CN102846661B - Compound nano-silver emulsifiable paste and preparation method thereof - Google Patents
Compound nano-silver emulsifiable paste and preparation method thereof Download PDFInfo
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- CN102846661B CN102846661B CN201210293061.2A CN201210293061A CN102846661B CN 102846661 B CN102846661 B CN 102846661B CN 201210293061 A CN201210293061 A CN 201210293061A CN 102846661 B CN102846661 B CN 102846661B
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Abstract
The invention discloses compound nano-silver emulsifiable paste and a preparation method thereof. The compound nano-silver emulsifiable paste is O/W or W/O type emulsifiable paste prepared from nano-silver and zinc oxide as main drugs by certain processes. Nano-silver has strong antibacterial effects and a wide antimicrobial spectrum and causes drug resistance of bacteria difficultly. Zinc oxide has convergence and wound heal promotion effects. The compound nano-silver emulsifiable paste prepared from nano-silver and zinc oxide has anti-infection and wound heal promotion effects. The compound nano-silver emulsifiable paste has treatment advantages of moisture exposed burn ointment and sulfadiazine silver cream and avoids treatment defects and adverse reactions of moisture exposed burn ointment and sulfadiazine silver cream. The compound nano-silver emulsifiable paste can be used for anti-infection treatment on burns and scalds, infected wounds caused by physical mechanical damages, and chronic surface ulcers, and promotion of wound heal. The compound nano-silver emulsifiable paste can also be used for treatment on skin diseases such as sores, carbuncles, furuncles, erysipelas and tinea caused by bacteria, fungi and viruses.
Description
Technical field
The present invention relates to field of medicaments, be specifically related to a kind of compound recipe nanometer silver emulsifiable paste and preparation method thereof.
Background technology
Burn and scald is more common clinically, particularly very common especially in wartime, and concerning burned patient, medicine for external use has important effect to the infection, the wound surface antibacterial that prevent wound surface to the healing of deep layer invasion and promotion wound surface.The medicine for external use for the treatment of burn and scald has the Chinese medicine taking moist expose burn ointment as representative and the Western medicine taking Sulfadiazine Silver Cream as representative at present, and the former can be wound surface a kind of moist environment that is conducive to wound surface regeneration is provided, but its antibacterial action is poor; The dual antibacterial action of the latter Yin Yin and sulfadiazine, and there is good anti-infectious function, but the existence of sulfanilamide group makes this medical instrument have the local untoward reaction of sulfadiazine, and percutaneous has again the systemic adverse reactions of sulfadiazine after absorbing; This medicine still has the untoward reaction of deepening wound surface, delayed healing in addition, and the clinical fastbacteria of having found silver sulfadiazine.Clinical in the urgent need to not only there is anti-infectious function but also there is wound healing effect and medicine that untoward reaction is little for the treatment of empyrosis wound surface.
Summary of the invention
For the problems referred to above, the invention provides a kind of compound recipe nanometer silver emulsifiable paste, this emulsifiable paste is O/W type emulsifiable paste or the w/o type emulsifiable paste of making through certain preparation process as principal agent taking nanometer silver and zinc oxide, nanometer silver antimicrobial effect is strong, has a broad antifungal spectrum, antibacterial are difficult for producing drug resistance to it, zinc oxide has convergence and promotes the effect of wound healing, two medicines are share to the emulsifiable paste of making, existing anti-infectious function has again the effect of wound healing of promotion, and the treatment advantage that this emulsifiable paste combines moist expose burn ointment and Sulfadiazine Silver Cream has been avoided again deficiency and the untoward reaction of its treatment.This emulsifiable paste can be used for burn and scald, physical mechanical damages the infective wound surface causing, anti-infective therapy and the promotion wound healing of chronic surface ulcers (venous ulcer, pressure ulcer etc.).
The synthesis technique of nanometer silver and purification process thereof, referring to application number: 201010566598.2, utilize the method and technique can prepare highly purified nanometer silver, their full text content is all included in this description as a reference, just look like its in full content repeated description is excessively the same in this manual.
