during transformation temperature higher than phase change material, generation solid-liquid phase changes, and can keep the balance of inner temperature in a long time.
Two of object of the present invention is to provide the preparation method of above-mentioned a kind of cool feeling temperature control microcapsule, namely adopts emulsion polymerization synthesis cool feeling temperature control microcapsule.
Know-why of the present invention
Emulsion polymerization is that the free radical generated in water medium enters in the micella or emulsion particle generated by emulsifying agent or other modes the heterogeneous polymerization causing wherein monomer and carry out being polymerized.System is at least made up of monomer, emulsifying agent, initiator and water, in this experimental system, also has core organic phase change material.Particularly, letex polymerization is under the effect of emulsifying agent and by means of mechanical stirring, makes monomer be dispersed into milk sap in water, is caused and the polyreaction of carrying out by initiator.Adjoint in emulsion polymerization process is the radical polymerization of methyl methacrylate.Therefore, emulsion polymerization synthesis polymethylmethacrylate organic phase change material microcapsule principle divides two portions to illustrate:
(1), the three phases (speedup phase, constant speed phase and reduction of speed phase) of letex polymerization
1., the first stage of letex polymerization-----the speedup phase (emulsion particle generation)
First stage indicates:
Micella to non-nucleation from polymerization all disappears;
Transformation efficiency is from 0% ~ 15%, and this one-phase emulsion particle diameter rises to 20nm ~ more than 40nm from 6nm ~ 10nm;
2., the second stage of the letex polymerization----constant speed phase
Subordinate phase mark:
Monomer droplet all disappears, and transformation efficiency is from 15% ~ 50%;
In monomer-polymer emulsion particle, monomer and polymkeric substance respectively account for half, and in emulsion particle, monomer concentration remains unchanged substantially, and emulsion particle number is constant, and rate of polymerization is constant, and monomer-polymer emulsion particle largest diameter is 50nm ~ 150nm;
3., the three phases of letex polymerization---the reduction of speed phase
Phase III indicates:
Transformation efficiency increases to 100% from 50%;
Rate of polymerization declines with the decline of monomer concentration in monomer-polymer emulsion particle, and last monomer is transformed into polymkeric substance completely;
(2), the radical polymerization mechanism of methyl methacrylate
1., chain starting reaction
Decomposition of initiator produces primary group of free radicals, and primary group of free radicals and monomer addition generate the reaction process of monomer radical;
2., transfer reaction
Monomer radical and monomer addition generate new free radical, so repeatedly generate the process of chain free radical.
3., chain termination reaction
Free radical activity is high, and having interacts stops and deactivated tendency.Chain free radical loses activity and forms the reaction of stabilization of polymer and be called chain termination reaction.
Technical scheme of the present invention
A kind of cool feeling temperature control microcapsule, being wall material with polymethylmethacrylate, take organic phase change material as core, adopts the organic phase change material microcapsule of emulsion polymerization synthesis to be cool feeling temperature control microcapsule; The consumption of wall material methyl methacrylate, core organic phase change material, calculates in mass ratio, wall material methyl methacrylate: core organic phase change material is 1:1-2;
Described organic change material is n-dodecanol, n-butyl stearate or n-Hexadecane.
