CN103451939A - Double-layer aromatic phase change microcapsule textile finishing liquor as well as preparation method and application thereof - Google Patents

Double-layer aromatic phase change microcapsule textile finishing liquor as well as preparation method and application thereof Download PDF

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CN103451939A
CN103451939A CN2013104100663A CN201310410066A CN103451939A CN 103451939 A CN103451939 A CN 103451939A CN 2013104100663 A CN2013104100663 A CN 2013104100663A CN 201310410066 A CN201310410066 A CN 201310410066A CN 103451939 A CN103451939 A CN 103451939A
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organic phase
phase change
change material
essence
double
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CN103451939B (en
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宋晓秋
刘钦矿
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Shanghai Institute of Technology
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Shanghai Institute of Technology
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Abstract

The invention discloses double-layer aromatic phase change microcapsule textile finishing liquor as well as a preparation method and application thereof. The double-layer aromatic phase change microcapsule textile finishing liquor comprises 10-30% of double-layer aromatic phase change microcapsules, 5-15% of low-temperature crosslinking agent, 1-5% of thickening agent, 1-3% of penetrant, 1-3% of emulsifier 1 and the balance of distilled water by mass percent. The preparation method comprises the following steps: firstly preparing the double-layer aromatic phase change microcapsules, then mixing the prepared double-layer aromatic phase change microcapsules, the low-temperature crosslinking agent, the thickening agent, the penetrant, the emulsifier and the distilled water, and stirring the materials at normal temperature and normal pressure for 10-20 minutes, thus obtaining the double-layer aromatic phase change microcapsule textile finishing liquor. Textiles are flavoured by coating or spraying the double-layer aromatic phase change microcapsule textile finishing liquor, and the flavoured textiles not only have good aroma retaining capacities and slow release performances but also have good temperature adjusting functions, and improve the comfort, wherein the aroma can be retained for 7 months.

Description

The fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer and preparation method and application
Technical field
The present invention relates to a kind of method of applying double-deck fragrant phase-change microcapsule perfuming on textiles, more particularly relate to fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer and preparation method thereof and the application aspect the textiles perfuming.
Background technology
Microcapsules are as a kind of emerging technology, can Protective substances avoid the impact of environment, and control core discharges, and changes states of matter easy to carry and transport.Essence microcapsule can effectively be controlled the fragrance rate of release, to the people, brings lasting joyful fragrance, and long via the aromatic fabric fragrance remaining time of essence microcapsule processing, fragrance discharges evenly, has met the demand that people decorate, enjoy, keep healthy textiles.And the appearance of phase-change microcapsule, realized the permanent solid state of phase-change material, can be when phase transformation occurs, control the variation of phase-change material volume, can effectively increase its heat transfer area, the minimizing phase-change material reacts with external environment, has been applied to the fields such as heat-storage thermoregulation material, energy-saving building material, solar energy utilization.Phase-change microcapsule is applied to textiles and can further meets the demand of people to comfortable life.
Yet, simple aromatic fabric and temperature control textiles all have certain application restric-tion, how to utilize microcapsules technology to develop to possess slow release fragrance and the fragrant temperature control textiles of regulating temperature feature is current study hotspot simultaneously.
Summary of the invention
One of purpose of the present invention is to provide a kind of bilayer fragrant phase-change microcapsule fabric finishing liquor in order to solve above-mentioned technical problem, this bilayer fragrance phase-change microcapsule fabric finishing liquor carries out perfuming on textiles, can meet the demand that people have slow release fragrance simultaneously and regulate temperature function textiles.
Two of purpose of the present invention is to provide the preparation method of the above-mentioned fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer.
Three of purpose of the present invention is to provide utilizes the fragrant phase-change microcapsule fabric finishing liquor of above-mentioned a kind of bilayer to carry out the method for perfuming on textiles.
