CN106939260A - Silver-colored transparent soap of a kind of graphene nano and its production and use - Google Patents

Silver-colored transparent soap of a kind of graphene nano and its production and use Download PDF

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CN106939260A
CN106939260A CN201710122506.3A CN201710122506A CN106939260A CN 106939260 A CN106939260 A CN 106939260A CN 201710122506 A CN201710122506 A CN 201710122506A CN 106939260 A CN106939260 A CN 106939260A
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silver
graphene nano
colored
reducing solution
graphene
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郑寅
贺伟
马小平
邓玉敏
宋新建
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Hubei University for Nationalities
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Hubei University for Nationalities
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D10/00Compositions of detergents, not provided for by one single preceding group
    • C11D10/04Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap
    • C11D10/042Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap based on anionic surface-active compounds and soap
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/817Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions or derivatives of such polymers, e.g. vinylimidazol, vinylcaprolactame, allylamines (Polyquaternium 6)
    • A61K8/8176Homopolymers of N-vinyl-pyrrolidones. Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005Antimicrobial preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/10Washing or bathing preparations
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/008Polymeric surface-active agents
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/29Sulfates of polyoxyalkylene ethers

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Abstract

The invention belongs to commodity processing technique field, and in particular to silver-colored transparent soap of a kind of graphene nano and its production and use.The silver-colored transparent soap of graphene nano that the present invention is prepared, the dirt-removing power not only possessed with general transparent soap, also as addition graphene nano is silver-colored and has bactericidal action.In addition, also there is excessive reducing agent such as glycerine, Tea Polyphenols and jujube extract and there is moisturizing, effect of beauty.The present invention uses the preparation method of a step redox graphene and silver ion, and the reducing agent of addition not only can also bring special effect with redox graphene and silver ion, excessive reducing agent.In addition, the preparation method production cost of the present invention is low, dangerous small, raw material is cheap and easily-available, green non-pollution, is suitable for large-scale industrial production.

Description

Silver-colored transparent soap of a kind of graphene nano and its production and use
Technical field
The invention belongs in transparent soap plus agent material technical field, and in particular to a kind of silver-colored transparent soap of graphene nano and its Preparation method and purposes.
Background technology
Transparent soap was just developed success early in 1789 abroad, but its correlation technique is monopolized once.Due to Transparent soap formula is strict, the more difficult control of production technology, and therefore, the soap transparency that conventional technique productions go out is poor, and table occurs Face carries the more sliding phenomenon of water droplet or surface, is difficult to real life.
At present, several functions soap has been occurred in that on the market, and such as there is beautifying face and moistering lotion, the soap of preserving moisture and protecting skin effect Deng.Attention with people to personal and environmental sanitation, the perfumed soap product with sterilizing function is gradually paid attention to by market.
However, the Antibacterial Constituents in existing Antibacterial soaps may have side effect to human body, and in its preparation During usually using with stronger physiological-toxicity chemical reagent, these chemical substances not only in process of production can be to environment Have undesirable effect, and if remained in the product, human body can also be adversely affected.
Therefore, exploitation has multinomial difference in functionality simultaneously, can particularly keep the premise of beautifying face and moistering lotion, preserving moisture and protecting skin Under, also with good bactericidal property, dirt-removing power and environment amenable transparent soap, and improve the preparation of such transparent soap Method, helps to improve the quality of life of people, is easy to use, improves production efficiency and product quality.
The content of the invention
In order to solve said one or multiple problems, the present invention provides a kind of transparent soap, includes following component:Soap base, thoroughly Bright dose and the silver-colored reducing solution of graphene nano.
Wherein, the soap base can be 30~80 parts by weight, such as 44-46 parts by weight;The clarifier can for 10~ 50 parts by weight, such as 23-30 parts by weight;The silver-colored reducing solution of the graphene nano can be 1~10 parts by weight, such as 1-3 weight Part.
The soap base can be included:
One or more fatty acid alkali metal salts;With
One or more in dihydric alcohol and polyalcohol.
