CN109758383A - A kind of preparation method of gelatin-based ultra light sun block lotion - Google Patents

A kind of preparation method of gelatin-based ultra light sun block lotion Download PDF

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Publication number
CN109758383A
CN109758383A CN201910230386.8A CN201910230386A CN109758383A CN 109758383 A CN109758383 A CN 109758383A CN 201910230386 A CN201910230386 A CN 201910230386A CN 109758383 A CN109758383 A CN 109758383A
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parts
dopamine
gelatin
poly
added
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CN201910230386.8A
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Inventor
胡杨
余小月
朱士臣
陈雯欣
林源利
刀林睿
尤娟
尹涛
杨明涛
刘茹
熊善柏
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Huazhong Agricultural University
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Huazhong Agricultural University
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Abstract

The invention discloses a kind of preparation method of gelatin-based ultra light sun block lotion, it the steps include: that a. prepares nanometer poly-dopamine;B. polyvinylpyrrolidone grafted gelatin is prepared;C. after mixing nanometer poly-dopamine and polyvinylpyrrolidone grafted gelatin in proportion, the ultra light sun block lotion of poly-dopamine containing nanometer is obtained.Also disclose application of nanometer poly-dopamine in ultra light sun block lotion.The present invention has the advantages that being modified with polyvinylpyrrolidone to gelatin, nanometer poly-dopamine has good uv absorption property, and the uviolresistance of ultra light sun block lotion can be improved.

