CN103464063A - Temperature-control aromatic double-layer microcapsule and preparation method thereof - Google Patents
Temperature-control aromatic double-layer microcapsule and preparation method thereof Download PDFInfo
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- CN103464063A CN103464063A CN201310409905XA CN201310409905A CN103464063A CN 103464063 A CN103464063 A CN 103464063A CN 201310409905X A CN201310409905X A CN 201310409905XA CN 201310409905 A CN201310409905 A CN 201310409905A CN 103464063 A CN103464063 A CN 103464063A
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Abstract
The invention discloses a temperature-control aromatic double-layer microcapsule and a preparation method thereof. The temperature-control aromatic double-layer microcapsule is prepared by the following steps: firstly, synthesizing an organic phase-change material microcapsule by using polymethyl methacrylate as an inner layer wall material through an emulsion polymerization method; then, fully mixing essence with the organic phase-change material microcapsule under high-speed stirring to uniformly distribute the essence on the surface of the organic phase-change material microcapsule to obtain an organic phase-change material microcapsule with adsorbed essence; finally, wrapping beta-cyclodextrin on the organic phase-change material microcapsule with adsorbed essence to obtain the temperature-control aromatic double-layer microcapsule with aromatic flavor and capable of regulating temperature. The temperature-control aromatic double-layer microcapsule prepared in the invention is environment-friendly, non-toxic, high in mechanical strength and good in heat resistance, and the organic phase-change material is entitled with pleasurable aromatic flavor while having a phase-change function, so that the application field of the organic phase-change material is broadened.
Description
Technical field
What the present invention relates to is a kind of bilayered microcapsule and preparation method thereof, and specifically a kind of have temp regulating function, and can discharge bilayered microcapsule of fragrant breath and preparation method thereof.
Background technology
phase-change material micro-capsule (MEPCMs), small " container " that comprises phase-change material in the Nang core, it is as a kind of composite, Volume Changes and leakage problem while having solved the solid-liquid phase change material phase transformation, realized being permanently fixed of phase-change material, make core material and external environment isolated, can resist the effect of oxygen, light etc., thereby make use, storage and the transportation of phase-change material convenient.Phase-change material micro-capsule provides large heat transfer area to improve heat transfer simultaneously, thereby has expanded the scope of application of phase-change material.The reaction monomers that current emulsion polymerization prepares organic phase-change material micro-capsule mainly contains methacrylic acid, methyl methacrylate, hydroxyethyl methacrylate, styrene etc., wherein polymethyl methacrylate, due to advantages such as environment-protecting asepsis, mechanical strength are high, good heat resistances, is the preferred wall material of the organic phase-change material micro-capsule of preparation.
Fragrance not only can make people's mood happy, also has treating disease, optimizes the environment, gives prominence to the effects such as vivid.The appearance of essence microcapsule has solved the short problem of the volatile fragrance remaining time of essence.But in recent years, along with expanding economy, growth in the living standard, simple aromatic micro-capsule or phase-change microcapsule can not meet the pursuit of people to fashionable life, and the variations in temperature fragrance that impact causes more greatly it to discharge on the slow release speed of essence microcapsule inhomogeneous be also one of problem to be solved.
Summary of the invention
One of purpose of the present invention is for the variations in temperature inhomogeneous problem of fragrance that impact causes more greatly it to discharge on the slow release speed of essence microcapsule, proposes a kind of temperature control fragrance bilayered microcapsule, and fragrance is evenly discharged in certain temperature range.
Two of purpose of the present invention is to provide a kind of preparation method of temperature control fragrance bilayered microcapsule.
Know-why of the present invention
A kind of preparation method of temperature control fragrance bilayered microcapsule.First, it is the preparation of polymethyl methacrylate organic phase change material microcapsules, under the effect of emulsifying agent and assistant for emulsifying agent, phase-change material is divided equably in aqueous dispersion mutually, then under uniform temperature and mixing speed, methyl methacrylate is added drop-wise in above-mentioned emulsification system, be warming up to uniform temperature and cause radical polymerization under the effect of initator, be i.e. the synthetic organic phase change material microcapsules of emulsion polymerization; The second, essence is fully mixed with the organic phase change material microcapsules, make essence evenly be adsorbed on the surface of organic phase change material microcapsules; The 3rd, the secondary embedding of beta-schardinger dextrin-to the organic phase change material microcapsules that adsorbed essence, utilize the inclusion complexation method, take beta-schardinger dextrin-as the wall material, and preparation temperature control fragrance bilayered microcapsule, give the microcapsules odor characteristic by essence.