Wherein, in the fatty acid alkali metal salt, aliphatic acid can be selected from fatty monoacid or binary acid;For example, described Aliphatic acid can be carbon number be more than 10, preferably carbon number be 11~20 (such as 11,12,13,14,15,16,17,18, 19 or fatty monoacid or binary acid 20) in one or more;Alkali metal can be selected from sodium or potassium;As example, The fatty acid alkali metal salt can be selected from one kind in odium stearate, sodium palmitate, Sodium myristate, sodium laurate or many Kind;
The dihydric alcohol can be selected from aliphatic dihydric alcohol, such as ethylene glycol, diglycol, propane diols, a contracting dipropyl Glycol, 1,3- propane diols, 1,2- propane diols, 1,3 butylene glycol, 1,4- butanediols, 2- methyl isophthalic acids, 2- propane diols, 2- methyl isophthalic acids, One kind in the dihydric alcohols such as ammediol, 1,2- pentanediols, 1,3- pentanediols, 1,4- pentanediols, 1,5- pentanediols, neopentyl glycol Or it is a variety of;The polyalcohol can be selected from aliph polyols, such as glycerine, two glycerine, three glycerine, four glycerine, three Hydroxymethyl ethane, trimethylolpropane, tri hydroxy methyl butane, pentaerythrite, 1,2,4- butantriols, the triols of 1,3,5- penta, 1,2, 6- hexanetriols, 1,2,3,4- erythrol, D-sorbite, sorbitan, D-sorbite glycerine condensation product, ribitol, Ah Draw the one or more in the polyalcohols such as primary sugar alcohol, xylitol, mannitol;As example, the dihydric alcohol is selected from propane diols, The trihydroxylic alcohol is selected from glycerine;
According to the present invention, it is not particularly limited for the clarifier, as long as it can make soap base that transparence is presented; For example, the clarifier can be selected from the one or more in ethanol, honey, sucrose.
According to the present invention, the transparent soap can also include non-fat Examples of carboxylic anionic's surfactant, such as bay Alcohol polyethenoxy ether sodium sulfovinate;
For example, the content of non-fat Examples of carboxylic anionic's surfactant can be 18~22 parts by weight.
According to the present invention, the transparent soap can also include water;
According to the present invention, the water is preferably deionized water;Preferably, the content of water is 8~10 parts by weight.
According to the present invention, the transparent soap can also include other optional additives.
According to the present invention, described other optional additives can selected from cationic surfactant, vitamin, essence, One or more in pigment or other compositions.The amount of the additive is not particularly limited, for example, can be 15~25 weight Part.
According to the present invention, the silver-colored reducing solution of the graphene nano can be selected from the silver-colored slycersol of graphene nano, graphite One or more in alkene Nano Silver Tea Polyphenols reducing solution, graphene nano pale rose colour jujube reducing solution.
In accordance with the present invention it is preferred that, the silver-colored slycersol of the graphene nano, the silver-colored Tea Polyphenols reducing solution of graphene nano and In graphene nano pale rose colour jujube reducing solution, the particle diameter of Nano Silver is preferably more than 100nm, such as no more than 50nm, and such as particle diameter is 2 ~20nm.
In accordance with the present invention it is preferred that, the silver-colored slycersol of the graphene nano, the silver-colored Tea Polyphenols reducing solution of graphene nano and In graphene nano pale rose colour jujube reducing solution, the concentration of graphene nano silver can be 0.4mg/ml~1.0mg/ml, for example 0.5mg/ml。
Preferably, in the transparent soap in addition to the silver-colored reducing solution of the graphene nano, not containing other has bactericidal activity Component.
The present invention also provides the preparation method of the transparent soap, including the soap base, clarifier and graphene nano is silver-colored Reducing solution is mixed.
According to the present invention, the preparation method includes reducing addition method using a step or the preparation of step-by-step reduction addition method is described Graphene nano silver reducing solution.
In accordance with the present invention it is preferred that, the preparation method may include steps of:
1) heat, then reacted with alkali metal hydroxide after mixing aliphatic acid, dihydric alcohol and/or polyalcohol;
2) to step 1) other components are added in the product for preparing, the silver-colored reducing solution of graphene nano is added after stirring, Stir, cooling obtains product.
Wherein it is preferred to, in step 1) in, heating stirring is to saturating after aliphatic acid, dihydric alcohol and/or polyalcohol are mixed It is bright, then add the reactant aqueous solution of alkali metal hydroxide;Reaction temperature can be 70~80 DEG C, such as 75 DEG C;
The concentration of the aqueous solution of the alkali metal hydroxide can be 7~8mol/L, such as 7.35~7.42mol/L, Such as 7.37mol/L;
Preferably, alkali metal hydroxide and the mol ratio sum of all aliphatic acid can be 1:(1~2), such as 1: (1.0~1.1), such as 1:1.05;
Preferably, alkali metal hydroxide and stearic mass ratio can be 0.14~0.15:1, the matter with palmitic acid It can be 0.15~0.16 to measure ratio:1, the mass ratio with myristic acid can be 0.17~0.18:1, with lauric mass ratio Can be 0.17~0.18:1.As example, the quality of alkali metal hydroxide can be calculated by equation below:
The quality of alkali metal hydroxide=stearic acid quality × 0.1406+ palmitic acid quality × 0.1560+ myristic acids Quality × 0.1751+ laurate quality × 0.2000.
