Composite nano germicide and its preparation method and application
Technical field
The present invention relates to antiseptic technical field, in particular to a kind of composite nano germicide and preparation method thereof
And application.
Background technology
With the raising of our people's living standard and health perception, the demand of antiseptic greatly increases, various
Antiseptic be continuously developed and apply.It is big that antiseptic mainly includes inorganic antiseptic, organic antibacterial agent and natural antibacterial agent three
Class.Although organic antibacterial agent and natural antibacterial agent are respectively provided with certain antibacterial ability, but the problem of different is individually present.Have
Machine antiseptic heat resistance is poor, facile hydrolysis, and service life is short, and antibiotic effect is low, kill pathogenic bacteria and it is viral while can
Injury can be brought to normal cell.And natural antibacterial agent is mainly restricted by security and processing conditions, extensive city
The problem of certain be present in fieldization.Compared to organic antibacterial agent and natural antibacterial agent, inorganic antiseptic have high temperature resistant, broad-spectrum antiseptic,
The features such as safe, long-acting, have become the research emphasis in antibacterial field.
Wherein, Nano Silver is as a kind of New Inorganic Antibacterial Agents, with permeability is strong, antibacterial is lasting, has no drug resistance and pacifies
Congruent feature, antimicrobial product field has been widely used in it.The cell membrane of the general Gonna breakthrough bacterium of antibacterial mechanisms of Nano Silver
And cell membrane barrier, into cytoplasm after could destroy the enzyme system in cytoplasm, disturb the metabolism of bacterium, or into core
Matter, destroy DNA of bacteria.So it can be seen from the antibacterial mechanisms of Nano Silver, Nano Silver needs and carrier combination, through the thin of bacterium
Cell wall and cell membrane barrier, play antibacterial the effect of.And the nano silver antimicrobials that existing Nano Silver is formed with carrier combination
Generally existing is not sufficiently stable, and the problem of a kind of anti-biotic material antibiotic effect of Nano Silver needs to be further improved is used alone.
In view of this, it is special to propose the present invention to solve above-mentioned technical problem.
The content of the invention
The present invention first purpose be to provide a kind of composite nano germicide, the composite nano germicide is mainly by base
Plinth oil, Nano Silver, graphene, protein, phosphatide, polysaccharide, cholesterol, vitamin, solubilizer, emulsifying agent, antioxidant, anti-polymerization
The raw material such as agent and water is made, and is acted on by the coordinated of each raw material so that the composite nano germicide formed has good
Antibiotic effect and stability.
Second object of the present invention is to provide a kind of preparation method of composite nano germicide, and the preparation method passes through
After each raw material mixing homogeneous super-voltage micro jet nano-equipment will be used to carry out super-voltage micro jet circular treatment, you can be received
Rice complex antimicrobials, the preparation method is simple, and operation is easy, and whole production process is green, can industrial mass production.
And the composite nano germicide particle prepared by the method is uniform, stability is high, has good antibiotic effect.
Third object of the present invention is to provide a kind of application of composite nano germicide.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme:
The present invention provides a kind of composite nano germicide, is mainly made up of following raw material:Base oil, Nano Silver, graphene,
Protein, phosphatide, polysaccharide, cholesterol, vitamin, solubilizer, emulsifying agent, antioxidant, anti-polymerizer and water.
Further, the composite nano germicide is mainly made up of the raw material of following mass fraction:Base oil 1-30%,
Nano Silver 0.01-30%, graphene 0.01-10%, protein 0.1-10%, phosphatidase 1-15%, polysaccharide 0.1-10%, cholesterol
0.1-3%, vitamin 0.1-5%, solubilizer 1-30%, emulsifying agent 1-10%, antioxidant 0.1-1%, anti-polymerizer 0.5-
10%, water polishing surplus to 100%.
Further, the composite nano germicide is mainly made up of the raw material of following mass fraction:Base oil 5-30%,
Nano Silver 0.01-25%, graphene 0.1-10%, protein 0.1-8%, phosphatidase 1-12%, polysaccharide 0.1-8%, cholesterol
0.3-3%, vitamin 0.5-5%, solubilizer 1-25%, emulsifying agent 1-8%, antioxidant 0.2-1%, anti-polymerizer 1-10%,
Water polishing surplus is to 100%;
Preferably, the composite nano germicide is mainly made up of the raw material of following mass fraction:Base oil 6-30%, receives
Rice silver-colored 0.01-20%, graphene 0.1-9%, protein 1-8%, phosphatidase 2-10%, polysaccharide 1-8%, cholesterol 0.5-2.5%,
Vitamin 0.6-5%, solubilizer 2-25%, emulsifying agent 2-8%, antioxidant 0.4-1%, anti-polymerizer 1-8%, water polishing surplus
To 100%.
Further, the composite nano germicide also includes the adsorbent that mass fraction is 0.01-2%, the absorption
Agent include CNT, silica or zeolite in it is a kind of or at least two combination;
Preferably, the composite nano germicide also includes the sustained release agent that mass fraction is 0.01-2%, the sustained release agent
One kind in carboxymethyl cellulose, hydroxypropyl methyl cellulose, polyvinylpyrrolidone, fat or Wax or at least
Two kinds of combination.
