CN108624409A - A kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent - Google Patents

A kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent Download PDF

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Publication number
CN108624409A
CN108624409A CN201810636420.7A CN201810636420A CN108624409A CN 108624409 A CN108624409 A CN 108624409A CN 201810636420 A CN201810636420 A CN 201810636420A CN 108624409 A CN108624409 A CN 108624409A
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graphene oxide
detergent
silver
prepared
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曾宣
吴珍
周永青
赵丹丹
江良梁
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/37—Mixtures of compounds all of which are anionic
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16—Heavy metals; Compounds thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/40—Liliopsida [monocotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9789—Magnoliopsida [dicotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9794—Liliopsida [monocotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00—Barrier 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
    • A61Q17/005—Antimicrobial preparations
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • A61Q19/10—Washing or bathing preparations
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/08—Silicates
    • C—CHEMISTRY; METALLURGY
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    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/10—Carbonates ; Bicarbonates
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    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/20—Organic compounds containing oxygen
    • C11D3/22—Carbohydrates or derivatives thereof
    • C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
    • C11D3/225—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin etherified, e.g. CMC
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    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/34—Organic compounds containing sulfur
    • C11D3/3472—Organic compounds containing sulfur additionally containing -COOH groups or derivatives thereof
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    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/38—Products with no well-defined composition, e.g. natural products
    • C11D3/382—Vegetable products, e.g. soya meal, wood flour, sawdust
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    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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    • C11D3/42—Brightening agents ; Blueing agents
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    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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    • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
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Abstract

The present invention proposes a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent, including following raw material is prepared：Graphene oxide silver-colored zinc nano-complex, Traditional Chinese medicine bacteriostatic composition, surfactant system, foam stabiliser, softening agent, fluorescent whitening agent, auxiliary material, the graphene oxide silver-colored zinc nano-complex are prepared by following methods：Step 1: preparing graphene oxide using improved Hummers methods, the nitration mixture of concentrated nitric acid and the concentrated sulfuric acid is added, is stirred at room temperature, filter, washs solid, be dried to obtain the graphene oxide of nitrification；Step 2: weighing step Step 1: the graphene oxide of the nitrification prepared is scattered in ethanol solution, ammonia spirit is added under ultrasonication, then the ethanol solution dissolved with silver acetate and zinc acetate is added dropwise, freeze-drying after reaction is washed repeatedly with ethyl alcohol afterwards for 24 hours, obtains graphene oxide silver-colored zinc nano-complex.Detergent clean effect provided by the invention is good, plays the role of apparent inhibiting bacteria and diminishing inflammation, has broad application prospects.

Description

A kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent
Technical field
The present invention relates to chemical industry agent technical fields, and in particular to a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent.
Background technology
With social progress and the improvement of people's living standards, house detergent demand increases, formula technique and Production technology is developed rapidly therewith.In addition with the enhancing of people's environmental consciousness, to the pass of itself and domestic hygiene health Note degree is higher and higher, is also constantly increasing to detergent product variety requirement, is being mainly reflected in consumer to detergent product Bacteria resistance function, ease of use and environmentally protective aspect.Liquid detergent with its water and electric saving, it is easy to use the advantages that, more Doted on by young man to get over, especially the liquid detergent with specific function, becomes the new lover of current detergent market.
Metal nanoparticle is dispersed in the surface of graphene, not only increases the distance between graphene sheet layer, resistance The aggregation of graphene film is stopped, and has served as the conductive channel between graphene film so that laminated film has high specific surface Product and electric conductivity.Meanwhile graphene and its derivative are remarkably improved the stabilization of nano-particle as metallic nanoparticle subcarrier Property.Therefore, with the graphene-based material of metal composite both can retained fraction itself performance, moreover it is possible to pass through synergistic effect, enhancing The characteristic of basis material simultaneously assigns some new function.Faria et al. has studied one argentum nano composite material of graphite oxide Antibacterial activity finds that composite material is only 2.5~5.0g/mL to the minimum inhibitory concentration of Pseudomonas aeruginosa.They also measured were attached The compound antibiont film in stainless steel surface to the antibacterial activity of Pseudomonas aeruginosa, as a result shows GO/Ag nanocomposites pair The inhibiting rate of attached cell is 100%, illustrates that this composite film material can inhibit the growth of microorganism adhering cell, to prevent giving birth to The formation of object film.Therefore, GO/Ag nanocomposites can be used as food packaging and Medical Devices antimicrobial coating material.Meanwhile GO/Ag nanocomposites also have prodigious potentiality in clinical and antifungal therapy.The present invention is studies have shown that graphite oxide Alkene-silver-colored zinc nanocomposite all shows significantly more antibacterial activity to various pathogen.Therefore, by graphene oxide- The effect for increasing the antibacterial anti-inflammatory of detergent in silver-colored zinc nano-complex and Traditional Chinese medicine bacteriostatic anti-inflammatory extract application detergent has Good application prospect.