Generally, the temperature of the aqueous solution of the alkali metal hydroxide before addition can be by those skilled in the art according to tool Body experiment condition, such as temperature selection when stirring.As example, the aqueous solution of the alkali metal hydroxide is before addition Temperature is 70~80 DEG C, such as 75 DEG C;
In accordance with the present invention it is preferred that, the step 1) reaction time can be 30~50min, for example, 40min;It is excellent Selection of land, after the reaction by temperature adjustment to 60~70 DEG C, such as 65 DEG C;
According to embodiment of the present invention, in step 2) in, to step 1) product in add non-fat carboxylic acids it is cloudy from Sub- surfactant, stirring adds clarifier and other optional additives, and graphene nano silver reduction is added after stirring Liquid, cools down after stirring, produces product.
Preferably, add after non-fat Examples of carboxylic anionic's surfactant, stir 3~10min, such as 5min;
Preparation in accordance with the present invention, it is preferable that methods described maintains the temperature at more than 60 DEG C, preferably more than 62 DEG C, Such as more than 63 DEG C;
It is further preferred that the addition temperature of each component or reagent is maintained at more than 60 DEG C, preferably 62 DEG C in methods described More than, such as more than 63 DEG C;
Preferably, the mixing time added after non-fat Examples of carboxylic anionic's surfactant is 1-15min, such as 5~ 10min;Preferably, the mixing time added after clarifier and other optional additives is 3~5min, such as 3min;
Preferably, add after the silver-colored reducing solution of graphene nano, mixing speed can be 300r/min.
Preferably, in step 2) in, the silver-colored reducing solution of graphene nano is added, is stirred, mould is put into, cooling is produced Product.The mould can select required shapes and sizes as needed.
In accordance with the present invention it is preferred that, the silver-colored slycersol of the graphene nano can be by graphene oxide, polyvinyl pyrrole It is prepared by alkanone, silver nitrate and glycerine hybrid reaction;Wherein, graphene oxide (g), silver nitrate (g), polyvinylpyrrolidone (g) Ratio with glycerine (ml) can be 1:(0.5~2):(2~10):(100~800), such as 1:(0.5~1.5):5:400.Root According to the present invention, the preparation method of the silver-colored slycersol of the graphene nano may include following steps:
A1) in a heated condition, glycerine, polyvinylpyrrolidone, silver nitrate are mixed;
A2) to step a1) obtained by mixture in add dispersion liquid of the graphene oxide in glycerine, obtain stone after mixing Black alkene Nano Silver slycersol.
Wherein, step a1) in, heating-up temperature can be 80~100 DEG C, such as 90 DEG C;
Preferably, step a1) and a2) in glycerine volume ratio be 1:1;
Preferably, step a2) in, to step a1) obtained by mixture in add graphene oxide scattered in glycerine After liquid, ultrasonic mixing 0.2-24h, such as 0.5-1h;
As example, the preparation method of the silver-colored slycersol of the graphene nano includes:
Glycerine is taken in container, 90 DEG C are heated to, polyvinylpyrrolidone, magneton stirring 20min is added;Weigh silver nitrate Add, 300r/min stirs 1~2.5h;
Graphene oxide 2~3h of ultrasonic disperse in glycerine is taken, dispersion liquid of the graphene oxide in glycerine is obtained;It is above-mentioned Continue to obtain the silver-colored slycersol of graphene nano after 0.5~1h of ultrasound after both mixing.
In accordance with the present invention it is preferred that, the silver-colored Tea Polyphenols reducing solution of the graphene nano can be by graphene oxide, nitric acid It is prepared by silver, tea (such as green tea or black tea) and water hybrid reaction;Wherein, graphene oxide (g), silver nitrate (g), tea (g) and water (ml) ratio can be:1:(0.5~2):(20~60):(800~3000), preferably 1:(0.5~1.5):40:2000.
According to the present invention, the preparation method of the silver-colored Tea Polyphenols reducing solution of the graphene nano may include following steps:
In a heated condition, tea, water, graphene oxide and silver nitrate are mixed, it is many that reaction obtains the silver-colored tea of graphene nano Phenol reducing solution.
