CN103642462A - Millimeter temperature-control slow-release aromatic gel capsule and preparation method thereof - Google Patents
Millimeter temperature-control slow-release aromatic gel capsule and preparation method thereof Download PDFInfo
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- CN103642462A CN103642462A CN201310625592.1A CN201310625592A CN103642462A CN 103642462 A CN103642462 A CN 103642462A CN 201310625592 A CN201310625592 A CN 201310625592A CN 103642462 A CN103642462 A CN 103642462A
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Abstract
The invention discloses a millimeter temperature-control slow-release aromatic gel capsule and a preparation method thereof. The preparation method of the millimeter temperature-control slow-release aromatic gel capsule comprises the following steps: synthesizing an organic phase-change material microcapsule through emulsion polymerization by taking an organic phase-change material as a core material and polymethyl methacrylate as a wall material; sequentially pouring the organic phase-change material microcapsule and essence to a sodium alginate solution and completely stirring to obtain a mixed solution; and gradually dropwise adding the mixed solution to a calcium chloride of which the mass concentration is 10% through a 2.5mm injection needle, standing still, washing and carrying out suction filtering to obtain the millimeter temperature-control slow-release aromatic gel capsule which is white particle with clean surface; the prepared aromatic gel capsule is 1.68-2.16mm in granularity, and the shortcomings of millimeter temperature-control slow-release aromatic gel capsule which easily disperses in wind and leaks when applied to textiles are solved. The millimeter temperature-control slow-release aromatic gel capsule has a function of regulating temperature and can disperse certain aromatic smell, thus widening application field of the organic phase-change material.
Description
Technical field
The present invention relates to a kind ofly there is temp regulating function and there is grade temperature control sustained-release fragrant gel capsule of fragrant breath and preparation method thereof.
Background technology
Phase-change material micro-capsule (micro-encapsulated phase change materials, be called for short MEPCM), apply exactly the matrix material with core-shell (core-shell) structure that microcapsulary forms at the film of the coated one deck stable performance of solid-liquid phase change material microparticle surfaces, MEPCM is comprised of inner nuclear material and sheating material two portions, wall material is generally natural macromolecular material, semi-synthetic macromolecular material or complete synthesis macromolecular material, wherein complete synthesis macromolecular material polymethylmethacrylate is due to environment-protecting asepsis, physical strength is high, the advantages such as good heat resistance, it is the preferred wall material of the organic phase-change material micro-capsule of preparation.The phase change material of micro encapsulation is maximum with paraffin hydro carbons at present, normal paraffin C
14～c
20transformation temperature within the scope of 5.8 ℃～36.8 ℃, can be widely used in the field such as cooling, material of construction, intelligent temperature-regulation fabric of accurate mechanical equipment.
The fragrant bilayered microcapsule of temperature control that the beta-cyclodextrin of take obtains as the coated essence of outer wall material and organic phase change material microcapsule mixture, solved the slow release speed impact fragrance inhomogeneous problem that millimeter cause it discharge of temperature variation on essence microcapsule, make to carry out in the certain temperature range of being released in of fragrance, but micron-sized capsule particle is less, causes and in textiles, have the technical problems such as seepage having easily to fly away under the condition of wind to fill the air and to be applied in.
summary of the invention
One of object of the present invention is less in order to solve the particle of above-mentioned micron-sized temperature control fragrance bilayered microcapsule, causes and in textiles, has the technical problem of seepage and proposed a kind of grade temperature control fragrant gel capsule having easily to fly away under the condition of wind to fill the air and to be applied in.
Two of object of the present invention is the preparation methods that propose above-mentioned a kind of grade temperature control sustained-release fragrant gel capsule.
Know-why of the present invention
A kind of preparation method of grade temperature control fragrant gel capsule.First, it is the preparation of polymethylmethacrylate organic phase change material microcapsule, under the effect of emulsifying agent and assistant for emulsifying agent, organic phase change material is divided equably and in water-dispersion mutually, obtains emulsification system, then under certain temperature and stirring velocity, methyl methacrylate is added drop-wise in above-mentioned emulsification system, be warming up to certain temperature and cause radical polymerization under the effect of initiator, be i.e. the synthetic organic phase change material microcapsule of emulsion polymerization; The second, organic phase change material microcapsule and essence are added to the sodium alginate of clear by a certain percentage successively, stir and obtain the sodium alginate mixed solution that contains microcapsule and essence; The 3rd, the sodium alginate mixed solution that contains microcapsule and essence is splashed in calcium chloride solution with the injection needles of 2.5 ㎜, thereby by alginate calcium coated to microcapsule and essence, obtain grade temperature control sustained-release fragrant gel capsule.