The preparation method of above-mentioned a kind of temperature control fragrance bilayered microcapsule, its principle has emulsion polymerization and inclusion complexation method.Be specifically described as follows:
1, emulsion polymerization principle
Emulsion polymerization is to enter in the micella that generated by emulsifying agent or other modes or emulsion particle and cause the heterogeneous polymerization that monomer wherein carries out polymerization at the free radical generated in aqueous medium.System at least is comprised of monomer, emulsifying agent, initator and water, in this experimental system, also has the core organic phase change material.Particularly, emulsion polymerisation (emulsion polymerization) is under the effect of emulsifying agent and by means of mechanical agitation, makes monomer be dispersed into emulsion in water, the polymerisation of being undertaken by the initator initiation.What in emulsion polymerization process, follow is the radical polymerization of methyl methacrylate.Therefore, the synthetic polymethyl methacrylate organic phase change material microcapsules principle of emulsion polymerization is divided two parts explanation:
(1), the three phases of emulsion polymerisation (speedup phase, constant speed phase and reduction of speed phase)
1.,-----the speedup phase first stage of emulsion polymerisation (emulsion particle generation)
The first stage sign:
From polymerization, start all to disappear to the micella of nucleation not;
Conversion ratio is from 0%～15%, more than this one-phase emulsion particle diameter rises to 20nm～40nm from 6nm～10nm;
2., the second stage of the emulsion polymerisation----constant speed phase
The second stage sign:
Monomer droplet all disappears, and conversion ratio is from 15%～50%;
In monomer-polyalcohol emulsion particle, monomer and polymer respectively account for half, and in emulsion particle, monomer concentration remains unchanged substantially, and the emulsion particle number is constant, and rate of polymerization is constant, and monomer-polyalcohol emulsion particle diameter is 50nm～150nm to the maximum;
3., the three phases of emulsion polymerisation---the reduction of speed phase
The phase III sign:
Conversion ratio increases to 100% from 50%;
Rate of polymerization descends with the decline of monomer concentration in monomer-polyalcohol emulsion particle, and last monomer is transformed into polymer fully;
(2), the radical polymerization mechanism of methyl methacrylate
1., chain initiation reaction
Decomposition of initiator produces elementary free radical, and elementary free radical and monomer addition generate the course of reaction of monomer free radical;
2., chain propagation reaction
New free radical is produced in monomer free radical and monomer addition, so repeatedly generates the process of chain free radical.
3., chain termination reaction
Free radical activity is high, and having interacts stops and deactivated tendency.The reaction that forms stabilization of polymer that loses activity of chain free radical is called chain termination reaction;
(2) inclusion complexation method principle
The inclusion complexation method is to take the microcapsule preparation method of beta-schardinger dextrin-as the wall material.Beta-schardinger dextrin-is that 7 glucopyranoses connect into by α-Isosorbide-5-Nitrae glycosidic bond, has the material of ring shaped molecule structure.Its molecule becomes oil cake shape, has the structure of hollow, and center has hydrophobicity, and skin is hydrophily.Simultaneously, beta-schardinger dextrin-has the spatial volume matching effect, with there is the interaction by non-covalent bond of suitable size, shape and hydrophobic molecule and form stable inclusion compound, therefore, many hydrophobic essence materials, pigment and vitamin can replace the hydrone at its center and and its strong complexing.
Technical scheme of the present invention
A kind of temperature control fragrance bilayered microcapsule, take organic phase change material as core, organic phase change material microcapsules that the polymethyl methacrylate of take obtains as the inner layer wall material adsorbed gained after essence absorption the organic phase change material microcapsules after essence, take beta-schardinger dextrin-as the outer wall material is coated again, obtain temperature control fragrance bilayered microcapsule; This temperature control fragrance bilayered microcapsule not only has temp regulating function, the breath that can give out a sweet perfume simultaneously;
The amount of above-mentioned organic phase change material used, polymethyl methacrylate, essence, calculate in mass ratio, i.e. organic phase change material: polymethyl methacrylate: essence is 1～4:1:0.05～0.2;
The amount of beta-schardinger dextrin-used, by itself and the mass ratio that has adsorbed the organic phase change material microcapsules after essence, calculate, i.e. beta-schardinger dextrin-: having adsorbed the organic phase change material microcapsules after essence is 1:1;
Described organic change material is atoleine, hexadecane, n-octadecane, n-docosane or solid slice paraffin;
Described essence is orange oil essence, lily essence or flavoring rose essence.