The preparation method of above-mentioned a kind of cool feeling temperature control microcapsule, specifically comprises the following steps:
(1), organic phase change material, emulsifying agent, assistant for emulsifying agent, initiator and distilled water are joined in container, control temperature is 50 DEG C, under rotating speed 500rpm condition, stir and make organic phase change material in distilled water, form stable emulsification system under the effect of emulsifying agent, assistant for emulsifying agent;
Above-mentioned organic phase change material, emulsifying agent, assistant for emulsifying agent, initiator and distilled water calculate in mass ratio, i.e. organic phase change material: emulsifying agent: assistant for emulsifying agent: initiator: distilled water is 100:5:2:2-4:1400-1700;
Described emulsifier agent is that Tween-80 and Span-80 calculates in mass ratio, is the mixture that Tween-80:Span-80 is 55:45 composition;
Described assistant for emulsifying agent is Pentyl alcohol or n-hexyl alcohol;
Described initiator is benzoyl peroxide or Diisopropyl azodicarboxylate;
(2), controlling drop rate is 1ml/min; methyl methacrylate is added drop-wise in the emulsification system of step (1), after dripping, is warming up to 65 DEG C; carry out prepolymerization reaction 1h under nitrogen protection; and then be warming up to 80 DEG C and carry out polyreaction 5-7h, after polyreaction terminates, gained reaction solution is left standstill; suction filtration; filter cake through being that the aqueous ethanolic solution of 20% carries out washing to effluent liquid clarification with concentration of volume percent, control temperature is 50 DEG C and carries out drying, obtains cool feeling temperature control microcapsule.
Beneficial effect of the present invention
A kind of cool feeling temperature control microcapsule of the present invention, owing to adopting environment-protecting asepsis, physical strength is high, compactness is good, the polymethylmethacrylate of good heat resistance is wall material, adopt cheap and the organic phase change material with high latent heat of phase change is core, therefore the polymethylmethacrylate prepared is the cool feeling temperature control microcapsule environment-protecting asepsis of wall material, physical strength is high, good heat resistance, its core is not revealed, latent heat of phase change is high, there is temp regulating function, thus solve the leakage problem of phase change material in the unidirectional temp regulating function of textiles in prior art and solid-liquid conversion process.
Further, a kind of cool feeling temperature control microcapsule of the present invention, add in textiles, clothing is made to have phase transition function, regulate the balance of inner temperature, realize the unification of clothing moment cool feeling and lasting cool feeling, maintain thermostasis, creates one neither hot also not cold " moist heat " widened the field that phase change material applies.
Embodiment
Below by embodiment, the present invention is set forth further, but content of the present invention can not be limited.
Various raw material used in various embodiments of the present invention or the specification of reagent and the information of manufacturer as follows:
Methyl methacrylate, analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Diisopropyl azodicarboxylate, analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Lauryl alcohol, analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
N-butyl stearate, analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Tween-80, analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Span-80, analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
The model of the plant and instrument that the present invention is used and the information of manufacturer as follows:
Electronic balance, PL403, plum Teller-Tuo benefit Instrument Ltd.;
Constant temperature blender with magnetic force, 524G, Mei Ying Pu, Shanghai instrument Manufacturing Co., Ltd;
The multiplex vacuum pump of circulating water type, SHZ-D III, Shanghai Yao Te plant and instrument company limited;
Digital display blast drier, 101, Shanghai Ye Tuo instrument company limited;
Biomicroscope, XSP-BM-8CAS, Shanghai Bi Aimu opticinstrument company limited;
Thermogravimetric analyzer, TGA-Q5000, TA instrument company of the U.S.;
Differential scanning calorimeter, DSC-Q2000, TA instrument company of the U.S..
embodiment 1
A kind of cool feeling temperature control microcapsule, being wall material with polymethylmethacrylate, take organic phase change material as core, adopts the organic phase change material microcapsule of emulsion polymerization synthesis to be cool feeling temperature control microcapsule;
The consumption of wall material methyl methacrylate, core organic phase change material, calculates in mass ratio, wall material methyl methacrylate: core organic phase change material is 1:1;
Described organic change material is n-dodecanol.