The preparation method of above-mentioned a kind of grade temperature control sustained-release fragrant gel capsule, its principle has phase-change mechanism and orifice-precipitation bath method of phase-change material micro-capsule.Be specifically described as follows:
1, the phase-change mechanism of phase change material
Phase change material (phase change material, PCM) be a kind of novel material of developing in recent years, it is a kind of general hot energy storage material of applying, it is to utilize the heat absorption and release of material in phase transition process, carry out storage and the release of heat energy, thereby reach the object that controls environment temperature and carry out heat use.When envrionment temperature is during higher than the transformation temperature of phase change material, under thermograde effect, heat is transferred to phase change material by the external world, carries out thaw process; When envrionment temperature is during lower than transformation temperature, phase change material carries out process of setting, to external environment releases heat.The banking system of heat energy has sensible heat formula, latent heat formula and chemical equation accumulation of heat.The heat that phase change material absorbs and discharges in phase transition process is called latent heat, compares with chemical reaction heat with sensible heat, and latent heat storage density is high, inhales the approximate isothermal of exothermic process, good reversibility, and this has very important effect in actual applications.
2, orifice-precipitation bath method principle
Orifice-precipitation bath method is a kind of microcapsule method that chemical method and physical mechanical method are combined, and to be Mabbs propose in nineteen fifty in 1940 and Rabbool this method.Take soluble polymer as wall material, by polymkeric substance wiring solution-forming, with this solution parcel core and be spherical drop and enter in precipitation bath, make polymkeric substance precipitation or crosslinking curing become membranous wall and make microcapsule.
Orifice method is prepared microcapsule and mainly 3 stages, is consisted of:
(1) forming drop is dissolved in polymers soln by core or is dispersed in the melts of polymkeric substance, by this solution or dispersion liquid add with the inconsistent liquid of polymkeric substance (suspension medium) in, under the effect of agitator, homogenizer, ultrasonic mixer etc., make two-phase mix.
(2) crosslinked polymer, by adding linking agent, makes polymkeric substance drop solidify under proper temperature, under the stable condition that is uniformly mixed.
(3) product reclaims by flotation, filtration or centrifugal method recovery microcapsule, and with suitable solvent wash and remove the remaining materials such as stablizer.
Technical scheme of the present invention
A grade temperature control sustained-release fragrant gel capsule, by the following method preparation:
First, using organic phase change material as core, take polymethylmethacrylate as wall material is by the synthetic organic phase change material microcapsule of emulsion polymerization;
Organic phase change material, polymethylmethacrylate used calculate in mass ratio, organic phase change material: polymethylmethacrylate is 1～4:1;
Described organic change material is whiteruss, n-tetradecane, n-hexadecane, Octadecane, NSC 62789 or solid slice paraffin;
Then, organic phase change material microcapsule and essence are poured into successively in sodium alginate soln and fully stirred and obtain mixed solution;
The mass ratio that essence used and the amount of sodium alginate are pressed the synthetic organic phase change material microcapsule of emulsion polymerization calculates, i.e. essence: sodium alginate: organic phase change material microcapsule are 1:1:1～5;
Described essence is violet compound, lemon flavour or all sorts of flowers essence;
Finally, it is in 10% calcium chloride water that the injection needles that adopts 2.5 ㎜ dropwise splashes into mass percent concentration by the mixed solution of above-mentioned gained, standing, washing, suction filtration, and the white particle of gained surface clean is grade temperature control sustained-release fragrant gel capsule.