Technical scheme of the present invention
The fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer, calculate by mass percentage, and its raw material composition and content are as follows:
Double-deck fragrant phase-change microcapsule 10~30%
Crosslinked at low temperature agent 5~15%
Thickener 1~5%
Bleeding agent 1~3%
Emulsifying agent 1~3%
Surplus is distilled water;
Prepared by the following method by the fragrant phase-change microcapsule of wherein said bilayer:
At first, take polymethyl methacrylate as the wall material coats organic phase change material, obtain the organic phase change material microcapsules, wherein methyl methacrylate and organic phase change material calculate in mass ratio, i.e. methyl methacrylate: organic phase change material is 1:2;
Described organic phase change material is atoleine, hexadecane or octadecane;
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, the consumption of described essence calculates by its mass ratio with respect to the organic phase change material microcapsules, i.e. essence: the organic phase change material microcapsules are 4:100;
Described essence is lavender oil, lily essence, flavoring rose essence or cream jasmin france;
Finally, coat and adsorbed the organic phase change material microcapsules of essence with beta-schardinger dextrin-, thereby obtain double-deck fragrant phase-change microcapsule; Wherein said beta-schardinger dextrin-and adsorbed the organic phase change material microcapsules of essence, by beta-schardinger dextrin-and the mass ratio that adsorbed the organic phase change material microcapsules of essence, calculate, i.e. organic phase change material: beta-schardinger dextrin-is 1:2;
Described crosslinked at low temperature agent CX-100 is the polyfunctional aziridines crosslinking agent;
Described thickening agent PTF is the anionic species polyelectrolyte;
Described penetrating agent JFC, be fatty alcohol-polyoxyethylene ether, non-ionic surface active agent;
Described emulsifying agent 1 is Tween-80.
The preparation method of the above-mentioned fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer, its feature specifically comprises the steps:
(1), the preparation of double-deck fragrant phase-change microcapsule
1., adopt emulsion polymerization, take polymethyl methacrylate as the wall material, take organic phase change material as core, synthetic organic phase change material microcapsules, its concrete steps are as follows:
At first, organic phase change material, methyl methacrylate, initator are stirred to dissolving after mixing, obtain oil phase component;
Described organic phase change material is atoleine, hexadecane or octadecane;
Described initator is azodiisobutyronitrile;
By emulsifying agent 2 and distilled water, 55 ℃ of lower agitation as appropriate, to evenly, obtain the water component again;
Described emulsifying agent 2 is Tween-80:Span-80, calculates in mass ratio, and being Tween-80:Span-80 is the mixture that 55:45 forms;
Then, under the 600rpm rotating speed, oil phase component is joined in the water component, temperature remains on 55 ℃ and stirs 30min, forms the O/W emulsion;
Above-mentioned organic phase change material used, methyl methacrylate, initator, emulsifying agent 2, distilled water calculate in mass ratio, i.e. organic phase change material: methyl methacrylate: initator: emulsifying agent 2: distilled water is 80:40:3:4:1500;
Then, by gained O/W emulsion under the high speed shear of 13000rpm after homogeneous 5min reflux condensation mode pass into nitrogen protection, prepolymerization 1h under 65 ℃ of waters bath with thermostatic control, 1000rpm are stirred simultaneously;
Then, under water bath condition, by temperature increase to 85 ℃ polymerisation 5h, standing 12h after reaction finishes, be that 30% ethanol-water solution washs three times with 50 ℃, mass percent concentration after suction filtration, and finally dry 24h under 50 ℃, obtain the organic phase change material microcapsules;
The preparation of 2., having adsorbed the organic phase change material microcapsules of essence
1. prepared organic phase change material microcapsules in are evenly mixed with essence, obtained the organic phase change material microcapsules of absorption essence;
The consumption of described essence calculates by its mass ratio with respect to organic phase change material in the organic phase change material microcapsules, i.e. essence: in the organic phase change material microcapsules, organic phase change material is 4:100;
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 step 2. gained absorption 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, make slowly Precipitation from solution of the bilayer fragrance phase-change microcapsule crude product that forms, filter the gained filter cake and wash to controlling temperature after the filtrate clarification and be 50 ℃ and be drying to obtain double-deck fragrant phase-change microcapsule through ethanol;
Wherein said beta-schardinger dextrin-and adsorbed the organic phase change material microcapsules of essence, by beta-schardinger dextrin-and the mass ratio that adsorbed the organic phase change material microcapsules of essence, calculate, i.e. organic phase change material: beta-schardinger dextrin-is 1:2;
(2), the preparation of double-deck fragrant phase-change microcapsule fabric finishing liquor
(1), after bilayer fragrance phase-change microcapsule, crosslinked at low temperature agent, thickener, bleeding agent, emulsifying agent 1 prepared by step mixes, magnetic agitation 10~20min obtains double-deck fragrant phase-change microcapsule fabric finishing liquor at normal temperatures and pressures.