Further, the composite nano germicide also includes the magnetic component that mass fraction is 0.01-10%;
Preferably, the magnetic component is ferroso-ferric oxide.
Further, the composite nano germicide also includes the titanium dioxide that mass fraction is 0.01-10%;
And/or the composite nano germicide also includes the zinc oxide that mass fraction is 0.01-10%.
Present invention also offers a kind of preparation method of composite nano germicide, comprise the following steps:
(a) by the base oil of formula ratio, protein, phosphatide, polysaccharide, cholesterol, vitamin, the solubilizer of respective part,
Emulsifying agent, antioxidant, anti-polymerizer and the mixing of part water, homogeneous, through super-voltage micro jet circular treatment, are made liposome and mix
Compound;
(b) by the Nano Silver and graphene of formula ratio, respective optional adsorbent, sustained release agent, magnetic component, titanium dioxide
And zinc oxide, and each solubilizer of surplus, emulsifying agent, antioxidant, anti-polymerizer and water mixing, homogeneous, through super-pressure
Microjet circular treatment, is made nanoparticles solution;
(c) liposomal mixtures obtained by step (a) and the nanoparticles solution obtained by step (b) are mixed, through superelevation
After pressing microjet circular treatment, composite nano germicide is obtained.
Further, in step (a), the temperature of the mixing is 50-70 DEG C, the pressure of super-voltage micro jet circular treatment
Power is 180-250MPa, and circular treatment number is 1-3 times;
Preferably, the particle diameter of the liposomal mixtures is 1-20nm.
Further, in step (b), the temperature of the mixing is 50-70 DEG C, the pressure of super-voltage micro jet circular treatment
Power is 180-250MPa, and circular treatment number is 1-3 times;
Preferably, the particle diameter of the nano particle in nanoparticles solution is 1-100nm.
Present invention also offers a kind of application of composite nano germicide in commodity or medical product.
Compared with prior art, the invention has the advantages that:
(1) the invention provides a kind of composite nano germicide, the composite nano germicide is mainly by base oil, nanometer
Silver, graphene, protein, phosphatide, polysaccharide, cholesterol, vitamin, solubilizer, emulsifying agent, antioxidant, anti-polymerizer and water etc.
Raw material forms, wherein, the liposome that the raw material such as protein, phosphatide, cholesterol is formed wraps up the functional materials such as vitamin, and
The compound back loading of the raw material such as Nano Silver and graphene is closely similar with eucaryotic cell structure so as to be formed on liposome interior or surface
Composite nano germicide, the speed that the complex antimicrobials enter microbial cell is fast, and can assemble to form height in perilesional
The drug effect of concentration, due to its surface positively charged, it can optionally adsorb, wrap up, shielding, killing the electronegative cause in surface
Germ and virus, there is stronger antibiotic effect, improve the nanometer silver antimicrobial that existing Nano Silver is formed with carrier combination
Agent generally existing is not sufficiently stable, and the problem of a kind of anti-biotic material antibiotic effect of Nano Silver needs to be further improved is used alone.
(2) it is simple to operate the invention provides a kind of preparation method of composite nano germicide, production process green ring
Protect, can industrial mass production, in addition, the uniform mixing of each raw material can be realized by this method, so as to be advantageous to be prepared into
The lifting of the stability of the composite nano germicide arrived.
(3) the invention provides a kind of application of composite nano germicide, in view of the advantage of above-mentioned composite nano germicide,
Composite nano germicide can be widely applied in commodity or medical product.
Brief description of the drawings
, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art
The required accompanying drawing used is briefly described in embodiment or description of the prior art, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 be human body acne experiment, wherein, (a) be using the composite nano germicide of embodiment 2 before;(b) it is using real
Apply after the composite nano germicide of example 2 48 hours;
Fig. 2 is that bacterium infection caused by human buttock's hair follicle inflammation is tested, wherein, (a) is nano combined using embodiment 2
(apocenosis cleaning treatment has been done before antiseptic);(b) it is to use 48 hours after the composite nano germicide of embodiment 2;
Fig. 3 be human body foot fungus infection experiment, wherein, (a) be using before the composite nano germicide of embodiment 4 (
There are 3 years medical histories);(b) it is using 15 days after the composite nano germicide of embodiment 4 (lasting daily to use);
Fig. 4 be human hands fungal infection experiment, wherein, (a) be using before the composite nano germicide of embodiment 6 (
There are 7 years medical histories);(b) it is using 20 days after the composite nano germicide of embodiment 6 (lasting daily to use);
Fig. 5 be human body psoriasis experiment 1, wherein, (a) be using the composite nano germicide of embodiment 8 before;(b) it is to make
With 21 days after the composite nano germicide of embodiment 8 (lasting daily to use);
Fig. 6 be human body psoriasis experiment 2, wherein, (a) be using the composite nano germicide of embodiment 1 before;(b) it is to make
With 14 days after the composite nano germicide of embodiment 1 (lasting daily to use).