The preparation method of above-mentioned grade temperature control sustained-release fragrant gel capsule, specifically comprises the steps:
(1), the preparation of organic phase change material microcapsule
1., organic phase change material, emulsifying agent, assistant for emulsifying agent, initiator and distilled water are put into container, control temperature and be 55 ℃, stir, obtain emulsion;
Above-mentioned organic phase change material used, 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 1:0.05:0.02:0.01-0.04:11.25～18;
Described emulsifying agent is that Tween-80 and Span-80 calculate in mass ratio, and being Tween-80:Span-80 is the mixture that 55:45 forms;
Described assistant for emulsifying agent is Pentyl alcohol or n-hexyl alcohol;
Described initiator is benzoyl peroxide or Diisopropyl azodicarboxylate;
2., by step 1. gained emulsion to control temperature be 55 ℃, rotating speed 600～1000rpm stirs 0.5～1h, makes the organic phase change material in emulsion under the effect of emulsifying agent, in water, form stable emulsification system;
3., controlling drop rate is that 2～3ml/min is added drop-wise to methyl methacrylate in emulsification system 2., then temperature is risen to 65 ℃, under nitrogen protection, carry out prepolymerization reaction 0.5～1h simultaneously, then be warming up to 85 ℃ and carry out polyreaction 5～8h, after polyreaction finishes, gained reaction solution is standing, suction filtration, gained filter cake washs to controlling temperature after elutant clarification and is 50 ℃ and is dried after 24h with 30% ethanolic soln, obtains organic phase change material microcapsule;
(2) preparation of the sodium alginate mixed solution that, contains organic phase change material microcapsule and essence
At 50 ℃, compound concentration is the sodium alginate soln of 5% clear, after the organic phase change material microcapsule of gained in step (1) and essence priority are joined in sodium alginate soln successively, controlling stir speed (S.S.) is that 500～800r/min stirs 0.5～1h, must contain the sodium alginate mixed solution of organic phase change material microcapsule and essence;
(3), the preparation of grade temperature control sustained-release fragrant gel capsule
By the sodium alginate mixed solution that contains organic phase change material microcapsule and essence of gained in (2) with in the injection needles of the 2.5 ㎜ calcium chloride water that dropwise to enter to mass percent concentration be 10%, standing 12h, millimeter is with after the hot wash of 60 ℃ 3 times, suction filtration, the white particle of the surface clean of gained, is grade temperature control sustained-release fragrant gel capsule.
Beneficial effect of the present invention
A kind of grade temperature control sustained-release fragrant gel capsule of the present invention, because its particle diameter has reached grade, therefore this grade temperature control sustained-release fragrant gel capsule can overcome and has and easily fly away the defect of filling the air and be applied in the technological deficiency that has seepage in textiles having under the condition of wind, can be widely used in wardrobe, indoor, car etc.
Further, a kind of grade temperature control sustained-release fragrant gel capsule of the present invention, the method for employing double-coated, makes material can also distribute certain fragrant breath, the Application Areas of having widened phase change material when having the function that regulates temperature.
Embodiment
Below by embodiment, the present invention is further set forth, but can not limit content of the present invention.
In various embodiments of the present invention, various raw materials used or the specification of reagent and the information of manufacturer are as follows:
Methyl methacrylate, analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Diisopropyl azodicarboxylate, analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
N-hexadecane, analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Whiteruss, 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;
Dehydrated alcohol, analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
N-hexyl alcohol, analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Sodium alginate, chemical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Calcium Chloride Powder Anhydrous, analytical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Violet compound, the international essence and flavoring agent (China) of American I FF company limited
Lemon flavour, Shenzhen GuanLiDa BoDun spice Co., Ltd
All sorts of flowers essence, Shenzhen GuanLiDa BoDun spice Co., Ltd
In various embodiments of the present invention, the model of plant and instrument used and the information of manufacturer are as follows:
Clarifixator, FA25 type, Shanghai Frock Fluid Machinery Manufacture Co., Ltd. produces;
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, U.S. TA instrument company;
Fourier transformation infrared spectrometer, VERTEX70, Brooker spectral instrument company;
Differential scanning calorimeter, DSC-Q2000, U.S. TA instrument company;
Vernier callipers, 1139-150, the prompt north material electronic digital indicator in Guan County.
embodiment 1
A grade temperature control sustained-release fragrant gel capsule, by the following method preparation:
First, using organic phase change material as core, take polymethylmethacrylate as wall material is by the synthetic organic phase change material microcapsule of emulsion polymerization;
Organic phase change material, polymethylmethacrylate used calculate in mass ratio, organic phase change material: polymethylmethacrylate is 1:1;
Described organic change material is n-tetradecane;
Then, organic phase change material microcapsule and essence are poured into successively in sodium alginate soln and fully stirred and obtain mixed solution;
The mass ratio that essence used and the amount of sodium alginate are pressed the synthetic organic phase change material microcapsule of emulsion polymerization calculates, i.e. essence: sodium alginate: organic phase change material microcapsule are 1:1:1;
Described essence is violet compound;
Finally, it is in 10% calcium chloride water that the injection needles that adopts 2.5 ㎜ dropwise splashes into mass percent concentration by the mixed solution of above-mentioned gained, standing, washing, suction filtration, and the white particle of gained surface clean is grade temperature control sustained-release fragrant gel capsule.