Invention content
In order to solve the above technical problems, the present invention provides a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent, and provides The wherein preparation method of active ingredient graphene oxide-silver-colored zinc nano-complex and Traditional Chinese medicine bacteriostatic anti-inflammatory extract, will aoxidize stone Black alkene-silver-colored zinc nano-complex is used together with Traditional Chinese medicine bacteriostatic anti-inflammatory extract, has the function of synergy, can be played bright The effect of aobvious inhibiting bacteria and diminishing inflammation.
The present invention provides a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent, and the detergent presses quality percentage by following raw material Than being prepared：Graphene oxide-silver-colored zinc nano-complex 0.1-1%, Traditional Chinese medicine bacteriostatic composition 1-10%, surfactant body It is 10-40%, foam stabiliser 0.1-2%, softening agent 1-5%, fluorescent whitening agent 0.01-0.1%, auxiliary material 5-10%, Water complements to 100%, and 15-20 parts of Cortex Phellodendri, the Qin is prepared by following raw material in the Traditional Chinese medicine bacteriostatic composition extract 15-20 parts of skin, 10-15 parts of the bletilla striata, 10-15 parts of honeysuckle, 10-15 parts of Schisandra chinensis, 5-10 parts of cloves, 5-10 parts of kuh-seng, stone Chang 5-10 parts of Pu, 2-7 parts of guava；The surfactant system includes sodium alkyl benzene sulfonate, sodium alkyl sulfate, alkyl sulfonic acid One or more of sodium；The foam stabiliser is the castor-oil plant sodium alkoxide of sulfonation；The softening agent is quaternary, aliphatic acid One kind in ester type, right wax pattern, polyethylene, organic siliconresin type cationic softener；The fluorescent whitening agent hexichol second Auxiliary material described in alkenyl biphenyl fluorescent brightener includes sodium phosphate, silicate, soda ash, carboxymethyl cellulose, borax, peroxide One or more of sour sodium, fluorite.
As further improvement of the invention, detergent is prepared by mass percentage by following raw material：Graphite oxide Alkene-silver-colored zinc nano-complex 0.1-0.5%, Traditional Chinese medicine bacteriostatic composition 1-6%, surfactant system 20-35%, foam are stablized Agent 0.5-1%, softening agent 2-4%, fluorescent whitening agent 0.05-0.1%, auxiliary material 7-9%, water complement to 100%, in described 17-19 parts of Cortex Phellodendri, 16-19 parts of the bark of ash, bletilla striata 11-13 is prepared by following raw material in medicine bacteria inhibiting composition extract Part, 12-14 parts of honeysuckle, 11-14 parts of Schisandra chinensis, 6-8 parts of cloves, 7-10 parts of kuh-seng, 6-9 parts of grass-leaved sweetflag, 4-6 parts of guava.
As further improvement of the invention, detergent is prepared by mass percentage by following raw material：Graphite oxide Alkene-silver-colored zinc nano-complex 0.2%, Traditional Chinese medicine bacteriostatic composition 5%, surfactant system 32%, foam stabiliser 0.7%, Softening agent 3%, fluorescent whitening agent 0.07%, auxiliary material 7%, water complement to 100%, the Traditional Chinese medicine bacteriostatic composition extract 17 parts of Cortex Phellodendri, 17 parts of the bark of ash, 12 parts of the bletilla striata, 13 parts of honeysuckle, 13 parts of Schisandra chinensis, cloves are prepared by following raw material 7 parts, 8 parts of kuh-seng, 7 parts of grass-leaved sweetflag, 5 parts of guava.
