CN108940146A - A kind of preparation method of natural perfume material liquid nanometer capsule - Google Patents

A kind of preparation method of natural perfume material liquid nanometer capsule Download PDF

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Publication number
CN108940146A
CN108940146A CN201810702523.9A CN201810702523A CN108940146A CN 108940146 A CN108940146 A CN 108940146A CN 201810702523 A CN201810702523 A CN 201810702523A CN 108940146 A CN108940146 A CN 108940146A
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Prior art keywords
natural perfume
preparation
emulsifier
perfume material
liquid nanometer
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CN201810702523.9A
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Chinese (zh)
Inventor
纪红兵
刘璇
冯羽
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Huizhou Research Institute of Sun Yat Sen University
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Huizhou Research Institute of Sun Yat Sen University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/04Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Dispersion Chemistry (AREA)
  • Cosmetics (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

The invention discloses a kind of preparation methods of natural perfume material liquid nanometer capsule, comprising the following steps: (1) measures the RHLB value of core material;(2) it weighs 1 part of wall material to be dissolved in 99 parts of deionized water, sufficiently dissolve, be prepared into the wall material solution that mass fraction is 1%;(3) assistant for emulsifying agent is added and stirs obtained blended emulsifier;(4) 10-30 parts of core materials are weighed, 70-90 parts of blended emulsifiers are added in beaker, obtained self-emulsifying microemulsion system;(5) wall material solution is mixed with self-emulsifying microemulsion system, stirs, obtains natural perfume material liquid nanometer capsule.The effect of product has the characteristics that spontaneously form, optical clear, stability are good, solubilized property is good, solves the problems, such as the solubilized of oil-soluble natural perfume material, while protecting natural perfume material free from the influence of the external environment, preferably plays active constituent.The suspending power for increasing nanoparticle, keeps system more stable.Nano capsule partial size is in 50 nm or less, dispersion degree is small, thermal stability and centrifugal stability are good.

Description

A kind of preparation method of natural perfume material liquid nanometer capsule
Technical field
The present invention relates to Nano capsule technologies of preparing, specifically, being related to a kind of system of natural perfume material liquid nanometer capsule Standby technology.
Background technique
Flavors and fragrances is the important raw material of the industries such as food, daily use chemicals, medicine, printing.But natural perfume material directly adds It is easy to be influenced by factors such as light, heat, radiation when into liquid daily chemical product, causes the volatilization and degradation of its constituent. The change of natural perfume material state may be implemented by microencapsulation, at the same can also play protection sensitive component, controlled release, The effects of variant component is isolated.Therefore, microencapsulation becomes the effective means for overcoming these problems.
Microcapsules technology provides protection for natural perfume material, enhances their stability, and realizes the controllable of them Release, it is all very attractive in different industries.The wall material of microcapsules can be mainly divided into natural polymer, semi-synthetic high score Son, synthesis macromolecule and inorganic material.Microcapsules are received as the natural perfume material used in daily chemical products, usually require that use Wall material have it is immiscible or do not react, the low stickiness of high concentration, hypotoxicity, biodegradable and biocompatibility with core material The characteristics of.Therefore the wall materials of microcapsules is received as natural perfume material frequently with natural polymer.As Nano capsule wall material Natural polymer also require it with good water-soluble, low stickiness, transparency and be not easy to form gel.
With the continuous excavation of nano material good characteristic, nanotechnology becomes an important branch of microcapsule systems, Protection, the sustained release that core material is realized using nanoparticle and Nano capsule, improve its bioactivity.Microemulsion is capsule of nano skill The extension of art.DaMelsson and Lindman in 1981 etc. gives microemulsion definition acknowledged at present: by water, oil and table Transparent, the optical isotropy, thermodynamically stable liquid system that face activating agent is constituted.It compares and ordinary emulsion, microemulsion has There are thermodynamic stability and appearance clear, though lotion is dynamic stabilization due to thermodynamic (al) unstability, most To also mutually separation occur eventually, another difference is exactly that the preparation of lotion needs a large amount of energy, and microemulsion emulsifier with It can be spontaneously formed under the action of assistant for emulsifying agent, therefore have the advantages that low energy consumption, industrial production cost is lower.
