CN101816911A - Method for preparing nano rose essence capsules - Google Patents
Method for preparing nano rose essence capsules Download PDFInfo
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- CN101816911A CN101816911A CN 201010147881 CN201010147881A CN101816911A CN 101816911 A CN101816911 A CN 101816911A CN 201010147881 CN201010147881 CN 201010147881 CN 201010147881 A CN201010147881 A CN 201010147881A CN 101816911 A CN101816911 A CN 101816911A
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Abstract
The invention discloses a method for preparing nano rose essence capsules, which comprises the following steps of: a, mixing 0.3 to 0.8 weight percent of rose essence and 2.0 to 3.2 weight percent of polyoxyethylene (20) sorbitan monolaurate, stirring the mixture at the rotation speed of 1,100rpm, adding deionized water into the mixture and stirring to form a uniform emulsion; and b, dripping 0.6 to 1.6 weight percent of N-butyl cyanoacrylate into the emulsion, reacting for 2 to 4 hours, adjusting the pH value of the system with 1mol/L solution of sodium hydroxide to 7.0, and continuously reacting for 0.5 hour until the reaction is completed. The nano rose essence capsules prepared by the emulsion polymerization method of the invention have an average particle size of 91nm and a peak width of 16.8nm, have uniform particle size distribution and can be applied to goods for everyday consumption, such as textiles, cosmetics and detergents and the like.
Description
Technical field
The present invention relates to a kind of preparation method of essential oil or fragrant sample of rose local flavor, more particularly relate to a kind of method for preparing nano rose essence capsules of passing through.
Background technology
Flavoring rose essence is a kind of important additive, liked by the consumer, is mainly used in daily necessities such as weaving, cosmetics, washing agent at present, and rose fragrance plays crucial effects to the quality of end product.But owing to contain a large amount of volatile terpenoid substances in the flavoring rose essence, so problems such as end product fragrance is stable inadequately, aroma-keeping time weak point never are resolved.Only rest on the microencapsulation technology aspect around the research that improves essence fragrance stability aspect both at home and abroad, the particle diameter of essence can reach 3～500 μ m.Because the Nano capsule particle is less, be easy to disperse and be suspended in to form colloidal solution in the water, as clear as crystal in appearance, have the peculiar property different with conventional capsule, the essence Nano capsuleization can improve the quality of essence, makes product have certain advantage at aspects such as the stability of fragrance and fragrance remaining time than conventional capsule.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method for preparing nano rose essence capsules, and the nano rose essence capsules average grain diameter of the present invention's preparation is less than 100nm.
Technical solution of the present invention: a kind of method for preparing nano rose essence capsules, its each component consists of:
0.3～0.8 percentage by weight flavoring rose essence
0.6 the positive butyl ester of～1.6 percentage by weight alpha-cyanoacrylates
2.0～3.2 percentage by weight polyoxyethylene (20) sorbitan mono-laurates
Surplus is a deionized water;
The preparation method of described nano rose essence capsules comprises the following steps:
A. the flavoring rose essence of 0.3～0.8 percentage by weight and polyoxyethylene (20) sorbitan mono-laurate of 2.0～3.2 percentage by weights are blended in 1100rpm rotating speed lower magnetic force stirring five minutes, slowly inject deionized water, magnetic agitation is until forming homogenous emulsion, and the pH value with the hydrochloric acid solution regulation system of 1mol/L is 2.0 then;
B. under stirring condition, speed with 3/min slowly joins the positive butyl ester of the alpha-cyanoacrylate of 0.6～1.6 percentage by weight in the emulsion of step a preparation, dropwised the back stirring reaction 2～4 hours, then with the pH value to 7.0 of the sodium hydroxide solution regulation system of 1mol/L, the continuation stirring reaction obtained target product until reaction terminating in 0.5 hour.