Utilize the fragrant phase-change microcapsule fabric finishing liquor of above-mentioned a kind of bilayer textiles to be carried out to the method for perfuming, by spray-on process or coating;
Described spray-on process, spray double-deck fragrant phase-change microcapsule fabric finishing liquor with watering can in textile surfaces, natural air drying, and wetting, 40~70 ℃ of oven dry complete the perfuming of double-deck fragrant phase-change microcapsule fabric finishing liquor on textiles;
Described coating, use scraper after the double-deck fragrant phase-change microcapsule fabric finishing liquor of textile surfaces blade coating, controls 70~120 ℃ of temperature, completes the perfuming of double-deck fragrant phase-change microcapsule fabric finishing liquor on textiles after drying 30~80s.
Beneficial effect of the present invention
The fragrant phase-change microcapsule fabric of a kind of bilayer of the present invention, owing to containing double-deck fragrant phase-change microcapsule, therefore it is applied on textiles and carries out perfuming, give textiles two large critical function: the rate of release that can meet fragrance is effectively controlled, bring lasting joyful fragrance to the people, the health-care function such as play calmness, sterilization, calm the nerves; Simultaneously because but the phase-change material in the fragrant phase-change microcapsule of bilayer can, according to variation free adjustment textiles internal temperature in certain temperature range of ambient temperature, therefore have more comfortableness than conventional textiles.
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, chemical pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Azodiisobutyronitrile, chemical 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;
Thickening agent PTF, Jiangsu Hai'an Petrochemical Plant produces;
Penetrating agent JFC, Jiangsu Hai'an Petrochemical Plant produces;
Absolute ethyl alcohol, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Beta-schardinger dextrin-, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Lavender oil, the international essence and flavoring agent (China) of American I FF Co., Ltd produces;
Lily essence, the international essence and flavoring agent (China) of American I FF Co., Ltd produces;
Crosslinked at low temperature agent CX-100, Guangzhou Zhong Guanmei Co., Ltd produces.
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;
Coating machine MU572C, Beijing textile equipment research institute.
embodiment 1
The fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer, calculate by mass percentage, and its raw material composition and content are as follows:
Double-deck fragrant phase-change microcapsule 20g (20%)
Crosslinked at low temperature agent 10g (10%)
Thickener 3g (3%)
Bleeding agent 2g (2%)
Emulsifying agent 1 2g (2%)
Distilled water 63g (63%);
Prepared by the following method by the fragrant phase-change microcapsule of wherein said bilayer:
At first, take polymethyl methacrylate as the wall material coats organic phase change material, obtain the organic phase change material microcapsules; Wherein methyl methacrylate and organic phase change material calculate in mass ratio, i.e. methyl methacrylate: organic phase change material is 1:2, and described organic phase change material is atoleine;
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; The consumption of wherein said essence calculates by its mass ratio with respect to the organic phase change material microcapsules, i.e. essence: the organic phase change material microcapsules are 4:100, and described essence is lavender oil;
Finally, coat and adsorbed the organic phase change material microcapsules of essence with beta-schardinger dextrin-, thereby obtain double-deck fragrant phase-change microcapsule; Wherein said beta-schardinger dextrin-and adsorbed the organic phase change material microcapsules of essence, by beta-schardinger dextrin-and the mass ratio that adsorbed the organic phase change material microcapsules of essence, calculate, i.e. organic phase change material: beta-schardinger dextrin-is 1:2;
Described crosslinked at low temperature agent is CX-100, is the polyfunctional aziridines crosslinking agent that Guangzhou Zhong Guanmei Co., Ltd produces;
Described thickener is PTF, is the anionic species polyelectrolyte that Jiangsu Hai'an Petrochemical Plant produces;
Described bleeding agent is JFC, is the fatty alcohol-polyoxyethylene ether that Jiangsu Hai'an Petrochemical Plant produces, non-ionic surface active agent;
Described emulsifying agent 1 is Tween-80.
