CN104073346A - Nanometer level microcapsule sweet orange essence and preparing method thereof - Google Patents
Nanometer level microcapsule sweet orange essence and preparing method thereof Download PDFInfo
- Publication number
- CN104073346A CN104073346A CN201310101829.6A CN201310101829A CN104073346A CN 104073346 A CN104073346 A CN 104073346A CN 201310101829 A CN201310101829 A CN 201310101829A CN 104073346 A CN104073346 A CN 104073346A
- Authority
- CN
- China
- Prior art keywords
- orange flavor
- chitosan
- microcapsule
- preparation
- essence
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Fats And Perfumes (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses nanometer level microcapsule sweet orange essence and a preparing method thereof. The nanometer level microcapsule sweet orange essence is prepared from following raw materials by weight: 5-20% of sweet orange essence, 3-10% of a surfactant, 5-20% of an organosilicone sol precursor, 0.5-5% of chitosan and 0.5-5% of ethanol, with the balance being deionized water. The nanometer level microcapsule sweet orange essence is prepared by steps of essence emulsification, preparation of the organosilicone sol precursor, preparation of a chitosan solution, microcapsule covering, and the like. The chitosan is adopted as a nanometer wall material, silicon dioxide skeleton is adopted as a carrier and the essence after emulsification is covered to obtain the nanometer level microcapsule sweet orange essence. Volatile components do not volatilize completely firstly. Specific surface area is large. Fragrance generation is natural and durable. A polyhydroxy structure on the surface of the chitosan can facilitate better adsorption on textile products. The original fragrance can be maintained even after washing for many times. The preparing method is short in covering time and high in covering efficiency.
Description
Technical field
The present invention relates to the essence that household chemicals field is used, be specifically related to a kind of nano level microcapsule orange flavor and preparation method thereof, be mainly used in washing composition.
Background technology
In fruit essence, the most common with several odor types such as sweet orange, lemon, strawberry, banana, pineapple, apples, wherein again with the favor that is subject to most people of sweet orange odor type, range of application is the widest, and almost most daily use chemicals commodity have sweet orange odor type.At present, on market, in orange flavor used, contain a large amount of volatile terpenoid substances, cause commodity aroma quality unstable, easily distortion, and fragrance loss speed is fast, is used in product, and fragrance is difficult to lasting.
Chinese patent application CN101142997A discloses a kind of preparation method of nanometer sweet orange essence, the median size of the nanometer sweet orange essence of preparing by the method is less than 1000nm, and can effectively solve the problem of essence fragrance slowly-releasing, and be mainly used in the food such as chewing gum, soft sweets, biscuit, but this preparation method also exists the parcel time long, the defects such as parcel weak effect.
Summary of the invention
For overcoming the defect of prior art, the object of the present invention is to provide a kind of nano level microcapsule orange flavor, stability and slow-releasing are good, and the nano essence after being coated can form effective absorption to yarn fabric, makes fabric fragrance lasting.
Another object of the present invention is to provide a kind of preparation method of nano level microcapsule orange flavor, shorten the parcel time, improve parcel efficiency, the slow-release time that extends essence.
The technical solution adopted in the present invention is as follows for achieving the above object:
A nano level microcapsule orange flavor, it is prepared from by following raw material by percentage to the quality:
Orange flavor 5-20%;
Tensio-active agent 3-10%;
Organic silicon sol precursor 5 ~ 20%;
Chitosan 0.5 ~ 5%;
Ethanol 0.5 ~ 5%;
Deionized water water surplus.
In such scheme, the effect of adding organic silicon sol precursor in formula is to guarantee that in gelation process, chitosan can effectively wrap up the essence after emulsification, in preferred scheme, described organic silicon sol precursor is that the ratio that is 1:1 with tetraethoxy 40 according to mass ratio by organic silicon sol is mixed, and adds the salt acid for adjusting pH value of 0.1-1mol/L to 1.5-2.0.Tetraethoxy is hydrolyzed and ethanol synthesis under acidic conditions, forms fast a kind of silica skeleton, and as the carrier of perfume formulation, essence is adsorbed on carrier and contributes to chitosan effectively to wrap up it, forms nano-scale particle material; Nano essence after coated by hydrogen bond and van der Waals interaction can form effective absorption to yarn fabric, in chitosan outer wall slow release, essence can be on yarn fabric lasting lasting; In Hydrolysis of Ethyl Silicate, add a kind of silicon sol, and constantly stir, contribute to shorten hydrolysis time, deepen hydrolysis degree, make the silica skeleton structure size of generation evenly, fixing formula essence, thus the encapsulation ratio of chitosan to essence improved.The more difficult control of tetraethoxy hydrolysis reaction in alkaline medium, therefore, when being hydrolyzed under acidic conditions, must control pH value, and pH value is larger, and hydrolyzed solution is more unstable, and for example, when pH value is 6, hydrolyzed solution is approximately through just possibility gel in 1 minute; Consider the stability of hydrolyzed solution, in such scheme, selected pH value is 1.5-2.0, and preferably pH value is 2.0.