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition suggested according to normal condition or manufacturer are carried out.Agents useful for same or the unreceipted production firm person of instrument, it is
The conventional products that can be obtained by commercially available purchase.
According to an aspect of the invention, there is provided a kind of composite nano germicide, the composite nano germicide mainly by
Following raw material is made:Base oil, Nano Silver, graphene, protein, phosphatide, polysaccharide, cholesterol, vitamin, solubilizer, emulsification
Agent, antioxidant, anti-polymerizer and water.
A kind of composite nano germicide provided by the invention, the composite nano germicide is mainly by base oil, Nano Silver, stone
The raw material groups such as black alkene, protein, phosphatide, polysaccharide, cholesterol, vitamin, solubilizer, emulsifying agent, antioxidant, anti-polymerizer and water
Into, wherein, the liposome that the raw material such as protein, phosphatide, cholesterol is formed wraps up the functional materials such as vitamin, and Nano Silver
With the compound back loading of raw material such as graphene on liposome interior or surface, so as to form the nanometer closely similar with eucaryotic cell structure
Complex antimicrobials, the speed that the complex antimicrobials enter microbial cell is fast, and can assemble to form high concentration in perilesional
Drug effect, due to its surface positively charged, can optionally adsorb, wrap up, shielding, kill the electronegative pathogenic bacteria in surface and
Virus, there is stronger antibiotic effect, it is universal with nano silver antimicrobials that carrier combination is formed to improve existing Nano Silver
In the presence of being not sufficiently stable, and the problem of a kind of anti-biotic material antibiotic effect of Nano Silver needs to be further improved is used alone.
As a kind of preferred embodiment of the present invention, the composite nano germicide is mainly by the raw material of following mass fraction
It is made:Base oil 1-30%, Nano Silver 0.01-30%, graphene 0.01-10%, phosphatidase 1-15%, cholesterol 0.1-3% are more
Sugared 0.1-10%, protein 0.1-10%, vitamin 0.1-5%, solubilizer 1-30%, emulsifying agent 1-10%, antioxidant 0.1-
1%, anti-polymerizer 0.5-10%, water polishing surplus to 100%.
Specifically, base oil belongs to lipid, main function forms emulsion, helps to maintain the stabilization of system, contributes to thin
The fusion of intercellular.Base oil is typical but non-limiting to elect evening primrose oil, grape-kernel oil, SIMMONDSIA CHINENSIS SEED OIL, olive oil, wheat as
Bud oil, apricot kernel oil, shea butter, peanut oil, avocado oil, rose hip oil, macadamia nut oil, safflower oil, sesame oil, soybean oil, rice bran
Oil, sun caul-fat, castor oil, coconut oil, marigold oil, snake oil, ostrich oil or lanolin are therein a kind of or at least two
Combination, preferably evening primrose oil.
The typical but non-limiting mass fraction of base oil be 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%,
10%th, 12%, 14%, 16%, 18%, 20%, 22%, 25%, 28% or 30%.
Main antimicrobial component of the Nano Silver as this composite nano germicide, with permeability is strong, antibacterial is lasting, without resistance
Property and it is safe the features such as.
The typical but non-limiting mass fraction of Nano Silver be 0.01%, 0.05%, 0.1%, 0.25%, 0.5%,
0.8%th, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 12%, 14%, 16%, 18%, 20%, 22%,
25%th, 28% or 30%.
In the present invention, Nano Silver is used in combination with graphene so that antibacterial effect is more notable.Graphene is typical but non-
Restricted mass fraction be 0.01%, 0.05%, 0.1%, 0.25%, 0.5%, 0.8%, 1%, 2%, 3%, 4%, 5%,
6%th, 7%, 8%, 9%, 10%.
Phosphatide and cholesterol collectively form liposome, and the liposome formed has the knot similar with biological cell
Structure, therefore by good biocompatibility, can be merged with human body cell film, so as to loaded Nano Silver, graphene and
Nutritional ingredient is sent into cell interior, improves the ability that antibacterial components break through human body cell barrier, adds Nano Silver, graphene
Sustained release stability, reach effectively, the purpose of enduringly antibacterial;And the nutriment of liposome is passed while antibacterial
Cell is passed, cellular energy is supplemented, promotes the growth of cell, improve the self-repairing capability of cell.In addition, liposome can also be prevented
Only Nano Silver is oxidized, and improves the stability of composite nano germicide.
The typical but non-limiting mass fraction of phosphatide be 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%,
10%th, 12%, 14% or 15%.
The typical but non-limiting mass fraction of cholesterol is 0.1%, 0.5%, 1%, 2% or 3%.
Protein, polysaccharide can be used as nutriment, wrap up or are supported on liposome.Protein is typical but unrestricted
Property mass fraction for 0.1%, 0.25%, 0.5%, 0.8%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or
10%.The typical but non-limiting mass fraction of polysaccharide be 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%,
8%th, 9% or 10%.
Vitamin, as the nutriment of the composite nano germicide, vitamin is given birth to including but not limited to vitamin A, dimension
One or more in plain B, vitamin C, vitamin D, vitamin E, vitamin K and derivative, preferred vitamin E.Vitamin
Typical but non-limiting mass fraction is 0.1%, 0.5%, 1%, 2%, 3%, 4% or 5%.By lipid while antibacterial
The nutriment of body parcel passes to cell, supplements cellular energy, promotes the growth of cell, improve the self-regeneration energy of cell
Power.
