CN110074993A - A method of preparing ultraviolet absorber nano particle - Google Patents

A method of preparing ultraviolet absorber nano particle Download PDF

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Publication number
CN110074993A
CN110074993A CN201910484284.9A CN201910484284A CN110074993A CN 110074993 A CN110074993 A CN 110074993A CN 201910484284 A CN201910484284 A CN 201910484284A CN 110074993 A CN110074993 A CN 110074993A
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CN
China
Prior art keywords
ultraviolet absorber
nano particle
room temperature
nanoemulsions
ethyl acetate
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Pending
Application number
CN201910484284.9A
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Chinese (zh)
Inventor
孙德军
郑晓阳
任改焕
谷慧
郭彦麟
刘尚营
武清林
骆兴伟
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Anhui Juyou Supply Chain Technology Development Co ltd
Shandong University
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Anhui Juyou Supply Chain Technology Development Co ltd
Shandong University
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Priority to CN201910484284.9A priority Critical patent/CN110074993A/en
Publication of CN110074993A publication Critical patent/CN110074993A/en
Pending legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241Containing particulates characterized by their shape and/or structure
    • A61K8/025Explicitly spheroidal or spherical shape
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/35Ketones, e.g. benzophenone
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37Esters of carboxylic acids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4973Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4993Derivatives containing from 2 to 10 oxyalkylene groups
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/413Nanosized, i.e. having sizes below 100 nm
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/56Compounds, absorbed onto or entrapped into a solid carrier, e.g. encapsulated perfumes, inclusion compounds, sustained release forms

Abstract

A method of preparing ultraviolet absorber nano particle, comprising the following steps: (1) weigh ethyl acetate, ethyl cellulose, surfactant, ultraviolet absorber and ultrapure water respectively in proportion;(2) ethyl cellulose is dissolved in ethyl acetate, is stirred at room temperature;Surfactant is added, is stirred at room temperature;It is eventually adding ultraviolet absorber, is stirred at room temperature, miscella phase is formed;(3) ultrapure water is instilled in oily phase at room temperature, and stirred, obtain the nanoemulsions of blue-opalescent;(4) it prepares dispersions of nanoparticles: obtained nanoemulsions is transferred in distilling flask, pass through evaporative removal ethyl acetate.The present invention prepares ultraviolet absorber nano particle by template of nanoemulsions, and obtained ultraviolet absorber nano particle regular appearance, good dispersion, particle diameter distribution are uniformly, granular size particle diameter distribution is controllable, ultraviolet absorption effect is good and preparation cost is effectively reduced.

