CN101928641B - Essence microcapsule with long-term effectiveness and preparation method thereof - Google Patents
Essence microcapsule with long-term effectiveness and preparation method thereof Download PDFInfo
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- CN101928641B CN101928641B CN2010102966511A CN201010296651A CN101928641B CN 101928641 B CN101928641 B CN 101928641B CN 2010102966511 A CN2010102966511 A CN 2010102966511A CN 201010296651 A CN201010296651 A CN 201010296651A CN 101928641 B CN101928641 B CN 101928641B
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Abstract
The invention relates to an essence microcapsule with long-term effectiveness and a preparation method thereof, belonging to the technical filed of microcapsule preparation. The essence microcapsule of the invention is prepared from essence, chitosan, compound emulsifier and other components. The microcapsule greatly reduces the essence loss during the storage and washing processes, improves the aroma retaining effect after washing and has the long-term effectiveness. When being added into washing powder, the essence microcapsule with slow releasing property is used to replace traditional aromatized washing powder, thus significantly retaining the essence no matter in production or in application, and prolonging the aroma retaining time after washing. When aromatized washing powder is produced according to the technology, the process is simple and the operation is simple; and when being added into the washing powder, the essence microcapsule has no toxic or side effect, and can slowly release aroma during washing and prolong the aroma retaining time after washing.
Description
Technical field
A kind of have long-lasting essence microcapsule and preparation method thereof; The present invention relates to the long-acting essence microcapsule that adds in a kind of washing powder, a kind of specifically have a slow-releasing, water-fast; Microcapsule that particle diameter is less and preparation method thereof belong to the microcapsule preparing technical field.
Background technology
Microcapsule are a kind of miniature vessel packing materials with polymer shell wall.The intracardiac corpuscle of its capsule (dripping) can sealed and protect to microcapsule.Cyst wall is normally by seamless, and firm film is formed.Generally in 1 ~ 1000 mu m range, diameter is called nano particle or Nano capsule less than the particle of 1 μ m to the size of microcapsule, is called particulate or large capsule greater than the particle of 1000 μ m.Because essence receives air easily, therefore the influence of ambient conditionss such as temperature and light often is prepared into micro encapsulation essence in actual application, and this application can be so that essence be stored effectively and discharges.Spray-dired micro encapsulation essence has been widely used in food, hospital, and a plurality of fields such as cosmetics of everyday use, and become a kind of general essence product rapidly.
Chitosan is also claimed soluble chitin, and chemistry is by name to gather-1, and 4-2-amino-2-deoxidation-β-D-glucose is to take off by chitin through concentrated base that acyl group makes.Chitosan is a kind of linear polymeric with the plain structure of like fibrous; Being a kind of alkaline polysaccharide that occurring in nature exists, also is a kind of natural cationic polymers, good mechanical stability; Have excellent biological compatibility and biological degradability; Wherein containing hydrophilic hydroxyl and protonated amino under certain condition, good adsorptivity is arranged, become characteristic of stock and permeability, fiberizability, water absorbability and moisture retention, is a kind of ideal microcapsule wall material.
Since the eighties of last century the eighties, chitosan is used to wrap up conventional medicament and protein etc. and is prepared into sustained-release microparticle, because of its good mucous membrane property is widely used in the biologic medical field.The method for preparing chitosan microcapsules of lot of documents report mainly contains four kinds: single coacervation, complex coacervation, solvent evaporation method and spray-drying process.The surface of microcapsule that wherein obtains with spray-drying process is smooth, and it is spherical to be rule, and body surface area is big, can improve controlled drug release, and that therefore uses is the most extensive.
To be direct perfuming add with being adsorbed in the porous mass the most frequently used perfuming mode of traditional aromatized washing powder, and this dual mode can not well protect essence not receive the influence of external environment, and especially essence receives very big loss in washing process.Since the last century the nineties, the neoteric microcapsule essence that makes an addition to washing powder is water-soluble because of its wall material, in washing process, will discharge whole essence, and the fabric that has washed can not discharge fragrance muchly.
Summary of the invention
The technical problem that the present invention will solve is to disclose a kind of long-acting essence microcapsule in the washing powder and preparation method thereof that makes an addition to; Promptly provide a kind of water insoluble; Has slow-releasing; The essence microcapsule of small particle size makes it in washing process, slowly discharge essence, after having washed, has long-time lasting.
Technical scheme of the present invention: a kind of long-acting essence microcapsule, its moity is:
The mass ratio of essence and chitosan is 1:1-4, and the ratio of compound emulsifying agent is a Tweens: the spans mass ratio is 4:1, and the addition of compound emulsifying agent is the 3%-7% of essence quality; Through high-speed stirring and the high-pressure homogeneous milk sap that makes uniform particle diameter; Spraying drying obtains long-acting essence microcapsule product then, and its embedding rate reaches more than 90%, and productive rate reaches more than 80%; Its essence fragrance has slow-releasing, and three months retention rates of storage reach more than 80% under the room temperature.