Composite nano germicide is a kind of suspension, aggregation, fusion easily occurs in storage process, and may cause institute
The drug leakage of embedding.To improve its stability, therefore need to add solubilizer, emulsifying agent, antioxidant and anti-polymerizer etc..
The one kind of solubilizer in ethanol, propane diols, 1-2 butanediols, 1-3 butanediols, preferably propane diols.Solubilizer allusion quotation
Type but nonrestrictive mass fraction are 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 12%, 14%,
16%th, 18%, 20%, 22%, 25%, 28% or 30%.
Emulsifying agent is selected from methyl glucoside sesquialter stearate, methyl glucoside sesquialter stearate, EG polypropylene
Sour sodium copolymer, stereth, tristerin/PEG-100 stearates, cetearyl alcohol ether, anhydro sorbitol sesquialter
Oleate, monoglyceride, sorbester p18, sorbester p17, polysorbate60, Tween 80, three polyglycereol double iso-stearate, peregal, quaternary ammonium salts
The one or more of one or more in ethanol, preferably stearine, stearate copolymer or monoglyceride.Emulsification
The typical but non-limiting mass fraction of agent is 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%.
Antioxidant is selected from butylated hydroxy anisole (BHA), dibutyl hydroxy toluene (BHT), propylgallate (PG), uncle
A kind of in butylhydroquinone (TBHQ) or at least two combination, preferably dibutyl hydroxy toluene.Antioxidant typical case but
Nonrestrictive mass fraction be 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9% or
0.10%.
Anti- polymerizer is selected from alkyl-glucoside, hexadecyltrimethylammonium chloride, OTAC, coconut palm
Seed oil fatty acid diethanolamine, dodecylic acid, tetradecanoic acid, hexadecanoic acid, EDETATE DISODIUM, sodium lauroyl sarcosine, bay
Alcohol ether phosphate potassium, monoalkyl ether ester sylvite, cocoyl isethionate or one kind in cocoyl isethionate or
The combination of person at least two, preferably alkyl-glucoside.The anti-typical but non-limiting mass fraction of polymerizer be 0.5%,
1%th, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%.
As a kind of preferred embodiment of the present invention, the composite nano germicide is mainly by the raw material of following mass fraction
It is made:Base oil 5-30%, Nano Silver 0.01-25%, graphene 0.1-10%, protein 0.1-8%, phosphatidase 1-12% are more
Sugared 0.1-8%, cholesterol 0.3-3%, vitamin 0.5-5%, solubilizer 1-25%, emulsifying agent 1-8%, antioxidant 0.2-1%,
Anti- polymerizer 1-10%, water polishing surplus to 100%;
Preferably, the composite nano germicide is mainly made up of the raw material of following mass fraction:Base oil 6-30%, receives
Rice silver-colored 0.01-20%, graphene 0.1-9%, protein 1-8%, phosphatidase 2-10%, polysaccharide 1-8%, cholesterol 0.5-2.5%,
Vitamin 0.6-5%, solubilizer 2-25%, emulsifying agent 2-8%, antioxidant 0.4-1%, anti-polymerizer 1-8%, water polishing surplus
To 100%.
The physical and chemical stability of composite nano germicide is related to Multiple factors, and is mutually restricted between each factor,
Therefore the proportioning between specific raw material composition and content is chosen, many factors must be just controlled, stablize effective nanometer to prepare
Complex antimicrobials.By to the raw material composition of composite nano germicide is further optimized so that the association between each raw material composition
Stronger with mating reaction, stability is more preferable, and the ability of penetration cell film is stronger, and antibacterial ability is more notable.
" mainly by ... be made " of the present invention, it is intended that it can also include other components in addition to the component, than
Such as thickener, these other components assign the composite nano germicide different characteristics.In addition, it is of the present invention
" mainly by ... be made ", may be replaced by enclosed " for " or " by ... be made ".
As a kind of preferred embodiment of the present invention, the composite nano germicide is 0.5-3% also including mass fraction
Thickener.Its denseness can be adjusted using thickener, it is actually required to meet.In the present invention, thickener is selected from
Polyethylene glycol, card ripple, acrylate copolymer, methyl glucoside polyoxyethylene, carbomer, polyvinylpyrrolidone, polyethylene
The poly- ammonium salt polymer of alcohol, alkyl, xanthan gum or one kind in sodium alginate or at least two combination, preferably xanthan gum or poly-
Ethylene glycol.The typical but non-limiting mass fraction of thickener is 0.5%, 1%, 1.5%, 2%, 2.5% or 3%.
As a kind of preferred embodiment of the present invention, the composite nano germicide is 0.01-2% also including mass fraction
Adsorbent.Adsorbent is added in composite nano germicide, can be by pathogenic bacteria and virus effectively absorption nano composite antibacterial
Around agent, then using the antibacterial components of composite nano germicide to reach to pathogenic bacteria and the purpose killed of virus.