Preferably, methods described comprises the following steps:
B1) tea is added in boiling water, boiling 5-40min, such as such as 10-30min, 20min is kept;
B2) by step b1) obtained by mixture cooling, be for example cooled to 70-90 DEG C, filtering, filtrate is in 70-90 DEG C of oil bath Middle insulation 1-20min, such as 5min;
B3 graphene oxide) is added, is added after being stirred until homogeneous after silver nitrate, 1~24h of backflow (such as 6h), obtains graphite Alkene Nano Silver Tea Polyphenols reducing solution.
As example, the preparation method of the silver-colored Tea Polyphenols reducing solution of the graphene nano includes:
By tea dry it is finely ground after be added in boiling water, keep boiling 20min, filtering;
Graphene oxide is added, is added after being stirred until homogeneous and the silver-colored Tea Polyphenols of graphene nano is obtained after silver nitrate, backflow 6h Reducing solution.
In accordance with the present invention it is preferred that, the graphene nano pale rose colour jujube reducing solution can by graphene oxide, silver nitrate, It is prepared by jujube and water reaction;Wherein, the ratio of graphene oxide (g), silver nitrate (g), jujube (g) and water (ml) can be 1: (0.5~2):(20~60):(800~3000), preferably 1:(0.5~1.5):40:2000.
According to the present invention, the preparation method of the graphene nano pale rose colour jujube reducing solution may include following steps:
In a heated condition, jujube, water, graphene oxide and silver nitrate are mixed, reaction obtains graphene nano pale rose colour Jujube reducing solution.
Preferably, methods described comprises the following steps:
C1) jujube is added in boiling water, boiling 5-40min, such as such as 10-30min, 20min is kept;
C2) by step c1) obtained by mixture cooling, be for example cooled to 70-90 DEG C, filtering, filtrate is in 70-90 DEG C of oil bath Middle insulation 1-20min, such as 5min;
C3 graphene oxide) is added, is added after being stirred until homogeneous after silver nitrate, 1~24h of backflow (such as 6h), obtains graphite Alkene Nano Silver Tea Polyphenols reducing solution.
As example, the preparation method of the graphene nano pale rose colour jujube reducing solution includes:
By jujube dry it is finely ground after be added in boiling water, seethe with excitement 20min, filtering;
Graphene oxide is added, graphene nano pale rose colour jujube is obtained also after silver nitrate, backflow 6h are added after being stirred until homogeneous Stoste.
According to the above-mentioned preparation method of the silver-colored reducing solution of graphene nano of the present invention, wherein graphene oxide and silver nitrate Mass ratio can be 1:(0.5~2), preferably 1:(0.5~1.5), is specifically as follows 1:(0.8~1.2), such as 1:1.
The present invention also provides the purposes of the silver-colored transparent soap of graphene nano as described above, and the silver-colored transparent soap of the graphene nano can Needed according to cleaning and as different types of cleansing soap, be such as used as human body clean soap, laundry soap.It is preferably used as human body clean Soap, such as cleaning available for face or other any parts, such as face soap, bath soap, the special bath soap of baby.
The present invention also provides described graphene nano silver-colored reducing solution.
The present invention also provides a kind of pharmaceutical composition, includes the silver-colored reducing solution of the graphene nano.
The present invention, which also provides the silver-colored reducing solution of the graphene nano, is used for sterilizing use, such as can be used as anti-in skin care item Bacterium, moisturizing Cosmetic Ingredient, such as purposes in mildy wash, face cream, suncream or cleansing soap, it is preferable that the graphene is received The silver-colored reducing solution of rice is as the antibacterial in transparent soap, moisturizing Cosmetic Ingredient.
Beneficial effects of the present invention
The silver-colored transparent soap of graphene nano that the present invention is prepared, the decontamination energy not only possessed with general transparent soap Power, also as addition graphene nano is silver-colored and has bactericidal action.
Simultaneously as the glycerine used in reduction, Tea Polyphenols and jujube extract are all excessive, can not only be abundant Reduced graphene and silver ion, moreover it is possible to retain glycerine, Tea Polyphenols and the jujube extract of suitable amount in Transparent soap base is added, make Transparent soap is obtained the characteristics of with general transparent soap on basis, due to also added Tea Polyphenols or jujube extract so that thoroughly Bright soap is provided with peat-reek and special moisturizing, beauty functions.The removing toxic substances of Tea Polyphenols tool and radiation resistance, can effectively prevent to put In penetrating property material intrusive body, and strontium and cobalt can be made to excrete rapidly, be the preferential choosing of working clan of the long-term work before computer Select, the vitamin content of jujube is very high.Glycerine, Tea Polyphenols and jujube are simultaneously as reducing agent, green non-hazardous.Also, tea is more Flavonoid substances in phenol also act as the effect of surfactant, prevent that reunion of the graphene caused by high surface tension from showing As.