The preparation method of said long-acting essence microcapsule, step is:
(1) dissolving of chitosan: by proportioning chitosan is dissolved in the acetum of mass concentration 1% and processes 1% chitosan wall material solution;
(2) kind of composite emulsifier and quality: it is composite to adopt a kind of among a kind of and spans Span24 among Tweens Tween20, Tween40, Tween60, the Tween80, Span40, Span60, the Span80 to treat with mass ratio 4:1 ratio, and the addition of composite emulsifier is the 3%-7% of essence quality;
(3) emulsification: Tweens is dissolved in the chitosan solution, spans is dissolved in the essence, mix then, high-pressure homogeneous twice under 40Mpa behind the 13500rpm high-speed stirring number minute, form the milk sap of uniform particle diameter;
(4) spraying drying: 150 ℃ of inlet temperatures, temperature out are 80 ℃, promptly get long-acting essence microcapsule product.
The application of said long-acting essence microcapsule: long-acting essence microcapsule is added in the washing powder, and addition is the 0.5%-1% of washing powder total amount, makes long-acting aromatized washing powder.
Beneficial effect of the present invention: from the characteristics of chitosan, adopt spray drying technology, essence and chitosan are processed water-fast small particle, directly add in the washing powder, avoided the fragrance of traditional aromatized washing powder to be prone to scatter and disappear the shortcoming that fragrance remaining time is short.
The contriver finds that in order to obtain the effect of microcapsule, the ratio of emulsifier type, composite emulsifier all is very crucial with core wall ratio and spraying drying condition.Different types of emulsifying agent has very big difference to the emulsifying effectiveness of chitosan essence, is committed step so select emulsifying agent, and finds that the emulsifying effectiveness of composite emulsifying agent is much better than the emulsifying effectiveness of single a kind of emulsifying agent.Though a large amount of emulsifying agents helps the effect of self-emulsifying microemulsion, they itself have certain toxicity, and the too much affiliation that adds has side effects.Under the prerequisite that does not influence the self-emulsifying microemulsion effect, the preferred emulsifier add-on is that the composite ratio of 3%-7%, the emulsifying agent of volatile oil is 4:1.The mass ratio of essence and chitosan is 0.25-1.
With essence, emulsifying agent and chitosan according to the prescription mixed after high-speed stirring, high-pressure homogeneous back spraying drying.
The present invention is prepared into long-acting aromatized washing powder first, and prepared essence microcapsule is water insoluble, has protected the essence that not exclusively discharges in the washing process, and small particle size can help microcapsule and embed in the clothes fiber, makes the clothing Longaacting fragrance-aretaining.
Description of drawings
The electromicroscopic photograph of Fig. 1 chitosan essence microcapsule.
The size distribution figure of Fig. 2 chitosan essence microcapsule.
Embodiment
The 20g chitosan is dissolved in the 2000g1% acetum, 0.4gTween40 is dissolved in the above-mentioned solution; Get 0.1gSpan20 in addition and be dissolved in the 10g sweet orange oil, above two kinds of solution medley relay 13500rpm rotating speeds are stirred 5min, homogeneous twice under 40Mpa, the emulsion spray drying that obtains.Inlet temperature is 150 ℃, and temperature out is 80 ℃, and flow is 1.5-2.5L/h.
Embodiment 2
The 20g chitosan is dissolved in the 2000g1% acetum, 0.2gTween40 is dissolved in the above-mentioned solution; Get 0.05gSpan20 in addition and be dissolved in the 5g sweet orange oil, above two kinds of solution medley relay 13500rpm rotating speeds are stirred 5min, homogeneous twice under 40Mpa, the emulsion spray drying that obtains.Inlet temperature is 150 ℃, and temperature out is 80 ℃, and flow is 1.5-2.5L/h.
Embodiment 3
The 20g chitosan is dissolved in the 2000g1% acetum, 0.4gTween40 is dissolved in the above-mentioned solution; Get 0.1gSpan80 in addition and be dissolved in the 10g PH 6968, above two kinds of solution medley relay 13500rpm rotating speeds are stirred 5min, homogeneous twice under 40Mpa, the emulsion spray drying that obtains.Inlet temperature is 150 ℃, and temperature out is 80 ℃, and flow is 1.5-2.5L/h.
Embodiment 4
Add in the common no fragrant washing powder having long-lasting chitosan essence microcapsule, addition is the 0.5%-1% of washing powder total amount, is used to make long-acting aromatized washing powder.Release rate shows that it has slow-releasing in washing process mensuration water, measures washing back aroma retaining effect experimental result and shows that fabric has slow release odour characteristics.