The typical but non-limiting mass fraction of adsorbent be 0.01%, 0.05%, 0.1%, 0.2%, 0.4%,
0.6%th, 0.8%, 0.10%, 0.12%, 0.14%, 0.16%, 0.18% or 0.20%.The adsorbent include CNT,
A kind of in silica or zeolite or at least two combination.
As a kind of preferred embodiment of the present invention, the composite nano germicide is 0.01-2% also including mass fraction
Sustained release agent.Sustained release agent can be with further such that the slow releasing function of composite nano germicide in the cell be more longlasting.
The typical but non-limiting mass fraction of sustained release agent be 0.01%, 0.05%, 0.1%, 0.2%, 0.4%,
0.6%th, 0.8%, 0.10%, 0.12%, 0.14%, 0.16%, 0.18% or 0.20%.Sustained release agent is selected from carboxymethyl cellulose
Element, hydroxypropyl methyl cellulose or one kind in polyvinylpyrrolidone or at least two combination.
As a kind of preferred embodiment of the present invention, the composite nano germicide is 0.01- also including mass fraction
10% magnetic component.Magnetic component is added in composite nano germicide, by the guiding of outer field of magnetic forece, is formed in diseased region
The drug effect of high concentration.
The typical but non-limiting quality digit of magnetic component be 0.1%, 0.5%, 1%, 2%, 3%, 4%, 5%,
6%th, 7%, 8%, 9% or 10%.The magnetic component can elect band as and be magnetic and harmless magnetic material.It is preferred that
, the magnetic component is ferroso-ferric oxide.
In order to further lift the antibacterial ability of composite nano germicide, as the present invention a kind of preferred embodiment,
The composite nano germicide also includes the titanium dioxide that mass fraction is 0.01-10%;
And/or the composite nano germicide also includes the zinc oxide that mass fraction is 0.01-10%.
Titanium dioxide, zinc oxide are respectively provided with certain antibacterial ability, add it in composite nano germicide, with nanometer
Silver and graphene coordinate jointly, so as to form the stronger antiseptic of antibacterial ability.
The typical but non-limiting quality digit of titanium dioxide be 0.01%, 0.1%, 0.5%, 1%, 2%, 3%, 4%,
5%th, 6%, 7%, 8%, 9% or 10%.The typical but non-limiting quality digit of zinc oxide be 0.01%, 0.1%, 0.5%,
1%th, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%.
Composite nano germicide provided by the invention can with Urine scent, absorption, shielding, kill electronegative pathogenic bacteria,
Repel the normal cell of positively charged, farthest safeguard the intercellular ecological balance.
According to another aspect of the present invention, a kind of preparation method of composite nano germicide, including following step are additionally provided
Suddenly:
(a) by the base oil of formula ratio, protein, phosphatide, polysaccharide, cholesterol, vitamin, the solubilizer of respective part,
Emulsifying agent, antioxidant, anti-polymerizer and the mixing of part water, homogeneous, through super-voltage micro jet circular treatment, are made liposome and mix
Compound;
(b) by the Nano Silver and graphene of formula ratio, respective optional adsorbent, sustained release agent, magnetic component, titanium dioxide
And zinc oxide, and each solubilizer, emulsifying agent, antioxidant, anti-polymerizer and water mixing homogeneous of surplus, it is micro- through super-pressure
Jet-loop processing, is made nanoparticles solution;
(c) liposomal mixtures obtained by step (a) and the nanoparticles solution obtained by step (b) are mixed, through superelevation
After pressing microjet circular treatment, composite nano germicide is obtained.
The preparation method of composite nano germicide provided by the invention, technique is simple, easy to operate, and whole production process is green
Colour circle is protected, can industrial mass production.And the uniform mixing of each raw material can be realized by this method, so as to be advantageous to be prepared into
The lifting of the stability of the composite nano germicide arrived.
Further, in step (a), the temperature of the mixing is 50-70 DEG C, the pressure of super-voltage micro jet circular treatment
Power is 180-250MPa, and circular treatment number is 1-3 times;
Preferably, the particle diameter of the liposomal mixtures is 1-20nm.
For the particle diameter of further refinement composite nano germicide, raw mixture is carried out using super-voltage micro jet equipment
Processing.In super-voltage micro jet circulating treatment procedure, cycle-index should not be too many, otherwise structure of phospholipid can be destroyed, make
Into the seepage of medicine.The selection of processing pressure has very big influence to the particle diameter and pattern of final composite nano germicide,
Processing pressure should not be too low, it is too low if liposomal mixtures particle diameter it is larger, and can have larger aggregation;Processing pressure
Also should not be too high, it otherwise can influence envelop rate of the liposomal mixtures to antibacterial components.
In the present invention, in step (a), the temperature of mixing is 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C or 70 DEG C.Super-pressure
Microjet circulate typical but non-limiting processing pressure for 180MPa, 190MPa, 200MPa, 205MPa, 210MPa,
220MPa, 225MPa, 230MPa, 235MPa, 240MPa, 245MPa or 250MPa.Circular treatment number is 1 time, 2 times or 3 times.