Description

A kind of preparation method of gelatin-based ultra light sun block lotion
Technical field
It is the present invention relates to technical field of skin care, in particular to a kind of to be prevented based on what nanometer poly-dopamine uvioresistant penetrated Shine the preparation method of lotion.
Background technique
It is proved through scientific research, ultraviolet light can make the structure or function of important component in cell that qualitative change occur, ultraviolet light Intensity is affected by region, season and weather.Sunlight medium wavelength is in 290nm ultraviolet light shortwave below, through atmospheric ozone layer Ground can not be reached after absorbing scattering.But these two types of ultraviolet lights of UVA (320~400nm) and UVB (290~230nm) can be to human body The skin corium or even subcutaneous tissue of skin cause centainly to injure.
Dopamine molecule contains catechol and amino structure, and in alkaline solution and oxidation environment, auto polymerization can occur Reaction forms the poly-dopamine particle with high-adhesiveness.Poly-dopamine has certain absorption to ultraviolet light, can mention for skin For ultraviolet shielded;Meanwhile poly-dopamine has excellent biodegradability and biocompatibility, has no to human skin toxic Illeffects;In addition, poly-dopamine can realize good adhesion effect by hydrogen bond association.
Polyvinylpyrrolidone has excellent adhesiveness, and hygroscopicity and biocompatibility etc. are a kind of more mature more Purposes medical auxiliary materials.After polyvinyl pyrrolidone modified, the retentiveness of gelatin, matter brittleness and film forming etc. can be improved.
It has been investigated that poly-dopamine has certain UV absorption effect, but there are no utilize to receive for currently available technology Rice poly-dopamine is applied to the technology of ultra light sun block lotion.
Summary of the invention
The present invention in view of the drawbacks of the prior art, provides a kind of preparation method of ultra light sun block lotion, can effectively solve State problem of the existing technology.
In order to realize the above goal of the invention, the technical solution adopted by the present invention is as follows:
A kind of preparation method of ultra light sun block lotion, comprising the following steps: below by weight;
A. it prepares a nanometer poly-dopamine particle: 2-4 parts of ammonium hydroxide (mass fraction 20%- being added in 250mL round-bottomed flask 30%) 40-50 parts of dehydrated alcohols and 90-120 parts of deionized waters, are added, are uniformly mixed.Take 4-6g Dopamine hydrochloride powder quick It is added in above-mentioned solution, poly-dopamine nanoparticle dispersion liquid, ie in solution A is made after 60-65 DEG C of water-bath 4-6h.It will be molten Liquid A is centrifuged 15min at 12000rpm, removes supernatant, obtains a nanometer poly-dopamine particle precipitating, appropriate deionization is then added Water cleans, and is centrifuged under the same terms, removes supernatant, and repeated washing operates three times, collects precipitating, and freeze-drying obtains nanometer and gathers Dopamine particle;
B. the preparation of polyvinylpyrrolidone grafted gelatin: 100-120 parts of deionized waters being added into three neck round bottom, 50-100 parts of gelatin, 20-30 parts of n-vinyl pyrrolidone (reaction monomers), 1-2 parts of azodiisobutyronitriles (initiator), logical Under conditions of nitrogen, 3-5h is at the uniform velocity stirred to react in 70-75 DEG C of water-bath and obtains solution B.To after the reaction was completed, into solution B Excessive propanone is added and obtains white or shallow thick white shape precipitating, is dried in vacuo at 40-60 DEG C after suction filtration.By petroleum ether Polyvinylpyrrolidone grafted gelatin is obtained after (60-90 DEG C of boiling point) extracting, freeze-drying;
C. the preparation of nanometer poly-dopamine ultra light sun block lotion: 20-80 parts of deionized water, polyvinylpyrrolidone grafted gelatin 10-30 parts, 2-10 parts of nanometer poly-dopamine, 40 DEG C of heating water bath stirrings obtain a nanometer poly-dopamine ultra light sun block lotion.
Preferably, 2 parts of ammonium hydroxide are added in step a in round-bottomed flask, 40 parts of dehydrated alcohols and 90 parts of deionizations are added Water is uniformly mixed.It takes 4 parts of Dopamine hydrochloride powder to be added rapidly in above-mentioned solution, is obtained after 60 DEG C of water-bath 4h poly- more Bar amine nanoparticle dispersion liquid, ie in solution A.
Preferably, 100 parts of deionized waters, 60 parts of gelatin, 20 parts of N- ethylene are added in step b into three neck round bottom Base pyrrolidones (reaction monomers), 1 part of azodiisobutyronitrile (initiator) are even in 70 DEG C of water-baths under conditions of logical nitrogen Speed is stirred to react 3h and obtains solution B.White or shallow thick white are obtained to which excessive propanone after the reaction was completed, is added into solution B Shape precipitates, and is dried in vacuo at 45 DEG C after suction filtration.Polyvinylpyrrolidone grafting is obtained after petroleum ether extracting, freeze-drying Gelatin.
Preferably, 110 parts of deionized waters, 85 parts of gelatin, 25 parts of N- ethylene are added in step b into three neck round bottom Base pyrrolidones (reaction monomers), 1.5 parts of azodiisobutyronitriles (initiator), under conditions of logical nitrogen, in 72 DEG C of water-baths It is at the uniform velocity stirred to react 4h and obtains solution B.To which after the reaction was completed, into solution B, it is viscous to obtain white or shallow white for addition excessive propanone Thick shape precipitates, and is dried in vacuo at 50 DEG C after suction filtration.Polyvinylpyrrolidone is obtained after petroleum ether extracting, freeze-drying to connect Branch gelatin.
Preferably, 50 parts of deionized water in step c, 10 parts of polyvinylpyrrolidone grafted gelatin, nanometer poly-dopamine 2 Part.
Preferably, 40 parts of deionized water in step c, 20 parts of polyvinylpyrrolidone grafted gelatin, nanometer poly-dopamine 5 Part.