Claims (3)
1. long-acting essence microcapsule is characterized in that its moity is:
The mass ratio of essence and chitosan is 1:1-4, and the ratio of compound emulsifying agent is a Tweens: the spans mass ratio is 4:1, and the addition of compound emulsifying agent is the 3%-7% of essence quality; Through high-speed stirring and the high-pressure homogeneous milk sap that makes uniform particle diameter; Spraying drying obtains long-acting essence microcapsule product then, and its embedding rate reaches more than 90%, and productive rate reaches more than 80%; Its essence fragrance has slow-releasing, and three months retention rates of storage reach more than 80% under the room temperature;
Said essence is citrus flavor.
2. the preparation method of the said long-acting essence microcapsule of claim 1 is characterized in that,
(1) dissolving of chitosan: by proportioning chitosan is dissolved in the acetum of mass concentration 1% and processes 1% chitosan wall material solution;
(2) kind of composite emulsifier and quality: it is composite to adopt a kind of among a kind of and spans Span24 among Tweens Tween20, Tween40, Tween60, the Tween80, Span40, Span60, the Span80 to treat with mass ratio 4:1 ratio, and the addition of composite emulsifier is the 3%-7% of essence quality;
(3) emulsification: Tweens is dissolved in the chitosan solution, spans is dissolved in the essence, mix then, high-pressure homogeneous twice under 40Mpa behind the 13500rpm high-speed stirring number minute, form the milk sap of uniform particle diameter;
(4) spraying drying: 150 ℃ of inlet temperatures, temperature out are 80 ℃, promptly get long-acting essence microcapsule product.
3. the application of the said long-acting essence microcapsule of claim 1: it is characterized in that long-acting essence microcapsule is added in the washing powder, addition is the 0.5%-1% of washing powder total amount, makes long-acting aromatized washing powder.
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| CN102921140B (en) * | 2012-11-07 | 2015-03-18 | 公安部天津消防研究所 | Liquid fire extinguishing agent for putting out edible oil fire hazards |
| CN103741496B (en) * | 2013-12-27 | 2016-04-20 | 天津城建大学 | The preparation method of long-acting height is affine essence microcapsule softener and application |
| CN105176677A (en) * | 2015-07-23 | 2015-12-23 | 安徽省三环纸业集团香料科技发展有限公司 | Spice for washing powder for preventing and treating cold and preparation method therefor |
| CN105725258A (en) * | 2016-02-25 | 2016-07-06 | 云南中烟工业有限责任公司 | Fragrant microcapsule for composite cigarettes and preparation method and application thereof |
| CN105997933A (en) * | 2016-05-09 | 2016-10-12 | 中山大学惠州研究院 | Vanillin microcapsule droplets and preparing method thereof |
| CN106967507A (en) * | 2017-03-10 | 2017-07-21 | 佛山市禅香新材料有限公司 | It is a kind of for lavender transparency liquid microcapsules of preserved flower and preparation method thereof |
| CN108531298B (en) * | 2018-04-10 | 2020-06-23 | 上海应用技术大学 | Washing powder containing fingered citron essential oil microcapsules and preparation method thereof |
| CN109124862B (en) * | 2018-07-12 | 2020-06-23 | 广州馥邦科技应用有限公司 | Controlled-release long-acting antipyretic patch and preparation method thereof |
| CN109173948A (en) * | 2018-09-27 | 2019-01-11 | 上海烟草集团有限责任公司 | A kind of slow-release microcapsule material and its preparation method and application discharging fragrance |
| CN112704762B (en) * | 2019-10-25 | 2022-12-27 | 广东爱车小屋电子商务科技有限公司 | Solid air freshener and preparation method thereof |
| CN112048922A (en) * | 2020-06-16 | 2020-12-08 | 江南大学 | Fragrance slow-release ultraviolet-proof textile coating and preparation method and application thereof |
| CN114405423B (en) * | 2022-01-11 | 2022-10-28 | 广州乐居日化用品有限公司 | Porous chitosan microcapsule fragrance retaining bead and high-stability laundry gel bead |
| CN114774216B (en) * | 2022-05-25 | 2023-08-08 | 浙江美生日化用品有限公司 | Fragrance-retaining bead and production process thereof |
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| CN1546557A (en) * | 2003-12-02 | 2004-11-17 | 武汉大学 | Preparation method and uses of carboxymethyl chitosan and sodium alginate blend microcapsule |
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| CN1546557A (en) * | 2003-12-02 | 2004-11-17 | 武汉大学 | Preparation method and uses of carboxymethyl chitosan and sodium alginate blend microcapsule |
| CN1883488A (en) * | 2005-06-21 | 2006-12-27 | 北京华禧联合科技发展有限公司 | Preparation method of minocycline hydrochloride chitosan microsphere and application thereof |
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