The particle diameter of liposomal mixtures is 1nm, 5nm, 8nm, 10nm, 12nm, 15nm, 18nm or 20nm.
Further, in step (b), the temperature of mixing is 50-70 DEG C, and the pressure of super-voltage micro jet circular treatment is
180-250MPa, circular treatment number are 1-3 times;
Preferably, the particle diameter of the nano particle in nanoparticles solution is 1-100nm.
In the present invention, in step (b), the temperature of mixing is 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C or 70 DEG C.Super-pressure
Microjet circulate typical but non-limiting processing pressure for 180MPa, 190MPa, 200MPa, 205MPa, 210MPa,
220MPa, 225MPa, 230MPa, 235MPa, 240MPa, 245MPa or 250MPa.Circular treatment number is 1 time, 2 times or 3 times.
The particle diameter of nano particle in nanoparticles solution be 10nm, 20nm, 30nm, 40nm, 50nm, 60nm, 70nm,
80nm, 90nm or 100nm.
By the research of the specific matching relationship between each parameter to being related in preparation method and each parameter, so that
Each parameter is determined, and then ensures that prepared composite nano germicide has good quality and effect.
According to the third aspect of the present invention, a kind of composite nano germicide is additionally provided in commodity or medical product
In application.
The composite nano germicide that the composite nano germicide is compounded to form by the component such as Nano Silver and graphene, has
Continue, permanent antibiotic effect, suitable formulation can be fabricated to and be applied to commodity or field of medicaments.
Composite nano germicide chemical property in the present invention is stable, may apply to daily necessities field, for example antibacterial disappears
The facial mask of inflammation, emulsion, Essence, face cream, foundation cream, thimerosal, hand cleanser, foot lotion, face sanitizer, disinfectant soap, liquid detergent, laundry
Powder, shampoo, hair cream, shower cream, toothpaste, mouthwash, hygenic towelette, sanitary napkin etc., or food antiseptic can also be applied to
Agent field etc..
Due to composite nano germicide to bacterium, fungi, spore, itch mite etc. infect caused by acne, scabies, acne rosacea,
The disease of skin such as eczema, burn, scald and vagina mycotic infection have an obvious curative effects, therefore the composite nano germicide in the present invention
It is also applied to pharmaceutical sanitary field, such as medical antibacterial anti-inflammatory ointment, medicinal powder, disinfecting, antimicrobial dressing, sterilization of instruments medicine
Health field;Or pharmaceutical test quarantine field is applied to, such as radioactively labelled substance, targeted drug are treated.
With reference to specific embodiment and comparative example, the invention will be further described.
Embodiment 1
A kind of composite nano germicide that the present embodiment provides, is made up of the raw material of following mass fraction:Evening primrose oil
1%, Nano Silver 0.01%, graphene 0.1%, protein 0.1%, phosphatidase 1 %, chitosan 0.2%, cholesterol 2%, vitamin
E 0.2%, ethanol 2%, monoglyceride 0.5%, dibutyl hydroxy toluene 0.2%, alkyl-glucoside 1%, water polishing surplus is extremely
100%.
Embodiment 2
A kind of composite nano germicide that the present embodiment provides, is made up of the raw material of following mass fraction:Grape-kernel oil
11%, Nano Silver 0.05%, graphene 1%, protein 0.3%, phosphatidase 3 %, chitosan 0.3%, cholesterol 1%, vitamin C
0.5%, vitamin E 0.5%, propane diols 4%, tristerin/PEG-100 stearates 1%, TBHQ
0.4%, alkyl-glucoside 0.8%, cocoyl isethionate 0.2%, xanthan gum 0.5%, polyethylene glycol 0.3%, two
Silica 0.2%, water polishing surplus to 100%.
Embodiment 3
A kind of composite nano germicide that the present embodiment provides, is made up of the raw material of following mass fraction:Evening primrose oil
12%, Nano Silver 5%, graphene 6%, protein 10%, phosphatide 7%, chitosan 10%, cholesterol 1%, vitamin C 5%,
Ethanol 25%, monoglyceride 8%, dibutyl hydroxy toluene 0.5%, alkyl-glucoside 0.5%, silica 0.2%, water polishing
Surplus is to 100%.
Embodiment 4
A kind of composite nano germicide that the present embodiment provides, is made up of the raw material of following mass fraction:Evening primrose oil
20%, Nano Silver 10%, graphene 10%, protein 8%, phosphatidase 1 2%, chitosan 1%, cholesterol 2%, vitamin E
1%, ethanol 5%, monoglyceride 2%, dibutyl hydroxy toluene 0.6%, alkyl-glucoside 2%, water polishing surplus to 100%.
Embodiment 5
A kind of composite nano germicide that the present embodiment provides, is that with the addition of mass fraction on the basis of embodiment 4 to be
0.2% silica and 1.5% sustained release agent, remaining raw material and dosage are same as Example 4.
Embodiment 6
A kind of composite nano germicide that the present embodiment provides, is that with the addition of mass fraction on the basis of embodiment 5 to be
1% titanium dioxide and 2% zinc oxide, remaining raw material and dosage are same as Example 5.