As further improvement of the invention, graphene oxide-silver-colored zinc nano-complex is prepared by following methods：
Step 1: prepared by the graphene oxide of nitrification：1mol graphene oxides are prepared using improved Hummers methods, are added Enter the concentrated nitric acid of 100mL and the nitration mixture of the concentrated sulfuric acid, reaction 10h is stirred at room temperature, filtering, distilled water washs solid repeatedly, until pH It is 6 or so, is dried to obtain the graphene oxide of nitrification；
Step 2: the preparation of graphene oxide-silver-colored zinc nano-complex：1mol steps are weighed Step 1: the nitrification prepared Graphene oxide be scattered in ethanol solution, under ultrasonication be added 1.5mol/L ammonia spirits, be then added dropwise dissolved with The ethanol solution of silver acetate and zinc acetate reacts at 45 DEG C and is repeatedly freeze-dried afterwards with ethyl alcohol centrifuge washing afterwards for 24 hours, obtains oxygen Graphite alkene-silver-colored zinc nano-complex.
As further improvement of the invention, the volume ratio of concentrated nitric acid and the concentrated sulfuric acid is 1:3.
As further improvement of the invention, ultrasound condition is 700W ultrasounds 1h.
As further improvement of the invention, the substance withdrawl syndrome ratio of silver acetate and zinc acetate is 1:1.2.
As further improvement of the invention, Traditional Chinese medicine bacteriostatic composition is prepared by following methods：
Step 1: weigh Cortex Phellodendri, the bark of ash, the bletilla striata, honeysuckle, Schisandra chinensis, cloves, kuh-seng, grass-leaved sweetflag, guava dry, It crushes, sieves with 100 mesh sieve, obtain herb powder；
Step 2: according to herb powder and bionic extraction liquid mass ratio 1:10 ratio mixing, 37 DEG C of heating water baths, plastics Diaphragm seal, magneton extract 3h, and filtrate is collected in filtering, and water-bath is concentrated into 1/4 volume, collects concentrate；
Step 3: by step Step 2: in concentrate according to volume ratio 1:4 is mixed with ethyl acetate-acetone mixed solution It closes, extracts 3 times, collect organic phase, vacuum rotary steam removes solvent, obtains faint yellow color powder to get Traditional Chinese medicine bacteriostatic composition.
Improved as of the invention further, bionic extraction liquid by 0.25% sodium chloride, 0.30% pepsin and 0.025mol/L hydrochloric acid and water are formulated.
As further improvement of the invention, bionic extraction liquid pH is 4.5~6.5.
The present invention has the advantages that：
1, Chinese medical extract of the present invention is all from natural Chinese medicine material, and preparation is easy, medicine source is wide, inhibiting bacteria and diminishing inflammation effect Significantly, it and has no toxic side effect；
2, graphene oxide-silver-colored zinc nano-complex of the present invention addition with apparent fungistatic effect, with Traditional Chinese medicine bacteriostatic group It closes object to be used in mixed way, has the effect of synergy, it can be so that detergent obviously inhibits bacterium, disease in the effect of potent decontamination The deleterious pathogens such as poison protect skin health.
Description of the drawings
Fig. 1 is the preparation technology figure of graphene oxide-silver-colored zinc nano-complex；
Fig. 2 is the preparation technology flow chart of Traditional Chinese medicine bacteriostatic composition.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete description, Obviously, the embodiment described is the embodiment of the part of representative of the present invention, rather than whole embodiments, this field are general Other all embodiments that logical technical staff is obtained without making creative work belong to the protection of the present invention Range.