For the ease of understanding the present invention, description of the present invention is stated synthesis technique and the purification process thereof of nanometer silver according to the concise and to the point example of content in above-mentioned patent application.The preparation of nanometer silver and purifying process comprise the steps: silver nitrate to be dissolved in that in deionized water, to make weight concentration be 1 × 10
-4molL
-1-4 × 10
-2molL
-1solution, under stirring, add the ammonia of weight ratio 25%-28%, make to form two amminos silver solution, the concentration of ammonia in solution is 1 × 10
-3molL
-1-2.5 × 10
-2molL
-1; Reducing agent (as maltose) is dissolved in in deionized water, to make concentration be 1 × 10
-3molL-1
-1× 10
-1molL
-1solution, 30-80 DEG C, reductant solution is slowly joined in two amminos silver solution it is fully reacted under stirring, make nanometer silver and other separating substances with " two step method of purification ", obtain highly purified nanometer silver." two step method of purification " successively removed impurity by two times of ultrafiltration and obtained high-purity nano silver, ultrafiltration is for the first time that reaction mixture is carried out to ultrafiltration, in the concentrated solution obtaining after ultrafiltration, contain nanometer silver, in the ultrafiltrate obtaining, except nanometer silver, also contain impurity, nanometer silver in ultrafiltrate is less than the aperture of ultrafilter membrane because of particle diameter, in ultra-filtration process, be lost in ultrafiltrate, for the nanometer silver that reclaims this part loss can be adopted with the following method: add nitric acid and stir in ultrafiltrate simultaneously, nano silver particles is reunited grows up, then add alkali neutralization, finally carry out ultrafiltration for the second time, the concentrated solution that the concentrated solution containing nanometer silver obtaining after ultrafiltration and ultrafiltration are for the first time obtained merges.
Concrete, accurately take 360.3g maltose, be dissolved in 50L deionized water; Accurately take 17g silver nitrate, be dissolved in 50L deionized water, under agitation 62.5ml ammonia is joined in silver nitrate solution, form two ammino silver solution; 40 DEG C, maltose solution is slowly added in two amminos silver solution the two is fully reacted under stirring, reaction mixture is carried out to ultrafiltration (ultrafiltration for the first time), in ultra-filtration process, collect containing the ultrafiltrate of nanometer silver for subsequent use, and measure the pH of ultrafiltrate in good time, in the time that ultrafiltrate pH is no longer alkalescence, collect concentrated solution, stop ultrafiltration (ultrafiltration for the first time completes).Measure the pH of the above-mentioned ultrafiltrate containing nanometer silver, under stirring to above-mentioned containing adding in the ultrafiltrate of nanometer silver nitric acid (volume ratio of 16mol/L concentrated nitric acid and deionized water be 1: 1 formulated) 30ml-2000ml to make its pH to 3-6, place 20 minutes-2400 hours, under stirring, add wherein sodium hydroxide to make pH value be increased to the level while not adding nitric acid, the above-mentioned ultrafiltrate containing nanometer silver is carried out to ultrafiltration (ultrafiltration for the second time), in ultra-filtration process, detect the pH value of ultrafiltrate in good time, in the time that pH value is no longer alkalescence, collect concentrated solution, stop ultrafiltration (ultrafiltration for the second time completes), the concentrated solution that this ultrafiltration obtained merges with the concentrated solution of ultrafiltration gained for the first time and obtains the solution containing high-purity nano silver.
The invention provides on this basis a kind of compound recipe nanometer silver emulsifiable paste that has not yet to see report, high-efficiency low-toxicity and preparation method thereof.
1, described compound recipe nanometer silver emulsifiable paste is made up of following component, and each constituent content is as follows:
Content of nanometer silver 60-100 μ gmL in described nano-silver water solution
-1.
One of above-mentioned compound recipe nanometer silver cream preparation method comprises the steps:
Water preparation: all or part of component of getting in glycerol, Calcium Disodium Versenate and oxybenzene second fat adds in nano-silver water solution, is heated to 45-95 DEG C, stirs evenly, for subsequent use;
Oil phase preparation: get stearic acid, octadecanol, 2,6 ditertiary butyl p cresol, laurocapram and mix with all or part of component in liquid Paraffin, be heated to 45-96 DEG C, stir evenly, for subsequent use;
Under stirring immediately, water is added in oil phase or by oil phase and added in water, then add triethanolamine, limit edged stirs, and complete when emulsifying, gradation adds zinc oxide fine powder, continues to be stirred to coagulate and obtain compound recipe nanometer silver emulsifiable paste.