Description

A method of preparing ultraviolet absorber nano particle
Technical field
The present invention relates to a kind of methods of nano particle for being used to prepare ultraviolet absorber, belong to nano particle technology of preparing Field.
Background technique
Ultraviolet light (UV) is the principal element for leading to skin sunburn and skin canceration, therefore sunscreen product is by increasingly It is more people's note that the photo-labile of ultraviolet absorber, skin irritation make its in cosmetics application receive it is certain Limitation.Therefore suitable encapsulation system such as nano particle is selected to encapsulate ultraviolet absorber, it is possible to reduce UV absorption Agent is directly contacted with skin, is reduced irritation, is increased its photostability.Polymer nano granules are high, raw due to its stability Object compatibility makes well it have good application prospect in food, medicine, cosmetic field.
Field of medicaments contains drug and active constituent usually using polymer nano granules, and common polymer has poly- cream Sour glycolic (PLGA), ethyl cellulose (EC), polylactic acid (PLA) etc..The preparation of polymer nano granules is generally divided into polymerization Object pre-dispersion method and monomer polymerization method, wherein monomer polymerization, which can generate by-product (residual monomer or initiator), leads to purification step Complexity, polymer pre-dispersion method include solvent evaporation method, solvent diffusion method, supercritical fluid technique etc..Wherein solvent, which volatilizees, is Most widely used a kind of technology, by polymer, drug, organic solvent, the thick lotion of surfactant preparation oil-in-water type, nanometer Lotion or microemulsion, then stable nano-colloid point is obtained by increasing temperature, reducing pressure or stirring removal organic solvent Granular media system, but since nanoemulsions are thermodynamic unstable systems, generally required when preparing nanoemulsions template it is high-pressure homogeneous or The instruments such as ultrasound input big energy to system, and instrument cost is higher, and energy charge is larger, and it is raw not to be suitable for industrial-scale It produces, and a large amount of heat can be generated under homogeneous or ultrasound condition, the preparation containing temperature sensitive active constituent is limited System, high energy may structure to active material and encapsulated condition have an impact, therefore by using the lower method of energy Preparing nano particle has preferable prospect.
The template that nanoemulsions are prepared as nano particle has the advantages that dilution stabilization, settlement stability, nanoemulsions Low-energy preparation method includes phase transition temperature method, phase transition component method, micro emulsion dilution method etc..Wherein phase transition component method by Aqueous phase content is gradually increased in the case where temperature-resistant promotes the spontaneous curvature of surfactant to change, and experience Water-In-Oil-is bis- Continuous phase microemulsion or the oil-in-water phase transition process of liquid crystalline phase-prepare nano oil-in-water emulsion.The preparation of phase transition component method is received Rice emulsion process is easy, can carry out under room temperature magnetic agitation, and capacity usage ratio is high, the nanoemulsions partial size being prepared It is smaller and be evenly distributed, nano particle is obtained after solvent evaporation in regular spherical morphology.
A kind of method of the multiple cohesion preparation sun-proof micron capsule of synergy disclosed in Chinese patent literature CN108969388A, this The wall material casein sodium of invention selection has ultraviolet absorption effect.Wall material casein sodium and sun-screening agent play UV absorption Cooperative synergism effect.
A kind of particle containing octyl methoxycinnamate and Avobenzone disclosed in Chinese patent literature CN108042382A Sunscreen composition and its application solve the problems, such as that octyl methoxycinnamate can not be applied in combination with Avobenzone, hence it is evident that mention The high photostability of composition, while also improving the stability of Avobenzone sun-screening agent.
Polymer-encapsulated colorant disclosed in american documentation literature US8709600 Nanoparticles (the colorant nano particle of polymer encapsulating), the resin of 10-250nm is prepared for by microfluidization The colorant nano particle of encapsulating.
Polymeric encapsulation of disclosed in american documentation literature US20030146529 Nanoparticles (nano particle of polymer encapsulating), provides in conjunction with ultrasonic treatment and the temperature-induced crystallization of non-solvent Polymer nanocomposite encapsulating method.
In the above-mentioned technology for preparing nano particle, polymerization reaction or crosslinking agent are used, obtaining nano particle need to be into one Step purifying or preparation process use the conditions such as high-pressure homogeneous, ultrasonic, high temperature, and high temperature and homogeneous may be for temperature sensitivities Active material or the encapsulated condition of particle impact.
Summary of the invention
The present invention is big for skin irritation existing for existing ultraviolet absorber, the required at high cost, consumption of nano particle preparation The big deficiency of energy, proposes a kind of method that temperate condition prepares ultraviolet absorber nano particle, to effectively reduce ultraviolet absorber Direct with skin contacts, and can be reduced the cost and energy loss of nano particle preparation process.