Improved Hummers methods prepare graphene oxide：
Step 1: weighing natural graphite powder (G) 10g, potassium peroxydisulfate 4g, phosphorus pentoxide 10g, add in the case of stirring Enter in the three-necked flask equipped with 24mL sulfuric acid, first react 3h in 60 DEG C of waters bath with thermostatic control, three-necked flask is then moved into people 25 again DEG C water bath with thermostatic control in react 5h, filter, be used in combination ionized water to clean to neutrality, dry in air, obtain pre-oxidation graphite (P- G)；
Step 2: weighing the pre-oxidation graphite of l g, it is added to the three-necked flask equipped with 25mL sulfuric acid in the case of stirring In, it puts in people's ice-water bath, after pre-oxidation graphite all dissolving, is added the potassium permanganate of 3g, react 2h, then by three-necked flask It moves in the water bath with thermostatic control of 35 DEG C of people and reacts 40min, be eventually adding deionized water, continue 35 DEG C of reaction 1h, be finally added dropwise 30% H：O：So that until being generated there is no gas, solution becomes glassy yellow.Centrifugal filtration while hot is used in combination a large amount of 5% hydrochloric acid and is gone Ionized water is cleaned to neutrality.By final sediment after the ultrasonic vibration of l h, dried for 24 hours at 90 DEG C in the culture dish of falling people Obtain the graphite oxide (GO) of sheet.
The preparation of 1 graphene oxide of embodiment-silver-colored zinc nano-complex
It carries out in accordance with the following methods：
Step 1: prepared by the graphene oxide of nitrification：1mol graphene oxides are prepared using improved Hummers methods, are added Enter the concentrated nitric acid of 100mL and the nitration mixture (volume ratio 1 of the concentrated sulfuric acid:1) reaction 10h, filtering, is stirred at room temperature, distilled water is washed repeatedly Solid is washed, until pH is 6 or so, is dried to obtain the graphene oxide of nitrification, yield 82%；
Step 2: the preparation of graphene oxide-silver-colored zinc nano-complex：1mol steps are weighed Step 1: the nitrification prepared Graphene oxide be scattered in ethanol solution, 500W ultrasound 30min, lower addition 1.5mol/L ammonia spirits, then dropwise plus Enter the ethanol solution dissolved with 1mol silver acetates and 1mol zinc acetates, is reacted at 45 DEG C after using ethyl alcohol centrifuge washing multiple afterwards for 24 hours Freeze-drying, obtains graphene oxide-silver-colored zinc nano-complex, yield 75%.
The preparation of 2 graphene oxides of embodiment-silver-colored zinc nano-complex
It carries out in accordance with the following methods：
Step 1: prepared by the graphene oxide of nitrification：1mol graphene oxides are prepared using improved Hummers methods, are added Enter the concentrated nitric acid of 100mL and the nitration mixture (volume ratio 1 of the concentrated sulfuric acid:3) reaction 10h, filtering, is stirred at room temperature, distilled water is washed repeatedly Solid is washed, until pH is 6 or so, is dried to obtain the graphene oxide of nitrification, yield 90%；
Step 2: the preparation of graphene oxide-silver-colored zinc nano-complex：1mol steps are weighed Step 1: the nitrification prepared Graphene oxide be scattered in ethanol solution, then 700W ultrasound 1h, lower addition 1.5mol/L ammonia spirits are added dropwise molten The ethanol solution for having 1mol silver acetates and 1.2mol zinc acetates reacts at 45 DEG C and uses ethyl alcohol centrifuge washing repeatedly rear cold afterwards for 24 hours It is lyophilized dry, obtains graphene oxide-silver-colored zinc nano-complex, yield 92%.
The preparation of 3 Traditional Chinese medicine bacteriostatic composition of embodiment
Raw material forms：20 parts of Cortex Phellodendri, 20 parts of the bark of ash, 15 parts of the bletilla striata, 15 parts of honeysuckle, 15 parts of Schisandra chinensis, 10 parts of cloves, hardship 10 parts of ginseng, 10 parts of grass-leaved sweetflag, 7 parts of guava.
It follows the steps below：
Step 1: weigh Cortex Phellodendri, the bark of ash, the bletilla striata, honeysuckle, Schisandra chinensis, cloves, kuh-seng, grass-leaved sweetflag, guava dry, It crushes, sieves with 100 mesh sieve, obtain herb powder；
Step 2: according to herb powder and bionic extraction liquid weight ratio 1:10 ratio mixing, bionic extraction liquid is by 0.2% Sodium chloride, 0.20% pepsin and 0.02mol/L hydrochloric acid and water are formulated, 6.7,37 DEG C of heating water baths of pH, and plastics are thin Film seals, and magneton extracts 3h, and filtrate is collected in filtering, and water-bath is concentrated into 1/4 volume, collects concentrate；
Step 3: by step Step 2: in concentrate according to volume ratio 1:4 is mixed with ethyl acetate-acetone mixed solution It closes, extracts 3 times, collect organic phase, vacuum rotary steam removes solvent, obtains faint yellow color powder to get Traditional Chinese medicine bacteriostatic composition, obtain Rate is 63%.