The preparation method of the above-mentioned fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer, specifically comprise the steps:
(1), the preparation of double-deck fragrant phase-change microcapsule
1., adopt emulsion polymerization, take polymethyl methacrylate as the wall material, take organic phase change material as core, synthetic organic phase change material microcapsules, its concrete steps are as follows:
At first, 8g organic phase change material, 4g methyl methacrylate, 0.3g initator are stirred to dissolving after mixing, obtain oil phase component;
Described organic phase change material is atoleine;
Described initator is azodiisobutyronitrile;
By 0.4g emulsifying agent 2 and 150g distilled water, 55 ℃ of lower agitation as appropriate, to evenly, obtain the water component again;
Described emulsifying agent 2 is Tween-80:Span-80, calculates in mass ratio, and being Tween-80:Span-80 is the mixture that 55:45 forms;
Then, under the 600rpm rotating speed, oil phase component is joined in the water component, temperature remains on 55 ℃ and stirs 30min, forms the O/W emulsion;
Above-mentioned organic phase change material used, methyl methacrylate, initator, emulsifying agent 2, distilled water calculate in mass ratio, i.e. organic phase change material: methyl methacrylate: initator: emulsifying agent 2: distilled water is 80:40:3:4:1500;
Then, by gained O/W emulsion under the high speed shear of 13000rpm after homogeneous 5min reflux condensation mode pass into nitrogen protection, prepolymerization 1h under 65 ℃ of waters bath with thermostatic control, 1000rpm are stirred simultaneously;
Then, under water bath condition, by temperature increase to 85 ℃ polymerisation 5h, standing 12h after reaction finishes, be that 30% ethanol-water solution washs three times with 50 ℃, mass percent concentration after suction filtration, and finally dry 24h under 50 ℃, obtain the organic phase change material microcapsules;
The preparation of 2., having adsorbed the organic phase change material microcapsules of essence
1. prepared organic phase change material microcapsules in are evenly mixed with 0.32g essence, obtained the organic phase change material microcapsules of absorption essence;
Described essence is lavender oil;
The consumption of described essence calculates by its mass ratio with respect to the organic phase change material in the organic phase change material microcapsules, i.e. essence: the organic phase change material in the organic phase change material microcapsules is 4:100;
3., beta-schardinger dextrin-coats the organic phase change material microcapsules that adsorbed essence
The 16g beta-schardinger dextrin-is dissolved in distilled water and makes the beta-schardinger dextrin-aqueous solution that concentration is 40%;
By step 2. gained absorption 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, make slowly Precipitation from solution of the bilayer fragrance phase-change microcapsule crude product that forms, filter the gained filter cake and wash to controlling temperature after the filtrate clarification and be 50 ℃ and be drying to obtain double-deck fragrant phase-change microcapsule through ethanol;
Described beta-schardinger dextrin-and the organic phase change material microcapsules that adsorbed essence, by beta-schardinger dextrin-and the organic phase change material microcapsules mass ratio that has adsorbed essence, calculate, i.e. organic phase change material: beta-schardinger dextrin-is 1:2;
(2), the preparation of double-deck fragrant phase-change microcapsule fabric finishing liquor
(1), after the double-deck fragrant phase-change microcapsule of 20g prepared by step, the agent of 10g crosslinked at low temperature, 3g thickener, 2g bleeding agent, 2g emulsifying agent 1,63g distilled water mix, magnetic agitation 15min obtains double-deck fragrant phase-change microcapsule fabric finishing liquor at normal temperatures and pressures.
Utilize the fragrant phase-change microcapsule fabric finishing liquor of above-mentioned a kind of bilayer textiles to be carried out to the method for perfuming, step is as follows:
Adopt coating, with after the double-deck fragrant phase-change microcapsule fabric finishing liquor of scraper blade coating on clip 40cmx40cm textile surfaces, control temperature 70 C, after baking 80s, complete the perfuming of double-deck fragrant phase-change microcapsule fabric finishing liquor on textiles.
Textiles Heat stability is good after perfuming, strong adhesion, aroma strength is better.By sensory evaluation, a larger reduction is relatively arranged when the smell of placing fabric after 3 months and just processing, 45% during for firm the processing, but fragrance is still obvious; The fabric fragrance remaining time was up to 9 months.