The preparation method of above-mentioned a kind of temperature control fragrance bilayered microcapsule, at first, take polymethyl methacrylate as the inner layer wall material coats organic phase change material, obtains the organic phase change material microcapsules;
Then, the organic phase change material microcapsules are fully mixed with essence, make essence evenly be adsorbed on the surface of organic phase change material microcapsules, obtained adsorbing the organic phase change material microcapsules of essence;
Finally, with beta-schardinger dextrin-, coat and adsorbed the organic phase change material microcapsules of essence, thereby obtain temperature control fragrance bilayered microcapsule, its preparation process specifically comprises the following steps:
(1), adopt emulsion polymerization, take polymethyl methacrylate as the inner layer wall material, take organic phase change material as core, synthetic organic phase change material microcapsules, its concrete steps are as follows:
1., organic phase change material, emulsifying agent, assistant for emulsifying agent, initator and distilled water are put into to container, heating, stir and obtain emulsion;
Above-mentioned organic phase change material used, emulsifying agent, assistant for emulsifying agent, initator and distilled water calculate in mass ratio, i.e. organic phase change material: emulsifying agent: assistant for emulsifying agent: initator: distilled water is 100:5:2:1～4:1125～1800;
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-amyl alcohol or n-hexyl alcohol;
Described initator is benzoyl peroxide or azodiisobutyronitrile;
2., by step 1. the gained emulsion stir 0.5～1h with the rotating speed of 600～1000rpm under 55 ℃, make organic phase change material form stable emulsification system under the effect of emulsifying agent in water;
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 ℃, carry out prepolymerization reaction simultaneously under nitrogen protection, time is 0.5～1h, then is warming up to 85 ℃ and carries out polymerisation 5～8h, after reaction finishes, the gained reactant liquor is standing, suction filtration, the gained filter cake washs to controlling temperature after filtrate clarification and is 50 ℃ and carries out drying with ethanol, obtains the organic phase change material microcapsules;
(2) preparation of, having adsorbed the organic phase change material microcapsules of essence
Organic phase change material microcapsules prepared in (1) are evenly mixed with essence, obtained adsorbing the organic phase change material microcapsules of essence;
(3), beta-schardinger dextrin-coats the organic phase change material microcapsules that adsorbed essence
Beta-schardinger dextrin-is dissolved in distilled water and makes the beta-schardinger dextrin-aqueous solution that concentration is 40%;
By the absorption of step (2) gained the organic phase change material microcapsules of essence join in the beta-schardinger dextrin-aqueous solution that concentration that temperature is 45 ℃ is 40%, cool while stirring to static spending the night after room temperature, the temperature control fragrance bilayered microcapsule crude product formed is Precipitation from solution slowly, filter, the gained filter cake washs to controlling temperature after filtrate clarification and is 50 ℃ and carries out drying through ethanol, obtains temperature control fragrance bilayered microcapsule.
Beneficial effect of the present invention
A kind of temperature control fragrance bilayered microcapsule of the present invention, at first adopt environment-protecting asepsis, mechanical strength is high, the polymethyl methacrylate of good heat resistance is that the inner layer wall material coats organic phase change material, obtain the organic phase change material microcapsules, then, the organic phase change material microcapsules are fully mixed with essence, make essence evenly be adsorbed on the surface of organic phase change material microcapsules, the organic phase change material microcapsules of essence have been obtained adsorbing, finally, coat with beta-schardinger dextrin-the organic phase change material microcapsules that adsorbed essence and obtain temperature control fragrance bilayered microcapsule, this temperature control fragrance bilayered microcapsule not only has temp regulating function, the breath that can give out a sweet perfume simultaneously.Solved technically the inhomogeneous problem of fragrance that variations in temperature causes more greatly it to discharge on the slow release speed impact of essence microcapsule, made to carry out in the certain temperature range of being released in of fragrance.