The preparation of 4 Traditional Chinese medicine bacteriostatic composition of embodiment
Raw material forms：17 parts of Cortex Phellodendri, 17 parts of the bark of ash, 12 parts of the bletilla striata, 13 parts of honeysuckle, 13 parts of Schisandra chinensis, 7 parts of cloves, hardship 8 parts of ginseng, 7 parts of grass-leaved sweetflag, 5 parts of guava.
It follows the steps below：
(1) Cortex Phellodendri, the bark of ash, the bletilla striata, honeysuckle, Schisandra chinensis, cloves, kuh-seng, grass-leaved sweetflag, guava is weighed to dry, crush, It sieves with 100 mesh sieve, obtains herb powder；
Step 2: according to herb powder and bionic extraction liquid weight ratio 1:10 ratio mixing, bionic extraction liquid is by 0.2% Sodium chloride, 0.20% pepsin and 0.02mol/L hydrochloric acid and water are formulated, 6.7,37 DEG C of heating water baths of pH, and plastics are thin Film seals, and magneton extracts 3h, and filtrate is collected in filtering, and water-bath is concentrated into 1/4 volume, collects concentrate；
Step 3: by step Step 2: in concentrate according to volume ratio 1:4 is mixed with ethyl acetate-acetone mixed solution It closes, extracts 3 times, collect organic phase, vacuum rotary steam removes solvent, obtains faint yellow color powder to get Traditional Chinese medicine bacteriostatic composition, obtain Rate is 63%.
A kind of preparations of graphene oxide inhibiting bacteria and diminishing inflammation detergent of embodiment 5-9
The combined amount that is respectively formed according to table 1 configures.
1 embodiment 5-9 of table respectively forms list of ingredients
First, after sodium alkyl benzene sulfonate and sodium alkyl sulfate being used as to the water dilution most probably for the amount that balance uses, With in the sulfuric acid of 0.2mol/L and adjustment pH to 7.5.Then, graphene oxide-silver-colored zinc nano-complex is added, ultrasonic disperse is equal It is even.Then, other whole components are mixed thereto, and uniform liquid is stirred at about 50 DEG C.Then, 0.2mol/L is added Sulphur acid for adjusting pH be 7.0 or so, finally add water be adjusted to 100%, be configured to each group inhibiting bacteria and diminishing inflammation containing graphene oxide and wash Wash agent.
The low-temperature stability of 1 liquid detergent of test example is evaluated
Experimental subjects：Liquid detergent prepared by embodiment 5-9, the Finish detergent of market purchase, carving board detergent, Super detergent.
For the liquid detergent of embodiment 5-9, the evaluation of low-temperature stability is carried out by evaluation method as shown below, As a result as shown in table 2-5.It takes in each liquid detergent 50mL to sample bottle, is respectively placed in 5 DEG C of thermostat, 0 DEG C of perseverance In warm slot, -5 DEG C of thermostat and -10 DEG C of thermostat, after 1 month, its appearance of visual observations passes through following evaluation bases Standard is evaluated.
Evaluation result indicates：V star：Under 5 DEG C, 0 DEG C, -5 DEG C and -10 DEG C of whole temperature conditions, it is transparent or without at Divide sedimentation；IV star：Under 5 DEG C, 0 DEG C and -5 DEG C three temperature conditions, it is transparent or without ingredient settle；III star：5 DEG C and 0 DEG C of temperature Under the conditions of degree, it is transparent or without ingredient settle；II star：Under 5 DEG C of temperature condition, it is transparent or without ingredient settle；I star：It is impermeable Bright or precipitation or solidification.
It the results are shown in Table 2.