Micro-emulsion technology application mostly important in daily use chemicals industry at present is exactly the solubilising to natural perfume material and essence.? In numerous daily use chemicals type of merchandises, aqua cosmetics are pursued by consumer.Aqua cosmetics are broadly divided into toner and perfume (or spice) Two class of water.In these products, main and core ingredient is exactly natural perfume material and essence.Often these essence, natural perfume Material, skin care raw material are all insoluble in water.Traditional handicraft be they are made to water-ethanol solution, but alcohol to skin damage compared with Greatly, and micro-emulsion technology can solve the solubilized problem of natural perfume material, while also reducing the irritation of product.In addition, micro- Emulsifying technology is also used for package and sustained release to effect type substance.By the theoretical knowledge application of microemulsion and micro-emulsion technology To in the research and preparation of liquid nanometer capsule, to be made, high stability, partial size are small, dispersion degree is low, the nanometer of appearance transparent Grade capsule has obvious and advantage and wide prospect.
Summary of the invention
It is an object of the invention to overcome the shortcomings of existing liquid nanometer capsule technology of preparing, providing one kind, low energy consumption, work The simple liquid nanometer capsule technology of preparing of skill, using this technology prepared liquid nanometer capsule have spontaneously form, optics Feature transparent, partial size is small, stability is good, solubilized property is good.
To achieve the goals above, the technical solution adopted by the present invention the following steps are included:
A kind of preparation method of natural perfume material liquid nanometer capsule, comprising the following steps:
(1) measurement of core material RHLB value:
A series of composite emulsifier for preparing different HLB values (hydrophilic lipophilic balance) is spare, selects emulsifying effectiveness optimal multiple It is the RHLB value of core material with emulsifier hlb value;
The composite emulsifier is that a kind of hydrophilic nonionic emulsifier and a kind of lipophilic nonionic emulsifier are mixed to get;
(2) preparation of wall material solution:
By weight, it weighs 1 part of wall material to be dissolved in 99 parts of deionized water, uniform stirring is allowed to sufficiently dissolve at room temperature, quiet Only 1h de-bubble is prepared into the wall material solution that mass fraction is 1%;
(3) preparation of blended emulsifier:
Assistant for emulsifying agent is added in the composite emulsifier of step (1) and 30 min are stirred at room temperature, blended emulsifier is made;
(4) preparation of self-emulsifying microemulsion system:
Weigh 10-30 parts of core materials, 70-90 parts of blended emulsifiers are added in beakers, after beaker is sealed immediately with prevent core material at The volatilization divided then stirs the mixture for that self-emulsifying microemulsion system is made;
(5) preparation of natural perfume material liquid nanometer capsule:
70-90 parts of wall material solution is mixed with 10-30 parts of self-emulsifying microemulsion systems, stirs, obtains natural perfume material liquid nanometer glue Capsule.
In the preparation method of above-mentioned natural perfume material liquid nanometer capsule, the wall material is poly- for natural polymer such as shell One of sugar, maltodextrin, casein sodium.
In the preparation method of above-mentioned natural perfume material liquid nanometer capsule, the hydrophilic nonionic emulsifier is poly- Glycols emulsifier;The lipophilic nonionic emulsifier is sorbitan fatty acid ester class emulsifier.Sorbitan Polyol fatty acid esters emulsifier is one of Span series.
In the preparation method of above-mentioned natural perfume material liquid nanometer capsule, the polyethylene glycols emulsifier is poly- second two One of alcohol hydrogenated castor oils (CO-40) or polyethylene glycol sorbitan fatty acid esters class (Tween series).
In the preparation method of above-mentioned natural perfume material liquid nanometer capsule, the assistant for emulsifying agent is that carbon chain lengths are 1-4 Short chain alcohol.