In such scheme, chitosan of the present invention is a kind of natural cationic polymers, and good mechanical stability wherein contains hydrophilic hydroxyl and protonated amino under certain condition, is a kind of desirable microcapsule wall material.
The effect of emulsifying agent is in the present invention that essence can be dissolved in water liquid completely, is fully utilized.In preferred scheme, tensio-active agent of the present invention is any one or the two or more mixing in sapn, tween, epoxy organosilicon.
A preparation method for nano level microcapsule orange flavor, it comprises the following steps:
1) essence emulsification: orange flavor, with after deionized water dissolving, is added to tensio-active agent, make core after stirring;
2) preparation of organic silicon sol precursor: organic silicon sol and tetraethoxy 40 are mixed and stirred, then obtain precursor with the salt acid for adjusting pH value of 0.1-1mol/L to 1.5-2.0;
3) prepare chitosan solution: chitosan is joined in ethanolic soln, and ultrasonication 20-50 minute, adds the oxalic acid solution of 0.5-1.5mol/L to regulate pH value to 4-6, obtains wall material;
4) in the precursor micro-capsule parcel: first the core in step 1) is joined to step 2), stir on interpolation limit, limit, after stirring, adds the wall material in step 3) again, after stirring in warm water heating in water bath 10-30 minute, then naturally cooling at room temperature, obtains product.
The consumption of its Raw is respectively orange flavor 5-20% by percentage to the quality; Tensio-active agent 3-10%; Organic silicon sol precursor 5 ~ 20%; Chitosan 0.5 ~ 5%; Ethanol 0.5 ~ 5%; Deionized water water surplus.
In above-mentioned preparation method, select ethanolic soln dispersion agent, be used for dissolving chitosan, be conducive to disperse oarse-grained chitosan, play the effect that disperses hydrotropy, adopt ultrasonication, chitosan is effectively hydrolyzed or is broken into finely ground particle substance, can further improve chitosan to emulsification after the encapsulation ratio of essence.In preferred scheme, in step 3) of the present invention, hyperacoustic frequency is 25-80kHz.
In preferred scheme, in above-mentioned preparation method's step 4), the temperature of warm water is 40-70 ℃.
Compared to existing technology, beneficial effect of the present invention is: it is nanometer wall material that the present invention adopts chitosan, take silica skeleton as carrier, formula essence after emulsification is wrapped up, preparing volatile component in the micro-capsule orange flavor of Nano grade can not take the lead in having dispersed, and surface-area is larger, send out perfume (or spice) more natural, more lasting, the poly-hydroxy structure on chitosan surface, can help to be better adsorbed on textiles, remove the technique of using linking agent and tackiness agent to process from, through repeatedly washing and also can keep its original fragrance.It is short that preparation method of the present invention wraps up the time, and parcel efficiency is high.
Below in conjunction with concrete embodiment, the present invention is described in further detail.
Embodiment
Embodiment 1
A nano level microcapsule orange flavor, is prepared from by the following method:
1) essence emulsification: orange flavor, with after deionized water dissolving, is added to tensio-active agent, make core after stirring;
2) preparation of organic silicon sol precursor: organic silicon sol and tetraethoxy 40 are mixed and stirred, then obtain precursor with the salt acid for adjusting pH value to 1.5 of 0.1l/L;
3) prepare chitosan solution: chitosan is joined in ethanolic soln, and ultrasonication 20 minutes, adds the oxalic acid solution of 1.5mol/L to regulate pH value to 4, obtains wall material;
4) in the precursor micro-capsule parcel: first the core in step 1) is joined to step 2), stir on interpolation limit, limit, after stirring, adds the wall material in step 3) again, after stirring in the warm water of 70 ℃ heating in water bath 10 minutes, then naturally cooling at room temperature, obtains product.