The invention also discloses nanometer poly-dopamines to be applied to ultra light sun block lotion.
Compared with prior art the present invention has the advantages that nanometer poly-dopamine is applied to ultra light sun block lotion, have excellent Biodegradability and biocompatibility have no poisonous and harmful effect to human skin;In addition, poly-dopamine can be formed by hydrogen bond The cooperation good adhesion effect of realization.Gelatin is modified with polyvinylpyrrolidone, nanometer poly-dopamine has good Uv absorption property, the uviolresistance of lotion can be improved.
Detailed description of the invention
Fig. 1 is the gelatin emulsion ultraviolet permeability curve graph of present invention load dopamine;
Fig. 2 is the gelatin infrared spectrogram of different proportion polyvinylpyrrolidone (PVP) of the present invention grafting.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, by the following examples, to the present invention do into One step is described in detail.
Embodiment 1
A kind of preparation method of ultra light sun block lotion, comprising the following steps: its formula meter;
A. the preparation of nanometer poly-dopamine;
In 250mL round-bottomed flask be added 2 parts of ammonium hydroxide (mass fraction 20%-30%), be added 40 parts of dehydrated alcohols and 90 parts of deionized waters are uniformly mixed.4 parts of Dopamine hydrochloride powder are taken to be added rapidly in above-mentioned solution, 60 DEG C of water-bath 4h After obtain poly-dopamine nanoparticle dispersion liquid, ie in solution A.Solution A is centrifuged 15min at 12000rpm, supernatant is removed, obtains It is precipitated to nanometer poly-dopamine particle, appropriate amount of deionized water cleaning is then added, is centrifuged under the same terms, removes supernatant, repeated Cleaning operation three times, collects precipitating, and freeze-drying obtains a nanometer poly-dopamine particle;
B. the preparation of polyvinylpyrrolidone grafted gelatin
100 parts of deionized waters, 60 parts of gelatin, 20 parts of N- ethenyl pyrrolidones are added into the three neck round bottom of 250mL Ketone (reaction monomers), 1 part of azodiisobutyronitrile (initiator), under conditions of logical nitrogen, at the uniform velocity stirring is anti-in 70 DEG C of water-baths 3h is answered to obtain solution B.White or shallow thick white shape precipitating are obtained to which excessive propanone after the reaction was completed, is added into solution B, is taken out It is dried in vacuo at 45 DEG C after filter.Polyvinylpyrrolidone is obtained after petroleum ether (60-90 DEG C of boiling point) extracting, freeze-drying The gelatin of grafting;
C. the preparation of nanometer poly-dopamine ultra light sun block lotion
50 parts of deionized water, 10 parts of polyvinylpyrrolidone grafted gelatin, 2 parts of nanometer poly-dopamine, 40 DEG C of heating water baths Stirring, obtains a nanometer poly-dopamine ultra light sun block lotion.
Embodiment 2
A kind of preparation method of ultra light sun block lotion, comprising the following steps: its formula meter.
A. the preparation of nanometer poly-dopamine
In 250mL round-bottomed flask be added 3 parts of ammonium hydroxide (mass fraction 20%-30%), be added 45 parts of dehydrated alcohols and 100 parts of deionized waters are uniformly mixed.5 parts of Dopamine hydrochloride powder are taken to be added rapidly in above-mentioned solution, 63 DEG C of water-bath 5h Poly-dopamine nanoparticle dispersion liquid, ie in solution A are made afterwards.Solution A is centrifuged 15min at 12000rpm, supernatant is removed, obtains It is precipitated to nanometer poly-dopamine particle, appropriate amount of deionized water cleaning is then added, is centrifuged under the same terms, removes supernatant, repeated Cleaning operation three times, collects precipitating, and freeze-drying obtains a nanometer poly-dopamine particle;
B. the preparation of polyvinylpyrrolidone grafted gelatin
110 parts of deionized waters, 85 parts of gelatin, 25 parts of N- ethenyl pyrrolidones are added into the three neck round bottom of 250mL Ketone (reaction monomers), 1.5 parts of azodiisobutyronitriles (initiator) are at the uniform velocity stirred in 72 DEG C of water-baths under conditions of logical nitrogen Reaction 4h obtains solution B.White or shallow thick white shape precipitating are obtained to which excessive propanone after the reaction was completed, is added into solution B, It is dried in vacuo at 50 DEG C after suction filtration.Polyvinylpyrrolidine is obtained after petroleum ether (60-90 DEG C of boiling point) extracting, freeze-drying The gelatin of ketone grafting;
C. the preparation of nanometer poly-dopamine ultra light sun block lotion
40 parts of deionized water, 20 parts of polyvinylpyrrolidone grafted gelatin, 5 parts of nanometer poly-dopamine, 40 DEG C of heating water baths Stirring, obtains a nanometer poly-dopamine ultra light sun block lotion.
As shown in Figure 1, having loaded the gelatin hydrogel of the nanometer dopamine transmitance at 200-800nm is 0, this and black Element (oxidation tyrosine, positive control) phenomenon is consistent, after illustrating nanometer dopamine and gelatin, gelatin is made to have significant uvioresistant Through effect
As shown in Fig. 2, lines 1: 50 parts of gelatin, PVP20 parts;Lines 2: 60 parts of gelatin, PVP20 parts;Lines 3: 70 parts of gelatin, PVP20 parts;Lines 4: 80 parts of gelatin, PVP20 parts
Feature peak type at 1284 wave numbers shows that gelatin is successfully grafted on PVP skeleton.
Those of ordinary skill in the art will understand that the embodiments described herein, which is to help reader, understands this hair Bright implementation method, it should be understood that protection scope of the present invention is not limited to such specific embodiments and embodiments.Ability The those of ordinary skill in domain disclosed the technical disclosures can make its various for not departing from essence of the invention according to the present invention Its various specific variations and combinations, these variations and combinations are still within the scope of the present invention.