Embodiment 7
A kind of composite nano germicide that the present embodiment provides, is that with the addition of mass fraction on the basis of embodiment 6 to be
8% ferroso-ferric oxide, remaining raw material and dosage are same as Example 6.
Embodiment 8
A kind of composite nano germicide that the present embodiment provides, is made up of the raw material of following mass fraction:Evening primrose oil
30%, Nano Silver 25%, graphene 2%, protein 6%, phosphatidase 1 5%, chitosan 5%, cholesterol 3%, vitamin B 1%,
Vitamin E 2%, ethanol 3%, monoglyceride 1%, polysorbate60 1%, butylated hydroxy anisole 0.8%, alkyl-glucoside 1%,
Water polishing surplus is to 100%.
Embodiment 9
The preparation method for the composite nano germicide that embodiment 1 provides, comprises the following steps:
(a) by the base oil of formula ratio, protein, phosphatide, polysaccharide, cholesterol, vitamin, the increasing of respective 1/2 formula ratio
Solvent, emulsifying agent, antioxidant, anti-polymerizer and water mixing, the temperature of mixing is 55 DEG C, homogeneous, is followed through super-voltage micro jet
Ring processing, processing pressure 200MPa, circular treatment number are 2 times, and liposomal mixtures are made;
(b) by the Nano Silver and graphene of formula ratio, respective optional adsorbent, sustained release agent, magnetic component, titanium dioxide
And zinc oxide, and each solubilizer of surplus, emulsifying agent, antioxidant, anti-polymerizer and water mixing, the temperature of mixing is 60
DEG C, homogeneous, through super-voltage micro jet circular treatment, processing pressure 200MPa, circular treatment number is 1 time, and nanometer is made
Grain solution;
(c) liposomal mixtures obtained by step (a) and the nanoparticles solution obtained by step (b) are mixed, through superelevation
After pressing microjet circular treatment, composite nano germicide is obtained.
Embodiment 10
The preparation method for the composite nano germicide that embodiment 2 provides, comprises the following steps:
(a) by the base oil of formula ratio, protein, phosphatide, polysaccharide, cholesterol, vitamin, the increasing of respective 1/2 formula ratio
Solvent, emulsifying agent, antioxidant, anti-polymerizer and water mixing, the temperature of mixing is 65 DEG C, homogeneous, is followed through super-voltage micro jet
Ring processing, processing pressure 220MPa, circular treatment number are 2 times, and liposomal mixtures are made;
(b) by the Nano Silver and graphene of formula ratio, respective optional adsorbent, sustained release agent, magnetic component, titanium dioxide
And zinc oxide, and each solubilizer of surplus, emulsifying agent, antioxidant, anti-polymerizer and water mixing, the temperature of mixing is 65
DEG C, homogeneous, through super-voltage micro jet circular treatment, processing pressure 220MPa, circular treatment number is 2 times, and nanometer is made
Grain solution;
(c) liposomal mixtures obtained by step (a) and the nanoparticles solution obtained by step (b) are mixed, through superelevation
After pressing microjet circular treatment, composite nano germicide is obtained.
Embodiment 11
The preparation method for the composite nano germicide that embodiment 3 provides, comprises the following steps:
(a) by the base oil of formula ratio, protein, phosphatide, polysaccharide, cholesterol, vitamin, the increasing of respective 2/3 formula ratio
Solvent, emulsifying agent, antioxidant, anti-polymerizer and water mixing, the temperature of mixing is 70 DEG C, homogeneous, is followed through super-voltage micro jet
Ring processing, processing pressure 250MPa, circular treatment number are 2 times, and liposomal mixtures are made;
(b) by the Nano Silver and graphene of formula ratio, respective optional adsorbent, sustained release agent, magnetic component, titanium dioxide
And zinc oxide, and each solubilizer of surplus, emulsifying agent, antioxidant, anti-polymerizer and water mixing, the temperature of mixing is 50
DEG C, homogeneous, through super-voltage micro jet circular treatment, processing pressure 250MPa, circular treatment number is 1 time, and nanometer is made
Grain solution;
(c) liposomal mixtures obtained by step (a) and the nanoparticles solution obtained by step (b) are mixed, through superelevation
After pressing microjet circular treatment, composite nano germicide is obtained.
Embodiment 12
The preparation method for the composite nano germicide that embodiment 4-7 is provided, comprises the following steps:
(a) by the base oil of formula ratio, protein, phosphatide, polysaccharide, cholesterol, vitamin, the increasing of respective 1/2 formula ratio
Solvent, emulsifying agent, antioxidant, anti-polymerizer and water mixing, the temperature of mixing is 50 DEG C, homogeneous, is followed through super-voltage micro jet
Ring processing, processing pressure 200MPa, circular treatment number are 2 times, and liposomal mixtures are made;
(b) by the Nano Silver and graphene of formula ratio, respective optional adsorbent, sustained release agent, magnetic component, titanium dioxide
And zinc oxide, and each solubilizer of surplus, emulsifying agent, antioxidant, anti-polymerizer and water mixing, the temperature of mixing is 70
DEG C, homogeneous, through super-voltage micro jet circular treatment, processing pressure 250MPa, circular treatment number is 3 times, and nanometer is made
Grain solution;
(c) liposomal mixtures obtained by step (a) and the nanoparticles solution obtained by step (b) are mixed, through superelevation
After pressing microjet circular treatment, composite nano germicide is obtained.