The consumption of its Raw (by percentage to the quality) proportion by subtraction is:
Orange flavor 20%;
Tensio-active agent 10%;
Organic silicon sol precursor 5%;
Chitosan 0.5%;
Ethanol 0.5%;
Deionized water water surplus.
Embodiment 2
A nano level microcapsule orange flavor, is prepared from by the following method:
1) essence emulsification: orange flavor, with after deionized water dissolving, is added to tensio-active agent, make core after stirring;
2) preparation of organic silicon sol precursor: organic silicon sol and tetraethoxy 40 are mixed and stirred, then obtain precursor with the salt acid for adjusting pH value to 2 of 1mol/L;
3) prepare chitosan solution: chitosan is joined in ethanolic soln, and ultrasonication 50 minutes, adds the oxalic acid solution of 0.5-1.5mol/L to regulate pH value to 5, obtains wall material;
4) in the precursor micro-capsule parcel: first the core in step 1) is joined to step 2), stir on interpolation limit, limit, after stirring, adds the wall material in step 3) again, after stirring in the warm water of 40 ℃ heating in water bath 30 minutes, then naturally cooling at room temperature, obtains product.
The consumption of its Raw (by percentage to the quality) proportion by subtraction is:
Orange flavor 5%;
Tensio-active agent 3%;
Organic silicon sol precursor 20%;
Chitosan 5%;
Ethanol 5%;
Deionized water water surplus.
performance test:
1. thermostability: in the baking oven of 120 ℃, dry 30min, then by GB GB/T 14454.2-2008, the fragrance of product is evaluated; Detected result is in Table 1.
2. slow-releasing (product carries out the fragrance remaining time after perfuming processing to yarn fabric): yarn fabric is placed in to the aqueous solution that is dissolved with 5% nano essence product, soak 1 hour, take out, wring out water, at 110 ℃, dry, then yarn fabric is placed under room temperature, by GB GB/T 14454.2-2008, the fragrance of perfuming yarn fabric is evaluated at set intervals; Detected result is in Table 1.
3. wash resistant degree (the wash resistant degree of perfuming yarn fabric): the yarn fabric that will arrange through perfuming, be placed in the water that is dissolved with 0.5% washing liquid, soak 30min, then with clear water washing 2 ~ 3 times, take out, wring out water, air-dry under room temperature, by GB GB/T 14454.2-2008, the fragrance of perfuming yarn fabric is evaluated; Repeated washing, disappears substantially to measure its fragrance after how many times washing, and detected result is in Table 1.
Table 1: detected result
| stability | slow-releasing | effect |
| at 120 ℃, toast 30 min, characteristic perfume quality and intensity are without considerable change. | room temperature, places 6 months naturally, and aroma quality and intensity are better. | without adding chemical glue crosslinking agent, the adsorption efficiency of nano essence reaches more than 80%, and the washing fastness of fabric reaches 60 times. |
Above-mentioned embodiment is only the preferred embodiment of the present invention; can not limit the scope of protection of the invention with this, the variation of any unsubstantiality that those skilled in the art does on basis of the present invention and replacement all belong to the present invention's scope required for protection.
Claims (7)
1. a nano level microcapsule orange flavor, is characterized in that its following raw material by is by percentage to the quality prepared from:
Orange flavor 5-20%;
Tensio-active agent 3-10%;
Organic silicon sol precursor 5 ~ 20%;
Chitosan 0.5 ~ 5%;
Ethanol 0.5 ~ 5%;
Deionized water water surplus.
2. nano level microcapsule orange flavor according to claim 1, it is characterized in that: wherein said organic silicon sol precursor is that the ratio that is 1:1 with tetraethoxy 40 according to mass ratio by organic silicon sol is mixed, add the salt acid for adjusting pH value of 0.1-1mol/L to 1.5-2.0.
3. nano level microcapsule orange flavor according to claim 1, is characterized in that: described tensio-active agent is any one or the two or more mixing in sapn, tween, epoxy organosilicon.