A kind of temperature control fragrance bilayered microcapsule of the present invention is given it and is made us the fragrant breath of feeling joyful when having phase transition function, has widened the field of organic phase change material application.
The specific embodiment
Below by specific embodiment, the present invention is further set forth, but can not limit content of the present invention.
The information of the various raw materials that the present invention is used or the specification of reagent and manufacturer is as follows:
Methyl methacrylate, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Azodiisobutyronitrile, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Hexadecane, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Atoleine, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Tween-80, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Span-80, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Absolute ethyl alcohol, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Beta-schardinger dextrin-, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Orange oil essence, Shenzhen GuanLiDa BoDun spice Co., Ltd;
Flavoring rose essence, the international essence and flavoring agent (China) of American I FF Co., Ltd.
The model of the instrument and equipment that the present invention is used and the information of manufacturer are as follows:
Homogenizer, the 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 and meter Manufacturing Co., Ltd;
The multiplex vavuum pump of circulating water type, the SHZ-D III, special instrument and equipment Co., Ltd shines in Shanghai;
The digital display blast drier, 101, the Shanghai leaf is opened up instrument and meter Co., Ltd;
Biomicroscope, XSP-BM-8CAS, Shanghai Bi Aimu optical instrument Co., Ltd;
Thermogravimetric analyzer, TGA-Q5000, U.S. TA instrument company;
High performance liquid chromatograph, UPLC, water generation Science and Technology Ltd.;
Fourier transformation infrared spectrometer, VERTEX70, Brooker spectral instrument company;
Differential scanning calorimeter, DSC-Q2000, U.S. TA instrument company.
embodiment 1
A kind of temperature control fragrance bilayered microcapsule, take organic phase change material as core, organic phase change material microcapsules that the polymethyl methacrylate of take obtains as the inner layer wall material adsorbed gained after essence absorption the organic phase change material microcapsules after essence, take beta-schardinger dextrin-as the outer wall material is coated again, obtain temperature control fragrance bilayered microcapsule;
The amount of above-mentioned organic phase change material used, polymethyl methacrylate, essence, calculate in mass ratio, i.e. organic phase change material: polymethyl methacrylate: essence is 1:1:0.05;
The amount of beta-schardinger dextrin-used, by itself and the mass ratio that has adsorbed the organic phase change material microcapsules after essence, calculate, i.e. beta-schardinger dextrin-: having adsorbed the organic phase change material microcapsules after essence is 1:1;
Described organic change material is atoleine;
Described essence is lily essence.
The preparation method of above-mentioned a kind of temperature control fragrance bilayered microcapsule specifically comprises the following steps:
(1), the preparation of polymethyl methacrylate atoleine microcapsules, adopt emulsion polymerization, take polymethyl methacrylate as the inner layer wall material, synthetic polymethyl methacrylate atoleine microcapsules, its concrete steps are as follows:
1., weighing 4g organic phase change material is that atoleine, 0.2g emulsifying agent, 0.08g assistant for emulsifying agent, 0.16g initator and the weighing of 72g distilled water enter in there-necked flask, heating, stir and obtain emulsion;
Above-mentioned organic phase change material used, emulsifying agent, assistant for emulsifying agent, initator and distilled water calculate in mass ratio, i.e. organic phase change material: emulsifying agent: assistant for emulsifying agent: initator: distilled water is 1:0.05:0.02:0.04:18;
Described emulsifying agent 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 initator is azodiisobutyronitrile;
2., by step 1. the gained emulsion stir 0.5h with the rotating speed of 800rpm under 55 ℃, make organic phase change material form stable emulsification system under the effect of emulsifying agent in water;