The preparation method of above-mentioned grade temperature control sustained-release fragrant gel capsule, specifically comprises the steps:
(1), the preparation of organic phase change material microcapsule
1., by 4g organic phase change material, be that n-tetradecane, 0.2g emulsifying agent, 0.08g assistant for emulsifying agent, 0.16g initiator and 72g distilled water weigh in there-necked flask, control temperature and be 55 ℃, stir, obtain emulsion;
Above-mentioned organic phase change material used, 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 1:0.05:0.02:0.04:18;
Described emulsifying agent is that Tween-80 and Span-80 calculate in mass ratio, and being Tween-80:Span-80 is the mixture that 55:45 forms;
Described assistant for emulsifying agent is n-hexyl alcohol;
Described initiator is Diisopropyl azodicarboxylate;
2., by step 1. gained emulsion to control temperature be 55 ℃, rotating speed 800rpm stirs 0.5h, makes the organic phase change material in emulsion under the effect of emulsifying agent, in water, form stable emulsification system;
3., controlling drop rate is that 2～3ml/min is added drop-wise to 4g methyl methacrylate in emulsification system 2., then temperature is risen to 65 ℃, under nitrogen protection, carry out prepolymerization reaction 0.5h simultaneously, then be warming up to 85 ℃ and carry out polyreaction 5h, after polyreaction finishes, on the surface of core organic phase change material, there is radical polymerization in methyl methacrylate drop, thereby make micro-encapsulation of core material, after polyreaction finishes, by the standing 12h of gained reaction solution, suction filtration, gained filter cake mass percent concentration is that 30% aqueous ethanolic solution washs to controlling temperature after elutant clarification and is 50 ℃ and is dried after 24h, obtain organic phase change material microcapsule,
(2) preparation of the sodium alginate mixed solution that, contains organic phase change material microcapsule and essence
Get 2.5g sodium alginate and under 50 ℃ of conditions, be dissolved to homogeneous transparent in 50mL distilled water, obtain the sodium alginate aqueous solution that mass percent concentration is 5% clear, by the organic phase change material microcapsule 2.5g of gained in (1), mass percent concentration that violet compound 2.5g joins above-mentioned gained successively, be in the sodium alginate soln of 5% clear after, controlling stir speed (S.S.) is that 500r/min stirs 0.5h, must contain the sodium alginate mixed solution of organic phase change material microcapsule and essence;
Essence used and the amount of sodium alginate are pressed the amount of the synthetic organic phase change material microcapsule of emulsion polymerization and are calculated, i.e. essence: sodium alginate: organic phase change material microcapsule are 1:1:1;
(3), the preparation of grade temperature control sustained-release fragrant gel capsule
Get 20g Calcium Chloride Powder Anhydrous and be dissolved in 200mL distilled water, obtain mass percent concentration and be 10% calcium chloride water;
It is in 10% calcium chloride water that the sodium alginate mixed solution that contains organic phase change material microcapsule and essence of gained in (2) is dropwise splashed into mass percent concentration with the injection needles of 2.5 ㎜, standing 12h, millimeter is with after the hot wash of 60 ℃ 3 times, suction filtration, the white particle of the surface clean of gained, is grade temperature control sustained-release fragrant gel capsule.
The grade temperature control sustained-release fragrant gel capsule of above-mentioned gained has natural violet breath, it is 7.1 ℃ that transformation temperature detects through differential scanning calorimeter, the content of core organic phase change material n-tetradecane detects and is about 50% through thermogravimetric analysis, and the grade temperature control sustained-release fragrant gel capsule of gained has good thermal stability below at 160 ℃.