4. a preparation method for nano level microcapsule orange flavor, is characterized in that it comprises the following steps:
1) essence emulsification: orange flavor, with after deionized water dissolving, is added to tensio-active agent, make core after stirring;
2) preparation of organic silicon sol precursor: organic silicon sol and tetraethoxy 40 are mixed and stirred, then obtain precursor with the salt acid for adjusting pH value of 0.1-1mol/L to 1.5-2.0;
3) prepare chitosan solution: chitosan is joined in ethanolic soln, and ultrasonication 20-50 minute, adds the oxalic acid solution of 0.5-1.5mol/L to regulate pH value to 4-6, obtains wall material;
4) in the precursor micro-capsule parcel: first the core in step 1) is joined to step 2), stir on interpolation limit, limit, after stirring, adds the wall material in step 3) again, after stirring in warm water heating in water bath 10-30 minute, then naturally cooling at room temperature, obtains product.
5. the preparation method of nano level microcapsule orange flavor according to claim 4, is characterized in that: the consumption of its Raw is respectively orange flavor 5-20% by percentage to the quality; Tensio-active agent 3-10%; Organic silicon sol precursor 5 ~ 20%; Chitosan 0.5 ~ 5%; Ethanol 0.5 ~ 5%; Deionized water water surplus.
6. the preparation method of nano level microcapsule orange flavor according to claim 4, is characterized in that: in step 3), hyperacoustic frequency is 25-80kHz.
7. the preparation method of nano level microcapsule orange flavor according to claim 4, is characterized in that: in step 4), the temperature of warm water is 40-70 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310101829.6A CN104073346A (en) | 2013-03-27 | 2013-03-27 | Nanometer level microcapsule sweet orange essence and preparing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310101829.6A CN104073346A (en) | 2013-03-27 | 2013-03-27 | Nanometer level microcapsule sweet orange essence and preparing method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104073346A true CN104073346A (en) | 2014-10-01 |
Family
ID=51594957
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310101829.6A Pending CN104073346A (en) | 2013-03-27 | 2013-03-27 | Nanometer level microcapsule sweet orange essence and preparing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104073346A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106190557A (en) * | 2016-07-28 | 2016-12-07 | 安徽省三环纸业集团香料科技发展有限公司 | A kind of have Longaacting fragrance-aretaining fabric detergent spice solving tired effect of refreshing oneself and preparation method thereof |
| CN108676615A (en) * | 2018-04-25 | 2018-10-19 | 上海应用技术大学 | A kind of preparation method of nano controlled-release essence |
| CN109125131A (en) * | 2018-10-09 | 2019-01-04 | 河北瑞龙生物科技有限公司 | A kind of nano essence mosquito-expelling bath lotion |
| CN109559888A (en) * | 2018-12-24 | 2019-04-02 | 凯杰森(天津)生物科技有限公司 | Fe3O4@SiO2The preparation method of composite Nano magnetic bead |
| CN110973575A (en) * | 2019-12-31 | 2020-04-10 | 上海华宝孔雀香精有限公司 | Orange-flavored microcapsule powder essence and preparation method thereof |
| CN112480895A (en) * | 2020-11-27 | 2021-03-12 | 中国石油大学(北京) | PH-responsive oil displacement agent composition, oil displacement agent, and preparation method and application thereof |
| CN112841773A (en) * | 2021-03-04 | 2021-05-28 | 杭州半边月文化创意有限公司 | Preparation process of tea breathing mask |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012168144A1 (en) * | 2011-06-07 | 2012-12-13 | Firmenich Sa | Core-shell capsules |
| WO2013004003A1 (en) * | 2011-07-04 | 2013-01-10 | 丽华（泰国）香精有限公司 | Nano-flavor and preparation method thereof |
| CN103263877A (en) * | 2013-05-17 | 2013-08-28 | 义乌市中力工贸有限公司 | Preparation method of essential oil-contained silicon dioxide microcapsule |
| CN104031740A (en) * | 2014-05-30 | 2014-09-10 | 上海应用技术学院 | Heat-resistant rose essence capsule and preparation method thereof |
-
2013
- 2013-03-27 CN CN201310101829.6A patent/CN104073346A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012168144A1 (en) * | 2011-06-07 | 2012-12-13 | Firmenich Sa | Core-shell capsules |
| WO2013004003A1 (en) * | 2011-07-04 | 2013-01-10 | 丽华（泰国）香精有限公司 | Nano-flavor and preparation method thereof |
| CN103263877A (en) * | 2013-05-17 | 2013-08-28 | 义乌市中力工贸有限公司 | Preparation method of essential oil-contained silicon dioxide microcapsule |