embodiment 2
The fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer, calculate by mass percentage, and its raw material composition and content are as follows:
Double-deck fragrant phase-change microcapsule 30g (30%)
Crosslinked at low temperature agent 15g (15%)
Thickener 5g (5%)
Bleeding agent 3g (3%)
Emulsifying agent 1 3g (3%)
Distilled water 44g (44%);
Prepared by the following method by the fragrant phase-change microcapsule of wherein said bilayer:
At first, take polymethyl methacrylate as the wall material coats organic phase change material, obtain the organic phase change material microcapsules; Wherein methyl methacrylate and organic phase change material calculate in mass ratio, i.e. methyl methacrylate: organic phase change material is 1:2, and described organic phase change material is atoleine;
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; The consumption of wherein said essence calculates by its mass ratio with respect to the organic phase change material in the organic phase change material microcapsules, i.e. essence: the organic phase change material in the organic phase change material microcapsules is 4:100, and described essence is lavender oil;
Finally, coat and adsorbed the organic phase change material microcapsules of essence with beta-schardinger dextrin-, thereby obtain double-deck fragrant phase-change microcapsule; Wherein said beta-schardinger dextrin-and adsorbed the organic phase change material microcapsules of essence, by beta-schardinger dextrin-and the mass ratio that adsorbed the organic phase change material microcapsules of essence, calculate, i.e. organic phase change material: beta-schardinger dextrin-is 1:2;
Described crosslinked at low temperature agent is CX-100, is the polyfunctional aziridines crosslinking agent that Guangzhou Zhong Guanmei Co., Ltd produces;
Described thickener is PTF, is the anionic species polyelectrolyte that Jiangsu Hai'an Petrochemical Plant produces;
Described bleeding agent is JFC, is the fatty alcohol-polyoxyethylene ether that Jiangsu Hai'an Petrochemical Plant produces, non-ionic surface active agent;
Described emulsifying agent 1 is Tween-80;
The preparation method of the above-mentioned fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer, specifically comprise the steps:
(1), the preparation of double-deck fragrant phase-change microcapsule
With embodiment 1;
(2), the preparation of double-deck fragrant phase-change microcapsule fabric finishing liquor
(1), after the double-deck fragrant phase-change microcapsule of 30g prepared by step, the agent of 15g crosslinked at low temperature, 5g thickener, 3g bleeding agent, 3g emulsifying agent 1,44g distilled water mix, magnetic agitation 10-20min obtains double-deck fragrant phase-change microcapsule fabric finishing liquor at normal temperatures and pressures.
Utilize the fragrant phase-change microcapsule fabric finishing liquor of above-mentioned a kind of bilayer textiles to be carried out to the method for perfuming, step is as follows:
Adopt coating, with the double-deck fragrant phase-change microcapsule fabric finishing liquor of scraper blade coating on clip 40cmx40cm textile surfaces, at 120 ℃, in 30s, oven dry completes the perfuming of double-deck fragrant phase-change microcapsule fabric finishing liquor on textiles.
Textiles better heat stability after perfuming, adhesive force is stronger, and aroma strength is good.By sensory evaluation, a larger reduction is relatively arranged when the smell of placing fabric after 4 months and just processing, 35% during for firm the processing, but fragrance is still obvious; Its fragrance remaining time reaches 8 months, and fabric was placed after 8 months, rubbed and still had light fragrance.
By the contrast of embodiment 1 and embodiment 2, result shows, by coating, the fragrant phase-change microcapsule fabric finishing liquor of bilayer is carried out to perfuming on textiles, the textiles Heat stability is good after perfuming, and strong adhesion, aroma strength is good; When bake out temperature is low, the essence rate of release is slower, and fragrance remaining time is longer.
embodiment 3
The fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer, calculate by mass percentage, and its raw material composition and content are as follows:
Double-deck fragrant phase-change microcapsule 20g (20%)
Crosslinked at low temperature agent 10g (10%)
Thickener 3g (3%)
Bleeding agent 2g (2%)
Emulsifying agent 1 2g (2%)
Distilled water 63g (63%);
Prepared by the following method by the fragrant phase-change microcapsule of wherein said bilayer:
At first, take polymethyl methacrylate as the wall material coats organic phase change material, obtain the organic phase change material microcapsules; Wherein methyl methacrylate and organic phase change material calculate in mass ratio, i.e. methyl methacrylate: organic phase change material is 1:2, and described organic phase change material is atoleine;
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; The consumption of wherein said essence calculates by its mass ratio with respect to the organic phase change material in the organic phase change material microcapsules, i.e. essence: the organic phase change material in the organic phase change material microcapsules is 4:100, and described essence is lily essence;
Finally, coat and adsorbed the organic phase change material microcapsules of essence with beta-schardinger dextrin-, thereby obtain double-deck fragrant phase-change microcapsule; Wherein said beta-schardinger dextrin-and adsorbed the organic phase change material microcapsules of essence, by beta-schardinger dextrin-and the mass ratio that adsorbed the organic phase change material microcapsules of essence, calculate, i.e. organic phase change material: beta-schardinger dextrin-is 1:2;
Described crosslinked at low temperature agent is CX-100, is the polyfunctional aziridines crosslinking agent that Guangzhou Zhong Guanmei Co., Ltd produces;
Described thickener is PTF, is the anionic species polyelectrolyte that Jiangsu Hai'an Petrochemical Plant produces;
Described bleeding agent is JFC, is the fatty alcohol-polyoxyethylene ether that Jiangsu Hai'an Petrochemical Plant produces, non-ionic surface active agent;
Described emulsifying agent 1 is Tween-80.