The mixed mixing speed of water and oil phase is 30-160rpm.
Two of above-mentioned compound recipe nanometer silver cream preparation method comprises the steps:
All components are placed in same container and are heated to 45-95 DEG C, then stop heating, be stirred to and coagulate and obtain compound recipe nanometer silver emulsifiable paste.
Above-mentioned compound recipe nanometer silver emulsifiable paste is O/W type or w/o type.
Above-mentioned compound recipe nanometer silver emulsifiable paste can not contain Calcium Disodium Versenate and/or oxybenzene second fat.
Above-mentioned compound recipe nanometer silver emulsifiable paste can not contain 2,6 ditertiary butyl p cresol and/or laurocapram.
In above-mentioned compound recipe nanometer silver emulsifiable paste, can also contain one or more in lanoline, vaseline, oleic acid, hexadecanol, Myrj 45, sodium lauryl sulphate, sodium sulfite.
2, compound recipe nanometer silver emulsifiable paste can also be made up of following component, and each constituent content is as follows:
Vaseline 350g, oleic acid 20g, hexadecanol 10g, octadecanol 30g, Myrj 45 21g, glycerol 100g, ethyl hydroxybenzoate 2g, nano-silver water solution 256mL, zinc oxide 20g, surplus is purified water or distilled water, altogether 1000g processed.Content of nanometer silver 60-100 μ gmL in described nano-silver water solution
-1.
Preparation method:
Get vaseline, oleic acid, hexadecanol, octadecanol and be mixed into oil phase; Separately get Myrj 45, glycerol, ethyl hydroxybenzoate, nano-silver water solution, zinc oxide and be mixed into water, biphase putting respectively in appropriate containers, be heated to after fusing or dissolving, keep 45-95 DEG C, under agitation water is slowly added in oil phase, and solidify with adding with being stirred to by same direction, obtain emulsifiable paste.
3, compound recipe nanometer silver emulsifiable paste can also be made up of following component, and each constituent content is as follows:
Sodium lauryl sulphate 9g, hexadecanol 81g, liquid paraffin 60g, vaseline 150g, sodium sulfite 3g, 2,6 ditertiary butyl p cresol 50g, glycerol 50g, nano-silver water solution 300mL, zinc oxide 30g, surplus is purified water or distilled water, altogether 1000g processed.Content of nanometer silver 60-100 μ gmL-1 in described nano-silver water solution.Does each constituent content need a scope?
Preparation method:
(1) oil phase preparation: get hexadecanol, liquid paraffin and vaseline, heat fused, in the time that temperature arrives 45-95 DEG C, adds 2,6 ditertiary butyl p cresol to dissolve.
(2) water preparation: get glycerol, zinc oxide and nano-silver water solution and mix, while being heated to 45-95 DEG C, add sodium sulfite and sodium lauryl sulphate, dissolve.
(3) oil phase is under agitation slowly added in water, be stirred to solidifyingly, obtain emulsifiable paste.
Nanometer silver is that particle diameter is accomplished to nano level argent simple substance, has very excellent characteristic at aspects such as electricity, optics and catalysis.Due to quantum effect, small-size effect with there is great specific surface area, nanometer silver has the incomparable antibacterial activity of traditional inorganic antiseptic, the disinfecting and sterilizing functions that silver is had has had qualitative leap, and the nanometer silver of minute quantity can produce powerful bactericidal action.In metal mold nano material, the antibacterial ability of nanometer silver is strong more than metals such as copper, zinc, lithium, magnesium.Its Antibacterial Mechanism may be: and the Peptidoglycan exposing on bacteria cell wall reaction, produce moldable compound, stop pathogenic bacteria activity, kill pathogens; Nano level particle diameter makes it directly enter thalline, with oxygen metabolism enzyme (SH) combination, thalline is suffocated and die etc.