Beneficial effect effect of the present invention, with the positive butyl ester of alpha-cyanoacrylate is carrier, the floral type flavoring rose essence is a core, in position on the basis of polymerization, prepare nano rose essence capsules by emulsion polymerization, under strong agitation and surfactant emulsification, the emulsification in water of the positive butyl ester of water-insoluble monomer alpha-cyanoacrylate disperses, and most of by solubilising among surfactant micella, regulate after the suitable pH value initiated polymerization, the monomer alpha-cyanoacrylate positive butyl ester very fast generation polymerization of solubilising in micella can constantly replenish and enter among the micella and still be dispersed in monomer in the water, and the polymer of generation has formed nano particle.PBCA is the package wall material, has favorable biological degradability and compatibility, prepares the controlled nano rose essence capsules of particle diameter by emulsion polymerization.Detect through dynamic laser determination of light scattering instrument, the nano rose essence capsules of the present invention's preparation is a milky blueing light emulsion, and average grain diameter is 91nm, peak width 16.8nm, particle diameter is evenly distributed, and fragrance is stable, can be applicable to daily necessities kinds such as weaving, cosmetics, washing agent.
Description of drawings
Fig. 1 is preparation method's flow chart of nano rose essence capsules;
Fig. 2 is the particle diameter distribution map of the nano rose essence capsules of embodiment 5 preparations.
The specific embodiment
By embodiment the present invention is described in further detail, a kind of nano rose essence capsules of emulsion polymerization preparation, its each component consists of:
0.3～0.8 percentage by weight flavoring rose essence
0.6 the positive butyl ester of～1.6 percentage by weight alpha-cyanoacrylates
2.0～3.2 percentage by weight polyoxyethylene (20) sorbitan mono-laurates
Surplus is a deionized water.
The preparation method of described nanometer rose slowly-releasing essence capsule comprises the following steps:
A. polyoxyethylene (20) sorbitan mono-laurate of the flavoring rose essence of 0.3～0.8 percentage by weight and 2.0～3.2 percentage by weights is blended under the 1100rpm magnetic agitation and stirred five minutes, slowly inject deionized water along walls of beaker, magnetic agitation is until forming homogenous emulsion.PH value with the hydrochloric acid solution regulation system of 1mol/L is 2.0 then;
B. under stirring condition, the positive butyl ester of the alpha-cyanoacrylate of 0.6～1.6 percentage by weight is slowly joined in the emulsion of step a preparation with the speed of 3/min.Dropwising, under the stirring condition, reacted 2～4 hours, is 7.0 with the pH value of 1mol/L sodium hydroxide solution regulation system, stirring condition down reaction 0.5 hour until reaction terminating.
In beaker, add the flavoring rose essence of 0.6 percentage by weight and polyoxyethylene (20) sorbitan mono-laurate of 2.6 percentage by weights, be blended under the speed of magnetic agitation 1100rpm and fully stirred five minutes, and in beaker, slowly add deionized water, continue identical speed and stir, until the emulsion homogeneous.Under magnetic agitation, slowly drip the pH value to 2.0 of the hydrochloric acid solution regulation system of 1mol/L then, the positive butyl ester of alpha-cyanoacrylate that then slowly adds 1.2 percentage by weights, stir while dripping, dropwise, seal a bottle, continue to stir, make its abundant polymerization, cessation reaction after 4 hours, the pH value to 7.0 of the sodium hydroxide solution regulation system of usefulness 1mol/L continues stirring and made the nano rose essence capsules emulsion in 0.5 hour.
Experiment has obtained nano essence capsule emulsion, this system stable existence, but the blue light phenomenon is not obvious.After the test of dynamic laser determination of light scattering instrument, the average grain diameter of prepared nano essence microcapsules is 41.8nm, and the size distribution coefficient is 0.318.
Embodiment 2
In beaker, add the flavoring rose essence of 0.8 percentage by weight and polyoxyethylene (20) sorbitan mono-laurate of 2.0 percentage by weights, be blended under the speed of magnetic agitation 1100rpm and fully stirred five minutes, and in beaker, slowly add deionized water, continue identical speed and stir, until the emulsion homogeneous.Under magnetic agitation, slowly drip the pH value to 2.0 of the hydrochloric acid solution regulation system of 1mol/L then, the positive butyl ester of alpha-cyanoacrylate that then slowly adds 1.6 percentage by weights, stir while dripping, dropwise, seal a bottle, continue to stir, make its abundant polymerization, cessation reaction after 2 hours, the pH value to 7.0 of the sodium hydroxide solution regulation system of usefulness 1mol/L continues stirring and made the nano rose essence capsules emulsion in 0.5 hour.