Claims (7)

1. a kind of preparation method of gelatin-based ultra light sun block lotion, which comprises the following steps: below by weight;
A. it prepares a nanometer poly-dopamine particle: 2-4 parts of ammonium hydroxide being added in 250mL round-bottomed flask, ammonium hydroxide mass fraction is 20%- 30%, 40-50 parts of dehydrated alcohols and 90-120 parts of deionized waters are added, are uniformly mixed;Take 4-6g Dopamine hydrochloride powder quick It is added in above-mentioned solution, poly-dopamine nanoparticle dispersion liquid, ie in solution A is made after 60-65 DEG C of water-bath 4-6h;It will be molten Liquid A is centrifuged 15min at 12000rpm, removes supernatant, obtains a nanometer poly-dopamine particle precipitating, appropriate deionization is then added Water cleans, and is centrifuged under the same terms, removes supernatant, and repeated washing operates three times, collects precipitating, and freeze-drying obtains nanometer and gathers Dopamine particle;
B. 100-120 parts of deionized waters, 50- the preparation of polyvinylpyrrolidone grafted gelatin: are added into three neck round bottom 100 parts of gelatin, 20-30 parts of n-vinyl pyrrolidone, 1-2 parts of azodiisobutyronitriles, under conditions of logical nitrogen, in 70-75 3-5h, which is at the uniform velocity stirred to react, in DEG C water-bath obtains solution B;To after the reaction was completed, excessive propanone be added into solution B and obtains white Or shallow thick white shape precipitates, and is dried in vacuo at 40-60 DEG C after suction filtration;Gathered after petroleum ether extracting, freeze-drying Vinylpyrrolidone grafted gelatin;
C. the preparation of nanometer poly-dopamine ultra light sun block lotion: 20-80 parts of deionized water, polyvinylpyrrolidone grafted gelatin 10-30 Part, 2-10 parts of nanometer poly-dopamine, 40 DEG C of heating water bath stirrings obtain a nanometer poly-dopamine ultra light sun block lotion.
2. according to the method described in claim 1, it is characterized by: 2 parts of ammonium hydroxide of addition, addition in round-bottomed flask in step a 40 parts of dehydrated alcohols and 90 parts of deionized waters are uniformly mixed;4 parts of Dopamine hydrochloride powder are taken to be added rapidly in above-mentioned solution, Poly-dopamine nanoparticle dispersion liquid, ie in solution A are obtained after 60 DEG C of water-bath 4h.
3. according to the method described in claim 1, it is characterized by: in step b into three neck round bottom be added 100 parts go from Sub- water, 60 parts of gelatin, 20 parts of n-vinyl pyrrolidone, 1 part of azodiisobutyronitrile, under conditions of logical nitrogen, in 70 DEG C of water It is at the uniform velocity stirred to react 3h in bath and obtains solution B;To which after the reaction was completed, into solution B, addition excessive propanone obtains white or shallow white Color thick precipitating is dried in vacuo after suction filtration at 45 DEG C;Polyvinylpyrrolidine is obtained after petroleum ether extracting, freeze-drying Ketone grafted gelatin.
4. according to the method described in claim 3, it is characterized by: 50 parts of deionized water in step c, polyvinylpyrrolidone connects 10 parts of gelatin, 2 parts of nanometer poly-dopamine of branch.
5. according to the method described in claim 1, it is characterized by: in step b into three neck round bottom be added 110 parts go from Sub- water, 85 parts of gelatin, 25 parts of n-vinyl pyrrolidone, 1.5 parts of azodiisobutyronitriles, under conditions of logical nitrogen, in 72 DEG C It is at the uniform velocity stirred to react 4h in water-bath and obtains solution B;White or shallow is obtained to which excessive propanone after the reaction was completed, is added into solution B Thick white shape precipitates, and is dried in vacuo at 50 DEG C after suction filtration;Polyvinyl pyrrole is obtained after petroleum ether extracting, freeze-drying Alkanone grafted gelatin.
6. according to the method described in claim 5, it is characterized by: 40 parts of deionized water in step c, polyvinylpyrrolidone connects 20 parts of gelatin, 5 parts of nanometer poly-dopamine of branch.
7. application of the described in claim 1 nanometer of poly-dopamine in ultra light sun block lotion.
CN201910230386.8A 2019-03-26 2019-03-26 A kind of preparation method of gelatin-based ultra light sun block lotion Pending CN109758383A (en)