Nanometer silver has strong inhibition and killing action to hundreds of pathogenic microorganism such as antibacterial, fungus, viruses, broad-spectrum sterilization and without any drug resistance, and can promote the healing of wound, growth and the impaired epithelial reparation of cell, skin is also found no to any stimulation.Explanation in public health bureau of U.S. nineteen ninety " about the investigation report of silver-colored toxicity ": " silver to human body without obvious toxic-side effects; Nanometer silver is local application, and silver content is few, is safest administering mode.Investigate and find through test, mice is at oral maximum tolerated dose 925mgkg-1, while being equivalent to 4625 times of clinical using dosage, without any toxic reaction; In the skin irritation test of rabbit, do not find any irritant reaction " yet.Nanometer silver is the natural antibacterial agent of latest generation.
Zinc oxide has the effect of good promotion wound healing.
The compound recipe nanometer silver emulsifiable paste that the application provides can be used for the anti-infective therapy of burn and scald, knife injury, gunshot wound etc., have antibacterial, promote the effect such as wound healing, be not only applicable at ordinary times, be more suitable for wartime, the particularly wartime, to rapid infection control, recover as early as possible wounded's health, reduce combat casualty and have great importance.
Detailed description of the invention
For the ease of understanding, below will be described in detail the present invention by specific embodiment.It needs to be noted, these descriptions are only exemplary descriptions, do not form limitation of the scope of the invention.In following proposal, the content of nanometer silver of nanometer silvering solution is 60-100 μ gmL
-1.
Embodiment 1
Component and the content of compound recipe nanometer silver emulsifiable paste: stearic acid 59.1g, octadecanol 59.1g, liquid Paraffin 118.2g, oxybenzene second fat 0.5g, triethanolamine 4.6g, laurocapram 10.1g, 2,6-ditertbutylparacresol 0.5g, Calcium Disodium Versenate 0.5g, glycerol 228g, nanometer silvering solution 232.6mL, zinc oxide 40g, adds water to 1000g.
Preparation method:
(1) water preparation: get zinc oxide, glycerol, Calcium Disodium Versenate and oxybenzene second fat and join in proper amount of nano silver solution, be heated to 80 DEG C, stir evenly, for subsequent use.
(2) oil phase preparation: get stearic acid, octadecanol, 2,6 ditertiary butyl p cresol, laurocapram and mix with liquid Paraffin, be heated to 75 DEG C, stir evenly.
(3) with adding oil phase by water, then add triethanolamine, stop heating, rapid stirring immediately, in the time that temperature is down to 50 DEG C, continues to be stirred to solidifying, obtains compound recipe nanometer silver emulsifiable paste.
Embodiment 2
Component and the content of compound recipe nanometer silver emulsifiable paste: stearic acid 59.1g, octadecanol 59.1g, liquid Paraffin 118.2g, triethanolamine 4.6g, glycerol 228g, nanometer silvering solution 200mL, zinc oxide 50g, adds water to 1000g.
Preparation method:
(1) water preparation: get glycerol, nanometer silver solution mixing, be heated to 80 DEG C, stir evenly, for subsequent use.
(2) oil phase preparation: get stearic acid, octadecanol, liquid Paraffin mixing, be heated to 75 DEG C, stir evenly, for subsequent use.
(3) with adding oil phase by water, then add triethanolamine, be stirred to emulsifying complete, gradation adds zinc oxide fine powder, stirs, and lets cool to room temperature, obtains compound recipe nanometer silver emulsifiable paste.
Embodiment 3
Component and the content of compound recipe nanometer silver emulsifiable paste: stearic acid 59.1g, octadecanol 59.1g, liquid Paraffin 118.2g, triethanolamine 4.6g, laurocapram 10.1g, 2,6 ditertiary butyl p cresol 0.5g, Calcium Disodium Versenate 0.5g, glycerol 228g, nanometer silvering solution 300mL, zinc oxide 45g, adds water to 1000g.
Preparation method:
(1) water preparation: get glycerol, Calcium Disodium Versenate, nanometer silver solution mixing, be heated to 80 DEG C, stir evenly, for subsequent use.
(2) oil phase preparation: get stearic acid, octadecanol, 2,6 ditertiary butyl p cresol, laurocapram and mix with liquid Paraffin, be heated to 75 DEG C, stir evenly, for subsequent use.