Conventional graphene preparation method can all use the noxious materials such as hydrazine hydrate, p-phenylenediamine, processing method It is improper all to cause harm and pollute to people, to environment.The preparation method of the present invention uses glycerine, Tea Polyphenols and jujube extract Graphene oxide is reduced, the theory of Green Chemistry is embodied.The preparation method production cost of the present invention is low, dangerous Small, raw material is cheap and easily-available, and green non-pollution is suitable for large-scale industrial production.
Embodiment
General formula compound of the present invention and its preparation method and application is done further below in conjunction with specific embodiment Detailed description.It should be appreciated that the following example is merely illustrative the ground description and interpretation present invention, and it is not necessarily to be construed as to this The limitation of invention protection domain.All technologies realized based on the above of the present invention are encompassed by the model it is contemplated that protecting In enclosing.
Unless otherwise indicated, the raw material and reagent used in embodiment is commercial goods, or can pass through known formula legal system It is standby to obtain.
Embodiment 1
1) stearic acid 3g, palmitic acid 10g, myristic acid 2g, laurate 3g, propane diols 20g, glycerine 5g is taken to be burnt in three necks In bottle, mechanical agitation is extremely clarified at 75 DEG C.Weigh 2.95g NaOH to be dissolved in 10ml water, 75 DEG C of insulation 5min slowly add Enter in flask, react 30~50min, adjust the temperature to 65 DEG C.
2) 10ml glycerine is taken in Boiling tube, in 90 DEG C of slightly hot rear addition 0.25g polyvinylpyrrolidones, magneton stirring 20min.Silver nitrate 0.05g additions are weighed, 300r/min stirs 1~2.5h;0.05g graphene oxides are taken to surpass in 10ml glycerine Sound continues the silver-colored slycersol of graphene nano that must can stablize after 0.5~1h of ultrasound to scattered after both above-mentioned mixing 26.35g。
3) 20g ethoxylated dodecyl alcohol sulfuric ester sodium salts are taken, 65-70 DEG C of insulation is added in soap base, stirs 5~10min. 20g honey is taken, is rapidly added after 65-70 DEG C of insulation in soap base, stirs 3~5min.The silver-colored slycersol of 2g graphene nanos is taken, It is added dropwise to after 65-70 DEG C of insulation in soap base rapidly, after 5~10min of insulation, soap base is taken out into injection mould, room temperature is cooled to, i.e., Obtain the silver-colored transparent soap of graphene nano.
Embodiment 2
1) stearic acid 3g, palmitic acid 10g, myristic acid 2g, laurate 3g, propane diols 20g, glycerine 5g is taken to be burnt in three necks In bottle, mechanical agitation is extremely clarified at a temperature of 75 DEG C.2.95g NaOH is taken to be dissolved in 10mL water, 75 DEG C of insulation 5min, slowly Add in flask, react 30~50min, adjust the temperature to 65 DEG C.
2) it is added to after taking the drying of 2g jujubes finely ground in 100ml boiling water, heats 20min, is cooled to 85 DEG C of filterings and will filter Liquid is transferred in 100ml flasks, is added magneton and is incubated 5min in 80 DEG C of oil baths, weighs the addition of 0.05g graphene oxides, 300r/min produces graphene nano pale rose colour jujube reducing solution after the addition of 0.05g silver nitrates, backflow 6h are weighed after being stirred until homogeneous 98g。
3) 22g ethoxylated dodecyl alcohol sulfuric ester sodium salts are taken, 65-70 DEG C of insulation, which is added, stirs 5~10min in soap base. 20g honey is taken, is rapidly added after 65-70 DEG C of insulation, stirs 3~5min.1g graphene nano pale rose colour jujube reducing solutions are taken, after insulation It is rapid to be added dropwise, soap base is incubated after 5~10min, injection mould is taken out, is cooled to room temperature, the silver-colored transparent soap of graphene nano is produced.
Embodiment 3
1) stearic acid 3g, palmitic acid 10g, myristic acid 2g, laurate 3g, propane diols 20g, glycerine 5g is taken to be burnt in three necks In bottle, mechanical agitation is extremely clarified at a temperature of 75 DEG C.2.95g NaOH is taken to be dissolved in 10mL water, 75 DEG C of insulation 5min, slowly Add in flask, react 30~50min, adjust the temperature to 65 DEG C.