The method for preparing ultraviolet absorber nano particle of the invention, comprising the following steps:
(1) raw material is weighed:
Ethyl acetate, ethyl cellulose, surface-active are weighed respectively by the mass ratio of 14:1.5:6:0.5-4:30-180 Agent, ultraviolet absorber and ultrapure water;
Ultraviolet absorber is one or both of octyl methoxycinnamate and Avobenzone in the step (1).
Surfactant is the Span80 and Tween80 mixture of example 4:2-1:5 in mass ratio in the step (1).
(2) oily phase is prepared:
1. ethyl cellulose is dissolved in ethyl acetate, stir evenly at room temperature;
2. surfactant is added, stir evenly at room temperature;
3. ultraviolet absorber is added, stir evenly at room temperature, forms miscella phase;
The step (2) 1. in stirring be magnetic agitation 30 minutes.
The step (2) 2. in stirring be magnetic agitation 10 minutes.
The step (2) 3. in stirring be magnetic agitation 10 minutes.
(3) nanoemulsions are prepared:
Ultrapure water is instilled in oily phase dropwise at room temperature, is stirred when instilling, obtains the nanoemulsions of blue-opalescent;
Mixing speed is 800-1200 revs/min in the step (3).
It is 0.1ml/min-0.6ml/min that rate is instilled in the step (3).
(4) dispersions of nanoparticles is prepared:
Obtained nanoemulsions are transferred in distilling flask, rotary evaporation removes ethyl acetate at room temperature.
The rate of rotary evaporation is 100 revs/min in the step (4), the vacuum of distilling flask during rotary evaporation Degree is 0.09MPa.
Final ultraviolet absorber nano particle diameter hydrated diameter obtained reaches 140-180nm, what transmission electron microscope obtained Partial size is 60-120nm.Ultraviolet absorber aqueous nanoparticle dispersions still have stronger UV absorption after tying up to 1000 times of dilution.
The present invention first prepares nanoemulsions template, then removes solvent and obtain nano particle.Prepare ultraviolet absorber nanometer The key of grain is by preparing nanometer with the variation of the spontaneous curvature for increasing generation of aqueous phase content using surfactant molecule Lotion needs to control the rate of addition and uniform stirring of water phase.
The present invention is directed to the characteristics of general ultraviolet sun-screening agent skin irritation, utilizes biodegradable high molecular polymer Ethyl cellulose encapsulates ultraviolet absorber, reduces contact of the ultraviolet absorber with skin;Nanometer is prepared by template of nanoemulsions Particle reduces the cost and energy loss of nano particle preparation process.
Detailed description of the invention:
Fig. 1 is the grain size distribution of 1 gained octyl methoxycinnamate nano particle of embodiment.
Fig. 2 is the UV absorption figure of 1 gained octyl methoxycinnamate nano particle of embodiment.
Fig. 3 and Fig. 4 is the transmission electron microscope picture of 1 gained octyl methoxycinnamate nano particle of embodiment.
Fig. 5 is the grain size distribution of 5 gained Avobenzone nano particle of embodiment.
Fig. 6 is the UV absorption figure of 5 gained Avobenzone nano particle of embodiment.
Fig. 7 is the transmission electron microscope picture of 5 gained Avobenzone nano particle of embodiment.
Fig. 8 is the particle diameter distribution of embodiment 8 gained octyl methoxycinnamate and Avobenzone nano particle.
Fig. 9 is the UV absorption figure of embodiment 8 gained octyl methoxycinnamate and Avobenzone nano particle.
Figure 10 is the transmission electron microscope picture of embodiment 8 gained octyl methoxycinnamate and Avobenzone nano particle.
Specific embodiment
Embodiment 1
Ethyl acetate 1.4g is taken, 0.15g ethyl cellulose is dissolved in ethyl acetate, at room temperature magnetic agitation 30 minutes. 0.4g Tween80 and 0.2g Span80 is added, at room temperature magnetic agitation 10 minutes.It is eventually adding octyl methoxycinnamate 0.2g.Magnetic agitation 10 minutes at room temperature form miscella phase.18g ultrapure water is weighed, water is instilled to oily phase dropwise at room temperature In, and with the stirring of 800 revs/min of revolving speed, instillation rate is 0.6ml/min, is added dropwise, obtains the nano-emulsion of blue-opalescent Liquid.Obtained nanoemulsions are transferred in distilling flask, by Rotary Evaporators evaporation of solvent ethyl acetate, distillation is burnt Bottle vacuum degree 0.09MPa obtains octyl methoxycinnamate and receives rotary evaporation 45 minutes under the conditions of 100 revs/min of the speed of rotation The aqueous dispersion of rice grain.
The particle diameter distribution of octyl methoxycinnamate nano particle obtained by the present embodiment is as shown in Figure 1, nano particle is average Hydrated diameter is 147.0nm, and UV absorption is as shown in Fig. 2, octyl methoxycinnamate aqueous nanoparticle dispersions tie up to dilution Still there is stronger UV absorption after 1000 times at 310nm.Transmission electron microscope picture is as shown in Figure 3 and Figure 4, the grain that transmission electron microscope obtains Diameter range is 60-120nm.
Embodiment 2
Ethyl acetate 1.4g is taken, 0.15g ethyl cellulose is dissolved in ethyl acetate, at room temperature magnetic agitation 30 minutes. 0.5g Tween80 and 0.1g Span80 is added, at room temperature magnetic agitation 10 minutes.It is eventually adding octyl methoxycinnamate 0.2g.Magnetic agitation 10 minutes at room temperature form miscella phase.3g ultrapure water is weighed, is at room temperature instilled water dropwise in oily phase, And with the stirring of 900 revs/min of revolving speed, instillation rate is 0.1ml/min, is added dropwise, obtains the nanoemulsions of blue-opalescent. Obtained nanoemulsions are transferred in distilling flask, Rotary Evaporators evaporation of solvent ethyl acetate, distilling flask are passed through Vacuum degree 0.09MPa obtains octyl methoxycinnamate nanometer rotary evaporation 15 minutes under the conditions of 100 revs/min of the speed of rotation The aqueous dispersion of particle.