The evaluation table of 2 embodiment 5-10 low-temperature stabilities of table
It can be seen that graphene oxide inhibiting bacteria and diminishing inflammation detergent prepared by the embodiment of the present invention 6 has good low temperature steady Qualitative, each composition and ratio is coordinated, still transparent no precipitation under the conditions of -10 DEG C, hence it is evident that better than the detergent of market purchase.
2 liquid detergent of test example freezes restoration evaluation
It takes in each liquid detergent 50mL to sample bottle, close the lid sealing.Liquid scrubbing will be accommodated under the state After the sample bottle of agent stands 12 hours at -25 DEG C, 12 hours are stood at 0 DEG C, 6 cycles is carried out continuously, observes each cycle In liquid detergent under 0 DEG C of state solid or solidification whether is precipitated.Then, not have in the liquid detergent under 0 DEG C of state There are precipitation or solidification and ensure that company's cycle-index of liquid stability is index, the restoration of freezing of liquid detergent is carried out Evaluation.Its result (the continuous cycle-index for ensuring liquid stability) is as shown in table 3.
3 embodiment 5-10 of table freezes restoration evaluation table
Embodiment Freeze restoration evaluation result
5 1
6 6
7 3
8 2
9 0
Finish detergent 2
Carve board detergent 2
Super detergent 1
It can be seen that graphene oxide inhibiting bacteria and diminishing inflammation detergent prepared by the embodiment of the present invention 6 to freeze restoration good, respectively Composition and ratio is coordinated, and 6 multigelations are still precipitated without apparent solid, and does not dissolve situation without there is solidification, hence it is evident that is better than The detergent of market purchase.
3 bacteriostatic experiment of test example
1, for trying strain：Escherichia coli, staphylococcus aureus, Escherichia coli, bacillus subtilis, Candida albicans Bacterium.
2, for reagent product：The Chinese medicine of graphene oxide inhibiting bacteria and diminishing inflammation detergent, the preparation of embodiment 4 prepared by embodiment 6 carries Graphene oxide-silver-colored zinc nano-complex solution prepared by object solution (being configured to equal size solution), embodiment 2 is taken (to be configured to Equal size solution), commercially available Safeguard protect antibacterial detergent, the antibacterial detergent of commercially available droplet dew only.
3, the preparation of culture medium：
LB liquid medium：Peptone 10g, yeast powder 5g, NaCl 10g add pure water to 1000m l, adjust pH value and reach 7.0；
LB solid mediums：Beef extract 3g, peptone 10g, yeast powder 5g, NaC1 10g, 15~20g of agar, add pure Water adjusts pH value to 7.0 autoclave sterilizations, makes culture medium to 1000mL；
Culture dish and test tube are wrapped with newspaper, solid medium is prepared according to formula, high pressure is then put into together and goes out It sterilizes in bacterium pot.Tablet is made in the solid medium culture dish of falling people, liquid aglucon pours into test tube.
4, the preparation of bacteria suspension：
Escherichia coli, staphylococcus aureus, Escherichia coli, bacillus subtilis, white are read with tablet setting-out method Pearl bacterium is inoculated in respectively on LB solid mediums, is sealed with sealed membrane, is set for 37 DEG C and is cultivated reactivated bacteria for 24 hours in biochemical cultivation case, After activation, with the bacterium of the same bacterium colony of oese picking, it is inoculated in the test tube equipped with LB liquid medium, is subsequently placed in gas bath 37 DEG C of culture 48h are used as experimental strain in constant-temperature table.