In the preparation method of above-mentioned natural perfume material liquid nanometer capsule, the short chain alcohol that the carbon chain lengths are 1-4 is One of ethyl alcohol, 1,2- propylene glycol, n-butanol.
In the preparation method of above-mentioned natural perfume material liquid nanometer capsule, the matter of the composite emulsifier and assistant for emulsifying agent Amount is than being 3:1 (Km=3).
In the preparation method of above-mentioned natural perfume material liquid nanometer capsule, the core material is natural perfume material, such as lavender Essential oil, lemon etc..
Compared with prior art, the invention has the following beneficial effects:
(1) product being prepared using microemulsion technology have spontaneously form, optical clear, stability are good, solubilized property is good Feature, solves the problems, such as the solubilized of oil-soluble natural perfume material, at the same microencapsulation operation can protect very well natural perfume material not by The influence of external environment, better the effect of playing wherein active constituent.
(2) viscosity by using natural polymer solution as the adjustable Nano capsule of wall material can increase nanometer The suspending power of particle keeps system more stable.Preparation-obtained Nano capsule partial size is in 50 nm or less, dispersion degree is small, tool There are good thermal stability and centrifugal stability.
Detailed description of the invention
Fig. 1 is the natural perfume material liquid nanometer capsule appearance figure that S/O ratio is respectively 7:3,8:2,9:1;Wherein, S/O ratio=mixed The ratio of co-emulsifier and core material;
Fig. 2 is natural perfume material liquid nanometer capsule grain diameter and its particle diameter distribution variation with temperature trend.
Specific embodiment
The preparation of 1 lavender liquid nanometer capsule of embodiment
Lavender is taken, it is 14 that experiment, which measures RHLB value, so that it is determined that composite emulsifier is rilanit special and Span-80;
Under 30 DEG C of bath temperatures, the chitosan solution that mass fraction is 1% is prepared;
14 g of rilanit special (CO-40), Span-80 (Span-80) 2 g and 5 g of 1,2-PD are added in beaker, in room Blended emulsifier is made in 30 min of the lower stirring of temperature;Add 3 g of core material Lavender, after immediately by beaker seal to prevent core The volatilization of material ingredient then stirs the mixture for that self-emulsifying microemulsion system is made;
Then it is placed under magnetic stirring apparatus at room temperature after stirring 1 h and 76 g chitosan solutions is added, then shear 10-15 min, i.e., Obtain lavender liquid nanometer capsule.Test gained lavender liquid nanometer capsule grain diameter and its particle diameter distribution variation with temperature Trend such as Fig. 2.
The preparation of 2 lavender liquid nanometer capsule of embodiment
Lavender is taken, it is 14 that experiment, which measures RHLB value, so that it is determined that composite emulsifier is Tween-60 and Span-80;
Under 30 DEG C of bath temperatures, the maltodextrin solution that mass fraction is 1% is prepared;
13 g of Tween-60 (Tween-60), Span-80 (Span-80) 1 g and 4 g of 1,2-PD are added in beaker, in room Blended emulsifier is made in 30 min of the lower stirring of temperature;Add 2 g of core material Lavender, after immediately by beaker seal to prevent core The volatilization of material ingredient then stirs the mixture for that self-emulsifying microemulsion system is made;
Then it is placed under magnetic stirring apparatus at room temperature after stirring 1 h and 80 g maltodextrin solutions is added, then shear 10-15 min, Obtain lavender liquid nanometer capsule.The S/O ratio of lavender liquid nanometer capsule appearance obtained as shown in figure 1 for 9:1 institute Show.