Gained octyl methoxycinnamate aqueous nanoparticle dispersions system obtained by the present embodiment dilutes 4 times of effect and implementation Example 1 is suitable.
Embodiment 3
Ethyl acetate 1.4g is taken, 0.15g ethyl cellulose is dissolved in ethyl acetate, at room temperature magnetic agitation 30 minutes. 0.3g Tween80 and 0.3g Span80 is added, at room temperature magnetic agitation 10 minutes.It is eventually adding octyl methoxycinnamate 0.2g.Magnetic agitation 10 minutes at room temperature form miscella phase.8g ultrapure water is weighed, is at room temperature instilled water dropwise in oily phase, And with the stirring of 1000 revs/min of revolving speed, instillation rate is 0.25ml/min, is added dropwise, obtains the nano-emulsion of blue-opalescent Liquid.Obtained nanoemulsions are transferred in distilling flask, by Rotary Evaporators evaporation of solvent ethyl acetate, distillation is burnt Bottle vacuum degree 0.09MPa obtains octyl methoxycinnamate and receives rotary evaporation 30 minutes under the conditions of 100 revs/min of the speed of rotation The aqueous dispersion of rice grain.
Gained octyl methoxycinnamate aqueous nanoparticle dispersions system obtained by the present embodiment dilutes 2 times of effect and implementation Example 1 is suitable.
Embodiment 4
The present embodiment the difference is that only that surfactant is 0.2g Tween80 and 0.4g with embodiment 1 Span80, the effect and embodiment 1 of gained octyl methoxycinnamate aqueous nanoparticle dispersions system are suitable.
Embodiment 5
Ethyl acetate 1.4g is taken, 0.15g ethyl cellulose is dissolved in ethyl acetate, at room temperature magnetic agitation 30 minutes. 0.4g Tween80 and 0.2g Span80 is added, at room temperature magnetic agitation 10 minutes.It is eventually adding Avobenzone 0.2g, room Temperature is magnetic agitation 10 minutes lower, forms miscella phase.18g ultrapure water is weighed, is at room temperature instilled water dropwise in oily phase, and with 1200 revs/min of revolving speed stirring, instillation rate is 0.6ml/min, is added dropwise, obtains the nanoemulsions of blue-opalescent.It will Obtained nanoemulsions are transferred in distilling flask, and by Rotary Evaporators evaporation of solvent ethyl acetate, distilling flask is true Reciprocal of duty cycle 0.09MPa, rotary evaporation 45 minutes, obtains the aqueous dispersion of Avobenzone nano particle by 100 revs/min of the speed of rotation System.
The particle diameter distribution of Avobenzone nano particle obtained by the present embodiment hydrated diameter as shown in figure 5, nano particle is averaged For 175.4nm, UV absorption is as shown in fig. 6, Avobenzone aqueous nanoparticle dispersions tie up to after 1000 times of dilution at 345nm Still there is stronger UV absorption.Transmission electron microscope picture is as shown in fig. 7, the particle size range that transmission electron microscope obtains is 60-120nm.
Embodiment 6
The present embodiment difference from example 1 is that: octyl methoxycinnamate 0.05g, ultrapure water 12g, It is 0.4ml/min that ultrapure water, which instills rate, and with the stirring of 1000 revs/min of revolving speed.Gained octyl methoxycinnamate nanometer The partial size and sem image and embodiment 1 of pellet moisture granular media system are suitable.
Embodiment 7
The present embodiment the difference is that only octyl methoxycinnamate 0.1g, gained methoxycinnamate with embodiment 1 The partial size and sem image and embodiment 1 of misery ester aqueous nanoparticle dispersions system are suitable.
Embodiment 8
Ethyl acetate 1.4g is taken, 0.15g ethyl cellulose is dissolved in ethyl acetate, at room temperature magnetic agitation 30 minutes. 0.4g Tween80 and 0.2g Span80 is added, at room temperature magnetic agitation 10 minutes.It is eventually adding octyl methoxycinnamate 0.2g and Avobenzone 0.2g, magnetic agitation 10 minutes, form miscella phase at room temperature.18g ultrapure water is weighed, at room temperature by water It is instilled in oily phase dropwise, and with the stirring of 1200 revs/min of revolving speed, instillation rate is 0.6ml/min, is added dropwise, obtains indigo plant The nanoemulsions of color opalescence.Obtained nanoemulsions are transferred in distilling flask, Rotary Evaporators evaporation of solvent is passed through Ethyl acetate, distilling flask vacuum degree 0.09MPa, rotary evaporation 45 minutes, obtain methoxyl group meat by 100 revs/min of the speed of rotation Cinnamate-Avobenzone nano particle aqueous dispersion.
Octyl methoxycinnamate-Avobenzone nano particle particle diameter distribution obtained by the present embodiment is as shown in figure 8, nanometer Particle is averaged hydrated diameter as 169.4nm, and UV absorption is as shown in figure 9, octyl methoxycinnamate-Avobenzone nano particle Aqueous dispersion has stronger UV absorption after tying up to 1000 times of dilution between 290nm-385nm.Transmission electron microscope picture such as Figure 10 Shown, the particle size range that transmission electron microscope obtains is 60-120nm.
Embodiment 9
The present embodiment and embodiment 8 the difference is that: octyl methoxycinnamate 0.1g, Avobenzone are 0.2g, ultrapure water 15g, it is 0.5ml/min that ultrapure water, which instills rate, and with the stirring of 1100 revs/min of revolving speed.Gained methoxyl group Cinnamic acid monooctyl ester-Avobenzone aqueous nanoparticle dispersions system partial size and sem image and embodiment 8 are suitable.