The grade temperature control sustained-release fragrant gel capsule of above-mentioned gained detects through vernier callipers instrument, and its particle diameter is 1.68-2.16mm.
embodiment 2
A grade temperature control sustained-release fragrant gel capsule, by the following method preparation:
First, using organic phase change material as core, take polymethylmethacrylate as wall material is by the synthetic organic phase change material microcapsule of emulsion polymerization;
Organic phase change material, polymethylmethacrylate used calculate in mass ratio, organic phase change material: polymethylmethacrylate is 2:1;
Described organic change material is Octadecane;
Then, organic phase change material microcapsule and essence are poured into successively in sodium alginate soln and fully stirred and obtain mixed solution;
The mass ratio that essence used and the amount of sodium alginate are pressed the synthetic organic phase change material microcapsule of emulsion polymerization calculates, i.e. essence: sodium alginate: organic phase change material microcapsule are 1:1:2.5;
Described essence is lemon flavour;
Finally, it is in 10% calcium chloride water that the injection needles that adopts 2.5 ㎜ dropwise splashes into mass percent concentration by the mixed solution of above-mentioned gained, standing, washing, suction filtration, and the white particle of gained surface clean is grade temperature control sustained-release fragrant gel capsule.
The preparation method of above-mentioned grade temperature control sustained-release fragrant gel capsule, specifically comprises the steps:
(1), the preparation of organic phase change material microcapsule
1., by 8g organic phase change material, be that Octadecane, 0.4g emulsifying agent, 0.16g assistant for emulsifying agent, 0.16g initiator and 108g distilled water weigh in there-necked flask, control temperature and be 55 ℃, stir, obtain emulsion;
Above-mentioned organic phase change material used, 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 1:0.05:0.02:0.02:13.5;
Described emulsifying agent is that Tween-80 and Span-80 calculate in mass ratio, and being Tween-80:Span-80 is the mixture that 55:45 forms;
Described assistant for emulsifying agent is n-hexyl alcohol;
Described initiator is Diisopropyl azodicarboxylate;
2., by step 1. gained emulsion to control temperature be 55 ℃, rotating speed 800rpm stirs 0.5h, makes the organic phase change material in emulsion under the effect of emulsifying agent, in water, form stable emulsification system;
3., controlling drop rate is that 2～3ml/min is added drop-wise to 4g methyl methacrylate in emulsification system 2., then temperature is risen to 65 ℃, under nitrogen protection, carry out prepolymerization reaction 0.5h simultaneously, then be warming up to 85 ℃ and carry out polyreaction 5h, after polyreaction finishes, on the surface of core organic phase change material, there is radical polymerization in methyl methacrylate drop, thereby make micro-encapsulation of core material, after polyreaction finishes, by the standing 12h of gained reaction solution, suction filtration, gained filter cake mass percent concentration is that 30% aqueous ethanolic solution washs to controlling temperature after elutant clarification and is 50 ℃ and is dried after 24h, obtain organic phase change material microcapsule,
(2) preparation of the sodium alginate mixed solution that, contains organic phase change material microcapsule and essence
Get 2.5g sodium alginate and under 50 ℃ of conditions, be dissolved to homogeneous transparent in 50mL distilled water, obtain the sodium alginate aqueous solution that mass percent concentration is 5% clear;
By the organic phase change material microcapsule 6.25g of gained in (1), mass percent concentration that lemon flavour 2.5g joins above-mentioned gained successively, be in the sodium alginate soln of 5% clear after, controlling stir speed (S.S.) is that 500r/min stirs 0.5h, must contain the sodium alginate mixed solution of organic phase change material microcapsule and essence;
Essence used and the amount of sodium alginate are pressed the amount of the synthetic organic phase change material microcapsule of emulsion polymerization and are calculated, i.e. essence: sodium alginate: organic phase change material microcapsule are 1:1:2.5;
(3), the preparation of grade temperature control sustained-release fragrant gel capsule
It is in 10% calcium chloride water that the sodium alginate mixed solution that contains organic phase change material microcapsule and essence of gained in (2) is dropwise splashed into mass percent concentration with the injection needles of 2.5 ㎜, standing 12h, millimeter is with after the hot wash of 60 ℃ 3 times, suction filtration, the white particle of the surface clean of gained, is grade temperature control sustained-release fragrant gel capsule.