5, the experiment of drug fungistatic effect：
After experimental strain culture is good, start bacteriostatic experiment on superclean bench.Experimental strain is shaken up, liquid-transfering gun is used 50 μ L bacteria suspensions are pipetted on the tablet made, tiling smoothens, 5 kinds of experimental bacterias, each applies 30 tablets, then will be sterilized Oxford cup is equidistantly placed on agar surface, quiet on super-clean bench to put 10min after all sequencing per 6, ware.It is sterilized with 1mL Liquid-transfering gun draws 200 μ L of target liquid, injects in the Oxford cup set, different detergent in 5 Oxford cups note people 5 in every ware, Another Oxford cup is injected the 200 μ L of bacterium pure water that gone out and is compared, and is then sealed with sealed membrane is careful.Each detergent corresponds to each Bacterium is cooked tablet respectively, and it is anti-to do graphene oxide inhibiting bacteria and diminishing inflammation detergent solution (n=25) prepared by embodiment 6 for totally 25 tablets Bacterium is control group with sterile pure water, and same 25 tablets do Chinese medical extract solution (n=25) antibacterial of the preparation of embodiment 4, is used Sterile pure water is control group, and 25 tablets do graphene oxide-silver-colored zinc nano-complex solution (n=25) of the preparation of embodiment 2 Antibacterial is control group with sterile pure water, and 25 tablets do Safeguard and protect antimicrobial cleaning agent solution (n=25) antibacterial only, and use is sterile Pure water is control group, and 25 tablets do the antibacterial detergent solution of droplet dew (n=25) antibacterial, are control group with sterile pure water.Later It is placed in 37 DEG C of biochemical cultivation cases the bacterial growth situation cultivated and observed afterwards for 24 hours in culture dish, is used in combination micrometer to correspond to measurement each The diameter and record of a processing group and control group inhibition zone, effective to be denoted as "+", no effect is denoted as "-", and it is total to count bacterium colony It counts, compared with the control group fungistatic effect.
Experimental result is shown in Table 4 and table 5.
The fungistatic effect table of 4 five kinds of detergent of table
The antibacterial result table of 5 five kinds of detergent of table
By the above experimental result it is found that graphite oxide prepared by Chinese medical extract solution and embodiment 2 prepared by embodiment 4 Alkene-silver-colored zinc nano-complex solution has apparent antibacterial and bacteriostasis, but respectively only to bacillus subtilis, Candida albicans It is obvious with escherichia coli, the inhibiting effect of staphylococcus aureus, two kinds of ingredients are added in detergent, Neng Gouming It is aobvious to inhibit five kinds of bacteriums, have the function of synergy.Meanwhile graphene oxide inhibiting bacteria and diminishing inflammation prepared by the embodiment of the present invention 6 Detergent protects antibacterial detergent and the antibacterial detergent of droplet dew only compared to commercially available Safeguard, and scope of restraining fungi is wider, better bright It is aobvious.
Those skilled in the art is not under conditions of departing from the spirit and scope of the present invention of claims determination, also Various modifications can be carried out to the above content.Therefore the scope of the present invention is not limited in above explanation, but by The range of claims determines.

Claims (10)

1. a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent, which is characterized in that the detergent presses quality percentage by following raw material Than being prepared：Graphene oxide-silver-colored zinc nano-complex 0.1-1%, Traditional Chinese medicine bacteriostatic composition 1-10%, surfactant body It is 10-40%, foam stabiliser 0.1-2%, softening agent 1-5%, fluorescent whitening agent 0.01-0.1%, auxiliary material 5-10%, Water complements to 100%, and 15-20 parts of Cortex Phellodendri, the Qin is prepared by following raw material in the Traditional Chinese medicine bacteriostatic composition extract 15-20 parts of skin, 10-15 parts of the bletilla striata, 10-15 parts of honeysuckle, 10-15 parts of Schisandra chinensis, 5-10 parts of cloves, 5-10 parts of kuh-seng, stone Chang 5-10 parts of Pu, 2-7 parts of guava；The surfactant system includes sodium alkyl benzene sulfonate, sodium alkyl sulfate, alkyl sulfonic acid One or more of sodium；The foam stabiliser is the castor-oil plant sodium alkoxide of sulfonation；The softening agent is quaternary, aliphatic acid One kind in ester type, right wax pattern, polyethylene, organic siliconresin type cationic softener；The fluorescent whitening agent hexichol second Auxiliary material described in alkenyl biphenyl fluorescent brightener includes sodium phosphate, silicate, soda ash, carboxymethyl cellulose, borax, peroxide One or more of sour sodium, fluorite.
2. a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent according to claim 1, which is characterized in that the detergent by with Lower raw material is prepared by mass percentage：Graphene oxide-silver-colored zinc nano-complex 0.1-0.5%, Traditional Chinese medicine bacteriostatic composition 1-6%, surfactant system 20-35%, foam stabiliser 0.5-1%, softening agent 2-4%, fluorescent whitening agent 0.05- 0.1%, auxiliary material 7-9%, water complement to 100%, and the Traditional Chinese medicine bacteriostatic composition extract is by following raw material system It is standby to form 17-19 parts of Cortex Phellodendri, 16-19 parts of the bark of ash, 11-13 parts of the bletilla striata, 12-14 parts of honeysuckle, 11-14 parts of Schisandra chinensis, cloves 6-8 Part, 7-10 parts of kuh-seng, 6-9 parts of grass-leaved sweetflag, 4-6 parts of guava.