The preparation method of the above-mentioned fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer, specifically comprise the steps:
(1), the preparation of double-deck fragrant phase-change microcapsule
With embodiment 1, just wherein essence used is lily essence;
(2), the preparation of double-deck fragrant phase-change microcapsule fabric finishing liquor
(1), after the double-deck fragrant phase-change microcapsule of 20g prepared by step, the agent of 10g crosslinked at low temperature, 3g thickener, 2g bleeding agent, 2g emulsifying agent 1,63g distilled water mix, magnetic agitation 10-20min obtains double-deck fragrant phase-change microcapsule fabric finishing liquor at normal temperatures and pressures.
Utilize the fragrant phase-change microcapsule fabric finishing liquor of above-mentioned a kind of bilayer textiles to be carried out to the method for perfuming, step is as follows:
Adopt spray-on process, with watering can, in the 40cmx40cm textile surfaces, spray double-deck fragrant phase-change microcapsule fabric finishing liquor, natural air drying, use water-wet, and 70 ℃ of oven dry complete the perfuming of double-deck fragrant phase-change microcapsule fabric finishing liquor on textiles.
Textiles fragrance after perfuming is pure and fresh, and aroma strength is better, resembles true degree better.By sensory evaluation, after placing 3 months, the fragrance of fabric obviously reduces, 40% during for just processing, and it is relatively large that essence content reduces amplitude, and the essence rate of release is relatively very fast; After fabric is placed 6 months, fabric still keeps light fragrance, and the minimizing of the essence content on fabric amplitude diminishes gradually afterwards, and the essence rate of release slows down relatively.
embodiment 4
The fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer, calculate by mass percentage, and its raw material composition and content are as follows:
Double-deck fragrant phase-change microcapsule 10g (10%)
Crosslinked at low temperature agent 5g (5%)
Thickener 1g (1%)
Bleeding agent 1g (1%)
Emulsifying agent 1 1g (1%)
Distilled water 82g (82%);
Prepared by the following method by the fragrant phase-change microcapsule of wherein said bilayer:
At first, take polymethyl methacrylate as the wall material coats organic phase change material, obtain the organic phase change material microcapsules; Wherein methyl methacrylate and organic phase change material calculate in mass ratio, i.e. methyl methacrylate: organic phase change material is 1:2, and described organic phase change material is atoleine;
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; The consumption of wherein said essence calculates by its mass ratio with respect to the organic phase change material in the organic phase change material microcapsules, i.e. essence: the organic phase change material in the organic phase change material microcapsules is 4:100, and described essence is lily essence;
Finally, coat and adsorbed the organic phase change material microcapsules of essence with beta-schardinger dextrin-, thereby obtain double-deck fragrant phase-change microcapsule; Wherein said beta-schardinger dextrin-and adsorbed the organic phase change material microcapsules of essence, by beta-schardinger dextrin-and the mass ratio that adsorbed the organic phase change material microcapsules of essence, calculate, i.e. organic phase change material: beta-schardinger dextrin-is 1:2;
Described crosslinked at low temperature agent is CX-100, is the polyfunctional aziridines crosslinking agent that Guangzhou Zhong Guanmei Co., Ltd produces;
Described thickener is PTF, is the anionic species polyelectrolyte that Jiangsu Hai'an Petrochemical Plant produces;
Described bleeding agent is JFC, is the fatty alcohol-polyoxyethylene ether that Jiangsu Hai'an Petrochemical Plant produces, non-ionic surface active agent;
Described emulsifying agent 1 is Tween-80.