The grade temperature control sustained-release fragrant gel capsule of above-mentioned gained has natural lemon breath, it is 30 ℃ that transformation temperature detects through differential scanning calorimeter, the content of core organic phase change material Octadecane detects and is about 55% through thermogravimetric analysis, and the grade temperature control sustained-release fragrant gel capsule of gained has good thermal stability below at 160 ℃.
embodiment 3
A grade temperature control sustained-release fragrant gel capsule, by the following method preparation:
First, using organic phase change material as core, take polymethylmethacrylate as wall material is by the synthetic organic phase change material microcapsule of emulsion polymerization;
Organic phase change material, polymethylmethacrylate used calculate in mass ratio, organic phase change material: polymethylmethacrylate is 4:1;
Described organic change material is NSC 62789;
Then, organic phase change material microcapsule and essence are poured into successively in sodium alginate soln and fully stirred and obtain mixed solution;
The mass ratio that essence used and the amount of sodium alginate are pressed the synthetic organic phase change material microcapsule of emulsion polymerization calculates, i.e. essence: sodium alginate: organic phase change material microcapsule are 1:1:5;
Described essence is all sorts of flowers essence;
Finally, it is in 10% calcium chloride water that the injection needles that adopts 2.5 ㎜ dropwise splashes into mass percent concentration by the mixed solution of above-mentioned gained, standing, washing, suction filtration, and the white particle of gained surface clean is grade temperature control sustained-release fragrant gel capsule.
The preparation method of above-mentioned grade temperature control sustained-release fragrant gel capsule, specifically comprises the steps:
(1), the preparation of organic phase change material microcapsule
1., by weighing 16g organic phase change material, be that NSC 62789,0.8g emulsifying agent, 0.32g assistant for emulsifying agent, 0.16g initiator and 180g distilled water weigh in there-necked flask, control temperature and be 55 ℃, stir, obtain emulsion;
Above-mentioned organic phase change material used, 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 1:0.05:0.02:0.01:11.25;
Described emulsifying agent is that Tween-80 and Span-80 calculate in mass ratio, and being Tween-80:Span-80 is the mixture that 55:45 forms;
Described assistant for emulsifying agent is Pentyl alcohol;
Described initiator is benzoyl peroxide;
2., by step 1. gained emulsion to control temperature be 55 ℃, rotating speed 800rpm stirs 0.5h, makes the organic phase change material in emulsion under the effect of emulsifying agent, in water, form stable emulsification system;
3., controlling drop rate is that 2～3ml/min is added drop-wise to 4g methyl methacrylate in emulsification system 2., then temperature is risen to 65 ℃, under nitrogen protection, carry out prepolymerization reaction 0.5h simultaneously, then be warming up to 85 ℃ and carry out polyreaction 5h, polyreaction starts, on the surface of core organic phase change material, there is radical polymerization in methyl methacrylate drop, thereby make micro-encapsulation of core material, after polyreaction finishes, by the standing 12h of gained reaction solution, suction filtration, gained filter cake washs to controlling temperature after elutant clarification and is 50 ℃ and is dried after 24h with the aqueous ethanolic solution that mass percent concentration is 30%, obtain white organic phase change material microcapsule,
(2) preparation of the sodium alginate mixed solution that, contains organic phase change material microcapsule and essence
Get 2.5g sodium alginate and be dissolved in 50mL distilled water and be dissolved to homogeneous transparent under 50 ℃ of conditions, obtain the sodium alginate aqueous solution that mass percent concentration is 5% clear;
By the organic phase change material microcapsule 12.5g of gained in (1), mass percent concentration that all sorts of flowers essence 2.5g joins above-mentioned gained successively, be in the sodium alginate soln of 5% clear after, controlling stir speed (S.S.) is that 800r/min stirs 1h, must contain the sodium alginate mixed solution of organic phase change material microcapsule and essence;
Essence used and the amount of sodium alginate are pressed the amount of the synthetic organic phase change material microcapsule of emulsion polymerization and are calculated, i.e. essence: sodium alginate: organic phase change material microcapsule are 1:1:5;
(3), the preparation of grade temperature control sustained-release fragrant gel capsule
It is in 10% calcium chloride water that the sodium alginate mixed solution that contains organic phase change material microcapsule and essence of gained in (2) is dropwise splashed into mass percent concentration with the injection needles of 2.5 ㎜, quiet 12h, millimeter is with after the hot wash of 60 ℃ 3 times, suction filtration, the white particle of the surface clean of gained, is grade temperature control sustained-release fragrant gel capsule.
The grade temperature control sustained-release fragrant gel capsule of above-mentioned gained has natural flower breath, it is 38.2 ℃ that transformation temperature detects through differential scanning calorimeter, the content of core organic phase change material NSC 62789 detects and is about 56% through thermogravimetric analysis, and the grade temperature control sustained-release fragrant gel capsule of gained has good thermal stability below at 160 ℃.