Embodiment 13
The preparation method for the composite nano germicide that embodiment 8 provides, comprises the following steps:
(a) by the base oil of formula ratio, protein, phosphatide, polysaccharide, cholesterol, vitamin, the increasing of respective 1/2 formula ratio
Solvent, emulsifying agent, antioxidant, anti-polymerizer and water mixing, the temperature of mixing is 50 DEG C, homogeneous, is followed through super-voltage micro jet
Ring processing, processing pressure 180MPa, circular treatment number are 3 times, and liposomal mixtures are made;
(b) by the Nano Silver and graphene of formula ratio, respective optional adsorbent, sustained release agent, magnetic component, titanium dioxide
And zinc oxide, and each solubilizer of surplus, emulsifying agent, antioxidant, anti-polymerizer and water mixing, the temperature of mixing is 60
DEG C, homogeneous, through super-voltage micro jet circular treatment, processing pressure 180MPa, circular treatment number is 3 times, and nanometer is made
Grain solution;
(c) liposomal mixtures obtained by step (a) and the nanoparticles solution obtained by step (b) are mixed, through superelevation
After pressing microjet circular treatment, composite nano germicide is obtained.
Comparative example 1
This comparative example provides a kind of composite nano germicide, except being not added with graphene in the raw material of embodiment 4, its
Remaining raw material and dosage and preparation method are same as Example 4.
Comparative example 2
This comparative example provides a kind of composite nano germicide, except be not added with the raw material of embodiment 4 antioxidant and
Anti- polymerizer, remaining raw material and dosage and preparation method are same as Example 4.
For the technique effect of checking embodiment and comparative example, ad hoc following experimental example.
Experimental example 1
Surface is weighed respectively uniformly coated with Escherichia coli (Escherichi a coli, 8099), staphylococcus aureus
The training of (Staphylococcusaureus, ATCC 6538), Candida albicans (Canidia albicans, ATCC 10331)
Plate is supported, the experiment scraps of paper for the composite nano germicide for being supported with each embodiment of same concentrations and comparative example are gently positioned over bacterium
The centre position of culture plate.Then, by culture plate as in 37 DEG C of incubators, observation inhibition zone is taken out in culture after 48 hours
Size.Inhibition zone is bigger, illustrates that antibacterial effect is better, specific testing result is as shown in table 1.
The antibacterial testing result of 1 each embodiment of table and comparative example
It can be seen from Table 1 that the composite nano germicide that various embodiments of the present invention provide is for Escherichia coli, golden yellow
Staphylococcus and Candida albicans are respectively provided with good antibacterial effect.
Wherein, embodiment 5-7 and comparative example 1-2 is the control experiment of embodiment 4.Compared with Example 4, embodiment 5
In adsorbent and sustained release agent are with the addition of on the basis of the raw material of embodiment 4, embodiment 6 is added on the basis of the raw material of embodiment 4
Adsorbent, sustained release agent, titanium dioxide and zinc oxide, embodiment 6 with the addition of on the basis of the raw material of embodiment 4 adsorbent, slow
Release agent and magnetic component.Adsorbent, sustained release agent, titanium dioxide, zinc oxide and magnetic component pair it can be seen from data in table 1
Has the effect of improving in composite nano germicide anti-microbial property.
Comparative example 1 is not added with graphene on the basis of the raw material of embodiment 4.As can be seen from the data in the table, comparative example 1
Antibacterial effect is far below the antibacterial effect of embodiment 4.This explanation graphene with Nano Silver is compound is obviously improved its antibacterial effect.
Comparative example 2 is not added with antioxidant and anti-polymerizer on the basis of the raw material of embodiment 4.The shortage of antioxidant and anti-polymerizer, no
Beneficial to the raising of composite nano germicide stability, so as to be unfavorable for the performance of antibacterial effect.
Experimental example 2
It is special by composite nano germicide system further to verify the antibacterial effect of composite nano germicide provided by the invention
The form of medicament is made, is applied at sufferer, and will be used before composite nano germicide with being contrasted afterwards at sufferer, is had
Body is as shown in figures 1 to 6.
By Fig. 1-6, it is apparent that composite nano germicide for mitigate human body face acne, epifolliculitis, foot or
Hand fungal infection, psoriasis etc. have certain effectiveness, and it is good that this illustrates that composite nano germicide provided by the invention has
Antibacterial effect.
Finally it should be noted that:Various embodiments above is merely illustrative of the technical solution of the present invention, rather than its limitations;To the greatest extent
The present invention is described in detail with reference to foregoing embodiments for pipe, it will be understood by those within the art that:Its according to
The technical scheme described in foregoing embodiments can so be modified, either which part or all technical characteristic are entered
Row equivalent substitution;And these modifications or replacement, the essence of appropriate technical solution is departed from various embodiments of the present invention technology
The scope of scheme.