The preparation method of the above-mentioned fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer, specifically comprise the steps:
(1), the preparation of double-deck fragrant phase-change microcapsule
With embodiment 1;
(2), the preparation of double-deck fragrant phase-change microcapsule fabric finishing liquor
(1), after the double-deck fragrant phase-change microcapsule of 10g prepared by step, the agent of 5g crosslinked at low temperature, 1g thickener, 1g bleeding agent, 1g emulsifying agent 1,82g distilled water mix, magnetic agitation 10-20min obtains double-deck fragrant phase-change microcapsule fabric finishing liquor at normal temperatures and pressures.
Utilize the fragrant phase-change microcapsule fabric finishing liquor of above-mentioned a kind of bilayer textiles to be carried out to the method for perfuming, step is as follows:
Adopt spray-on process, with watering can, in the 40cmx40cm textile surfaces, spray double-deck fragrant phase-change microcapsule fabric finishing liquor, natural air drying, use water-wet, dries and complete the perfuming of double-deck fragrant phase-change microcapsule fabric finishing liquor on textiles under 40 ℃.
Textiles fragrance after perfuming is pure and fresh, and aroma strength is good, resembles true degree well.By subjective organoleptic method evaluation, after placing 3 months, the fragrance of fabric obviously reduces, 30% during for just processing, and it is relatively large that essence content reduces amplitude, and the essence rate of release is relatively very fast; After fabric is placed 5 months, fabric still keeps light fragrance, 7% during for just processing, and the essence content on fabric reduces amplitude and diminishes gradually, and the essence rate of release slows down relatively.
By embodiment 3 and embodiment 4 contrasts, result shows, by spray-on process, the fragrant phase-change microcapsule fabric finishing liquor of bilayer is carried out to perfuming on textiles, and the textiles fragrance after perfuming is pure and fresh, resembles true degree well, and aroma strength is better; When bake out temperature is higher, the essence rate of release is slower, and fragrance remaining time is longer.
In sum, the fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer of the present invention, carry out perfuming by spray-on process or coating to textiles, and not only aroma strength is good for the textiles after perfuming, the fragrance duration is long, can regulate the textiles temperature, meet people's demand simultaneously.
Above said content 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 (6)

1. the fragrant phase-change microcapsule fabric finishing liquor of bilayer, is characterized in that the fragrant phase-change microcapsule dressing liquid of described bilayer calculates by mass percentage, its raw material form and content as follows:
Double-deck fragrant phase-change microcapsule 10~30%
Crosslinked at low temperature agent 5~15%
Thickener 1~5%
Bleeding agent 1~3%
Emulsifying agent 1 1~3%
Surplus is distilled water;
Prepared by the following method by the fragrant phase-change microcapsule of wherein said bilayer:
At first, take polymethyl methacrylate as the wall material coats organic phase change material, obtain the organic phase change material microcapsules; Wherein methyl methacrylate and organic phase change material calculate in mass ratio, i.e. methyl methacrylate: organic phase change material is 1:2, and described organic phase change material is atoleine, hexadecane or octadecane;
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; The consumption of wherein said essence calculates by its mass ratio with respect to the organic phase change material microcapsules, i.e. essence: the organic phase change material microcapsules are 4:100, and described essence is lavender oil, lily essence, flavoring rose essence or cream jasmin france;
Finally, coat and adsorbed the organic phase change material microcapsules of essence with beta-schardinger dextrin-, thereby obtain double-deck fragrant phase-change microcapsule; Wherein said beta-schardinger dextrin-and adsorbed the organic phase change material microcapsules of essence, by beta-schardinger dextrin-and the mass ratio that adsorbed the organic phase change material microcapsules of essence, calculate, i.e. organic phase change material: beta-schardinger dextrin-is 1:2;
Described crosslinked at low temperature agent is CX-100;
Described thickener is PTF;
Described bleeding agent is JFC;
Described emulsifying agent 1 is Tween-80.
2. the fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer as claimed in claim 1, is characterized in that calculating by mass percentage, and its raw material composition and content are as follows:
Double-deck fragrant phase-change microcapsule 20%
Crosslinked at low temperature agent 10%
Thickener 3%
Bleeding agent 2%
Emulsifying agent 1 2%
Surplus is distilled water.