The preparation method of above-mentioned a kind of cool feeling temperature control microcapsule, specifically comprises the following steps:
(1), 4g organic phase change material and n-dodecanol, 0.2g emulsifying agent, 0.08g assistant for emulsifying agent, 0.16g initiator and 60ml distilled water are joined in container, control temperature is 50 DEG C, rotating speed 500rpm stirs 30min, makes organic phase change material in distilled water, form stable emulsification system under the effect of emulsifying agent, assistant for emulsifying agent;
Above-mentioned organic phase change material, emulsifying agent, assistant for emulsifying agent, initiator and distilled water calculate in mass ratio, i.e. organic phase change material: emulsifying agent: assistant for emulsifying agent: initiator: distilled water is 100:5:2:4:1400;
Described emulsifier agent is that Tween-80 and Span-80 calculates in mass ratio, is the mixture that Tween-80:Span-80 is 55:45 composition;
Described assistant for emulsifying agent is n-hexyl alcohol;
Described initiator is Diisopropyl azodicarboxylate;
(2), control drop rate is 1ml/min, 4g methyl methacrylate is added drop-wise in the emulsification system of step (1), after dripping, be warming up to 65 DEG C, carry out prepolymerization reaction 0.5h under nitrogen protection, and then be warming up to 80 DEG C and carry out polyreaction 5h, after polyreaction terminates, after gained reaction solution is left standstill 12h, control pressure is carry out vacuum filtration under 0.05MPa condition, gained filter cake is through being that the aqueous ethanolic solution of 20% carries out washing to effluent liquid clarification with concentration of volume percent, control temperature is 50 DEG C and carries out drying, obtain the cool feeling temperature control microcapsule of white powder.
The cool feeling temperature control microcapsule of the white powder of above-mentioned gained have temp regulating function, can keep within a certain period of time taking interior normal temps, transformation temperature is detected as 24 DEG C through differential scanning calorimeter, enthalpy of phase change is 98J/g, the content of core organic phase change material n-dodecanol detects through thermogravimetric analysis and is about 47%, and the cool feeling temperature control microcapsule of the white powder of gained have good thermal stability below 160 DEG C.
embodiment 2
A kind of cool feeling temperature control microcapsule, being wall material with polymethylmethacrylate, take organic phase change material as core, and adopt emulsion polymerization, the organic phase change material microcapsule of synthesis are cool feeling temperature control microcapsule;
The consumption of wall material methyl methacrylate, core organic phase change material, calculates in mass ratio, wall material methyl methacrylate: core organic phase change material is 1:2;
Described organic change material is n-butyl stearate.
The preparation method of above-mentioned a kind of cool feeling temperature control microcapsule, specifically comprises the following steps:
(1), 4g organic phase change material, 0.2g emulsifying agent, 0.08g assistant for emulsifying agent, 0.16g initiator and 68ml distilled water are joined in container, control temperature is 50 DEG C, under rotating speed 500rpm agitation condition, stir and make organic phase change material in distilled water, form stable emulsification system under the effect of emulsifying agent, assistant for emulsifying agent;
Above-mentioned organic phase change material, emulsifying agent, assistant for emulsifying agent, initiator and distilled water calculate in mass ratio, i.e. organic phase change material: emulsifying agent: assistant for emulsifying agent: initiator: distilled water is 100:5:2:4:1700;
Described emulsifier agent is that Tween-80 and Span-80 calculates in mass ratio, is the mixture that Tween-80:Span-80 is 55:45 composition;
Described assistant for emulsifying agent is n-hexyl alcohol;
Described initiator is Diisopropyl azodicarboxylate;
(2), control drop rate is 1ml/min, 2g methyl methacrylate is added drop-wise in the emulsification system of step (1), after dripping, be warming up to 65 DEG C, carry out prepolymerization reaction 0.5h under nitrogen protection, and then be warming up to 80 DEG C and carry out polyreaction 7h, after polyreaction terminates, after gained reaction solution is left standstill 12h, control pressure is carry out vacuum filtration under 0.05MPa condition, gained filter cake is through being that the aqueous ethanolic solution of 20% carries out washing to effluent liquid clarification with concentration of volume percent, control temperature is 50 DEG C and carries out drying, obtain the cool feeling temperature control microcapsule of white powder.