Claims (9)

1. a kind of method for preparing ultraviolet absorber nano particle, characterized in that the following steps are included:
(1) raw material is weighed:
Ethyl acetate, ethyl cellulose, surfactant, purple are weighed respectively by the mass ratio of 14:1.5:6:0.5-4:30-180 Outer absorbent and ultrapure water;
(2) oily phase is prepared:
1. ethyl cellulose is dissolved in ethyl acetate, stir evenly at room temperature;
2. surfactant is added, stir evenly at room temperature;
3. ultraviolet absorber is added, stir evenly at room temperature, forms miscella phase;
(3) nanoemulsions are prepared:
Ultrapure water is instilled in oily phase dropwise at room temperature, is stirred when instilling, obtains the nanoemulsions of blue-opalescent;
(4) dispersions of nanoparticles is prepared:
Obtained nanoemulsions are transferred in distilling flask, rotary evaporation removes ethyl acetate at room temperature.
2. the method according to claim 1 for preparing ultraviolet absorber nano particle, characterized in that in the step (1) Ultraviolet absorber is one or both of octyl methoxycinnamate and Avobenzone.
3. the method according to claim 1 for preparing ultraviolet absorber nano particle, characterized in that in the step (1) Surfactant is the Span80 and Tween80 mixture of 4:2-1:5 in mass ratio.
4. the method according to claim 1 for preparing ultraviolet absorber nano particle, characterized in that the step (2) is 1. In stirring be magnetic agitation 30 minutes.
5. the method according to claim 1 for preparing ultraviolet absorber nano particle, characterized in that the step (2) is 2. In stirring be magnetic agitation 10 minutes.
6. the method according to claim 1 for preparing ultraviolet absorber nano particle, characterized in that the step (2) is 3. In stirring be magnetic agitation 10 minutes.
7. the method according to claim 1 for preparing ultraviolet absorber nano particle, characterized in that in the step (3) Mixing speed is 800-1200 revs/min.
8. the method according to claim 1 for preparing ultraviolet absorber nano particle, characterized in that in the step (3) Instillation rate is 0.1ml/min-0.6ml/min.
9. the method according to claim 1 for preparing ultraviolet absorber nano particle, characterized in that in the step (4) The rate of rotary evaporation is 100 revs/min, and the vacuum degree of distilling flask is 0.09MPa during rotary evaporation.
CN201910484284.9A 2019-06-05 2019-06-05 A method of preparing ultraviolet absorber nano particle Pending CN110074993A (en)

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Application publication date: 20190802