3. the fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer as claimed in claim 1, is characterized in that calculating by mass percentage, and its raw material composition and content are as follows:
Double-deck fragrant phase-change microcapsule 30%
Crosslinked at low temperature agent 15%
Thickener 5%
Bleeding agent 3%
Emulsifying agent 1 3%
Surplus is distilled water.
4. the fragrant phase-change microcapsule fabric finishing liquor of a kind of bilayer as claimed in claim 1, is characterized in that calculating by mass percentage, and its raw material composition and content are as follows:
Double-deck fragrant phase-change microcapsule 10%
Crosslinked at low temperature agent 5%
Thickener 1%
Bleeding agent 1%
Emulsifying agent 1 1%
Surplus is distilled water.
5. as the preparation method of claim 1,2, the fragrant phase-change microcapsule fabric finishing liquor of 3 or 4 arbitrary described a kind of bilayer, it is characterized in that specifically comprising the steps:
(1), the preparation of double-deck fragrant phase-change microcapsule
1., adopt emulsion polymerization, take polymethyl methacrylate as the wall material, take organic phase change material as core, synthetic organic phase change material microcapsules, its concrete steps are as follows:
At first, organic phase change material, methyl methacrylate, initator are stirred to dissolving after mixing, obtain oil phase component;
By emulsifying agent 2 and distilled water, 55 ℃ of lower agitation as appropriate, to evenly, obtain the water component again;
Described emulsifying agent 2 is Tween-80:Span-80, calculates in mass ratio, and being Tween-80:Span-80 is the mixture that 55:45 forms;
Then, under the 600rpm rotating speed, oil phase component is joined in the water component, temperature remains on 55 ℃ and stirs 30min, forms the O/W emulsion;
Above-mentioned organic phase change material used, methyl methacrylate, initator, emulsifying agent 2, distilled water calculate in mass ratio, i.e. organic phase change material: methyl methacrylate: initator: emulsifying agent 2: distilled water is 80:40:3:4:1500;
Then, by gained O/W emulsion under the high speed shear of 13000rpm after homogeneous 5min reflux condensation mode pass into nitrogen protection, prepolymerization 1h under 65 ℃ of waters bath with thermostatic control, 1000rpm are stirred simultaneously;
Then, under water bath condition, by temperature increase to 85 ℃ polymerisation 5h, standing 12h after reaction finishes, be that 30% ethanol-water solution washs three times with 50 ℃, mass percent concentration after suction filtration, and finally dry 24h under 50 ℃, obtain the organic phase change material microcapsules;
The preparation of 2., having adsorbed the organic phase change material microcapsules of essence
1. prepared organic phase change material microcapsules in are evenly mixed with essence, obtained the organic phase change material microcapsules of absorption 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 step 2. gained absorption 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, make slowly Precipitation from solution of the bilayer fragrance phase-change microcapsule crude product that forms, filter the gained filter cake and wash to controlling temperature after the filtrate clarification and be 50 ℃ and be drying to obtain double-deck fragrant phase-change microcapsule through ethanol;
(2), the preparation of double-deck fragrant phase-change microcapsule fabric finishing liquor
(1), after bilayer fragrance phase-change microcapsule, crosslinked at low temperature agent, thickener, bleeding agent, emulsifying agent 1 and distilled water prepared by step mixes, magnetic agitation 10~20min obtains double-deck fragrant phase-change microcapsule fabric finishing liquor at normal temperatures and pressures.
6. utilization is carried out the method for perfuming as claim 1,2, the fragrant phase-change microcapsule fabric finishing liquor of 3 or 4 arbitrary described a kind of bilayer to textiles, it is characterized in that by spray-on process or coating;
Described spray-on process, spray double-deck fragrant phase-change microcapsule fabric finishing liquor with watering can in textile surfaces, natural air drying, and wetting, 40~70 ℃ of oven dry complete the perfuming of double-deck fragrant phase-change microcapsule fabric finishing liquor on textiles;
Described coating, use scraper after the double-deck fragrant phase-change microcapsule fabric finishing liquor of textile surfaces blade coating, controls 70~120 ℃ of temperature, completes the perfuming of double-deck fragrant phase-change microcapsule fabric finishing liquor on textiles after drying 30~80s.
CN201310410066.3A 2013-09-11 2013-09-11 A kind of double-layer aromatic phase-change microcapsule fabric finishing liquor and preparation method and application Expired - Fee Related CN103451939B (en)

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