3. a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent according to claim 1, which is characterized in that the detergent by with Lower raw material is prepared by mass percentage：Graphene oxide-silver-colored zinc nano-complex 0.2%, Traditional Chinese medicine bacteriostatic composition 5%, Surfactant system 32%, foam stabiliser 0.7%, softening agent 3%, fluorescent whitening agent 0.07%, auxiliary material 7%, water 100% is complemented to, 17 parts of Cortex Phellodendri, the bark of ash 17 is prepared by following raw material in the Traditional Chinese medicine bacteriostatic composition extract Part, 12 parts of the bletilla striata, 13 parts of honeysuckle, 13 parts of Schisandra chinensis, 7 parts of cloves, 8 parts of kuh-seng, 7 parts of grass-leaved sweetflag, 5 parts of guava.
4. a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent according to claim 1, which is characterized in that the graphite oxide Alkene-silver-colored zinc nano-complex is prepared by following methods：
Step 1: prepared by the graphene oxide of nitrification：1mol graphene oxides are prepared using improved Hummers methods, are added Reaction 10h is stirred at room temperature in the concentrated nitric acid of 100mL and the nitration mixture of the concentrated sulfuric acid, and filtering, distilled water washs solid repeatedly, until pH is 6 Left and right, is dried to obtain the graphene oxide of nitrification；
Step 2: the preparation of graphene oxide-silver-colored zinc nano-complex：Weigh 1mol steps Step 1: prepare nitrification oxygen Graphite alkene is scattered in ethanol solution, and 1.5mol/L ammonia spirits are added under ultrasonication, are then added dropwise dissolved with acetic acid The ethanol solution of silver and zinc acetate, reacts at 45 DEG C and is repeatedly freeze-dried afterwards with ethyl alcohol centrifuge washing afterwards for 24 hours, obtains oxidation stone Black alkene-silver-colored zinc nano-complex.
5. a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent according to claim 4, which is characterized in that the concentrated nitric acid and dense The volume ratio of sulfuric acid is 1:3.
6. a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent according to claim 4, which is characterized in that the ultrasound condition is 700W ultrasounds 1h.
7. a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent according to claim 4, which is characterized in that the silver acetate and second The substance withdrawl syndrome ratio of sour zinc is 1:1.2.
8. a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent according to claim 1, which is characterized in that the Traditional Chinese medicine bacteriostatic group Object is closed to be prepared by following methods：
It dries, crush Step 1: weighing Cortex Phellodendri, the bark of ash, the bletilla striata, honeysuckle, Schisandra chinensis, cloves, kuh-seng, grass-leaved sweetflag, guava, It sieves with 100 mesh sieve, obtains herb powder；
Step 2: according to herb powder and bionic extraction liquid mass ratio 1:10 ratio mixing, 37 DEG C of heating water baths, plastic film Sealing, magneton extract 3h, and filtrate is collected in filtering, and water-bath is concentrated into 1/4 volume, collects concentrate；
Step 3: by step Step 2: in concentrate according to volume ratio 1:4 mix with ethyl acetate-acetone mixed solution, extraction It takes 3 times, collects organic phase, vacuum rotary steam removes solvent, obtains faint yellow color powder to get Traditional Chinese medicine bacteriostatic composition.
9. a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent according to claim 8, which is characterized in that the bionic extraction liquid It is formulated by 0.25% sodium chloride, 0.30% pepsin and 0.025mol/L hydrochloric acid and water.
10. a kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent according to claim 8, which is characterized in that the bionic extraction Liquid pH is 4.5~6.5.
CN201810636420.7A 2018-06-20 2018-06-20 A kind of graphene oxide inhibiting bacteria and diminishing inflammation detergent Pending CN108624409A (en)

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Application publication date: 20181009