3., controlling drop rate is that 2～3ml/min is added drop-wise to the 4g methyl methacrylate in emulsification system 2., then temperature is risen to 65 ℃ of whiles carries out the pre-polymerization back flow reaction under nitrogen protection, time is 0.5h, then be warming up to 85 ℃ and carry out polymerisation 5h, polymerisation starts, radical polymerization occurs on the surface of core organic phase change material in the methyl methacrylate drop, thereby make micro-encapsulation of core material, after polymerisation finishes, by the standing 12h of gained reactant liquor, suction filtration, the gained filter cake washs to controlling temperature after filtrate clarification and is 50 ℃ and carries out drying through ethanol, obtain white organic phase change material microcapsules,
The consumption of described methyl methacrylate, the mass ratio by it with respect to step organic phase change material used in 1. calculates, i.e. methyl methacrylate: organic phase change material is 1:1;
(2) preparation of, having adsorbed the organic phase change material microcapsules of lily essence
The organic phase change material microcapsules of gained in (1) are evenly mixed with 0.2g lily essence, obtained adsorbing the organic phase change material microcapsules of lily essence;
The consumption of lily essence is by itself and the calculating of the mass ratio of organic phase change material microcapsules, i.e. lily essence: the organic phase change material in the organic phase change material microcapsules is 0.05:1;
(3), beta-schardinger dextrin-coats the organic phase change material microcapsules that adsorbed lily essence
The 5g beta-schardinger dextrin-is dissolved in distilled water and makes the beta-schardinger dextrin-aqueous solution that concentration is 40%;
By the absorption of the 5g of step (2) gained the organic phase change material microcapsules of lily essence join in the beta-schardinger dextrin-aqueous solution that concentration that temperature is 45 ℃ is 40%, controlling speed of agitator is to be down to room temperature after 600r/min stirs 2h, static 24h, make slowly Precipitation from solution of the bilayer fragrance organic phase change material microcapsules crude product that forms, filter, the gained filter cake washs to controlling temperature after filtrate clarification and is 50 ℃ and carries out drying through ethanol, obtains temperature control fragrance bilayered microcapsule.
The temperature control fragrance bilayered microcapsule of above-mentioned gained has the natural lily breath, phase transition temperature detects as-20 ℃ through differential scanning calorimeter, the content of core organic phase change material atoleine detects and is about 47% through thermogravimetric analysis, and the temperature control of gained fragrance bilayered microcapsule has good thermal stability below 160 ℃.
embodiment 2
A kind of temperature control fragrance bilayered microcapsule, take organic phase change material as core, organic phase change material microcapsules that the polymethyl methacrylate of take obtains as the inner layer wall material adsorbed gained after essence absorption the organic phase change material microcapsules after essence, take beta-schardinger dextrin-as the outer wall material is coated again, obtain temperature control fragrance bilayered microcapsule;
The amount of above-mentioned organic phase change material used, polymethyl methacrylate, essence, calculate in mass ratio, i.e. organic phase change material: polymethyl methacrylate: essence is 4:1:0.2;
The amount of beta-schardinger dextrin-used, by itself and the mass ratio that has adsorbed the organic phase change material microcapsules after essence, calculate, i.e. beta-schardinger dextrin-: having adsorbed the organic phase change material microcapsules after essence is 1:1;
Described organic change material is hexadecane;
Described essence is flavoring rose essence.
The preparation method of above-mentioned a kind of temperature control fragrance bilayered microcapsule specifically comprises the following steps:
(1), adopt emulsion polymerization, take polymethyl methacrylate as the inner layer wall material, take organic phase change material as core, synthetic organic phase change material microcapsules, its concrete steps are as follows:
1., 16g organic phase change material, 0.8g emulsifying agent, 0.32g assistant for emulsifying agent, 0.16g initator and 180g distilled water are put into to container, heating, stir and obtain emulsion;
Above-mentioned organic phase change material used, emulsifying agent, assistant for emulsifying agent, initator and distilled water come by matter can be than calculating, i.e. organic phase change material: emulsifying agent: assistant for emulsifying agent: initator: distilled water is 1:0.05:0.02:0.01:11.25;
Described emulsifying agent 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 initator is azodiisobutyronitrile;
2., by step 1. the gained emulsion stir 0.5h with the rotating speed of 800rpm under 55 ℃, make organic phase change material form stable emulsification system under the effect of emulsifying agent in water;