2) it is added to after taking the drying of 2g green tea finely ground in 100ml boiling water, heats 20min, is cooled to 85 DEG C of filterings and will filter Liquid is transferred in 100ml flasks, is added magneton and is incubated 5min in 80 DEG C of oil baths, weighs the addition of 0.05g graphene oxides, 300r/min is weighed after being stirred until homogeneous produces the silver-colored green tea reducing solution of graphene nano after the addition of 0.05g silver nitrates, backflow 6h 99g。
3) 18g ethoxylated dodecyl alcohol sulfuric ester sodium salts are taken, 65-70 DEG C of insulation, which is added, stirs 5~10min in soap base. 20g honey is taken, is rapidly added after 65-70 DEG C of insulation, stirs 3~5min.Take the silver-colored Tea Polyphenols reducing solution of 3g graphene nanos, insulation It is rapid afterwards to be added dropwise, it is stirred vigorously after 1~2min, soap base is taken out into injection mould, room temperature is cooled to, produces graphene nano silver thoroughly Bright soap.
Embodiment 4:Bactericidal property is tested
Using antibacterial circle diameter method, to embodiment 1,2, the fungicide active ingredient graphene nano silver of 3 three kind of transparent soap it is sweet The silver-colored Tea Polyphenols reducing solution of oleosol, graphene nano and graphene nano pale rose colour jujube reducing solution do bacteriostatic experiment, and test result is such as Shown in table 1, table 2 and table 3.From test result, three kinds of compositions are respectively to bacillus subtilis, Escherichia coli, golden yellow Portugal Grape coccus, Candida albicans and Pseudomonas aeruginosa are respectively provided with good bactericidal potency.
Use the silver-colored slycersol of 0.05mg/ml graphene nano, the silver-colored Tea Polyphenols reducing solution of graphene nano and graphene Nano Silver jujube reducing solution is tested, and good inhibitory action can be produced to above-mentioned bacterium, when using higher concentration, 10~ 20min bacterium kill rate is to reach 99%.
The Bactericidal test of the graphene nano of table 1 silver slycersol (0.05mg/ml)
Strain Bacillus subtilis Escherichia coli Staphylococcus aureus Candida albicans Pseudomonas aeruginosa
Antibacterial circle diameter/mm 16.7 16.4 15.5 15.7 16.2
The Bactericidal test of the graphene nano of table 2 silver Tea Polyphenols reducing solution (0.05mg/ml)
Strain Bacillus subtilis Escherichia coli Staphylococcus aureus Candida albicans Pseudomonas aeruginosa
Antibacterial circle diameter/mm 16.8 16.4 15.5 15.8 16.2
The Bactericidal test of the graphene nano pale rose colour jujube reducing solution (0.05mg/ml) of table 3
Strain Bacillus subtilis Escherichia coli Staphylococcus aureus Candida albicans Pseudomonas aeruginosa
Antibacterial circle diameter/mm 16.8 16.3 15.4 15.7 16.3
Note:Data above takes the average value of three experimental results.
More than, embodiments of the present invention are illustrated.But, the present invention is not limited to above-mentioned embodiment.It is all Within the spirit and principles in the present invention, any modifications, equivalent substitutions and improvements done etc., should be included in the guarantor of the present invention Within the scope of shield.

Claims (10)

1. a kind of transparent soap, includes following component:The silver-colored reducing solution of soap base, clarifier and graphene nano;
Wherein, the soap base can be 30~80 parts by weight, such as 44-46 parts by weight;The clarifier can be 10~50 weights Measure part, such as 23-30 parts by weight;The silver-colored reducing solution of the graphene nano can be 1~10 parts by weight, such as 1-3 parts by weight;
The soap base can be included:
One or more fatty acid alkali metal salts;With
One or more in dihydric alcohol and polyalcohol;
The clarifier can be selected from the one or more in ethanol, honey, sucrose;
The silver-colored reducing solution of the graphene nano can be selected from the silver-colored slycersol of graphene nano, the silver-colored Tea Polyphenols of graphene nano also One or more in stoste, graphene nano pale rose colour jujube reducing solution;
Preferably, the transparent soap can also include non-fat Examples of carboxylic anionic's surfactant, such as laruyl alcohol polyoxy second Alkene ether sodium sulfovinate;For example, the content of non-fat Examples of carboxylic anionic's surfactant can be 18~22 parts by weight.