The cool feeling temperature control microcapsule of the white powder of above-mentioned gained have temp regulating function, can keep within a certain period of time taking interior normal temps, transformation temperature is detected as 22 DEG C through differential scanning calorimeter, enthalpy of phase change is 86J/g, the content of core organic phase change material n-butyl stearate detects through thermogravimetric analysis and is about 61%, and the cool feeling temperature control microcapsule of the white powder of gained have good thermal stability below 160 DEG C.
embodiment 3
A kind of cool feeling temperature control microcapsule, being wall material with polymethylmethacrylate, take organic phase change material as core, and adopt emulsion polymerization, the organic phase change material microcapsule of synthesis are cool feeling temperature control microcapsule;
The consumption of wall material methyl methacrylate, core organic phase change material, calculates in mass ratio, wall material methyl methacrylate: core organic phase change material is 1:1.5;
Described organic change material is n-Hexadecane.
The preparation method of above-mentioned a kind of cool feeling temperature control microcapsule, specifically comprises the following steps:
(1), 4g organic phase change material, 0.2g emulsifying agent, 0.08g assistant for emulsifying agent, 0.16g initiator and 68ml distilled water are joined in container, control temperature is 50 DEG C, under rotating speed 500rpm condition, stir and make organic phase change material in distilled water, form stable emulsification system under the effect of emulsifying agent, assistant for emulsifying agent;
Above-mentioned organic phase change material, emulsifying agent, assistant for emulsifying agent, initiator and distilled water calculate in mass ratio, i.e. organic phase change material: emulsifying agent: assistant for emulsifying agent: initiator: distilled water is 100:5:2:3:1550;
Described emulsifier agent is that Tween-80 and Span-80 calculates in mass ratio, is the mixture that Tween-80:Span-80 is 55:45 composition;
Described assistant for emulsifying agent is n-hexyl alcohol;
Described initiator is Diisopropyl azodicarboxylate;
(2), control drop rate is 1ml/min, 2.667g methyl methacrylate is added drop-wise in the emulsification system of step (1), after dripping, be warming up to 65 DEG C, carry out prepolymerization reaction 0.5h under nitrogen protection, and then be warming up to 80 DEG C and carry out polyreaction 6h, after polyreaction terminates, after gained reaction solution is left standstill 12h, control pressure is carry out vacuum filtration under 0.05MPa condition, gained filter cake is through being that the aqueous ethanolic solution of 20% carries out washing to effluent liquid clarification with concentration of volume percent, control temperature is 50 DEG C and carries out drying, obtain the cool feeling temperature control microcapsule of white powder.
The cool feeling temperature control microcapsule of the white powder of above-mentioned gained have temp regulating function, can keep within a certain period of time taking interior normal temps, transformation temperature is detected as 18 DEG C through differential scanning calorimeter, enthalpy of phase change is 128J/g, the content of core organic phase change material n-butyl stearate detects through thermogravimetric analysis and is about 56%, and the cool feeling temperature control microcapsule of the white powder of gained have good thermal stability below 160 DEG C.
In sum, cool feeling temperature control microcapsule of the present invention have temp regulating function, can keep within a certain period of time taking interior normal temps, transformation temperature is detected as 18-24 DEG C through differential scanning calorimeter, enthalpy of phase change is 86-128J/g, the content of core organic phase change material detects through thermogravimetric analysis and is about 47-61%, and the cool feeling temperature control microcapsule of the white powder of gained have good thermal stability below 160 DEG C.
The above is only the citing of embodiments of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement, these improvement also should be considered as protection scope of the present invention.
Claims (6)
1. cool feeling temperature control microcapsule, it is characterized in that described cool feeling temperature control microcapsule take polymethylmethacrylate as wall material, take organic phase change material as core, the consumption of wall material methyl methacrylate, core organic phase change material, calculate in mass ratio, wall material methyl methacrylate: core organic phase change material is 1:1-2.
2. a kind of cool feeling temperature control microcapsule as claimed in claim 1, is characterized in that described organic phase change material is n-dodecanol, n-butyl stearate or n-Hexadecane.
3. a kind of cool feeling temperature control microcapsule as claimed in claim 1, is characterized in that the consumption of wall material methyl methacrylate, core organic phase change material, calculate in mass ratio, wall material methyl methacrylate: core organic phase change material is 1:1;
Described organic change material is n-dodecanol.