3., controlling drop rate is that 2～3ml/min is added drop-wise to the 4g methyl methacrylate in emulsification system 2., then temperature is risen to 65 ℃, carry out pre-polymerization back flow reaction 1h simultaneously under nitrogen protection, then be warming up to 85 ℃ and carry out polymerisation 8h, after reaction finishes, by the standing 12h of gained reactant liquor, suction filtration, the gained filter cake washs to controlling temperature after filtrate clarification and is 50 ℃ and carries out drying through ethanol, obtains white organic phase change material microcapsules;
The consumption of described methyl methacrylate, the mass ratio by it with respect to step organic phase change material used in 1. calculates, i.e. methyl methacrylate: organic phase change material is 1:4;
(2) preparation of, having adsorbed the organic phase change material microcapsules of essence
The organic phase change material microcapsules of gained in (1) are evenly mixed with the 0.8g flavoring rose essence, obtained adsorbing the organic phase change material microcapsules of flavoring rose essence;
The consumption of flavoring rose essence is by itself and the calculating of the mass ratio of organic phase change material microcapsules, i.e. essence: the organic phase change material in the organic phase change material microcapsules is 0.2:1;
(3), beta-schardinger dextrin-coats the organic phase change material microcapsules that adsorbed flavoring rose essence
The 10g beta-schardinger dextrin-is dissolved in distilled water and makes the beta-schardinger dextrin-aqueous solution that concentration is 40%;
By the absorption of the 10g of step (2) gained the organic phase change material microcapsules of flavoring rose essence join in the beta-schardinger dextrin-aqueous solution that concentration that temperature is 45 ℃ is 40%, controlling speed of agitator is to be down to room temperature after 600r/min stirs 2h, static 24h, make slowly Precipitation from solution of the bilayer fragrance organic phase change material microcapsules crude product that forms, filter, the gained filter cake washs to controlling temperature after filtrate clarification and is 50 ℃ and carries out drying through ethanol, obtains temperature control fragrance bilayered microcapsule.
The temperature control fragrance bilayered microcapsule of above-mentioned gained has the natural rose breath, it is 35 ℃ that phase transition temperature detects through differential scanning calorimeter, the content of core organic phase change material n-octadecane detects and is about 50% through thermogravimetric analysis, and the temperature control fragrance bilayered microcapsule of gained has good thermal stability below 160 ℃.
Foregoing is the basic explanation under conceiving for the present invention only, 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 (3)
1. temperature control fragrance bilayered microcapsule, it is characterized in that described temperature control fragrance bilayered microcapsule take organic phase change material as core, organic phase change material microcapsules that the polymethyl methacrylate of take obtains as the inner layer wall material adsorbed gained after essence absorption the organic phase change material microcapsules after essence, take beta-schardinger dextrin-as the outer wall material is coated again, obtain temperature control fragrance bilayered microcapsule;
The amount of organic phase change material used, polymethyl methacrylate, essence, calculate in mass ratio, i.e. organic phase change material: polymethyl methacrylate: essence is 1～4:1:0.05～0.2;
The amount of beta-schardinger dextrin-used, by itself and the mass ratio that has adsorbed the organic phase change material microcapsules after essence, calculate, i.e. beta-schardinger dextrin-: having adsorbed the organic phase change material microcapsules after essence is 1:1;
Described organic change material is atoleine, hexadecane, n-octadecane, n-docosane or solid slice paraffin;
Described essence is orange oil essence, lily essence or flavoring rose essence.
2. the preparation method of a kind of temperature control fragrance bilayered microcapsule as claimed in claim 1 is characterized in that:
At first, take polymethyl methacrylate as the inner layer wall material coats organic phase change material, obtain the organic phase change material microcapsules;
Then, the organic phase change material microcapsules are fully mixed with essence, make essence evenly be adsorbed on the surface of organic phase change material microcapsules, obtained adsorbing the organic phase change material microcapsules of essence;
Finally, with beta-schardinger dextrin-, be that the outer wall material coats the organic phase change material microcapsules that adsorbed essence, obtain temperature control fragrance bilayered microcapsule.