The preparation of 3 lemon liquid Nano capsule of embodiment
Lemon is taken, it is 12 that experiment, which measures RHLB value,;So that it is determined that composite emulsifier is Tween-60 and Span-80;
Under 30 DEG C of bath temperatures, the na caseinate solution that mass fraction is 1% is prepared;
Beaker is added in 5 g of Tween-60 (Tween-60), 1.75 g of Span-80 (Span-80) 1.25 g and 1,2- propylene glycol In, 30 min are stirred at room temperature, blended emulsifier is made;Add 2 g of core material lemon, after immediately by beaker seal with The volatilization of core material ingredient is prevented, then stirs the mixture for that self-emulsifying microemulsion system is made;
Then it is placed under magnetic stirring apparatus at room temperature after stirring 1 h and 90 g na caseinate solutions is added, then shear 10-15 Min to get arrive lemon liquid Nano capsule.The S/O ratio of lemon liquid Nano capsule appearance obtained as shown in figure 1 for 8:2 institute Show.
The preparation of 4 lemon liquid Nano capsule of embodiment
Lemon is taken, it is 12 that experiment, which measures RHLB value,;So that it is determined that composite emulsifier is rilanit special and Span-80.
Under 30 DEG C of bath temperatures, the maltodextrin solution that mass fraction is 1% is prepared;
Beaker is added in 12 g of rilanit special (CO-40), 5.25 g of Span-80 (Span-80) 3.75 g and 1,2- propylene glycol In, 30 min are stirred at room temperature, blended emulsifier is made;Add 9 g of core material lemon, after immediately by beaker seal with The volatilization of core material ingredient is prevented, then stirs the mixture for that self-emulsifying microemulsion system is made;
Then it is placed under magnetic stirring apparatus at room temperature after stirring 1 h and 70 g maltodextrin solutions is added, then shear 10-15 min, Obtain lemon fluid body Nano capsule.The S/O ratio of lemon liquid Nano capsule appearance obtained as shown in figure 1 is shown in 7:3.
The preparation of 5 lavender liquid nanometer capsule of embodiment
Lavender is taken, it is 14 that experiment, which measures RHLB value,;So that it is determined that composite emulsifier is rilanit special and Span-80.
Under 30 DEG C of bath temperatures, the chitosan solution that mass fraction is 1% is prepared;
12 g of rilanit special (CO-40), Span-80 (Span-80) 3.75 g and 5 g of ethyl alcohol are added in beaker, in room temperature Blended emulsifier is made in 30 min of lower stirring;Add 9 g of core material Lavender, after immediately by beaker seal to prevent core material The volatilization of ingredient then stirs the mixture for that self-emulsifying microemulsion system is made;
Then it is placed under magnetic stirring apparatus at room temperature after stirring 1 h and 70 g chitosan solutions is added, then shear 10-15 min, i.e., Obtain lavender liquid nanometer capsule.

Claims (8)

1. a kind of preparation method of natural perfume material liquid nanometer capsule, it is characterised in that the following steps are included:
(1) measurement of core material RHLB value:
A series of composite emulsifier for preparing different HLB values is spare, and the selection optimal composite emulsifier HLB value of emulsifying effectiveness is The RHLB value of core material;
The composite emulsifier is that a kind of hydrophilic nonionic emulsifier and a kind of lipophilic nonionic emulsifier are mixed to get;
(2) preparation of wall material solution:
By weight, it weighs 1 part of wall material to be dissolved in 99 parts of deionized water, uniform stirring is allowed to sufficiently dissolve at room temperature, quiet Only 1h de-bubble is prepared into the wall material solution that mass fraction is 1%;
(3) preparation of blended emulsifier:
Assistant for emulsifying agent is added in the composite emulsifier of step (1) and 30 min are stirred at room temperature, blended emulsifier is made;
(4) preparation of self-emulsifying microemulsion system:
Weigh 10-30 parts of core materials, 70-90 parts of blended emulsifiers are added in beakers, after beaker is sealed immediately with prevent core material at The volatilization divided then stirs the mixture for that self-emulsifying microemulsion system is made;
(5) preparation of natural perfume material liquid nanometer capsule:
70-90 parts of wall material solution is mixed with 10-30 parts of self-emulsifying microemulsion systems, stirs, obtains natural perfume material liquid nanometer glue Capsule.