4. a kind of cool feeling temperature control microcapsule as claimed in claim 1, is characterized in that the consumption of wall material methyl methacrylate, core organic phase change material, calculate in mass ratio, wall material methyl methacrylate: core organic phase change material is 1:2;
Described organic change material is n-butyl stearate.
5. a kind of cool feeling temperature control microcapsule as claimed in claim 1, is characterized in that the consumption of wall material methyl methacrylate, core organic phase change material, calculate in mass ratio, wall material methyl methacrylate: core organic phase change material is 1:1.5;
Described organic change material is n-Hexadecane.
6. the preparation method of a kind of cool feeling temperature control microcapsule as claimed in claim 1, is characterized in that specifically comprising the following steps:
(1), organic phase change material, emulsifying agent, assistant for emulsifying agent, initiator and distilled water are put into container, control temperature is 50 DEG C, under rotating speed 500rpm condition, stir and make organic phase change material in distilled water, form stable emulsification system under the effect of emulsifying agent, assistant for emulsifying agent;
Above-mentioned organic phase change material, emulsifying agent, assistant for emulsifying agent, initiator and distilled water calculate in mass ratio, i.e. organic phase change material: emulsifying agent: assistant for emulsifying agent: initiator: distilled water is 100:5:2:2-4:1400-1700;
Described emulsifier agent is that Tween-80 and Span-80 calculates in mass ratio, is the mixture that Tween-80:Span-80 is 55:45 composition;
Described assistant for emulsifying agent is Pentyl alcohol or n-hexyl alcohol;
Described initiator is benzoyl peroxide or Diisopropyl azodicarboxylate;
(2), controlling drop rate is that methyl methacrylate is added drop-wise in the emulsification system of step (1) by 1ml/min; after dripping; be warming up to 65 DEG C, carry out prepolymerization reaction 1h under nitrogen protection, and then be warming up to 80 DEG C and carry out polyreaction 5-7h; after polyreaction terminates; gained reaction solution is left standstill, suction filtration, filter cake through being that the aqueous ethanolic solution of 20% carries out washing to effluent liquid clarification with concentration of volume percent; control temperature is 50 DEG C and carries out drying, obtains cool feeling temperature control microcapsule.
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| CN115627641A (en) * | 2022-09-26 | 2023-01-20 | 黛思(常州)无纺布有限公司 | Lasting mask cool feeling agent and preparation method thereof |
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| CN106592251A (en) * | 2016-11-17 | 2017-04-26 | 上海应用技术大学 | Microcapsule finishing agent for cool and refreshing functional fabric and preparation method |
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| JP7505711B2 (en) | 2019-10-24 | 2024-06-25 | アクトインテリア株式会社 | Cooling fabric, textile product having same, and method for manufacturing cooling fabric |
| GB2597373A (en) * | 2020-03-16 | 2022-01-26 | Istanbul Kultur Univ | Webs with coaxial nanofiber structure, a textile product containing these webs and a preparation method thereof |
| WO2021188073A1 (en) * | 2020-03-16 | 2021-09-23 | Istanbul Kultur Universitesi | Webs with coaxial nanofiber structure, a textile product containing these webs and a preparation method thereof |
| GB2597373B (en) * | 2020-03-16 | 2024-05-15 | Istanbul Kultur Univ | Webs with coaxial nanofiber structure, a textile product containing these webs and a preparation method thereof |
| CN112726199A (en) * | 2020-12-28 | 2021-04-30 | 福建冠泓工业有限公司 | Cool skin-friendly non-woven fabric and preparation method thereof |
| CN114808464A (en) * | 2021-09-29 | 2022-07-29 | 中国制浆造纸研究院有限公司 | Intelligent temperature-adjusting finishing agent and preparation method thereof |
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| CN115627641B (en) * | 2022-09-26 | 2024-02-13 | 黛思(常州)无纺布有限公司 | Lasting mask cool feeling agent and preparation method thereof |
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Application publication date: 20150715 |