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN110279613A (en) * 2019-07-08 2019-09-27 四川大学 A kind of melanin suncream of light color and preparation method thereof
CN111410887A (en) * 2020-05-11 2020-07-14 郑明光 Super-hydrophobic nano SiO2 modified epoxy acrylic resin coating and preparation method thereof
CN114209601A (en) * 2021-12-31 2022-03-22 华南理工大学 Sun-proof compressed tablet capable of being quickly coated and loaded with ultraviolet screening agent as well as preparation method and using method thereof
CN114983861A (en) * 2022-06-24 2022-09-02 温州中草集化妆品有限公司 Sunscreen cosmetic and preparation method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
CHANGPING WANG等: "Skin Pigmentation-Inspired Polydopamine Sunscreens", 《ADV. FUNCT. MATER.》 *
XING WANG等: "A Polydopamine Nanoparticle-Knotted Poly(ethylene glycol) Hydrogel for On-Demand Drug Delivery and Chemo-photothermal Therapy", 《CHEM. MATER》 *
高建平等: "明胶/乙烯基吡咯烷酮接枝共聚反应的研究", 《化学工业与工程》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110279613A (en) * 2019-07-08 2019-09-27 四川大学 A kind of melanin suncream of light color and preparation method thereof
CN111410887A (en) * 2020-05-11 2020-07-14 郑明光 Super-hydrophobic nano SiO2 modified epoxy acrylic resin coating and preparation method thereof
CN111410887B (en) * 2020-05-11 2021-06-15 黑龙江亿坪方科技有限公司 Super-hydrophobic nano SiO2Modified epoxy acrylic resin paint and its preparation
CN114209601A (en) * 2021-12-31 2022-03-22 华南理工大学 Sun-proof compressed tablet capable of being quickly coated and loaded with ultraviolet screening agent as well as preparation method and using method thereof
CN114983861A (en) * 2022-06-24 2022-09-02 温州中草集化妆品有限公司 Sunscreen cosmetic and preparation method thereof
CN114983861B (en) * 2022-06-24 2024-02-27 深圳市理然化妆品有限公司 A sunscreen cosmetic and its preparation method

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