2. transparent soap as claimed in claim 1, wherein:In the fatty acid alkali metal salt, aliphatic acid can be selected from fat one First acid or binary acid;For example, the aliphatic acid can be carbon number be more than 10, preferably carbon number be 11~20 (such as 11, 12nd, 13,14,15,16,17,18,19 or fatty monoacid or binary acid 20) in one or more;Alkali metal can be with Selected from sodium or potassium;As example, the fatty acid alkali metal salt can be selected from odium stearate, sodium palmitate, Sodium myristate, the moon One or more in sodium metasilicate;
The dihydric alcohol can be selected from aliphatic dihydric alcohol, for example ethylene glycol, diglycol, propane diols, dipropylene glycol, 1,3- propane diols, 1,2- propane diols, 1,3 butylene glycol, 1,4- butanediols, 2- methyl isophthalic acids, 2- propane diols, 2- methyl isophthalic acids, 3- the third two One kind or many in the dihydric alcohols such as alcohol, 1,2- pentanediols, 1,3- pentanediols, 1,4- pentanediols, 1,5- pentanediols, neopentyl glycol Kind;The polyalcohol can be selected from aliph polyols, such as glycerine, two glycerine, three glycerine, four glycerine, three hydroxyl first Base ethane, trimethylolpropane, tri hydroxy methyl butane, pentaerythrite, 1,2,4- butantriols, the triols of 1,3,5- penta, 1,2,6- oneself Triol, 1,2,3,4- erythrol, D-sorbite, sorbitan, D-sorbite glycerine condensation product, ribitol, Arab One or more in the polyalcohols such as sugar alcohol, xylitol, mannitol;As example, the dihydric alcohol is selected from propane diols, described Trihydroxylic alcohol is selected from glycerine;
Preferably, the silver-colored reducing solution of the graphene nano can be selected from the silver-colored slycersol of graphene nano, graphene nano silver One or more in Tea Polyphenols reducing solution, graphene nano pale rose colour jujube reducing solution;
Preferably, the silver-colored slycersol of the graphene nano, the silver-colored Tea Polyphenols reducing solution of graphene nano and graphene nano pale rose colour In jujube reducing solution, the particle diameter of Nano Silver is preferably more than 100nm, such as no more than 50nm, and such as particle diameter is 2~20nm;
Preferably, the silver-colored slycersol of the graphene nano, the silver-colored Tea Polyphenols reducing solution of graphene nano and graphene nano pale rose colour In jujube reducing solution, the concentration of graphene nano silver can be 0.4mg/ml~1.0mg/ml, such as 0.5mg/ml;
Preferably, in the transparent soap in addition to the silver-colored reducing solution of the graphene nano, not containing other has the group of bactericidal activity Point.
3. the preparation method of transparent soap as claimed in claim 1 or 2, including the soap base, clarifier and graphene nano is silver-colored Reducing solution is mixed;
Preferably, the preparation method may include steps of:
1) heat, then reacted with alkali metal hydroxide after mixing aliphatic acid, dihydric alcohol and/or polyalcohol;
2) to step 1) other components are added in the product for preparing, the silver-colored reducing solution of graphene nano, stirring are added after stirring Uniformly, cooling obtains product.
4. preparation method as claimed in claim 3, wherein:
In step 1) in, then heating stirring adds alkali metal to transparent after aliphatic acid, dihydric alcohol and/or polyalcohol are mixed The reactant aqueous solution of hydroxide;Reaction temperature can be 70~80 DEG C, such as 75 DEG C;
The concentration of the aqueous solution of the alkali metal hydroxide can be 7~8mol/L, such as 7.35~7.42mol/L, such as 7.37mol/L;
Preferably, alkali metal hydroxide and the mol ratio sum of all aliphatic acid can be 1:(1~2), such as 1:(1.0~ 1.1), such as 1:1.05;
Preferably, the temperature of the aqueous solution of the alkali metal hydroxide before addition is 70~80 DEG C, such as 75 DEG C;
Preferably, the step 1) reaction time can be 30~50min, for example, 40min;Preferably, after the reaction will Temperature adjustment is to 60~70 DEG C, such as 65 DEG C;
In step 2) in, to step 1) product in add non-fat Examples of carboxylic anionic's surfactant, stir, add Bright dose and other optional additives, add the silver-colored reducing solution of graphene nano, are cooled down after stirring, produce product after stirring;
Preferably, add after non-fat Examples of carboxylic anionic's surfactant, stir 3~10min, such as 5min;
Preferably, methods described maintains the temperature at more than 60 DEG C, such as preferably more than 62 DEG C, more than 63 DEG C;
Preferably, the addition temperature of each component or reagent is maintained at more than 60 DEG C, preferably more than 62 DEG C, such as 63 in methods described More than DEG C.