2. the preparation method of natural perfume material liquid nanometer capsule as described in claim 1, which is characterized in that the wall material For one of natural polymer such as chitosan, maltodextrin, casein sodium.
3. the preparation method of natural perfume material liquid nanometer capsule as described in claim 1, which is characterized in that described is hydrophilic Type nonionic emulsifier is polyethylene glycols emulsifier;The lipophilic nonionic emulsifier is sorbitan fatty acid ester Class emulsifier.
4. the preparation method of natural perfume material liquid nanometer capsule as described in claim 1, which is characterized in that the poly- second two Alcohols emulsifier is one of Cremophor RH40 class or polyethylene glycol sorbitan fatty acid esters class.
5. the preparation method of natural perfume material liquid nanometer capsule as described in claim 1, which is characterized in that
The assistant for emulsifying agent is the short chain alcohol that carbon chain lengths are 1-4.
6. the preparation method of natural perfume material liquid nanometer capsule as described in claim 5, which is characterized in that
The short chain alcohol that the carbon chain lengths are 1-4 is one of ethyl alcohol, 1,2- propylene glycol, n-butanol.
7. the preparation method of natural perfume material liquid nanometer capsule as described in claim 1, which is characterized in that
The mass ratio of the composite emulsifier and assistant for emulsifying agent is 3:1.
8. the preparation method of natural perfume material liquid nanometer capsule as described in claim 1, which is characterized in that
The core material is natural perfume material.
CN201810702523.9A 2018-06-30 2018-06-30 A kind of preparation method of natural perfume material liquid nanometer capsule Pending CN108940146A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111074674A (en) * 2020-01-08 2020-04-28 云南恩典科技产业发展有限公司 Slow-release essence forming paper
CN114903205A (en) * 2022-05-07 2022-08-16 江苏万腾新材料科技有限公司 Plant essential oil flavored capsule and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
PL394825A1 (en) * 2011-05-10 2012-11-19 Wroclawskie Centrum Badan Eit + Spólka Z Ograniczona Odpowiedzialnoscia Polymer nanocapsule, and method for manufacturing and use thereof
CN103691373A (en) * 2013-12-12 2014-04-02 上海应用技术学院 Method for preparing nano capsule
CN104437284A (en) * 2013-09-25 2015-03-25 王林 Preparation method of phase change microcapsule
CN107630366A (en) * 2017-09-01 2018-01-26 南通香佳纺织科技有限公司 A kind of Lavender and the microcapsules underwear finishing agent and preparation method of Blumea oil compounding
CN107858836A (en) * 2017-09-15 2018-03-30 南通香佳纺织科技有限公司 A kind of osmanthus flower fragrance microcapsules textile finish and its preparation application method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
PL394825A1 (en) * 2011-05-10 2012-11-19 Wroclawskie Centrum Badan Eit + Spólka Z Ograniczona Odpowiedzialnoscia Polymer nanocapsule, and method for manufacturing and use thereof
CN104437284A (en) * 2013-09-25 2015-03-25 王林 Preparation method of phase change microcapsule
CN103691373A (en) * 2013-12-12 2014-04-02 上海应用技术学院 Method for preparing nano capsule
CN107630366A (en) * 2017-09-01 2018-01-26 南通香佳纺织科技有限公司 A kind of Lavender and the microcapsules underwear finishing agent and preparation method of Blumea oil compounding
CN107858836A (en) * 2017-09-15 2018-03-30 南通香佳纺织科技有限公司 A kind of osmanthus flower fragrance microcapsules textile finish and its preparation application method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111074674A (en) * 2020-01-08 2020-04-28 云南恩典科技产业发展有限公司 Slow-release essence forming paper
CN114903205A (en) * 2022-05-07 2022-08-16 江苏万腾新材料科技有限公司 Plant essential oil flavored capsule and preparation method thereof

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