3. the preparation method of a kind of temperature control fragrance bilayered microcapsule as claimed in claim 2 is characterized in that specifically comprising the following steps:
(1), adopt emulsion polymerization, take polymethyl methacrylate as the inner layer wall material, take organic phase change material as core, synthetic organic phase change material microcapsules, its concrete steps are as follows:
1., organic phase change material, emulsifying agent, assistant for emulsifying agent, initator and distilled water are put into to container, heating, stir and obtain emulsion;
Above-mentioned organic phase change material used, emulsifying agent, assistant for emulsifying agent, initator and distilled water calculate in mass ratio, i.e. organic phase change material: emulsifying agent: assistant for emulsifying agent: initator: distilled water is 100:5:2:1～4:1125～1800;
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-amyl alcohol or n-hexyl alcohol;
Described initator is benzoyl peroxide or azodiisobutyronitrile;
2., by step 1. the gained emulsion stir 0.5～1h with the rotating speed of 600～1000rpm under 55 ℃, make organic phase change material form stable emulsification system under the effect of emulsifying agent in water;
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 ℃, carry out prepolymerization reaction simultaneously under nitrogen protection, time is 0.5～1h, then is warming up to 85 ℃ and carries out polymerisation 5～8h, after reaction finishes, the gained reactant liquor is standing, suction filtration, the gained filter cake washs to controlling temperature after filtrate clarification and is 50 ℃ and carries out drying with ethanol, obtains the organic phase change material microcapsules;
(2) preparation of, having adsorbed the organic phase change material microcapsules of essence
Organic phase change material microcapsules prepared in (1) are evenly mixed with essence, obtained adsorbing the organic phase change material microcapsules of essence;
(3), beta-schardinger dextrin-coats the organic phase change material microcapsules that adsorbed essence
Beta-schardinger dextrin-is dissolved in distilled water and makes the beta-schardinger dextrin-aqueous solution that concentration is 40%;
By the absorption of step (2) gained the organic phase change material microcapsules of essence join in the beta-schardinger dextrin-aqueous solution that concentration that temperature is 45 ℃ is 40%, cool while stirring to static spending the night after room temperature, the temperature control fragrance bilayered microcapsule crude product formed is Precipitation slowly, filter, the gained filter cake washs to controlling temperature after filtrate clarification and is 50 ℃ and carries out drying through ethanol, obtains temperature control fragrance bilayered microcapsule.
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| CN104774593A (en) * | 2015-03-11 | 2015-07-15 | 上海应用技术学院 | Cool temperature controlled microcapsule and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101530772A (en) * | 2009-03-13 | 2009-09-16 | 清华大学深圳研究生院 | Preparing method for phase transited stored energy microcapsule covered with an organic polymer material |
| CN102827586A (en) * | 2012-09-17 | 2012-12-19 | 上海菲康垫子制品厂 | Double-layer aromatic organic phase change material microcapsules and preparation method thereof |
-
2013
- 2013-09-11 CN CN201310409905XA patent/CN103464063A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101530772A (en) * | 2009-03-13 | 2009-09-16 | 清华大学深圳研究生院 | Preparing method for phase transited stored energy microcapsule covered with an organic polymer material |
| CN102827586A (en) * | 2012-09-17 | 2012-12-19 | 上海菲康垫子制品厂 | Double-layer aromatic organic phase change material microcapsules and preparation method thereof |
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| CN103805143A (en) * | 2014-02-19 | 2014-05-21 | 东华大学 | Phase-change material microcapsule with aromatic odor and preparation method thereof |
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| CN108142993B (en) * | 2017-12-29 | 2020-08-11 | 玉溪笃行创新科技有限公司 | Phase change filter stick additive and preparation method and application thereof |
| CN108940148A (en) * | 2018-07-27 | 2018-12-07 | 云南中烟工业有限责任公司 | A kind of preparation method of temperature control sustained-release essence micro-capsule |
| CN109294737A (en) * | 2018-10-26 | 2019-02-01 | 广州丽悦香精香料有限公司 | A kind of preparation method of essence microcapsule |
| CN109294737B (en) * | 2018-10-26 | 2022-04-22 | 广州丽悦香精香料有限公司 | Preparation method of essence microcapsule |
| CN110627402A (en) * | 2019-09-29 | 2019-12-31 | 北京工业大学 | Cement-based composite phase-change heat-storage temperature-regulating material based on mixed ester phase-change microcapsules |
| CN110627402B (en) * | 2019-09-29 | 2021-11-19 | 北京工业大学 | Cement-based composite phase-change heat-storage temperature-regulating material based on mixed ester phase-change microcapsules |
| CN111589387A (en) * | 2020-04-21 | 2020-08-28 | 同济大学 | Microcapsule composite material and preparation method thereof |
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| CN113913160B (en) * | 2021-11-09 | 2023-08-15 | 青岛尼希米生物科技有限公司 | Double-layer capsule wall energy storage temperature adjustment microcapsule, polyacrylonitrile fiber and preparation method thereof |
| CN114457594A (en) * | 2022-02-15 | 2022-05-10 | 绍兴柯桥春意居室用品有限公司 | Production method of aromatic home textile fabric |
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