| CN104031740A (en) * | 2014-05-30 | 2014-09-10 | 上海应用技术学院 | Heat-resistant rose essence capsule and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106190557A (en) * | 2016-07-28 | 2016-12-07 | 安徽省三环纸业集团香料科技发展有限公司 | A kind of have Longaacting fragrance-aretaining fabric detergent spice solving tired effect of refreshing oneself and preparation method thereof |
| CN108676615A (en) * | 2018-04-25 | 2018-10-19 | 上海应用技术大学 | A kind of preparation method of nano controlled-release essence |
| CN109125131A (en) * | 2018-10-09 | 2019-01-04 | 河北瑞龙生物科技有限公司 | A kind of nano essence mosquito-expelling bath lotion |
| CN109559888A (en) * | 2018-12-24 | 2019-04-02 | 凯杰森(天津)生物科技有限公司 | Fe3O4@SiO2The preparation method of composite Nano magnetic bead |
| CN110973575A (en) * | 2019-12-31 | 2020-04-10 | 上海华宝孔雀香精有限公司 | Orange-flavored microcapsule powder essence and preparation method thereof |
| CN112480895A (en) * | 2020-11-27 | 2021-03-12 | 中国石油大学(北京) | PH-responsive oil displacement agent composition, oil displacement agent, and preparation method and application thereof |
| CN112480895B (en) * | 2020-11-27 | 2022-02-01 | 中国石油大学(北京) | PH-responsive oil displacement agent composition, oil displacement agent, and preparation method and application thereof |
| CN112841773A (en) * | 2021-03-04 | 2021-05-28 | 杭州半边月文化创意有限公司 | Preparation process of tea breathing mask |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104073346A (en) | Nanometer level microcapsule sweet orange essence and preparing method thereof | |
| EP1196533B1 (en) | Improved encapsulated oil particles | |
| CN103361197A (en) | Laundry liquid using gel to stably disperse microcapsule essence and preparation technology thereof | |
| CN102776070A (en) | Transparent microcapsule flavoring rose essence and preparation method thereof | |
| CN104206561A (en) | Preparation process of peony seed oil micro-capsule powder | |
| WO2009100306A1 (en) | Consumer product packets with enhanced performance | |
| CN102776068A (en) | Paste type microcapsule flavoring rose essence and preparation method thereof | |
| CN101884415A (en) | DHA microcapsule and preparation process thereof | |
| CN104878610A (en) | Preparing method for aroma-releasing type baffeta | |
| TW201701863A (en) | Composition | |
| CN101416928A (en) | Matcha anti-senescence face mask added with superoxide dismutase and preparation method thereof | |
| CN109133070A (en) | A method of hydrophobic silica aerogel is prepared by the supper-fast normal pressure of raw material of waterglass | |
| CN102776071A (en) | Transparent microcapsule flavoring jasmine essence and preparation method thereof | |
| CN108531298B (en) | Washing powder containing fingered citron essential oil microcapsules and preparation method thereof | |
| CN105395378B (en) | A kind of sheet microcapsules containing refrigerant formula | |
| JP6980801B2 (en) | Consumer product composition containing microcapsules | |
| CN102776069B (en) | Paste microcapsule jasmine essence and preparation method thereof | |
| CN108948835A (en) | A kind of novel antibacterial thermal insulation coatings and preparation method thereof | |
| CN104607119A (en) | Acetic acid styracin nanometer capsule and preparation method thereof | |
| CN103747772B (en) | Comprise the benefit agent delivery particle of nonionic polysaccharide | |
| CN106753861A (en) | A kind of Closestool cleanser of antibacterial lasting and preparation method thereof | |
| CN101270548A (en) | Deodorizing colloidal sol-gel rubber finishing agent, preparation method and application thereof | |
| CN112522039A (en) | Clothing aroma-enhancing bead composition and preparation method thereof | |
| CN107459952A (en) | A kind of wet glue of wallpaper | |
| CN108676615A (en) | A kind of preparation method of nano controlled-release essence |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| CB02 | Change of applicant information |
Address after: Baiyun District of Guangzhou City, Guangdong province 510540 North Tai Road No. 1633 Guangzhou private science and Technology Park Branch Road No. 19 Applicant after: Li Hua (Guangzhou) Flavors & Fragrances Limited by Share Ltd Address before: Baiyun District of Guangzhou City, Guangdong province 510540 North Tai Road No. 1633 Guangzhou private science and Technology Park Branch Road No. 19 Applicant before: Li Hua (Guangzhou) essence Co., Ltd. |
|
| COR | Change of bibliographic data | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20141001 |
|
| RJ01 | Rejection of invention patent application after publication |