(3) with slowly adding in oil phase by water, with adding with stirring, then add triethanolamine, complete to emulsifying, gradation adds zinc oxide fine powder, stirs, and is chilled to room temperature, obtains compound recipe nanometer silver emulsifiable paste.
Embodiment 4
Component and the content of compound recipe nanometer silver emulsifiable paste: stearic acid 59.1g, octadecanol 59.1g, liquid Paraffin 118.2g, triethanolamine 4.6g, laurocapram 10.1g, 2,6 ditertiary butyl p cresol 0.5g, glycerol 228g, nanometer silvering solution 238mL, zinc oxide 48g, adds water to 1000g.
Preparation method:
(1) water preparation: get zinc oxide, glycerol, nanometer silver solution mixing, be heated to 80 DEG C, stir evenly, for subsequent use.
(2) oil phase preparation: get stearic acid, octadecanol, 2,6 ditertiary butyl p cresol, laurocapram and mix with liquid Paraffin, be heated to 75 DEG C, stir evenly, for subsequent use.
With slowly adding oil phase by water, then add triethanolamine, limit edged stirs, complete to emulsifying, stops heating, continues to be stirred to coagulate and obtain compound recipe nanometer silver emulsifiable paste.
Embodiment 5
Component and the content of compound recipe nanometer silver emulsifiable paste: stearic acid 59.1g, octadecanol 59.1g, liquid Paraffin 118.2g, triethanolamine 4.6g, 2,6 ditertiary butyl p cresol 0.5g, glycerol 228g, nanometer silvering solution 232.6mL, zinc oxide 36g, adds water to 1000g.
Preparation method:
(1) water preparation: get glycerol, nanometer silver solution mixing, be heated to 75 DEG C, stir evenly, for subsequent use.
(2) oil phase preparation: get stearic acid, octadecanol, 2,6 ditertiary butyl p cresol and mix with liquid Paraffin, be heated to 75 DEG C, stir evenly, for subsequent use.
(3) with slowly adding oil phase by water, with adding with stirring, then add triethanolamine, continue to be stirred to emulsifying complete, be cooled to room temperature and obtain nanometer silver emulsifiable paste.
(4) get zinc oxide fine powder, add a small amount of above-mentioned nanometer silver emulsifiable paste, grind well, then the substrate of progressively increasing is to full dose, grinds well, obtain compound recipe nanometer silver emulsifiable paste.
Embodiment 6
Component and the content of compound recipe nanometer silver emulsifiable paste: stearic acid 120g, lanoline 20g, vaseline 230g, glycerol 50g, triethanolamine 20g, nanometer silver solution 298mL, zinc oxide 100g, adds water to 1000g.
Preparation method:
Get stearic acid, lanoline, vaseline, glycerol, triethanolamine, nanometer silver solution, zinc oxide and put in appropriate containers, heat and remain on 70 DEG C of left and right, be stirred to emulsifying completely in a direction and get final product.
Embodiment 7
Component and the content of compound recipe nanometer silver emulsifiable paste: laurocapram 0.5g, octadecanol 75g, stearic acid 75g, liquid paraffin 105g, triethanolamine 5g, glycerol 200g, nanometer silver solution 278mL, zinc oxide 150g, adds water to 1000g.
Preparation method:
(1) oil phase preparation: get octadecanol, stearic acid, laurocapram and liquid paraffin, heating and melting, continues to be heated to approximately 70 DEG C of temperature.
(2) water preparation: get glycerol, nanometer silver solution, zinc oxide mixing, add triethanolamine, be heated to 70 DEG C.
(3) water is slowly added in oil phase, it is complete that limit edged is stirred to emulsifying, is chilled to room temperature and get final product.
Embodiment 8
Component and the content of compound recipe nanometer silver emulsifiable paste: vaseline 350g, oleic acid 20g, hexadecanol 10g, octadecanol 30g, Myrj 45 21g, glycerol 100g, ethyl hydroxybenzoate 2g, nanometer silver solution 256mL, zinc oxide 30g, adds water to 1000g.