Experiment has obtained having the nano essence capsule emulsion of blue light, this system stable existence.After the test of dynamic laser determination of light scattering instrument, prepared nano essence capsule average grain diameter is 101nm, and the size distribution coefficient is 0.109.
Embodiment 3
In beaker, add the flavoring rose essence of 0.6 percentage by weight and polyoxyethylene (20) sorbitan mono-laurate of 2.6 percentage by weights, be blended under the speed of magnetic agitation 1100rpm and fully stirred five minutes, and in beaker, slowly add deionized water, continue identical speed and stir, until the emulsion homogeneous.Under magnetic agitation, slowly drip the pH value to 2.0 of the hydrochloric acid solution regulation system of 1mol/L then, the positive butyl ester of alpha-cyanoacrylate that then slowly adds 0.6 percentage by weight, stir while dripping, dropwise, seal a bottle, continue to stir, make its abundant polymerization, cessation reaction after 2 hours, the pH value to 7.0 of the sodium hydroxide solution regulation system of usefulness 1mol/L continues stirring and made described nano rose essence capsules emulsion in 0.5 hour.
Experiment has obtained having the nano essence capsule emulsion of blue light, this system stable existence.Through the test of dynamic laser determination of light scattering instrument, the particle diameter skewness of prepared nano essence capsule, average grain diameter is 90nm, the size distribution coefficient is 0.207.
Embodiment 4
In beaker, add the flavoring rose essence of 0.3 percentage by weight and polyoxyethylene (20) sorbitan mono-laurate of 3.2 percentage by weights, be blended under the speed of magnetic agitation 1100rpm and fully stirred five minutes, and in beaker, slowly add deionized water, continue identical speed and stir, until the emulsion homogeneous.Under magnetic agitation, slowly drip the pH value to 2.0 of the hydrochloric acid solution regulation system of 1mol/L then, the positive butyl ester of alpha-cyanoacrylate that then slowly adds 0.9 percentage by weight, stir while dripping, dropwise, seal a bottle, continue to stir, make its abundant polymerization, cessation reaction after 3 hours, the pH value to 7.0 of the sodium hydroxide solution regulation system of usefulness 1mol/L continues stirring and made described nano rose essence capsules emulsion in 0.5 hour.
Experiment has obtained having the nano essence capsule emulsion of light blue light, this system stable existence.Through the test of dynamic laser determination of light scattering instrument, the particle diameter skewness of prepared nano essence capsule, average grain diameter is 43.8nm, the size distribution coefficient is 0.144.
Embodiment 5
In beaker, add the flavoring rose essence of 0.4 percentage by weight and polyoxyethylene (20) sorbitan mono-laurate of 2.0 percentage by weights, be blended under the speed of magnetic agitation 1100rpm and fully stirred five minutes, and in beaker, slowly add deionized water, continue identical speed and stir, until the emulsion homogeneous.Under magnetic agitation, slowly drip the pH value to 2.0 of the hydrochloric acid solution regulation system of 1mol/L then, the positive butyl ester of alpha-cyanoacrylate that then slowly adds 0.8 percentage by weight, stir while dripping, dropwise, seal a bottle, continue to stir, make its abundant polymerization, cessation reaction after 2 hours, the pH value to 7.0 of the sodium hydroxide solution regulation system of usefulness 1mol/L continues stirring and made described nano rose essence capsules emulsion in 0.5 hour.
Experiment has obtained having the nano essence capsule emulsion of obvious blue light, this system stable existence simultaneously, and fragrance is stable.After the test of dynamic laser determination of light scattering instrument, prepared nano essence capsule grain diameter is evenly distributed, and average grain diameter is 91nm, and the size distribution coefficient is 0.034, and the particle diameter distribution map is seen Fig. 2.Above said content only is the basic explanation of the present invention under conceiving, and according to appointing that the technical scheme of invention is done
How valency exchange all should belong to protection scope of the present invention.