In sum, a kind of grade temperature control sustained-release fragrant gel capsule of the present invention, because its particle diameter can reach 1.68-2.16mm, so this grade temperature control sustained-release fragrant gel capsule can overcome and easily flies away the defect of filling the air and be applied in the technological deficiency that has seepage in textiles having to have under the condition of wind.
Further, a kind of grade temperature control sustained-release fragrant gel capsule of the present invention, through differential scanning calorimeter, detect, its transformation temperature is 7.1-38.2 ℃, and there is below good thermal stability at 160 ℃, show that thus the grade temperature control sustained-release fragrant gel capsule that the present invention obtains can not only distribute certain fragrant breath, and there is wider phase transformation range, widened the Application Areas of phase change material.
Foregoing is only the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (2)
1. a grade temperature control sustained-release fragrant gel capsule, is characterized in that described grade temperature control sustained-release fragrant gel capsule prepared by the following method:
First, using organic phase change material as core, take polymethylmethacrylate as wall material is by the synthetic organic phase change material microcapsule of emulsion polymerization;
Organic phase change material, polymethylmethacrylate used calculate in mass ratio, organic phase change material: polymethylmethacrylate is 1～4:1;
Described organic change material is whiteruss, n-tetradecane, n-hexadecane, Octadecane, NSC 62789 or solid slice paraffin;
Then, organic phase change material microcapsule and essence are poured into successively in sodium alginate soln and fully stirred and obtain mixed solution;
The mass ratio that essence used and the amount of sodium alginate are pressed the synthetic organic phase change material microcapsule of emulsion polymerization calculates, i.e. essence: sodium alginate: organic phase change material microcapsule are 1:1:1～5;
Described essence is violet compound, lemon flavour or all sorts of flowers essence;
Finally, it is in 10% calcium chloride water that the injection needles that adopts 2.5 ㎜ dropwise splashes into mass percent concentration by the mixed solution of above-mentioned gained, standing, washing, suction filtration, and the white particle of gained surface clean is grade temperature control sustained-release fragrant gel capsule.
2. the preparation method of grade temperature control sustained-release fragrant gel capsule as claimed in claim 1, is characterized in that specifically comprising the steps:
(1), the preparation of organic phase change material microcapsule
1., organic phase change material, emulsifying agent, assistant for emulsifying agent, initiator and distilled water are put into container, control temperature and be 55 ℃, stir, obtain emulsion;
Above-mentioned organic phase change material used, 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 1:0.05:0.02:0.01-0.04:11.25～18;
Described emulsifying agent is that Tween-80 and Span-80 calculate in mass ratio, and being Tween-80:Span-80 is the mixture that 55:45 forms;
Described assistant for emulsifying agent is Pentyl alcohol or n-hexyl alcohol;
Described initiator is benzoyl peroxide or Diisopropyl azodicarboxylate;
2., by step 1. gained emulsion to control temperature be 55 ℃, rotating speed 600～1000rpm stirs 0.5～1h, makes the organic phase change material in emulsion under the effect of emulsifying agent, in water, form stable emulsification system;
3., controlling drop rate is that 2～3ml/min is added drop-wise to methyl methacrylate in emulsification system 2., then temperature is risen to 65 ℃, under nitrogen protection, carry out prepolymerization reaction 0.5～1h simultaneously, then be warming up to 85 ℃ and carry out polyreaction 5～8h, after polyreaction finishes, gained reaction solution is standing, suction filtration, gained filter cake washs to controlling temperature after elutant clarification and is 50 ℃ and is dried after 24h with 30% ethanolic soln, obtains organic phase change material microcapsule;
(2) preparation of the sodium alginate mixed solution that, contains organic phase change material microcapsule and essence
At 50 ℃, compound concentration is the sodium alginate soln of 5% clear, after the organic phase change material microcapsule of gained in step (1) and essence priority are joined in sodium alginate soln successively, controlling stir speed (S.S.) is that 500～800r/min stirs 0.5～1h, must contain the sodium alginate mixed solution of organic phase change material microcapsule and essence;
(3), the preparation of grade temperature control sustained-release fragrant gel capsule
By the sodium alginate mixed solution that contains organic phase change material microcapsule and essence of gained in (2) with in the injection needles of the 2.5 ㎜ calcium chloride water that dropwise to enter to mass percent concentration be 10%, standing 12h, millimeter is with after the hot wash of 60 ℃ 3 times, suction filtration, the white particle of gained surface clean, is grade temperature control sustained-release fragrant gel capsule.
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