Preparation method:
Get vaseline, oleic acid, hexadecanol, octadecanol and be mixed into oil phase; Separately get Myrj 45, glycerol, ethyl hydroxybenzoate, nanometer silver solution and be mixed into water, biphase putting respectively in appropriate containers, be heated to after fusing or dissolving, keep 70 DEG C of left and right, under agitation water is slowly added in oil phase, and it is complete to be stirred to emulsifying by same direction, the gradation of zinc oxide fine powder is added, limit edged is stirred to mix homogeneously, is chilled to room temperature and obtains compound recipe nanometer silver emulsifiable paste.
Embodiment 9
Component and the content of compound recipe nanometer silver emulsifiable paste: sodium lauryl sulphate 9g, hexadecanol 81g, liquid paraffin 60g, vaseline 150g, sodium sulfite 3g, 2,6 ditertiary butyl p cresol 50g, glycerol 50g, nanometer silver solution 300mL, zinc oxide 20g, adds water to 1000g.
Preparation method:
(1) oil phase preparation: get hexadecanol, liquid paraffin, vaseline, heat fused, in the time that temperature arrives approximately 70 DEG C, adds 2,6 ditertiary butyl p cresol to dissolve.
(2) water preparation: get glycerol, nanometer silvering solution mixes with appropriate distilled water, while being heated to approximately 70 DEG C, adds sodium sulfite, sodium lauryl sulphate, dissolving.
(3) oil phase is under agitation slowly added in water, continue to be stirred to emulsifying complete.
(4) gradation adds zinc oxide fine powder wherein, and limit edged is stirred to mix homogeneously, is placed to room temperature and obtains compound recipe nanometer silver emulsifiable paste.
The present embodiment agents useful for same is purchased from: glycerol (lot number 090625, Hunan Er-kang Pharmaceutical Co., Ltd. produces); Calcium Disodium Versenate, oxybenzene second fat (lot number 070703, Xinning, Taishan City pharmaceutical Co. Ltd); Stearic acid (lot number 080605, Hunan Er-kang Pharmaceutical Co., Ltd.); Octadecanol (090201, Hunan Er-kang Pharmaceutical Co., Ltd.); 2,6 ditertiary butyl p cresol, laurocapram (lot number 20090216, Xing Qing chemical plant, Ruicheng, Shanxi); Liquid Paraffin (lot number 090905, Nanchang white clouds pharmaceutcal corporation, Ltd); Triethanolamine (lot number 081201, Xi Xing pharmaceutcal corporation, Ltd of Guan County); Lanoline (lot number 090805, Nanchang white clouds pharmaceutcal corporation, Ltd); Vaseline (lot number 090505, Nanchang white clouds pharmaceutcal corporation, Ltd); Oleic acid, hexadecanol, Myrj 45, sodium lauryl sulphate (lot number 071102, Hunan Er-kang Pharmaceutical Co., Ltd. produces); Sodium sulfite (industrial and commercial shop routinizes).
Claims (1)
1. a compound recipe nanometer silver emulsifiable paste, its component and content are: stearic acid 59.1g, octadecanol 59.1g, liquid Paraffin 118.2g, triethanolamine 4.6g, 2,6 ditertiary butyl p cresol 0.5g, glycerol 228g, nanometer silvering solution 232.6mL, zinc oxide 36g, adds water to 1000g; The employing following methods of described compound recipe nanometer silver emulsifiable paste prepares:
(1) water preparation: get glycerol, nanometer silver solution mixing, be heated to 75 DEG C, stir evenly, for subsequent use;
(2) oil phase preparation: get stearic acid, octadecanol, 2,6 ditertiary butyl p cresol and mix with liquid Paraffin, be heated to 75 DEG C, stir evenly, for subsequent use;
(3) with slowly adding oil phase by water, with adding with stirring, then add triethanolamine, continue to be stirred to emulsifying complete, be cooled to room temperature and obtain nanometer silver emulsifiable paste;
(4) get zinc oxide fine powder, add a small amount of above-mentioned nanometer silver emulsifiable paste, grind well, then the substrate of progressively increasing is to full dose, grinds well, obtain compound recipe nanometer silver emulsifiable paste.
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