5. the preparation method as described in claim 3 or 4, wherein:
The silver-colored slycersol of the graphene nano can be mixed by graphene oxide, polyvinylpyrrolidone, silver nitrate and glycerine It is prepared by reaction;Wherein, the ratio of graphene oxide (g), silver nitrate (g), polyvinylpyrrolidone (g) and glycerine (ml) can be 1:(0.5~2):(2~10):(100~800), such as 1:(0.5~1.5):5:400;
Preferably, the preparation method of the silver-colored slycersol of the graphene nano may include following steps:
A1) in a heated condition, glycerine, polyvinylpyrrolidone, silver nitrate are mixed;
A2) to step a1) obtained by mixture in add dispersion liquid of the graphene oxide in glycerine, obtain graphene after mixing Nano Silver slycersol;
Wherein, step a1) in, heating-up temperature can be 80~100 DEG C, such as 90 DEG C;
Preferably, step a1) and a2) in glycerine volume ratio be 1:1;
Preferably, step a2) in, to step a1) obtained by mixture in add after dispersion liquid of the graphene oxide in glycerine, Ultrasonic mixing 0.2-24h, such as 0.5-1h.
6. the preparation method as described in claim any one of 3-5, wherein graphene nano silver Tea Polyphenols reducing solution can be with Prepared by graphene oxide, silver nitrate, tea (such as green tea or black tea) and water hybrid reaction;Wherein, graphene oxide (g), nitric acid Silver-colored (g), the ratio of tea (g) and water (ml) can be:1:(0.5~2):(20~60):(800~3000), preferably 1:(0.5~ 1.5):40:2000;
Preferably, the preparation method of the silver-colored Tea Polyphenols reducing solution of the graphene nano may include following steps:
In a heated condition, tea, water, graphene oxide and silver nitrate are mixed, reaction obtains the silver-colored Tea Polyphenols of graphene nano also Stoste;
Preferably, methods described comprises the following steps:
B1) tea is added in boiling water, boiling 5-40min, such as such as 10-30min, 20min is kept;
B2) by step b1) obtained by mixture cooling, be for example cooled to 70-90 DEG C, filtering, filtrate is protected in 70-90 DEG C of oil bath Warm 1-20min, such as 5min;
B3 graphene oxide) is added, is added after being stirred until homogeneous after silver nitrate, 1~24h of backflow (such as 6h), obtains graphene nitre Sour silver Tea Polyphenols reducing solution.
7. the preparation method as described in claim any one of 3-6, wherein the graphene nano pale rose colour jujube reducing solution can be by It is prepared by graphene oxide, silver nitrate, jujube and water reaction;Wherein, graphene oxide (g), silver nitrate (g), jujube (g) and water (ml) ratio can be 1:(0.5~2):(20~60):(800~3000), preferably 1:(0.5~1.5):40:2000;
Preferably, the preparation method of the graphene nano pale rose colour jujube reducing solution may include following steps:
In a heated condition, jujube, water, graphene oxide and silver nitrate are mixed, reaction obtains graphene nano pale rose colour jujube also Stoste;
Preferably, methods described comprises the following steps:
C1) jujube is added in boiling water, boiling 5-40min, such as such as 10-30min, 20min is kept;
C2) by step c1) obtained by mixture cooling, be for example cooled to 70-90 DEG C, filtering, filtrate is protected in 70-90 DEG C of oil bath Warm 1-20min, such as 5min;
C3 graphene oxide) is added, is added after being stirred until homogeneous after silver nitrate, 1~24h of backflow (such as 6h), is obtained graphene and receive The silver-colored Tea Polyphenols reducing solution of rice.
8. the purposes of transparent soap as claimed in claim 1 or 2, the transparent soap is used as human body clean soap, laundry soap;It is preferably used as Human body clean soap, such as cleaning available for face or other any parts, such as face soap, bath soap, the special bath soap of baby.
9. a kind of silver-colored reducing solution of graphene nano, the silver-colored reducing solution of the graphene nano is in claim any one of 1-7 One kind in graphene nano silver slycersol, the silver-colored Tea Polyphenols reducing solution of graphene nano and graphene nano pale rose colour jujube reducing solution Or it is a variety of.
10. the silver-colored reducing solution of graphene nano described in claim 9 is used for sterilized purposes, be such as used as antibacterial in skin care item, Moisturizing Cosmetic Ingredient, such as purposes in mildy wash, face cream, suncream or cleansing soap;
Preferably, the silver-colored reducing solution of the graphene nano is as the antibacterial in transparent soap, moisturizing Cosmetic Ingredient.
CN201710122506.3A 2017-03-02 2017-03-02 Silver-colored transparent soap of a kind of graphene nano and its production and use Pending CN106939260A (en)

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