Claims (2)
1. method for preparing nano rose essence capsules, its each component consists of:
0.3～0.8 percentage by weight flavoring rose essence
0.6 the positive butyl ester of～1.6 percentage by weight alpha-cyanoacrylates
2.0～3.2 percentage by weight polyoxyethylene (20) sorbitan mono-laurate surpluses are deionized water;
The preparation method of described nano rose essence capsules comprises the following steps:
A. the flavoring rose essence of 0.3～0.8 percentage by weight and polyoxyethylene (20) sorbitan mono-laurate of 2.0～3.2 percentage by weights are blended in 1100rpm rotating speed lower magnetic force stirring five minutes, slowly inject deionized water, magnetic agitation is until forming homogenous emulsion, and the pH value with the hydrochloric acid solution regulation system of 1mol/L is 2.0 then;
B. under stirring condition, speed with 3/min slowly joins the positive butyl ester of the alpha-cyanoacrylate of 0.6～1.6 percentage by weight in the emulsion of step a preparation, dropwised the back stirring reaction 2～4 hours, then with the pH value to 7.0 of the sodium hydroxide solution regulation system of 1mol/L, the continuation stirring reaction obtained target product until reaction terminating in 0.5 hour.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268493A (en) * | 2011-07-14 | 2011-12-07 | 上海应用技术学院 | Method for preparing rose-fragrance leather |
| CN102352282A (en) * | 2011-07-14 | 2012-02-15 | 上海应用技术学院 | Lilial nanometer capsule and preparation method thereof |
| CN102634415A (en) * | 2012-04-26 | 2012-08-15 | 华南师范大学 | Nanometer essence capsule and preparation method thereof |
| CN102776070A (en) * | 2012-08-15 | 2012-11-14 | 上海应用技术学院 | Transparent microcapsule flavoring rose essence and preparation method thereof |
| CN102776068A (en) * | 2012-08-15 | 2012-11-14 | 上海应用技术学院 | Paste type microcapsule flavoring rose essence and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037640A (en) * | 2007-04-25 | 2007-09-19 | 上海应用技术学院 | Preparation method of potpourri type nano microcapsule essence |
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2010
- 2010-04-15 CN CN 201010147881 patent/CN101816911A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037640A (en) * | 2007-04-25 | 2007-09-19 | 上海应用技术学院 | Preparation method of potpourri type nano microcapsule essence |
Non-Patent Citations (3)
| Title |
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| 《上海应用技术学院学报》 20081231 未知 《新型微胶囊香精的制备技术研究》项目通过市科委专家组验收 124页 1 第8卷, 2 * |
| 《第七届中国香料香精学术研讨会论文集》 20081231 肖作兵等 聚合法制备纳米玫瑰香精 第1节、第2节、第3节 1 , 2 * |
| 《药学服务与研究》 20040430 戴蔚荃等 聚alpha-氰基丙烯酸丁醋载药纳米微粒的研究进展 第33页右栏第2段，第34页左栏第2段、第3段 1 第4卷, 第1期 2 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102268493A (en) * | 2011-07-14 | 2011-12-07 | 上海应用技术学院 | Method for preparing rose-fragrance leather |
| CN102352282A (en) * | 2011-07-14 | 2012-02-15 | 上海应用技术学院 | Lilial nanometer capsule and preparation method thereof |
| CN102352282B (en) * | 2011-07-14 | 2013-02-20 | 上海应用技术学院 | Lilial nanometer capsule and preparation method thereof |
| CN102634415A (en) * | 2012-04-26 | 2012-08-15 | 华南师范大学 | Nanometer essence capsule and preparation method thereof |
| CN102634415B (en) * | 2012-04-26 | 2013-07-17 | 华南师范大学 | Nanometer essence capsule and preparation method thereof |
| CN102776070A (en) * | 2012-08-15 | 2012-11-14 | 上海应用技术学院 | Transparent microcapsule flavoring rose essence and preparation method thereof |
| CN102776068A (en) * | 2012-08-15 | 2012-11-14 | 上海应用技术学院 | Paste type microcapsule flavoring rose essence and preparation method thereof |
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Application publication date: 20100901 |