CN109021296A - A kind of bamboo charcoal/biology cellulose composite material and preparation method and application - Google Patents

A kind of bamboo charcoal/biology cellulose composite material and preparation method and application Download PDF

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CN109021296A
CN109021296A CN201710428104.6A CN201710428104A CN109021296A CN 109021296 A CN109021296 A CN 109021296A CN 201710428104 A CN201710428104 A CN 201710428104A CN 109021296 A CN109021296 A CN 109021296A
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bamboo charcoal
composite material
cellulose composite
biology cellulose
biology
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杨加志
李文萍
陈春涛
梁光芸
顾焱
刘晓慧
曾干敏
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Nanjing University of Science and Technology
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Nanjing University of Science and Technology
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0212Face masks
    • 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
    • A61K8/73Polysaccharides
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • 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
    • A61Q19/00Preparations for care of the skin
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075Macromolecular gels
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12NMICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
    • C12N1/00Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
    • C12N1/20Bacteria; Culture media therefor
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/04Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2301/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/02Cellulose; Modified cellulose
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/16Applications used for films

Abstract

The invention discloses a kind of bamboo charcoal/biology cellulose composite material and preparation method and applications.The bamboo charcoal/biology cellulose composite material is prepared by addition bamboo charcoal powder in situ, static fermentation culture.Preparation step is as follows: activated spawn Acetobacter xylinum NUST4.2;Prepare strain Acetobacter xylinum NUST4.2 seed liquor;The bamboo charcoal powder that different quality volume ratio is added in the fermentation medium of Acetobacter xylinum NUST4.2 carries out static fermentation production, obtains bamboo charcoal/biology cellulose composite material;Purification process is carried out to bamboo charcoal/biology cellulose composite material, obtains spongiform bamboo charcoal/biology cellulose composite material.The bamboo charcoal/application of the biology cellulose composite material in facial treatment mask.The present invention is tested for the property bamboo charcoal biological fiber composite membrane, and porosity, gas permeability are improved, and mechanical strength etc. does not decline, the application being more suitable in facial treatment mask.

Description

A kind of bamboo charcoal/biology cellulose composite material and preparation method and application
Technical field
The invention belongs to Biocomposite material technical field, especially a kind of bamboo charcoal/biology cellulose composite material and its Preparation method and application.
Background technique
Bacteria cellulose (bacterial cellulose, BC) is the one kind produced by bacteriums such as acetobacters Novel high-performance Microbe synthesis material has good bioaffinity, adaptability, compatibility, degradability, and has high hold Aqueous and crystallinity, good Nanofiber Network, high tension and intensity, the Optimalities such as especially good mechanical tenacity Can, the concern of people is increasingly subject in the application of medical material.
Bamboo charcoal powder is that high-quality bamboo charcoal carries out to powder is fine crushing forms, product adsorption function with super strength and generation bear from Sub, radiation infrared, increase alkalinity and other effects, can purify air and water quality, moisture absorption damping, and fungus-resistant blocks radiation, It can promote blood circulation with human contact and metabolic.It is different to be widely used in water quality and air cleaning, room damping, absorption The industries such as taste, make-up and beauty, coating, weaving, health-care medical, electronics and field.
Therefore, by the advantages of after bamboo charcoal incorporation biology cellulose, the composite material of the two synthesis has both the two.But mesh Before, there has been no the preparation method for being combined the two, when pure BC film is used for facial treatment mask, insufficient, cleaning force that there are porositys The disadvantages of degree difference.
Summary of the invention
The purpose of the present invention is to provide a kind of bamboo charcoal/biology cellulose composite material and preparation method and applications, obtain To the modification composite membrane of the excellent absorption property for the good characteristic and bamboo charcoal for having BC concurrently.
The technical solution for realizing the aim of the invention is as follows: a kind of bamboo charcoal/biology cellulose composite material, by In the fermentation medium of Acetobacter xylinum NUST4.2, the bamboo charcoal powder of addition different quality volume ratio carries out static Fermenting and producing forms, and bamboo charcoal particle is wrapped in the reticular fiber structure of biology cellulose.
Further, the bamboo charcoal powder of the different quality volume ratio, respectively 0.1%, 0.25%, 0.5%, 1.0%, 5.0%.
A kind of bamboo charcoal/biology cellulose composite material preparation method, comprising the following steps:
Step 1, activated spawn Acetobacter xylinum NUST4.2;
Step 2, strain Acetobacter xylinum NUST4.2 seed liquor is prepared;
Step 3, different quality volume ratio is added in the fermentation medium of Acetobacter xylinum NUST4.2 Bamboo charcoal powder carries out static fermentation production, obtains bamboo charcoal/biology cellulose composite material;
Step 4, purification process is carried out to bamboo charcoal/biology cellulose composite material, obtains spongiform bamboo charcoal/biological fiber Plain composite material.
Further, activated spawn Acetobacter xylinum NUST4.2 described in step 1, specific as follows:
Required ingredient is weighed according to solid culture based formulas and adds water constant volume, is adjusted to required pH, sterilize 30min at 121 DEG C; After sterilizing, it is cooled to room temperature to obtain solid medium;Strain Acetobacter xylinum NUST4.2 is connected to solid In culture medium, and constant incubator is put it into stationary culture 5-7 days at 30 DEG C, finally obtain activation bacterium;Wherein solid is trained Support base w/v: glucose 2.0%, sucrose 1.0%, peptone 1.0%, yeast extract 0.1%, agar 1.8%, sodium dihydrogen phosphate 0.25%, citric acid 0.11%, magnesium sulfate 0.04%;PH=6.0.
Further, strain Acetobacter xylinum NUST4.2 seed liquor is prepared described in step 2, specific as follows:
Required ingredient is weighed according to seed culture based formulas and adds water constant volume, is placed on and is contained in the triangular flask that liquid measure is 25%, Sterilize 30min at 121 DEG C, and sterilizing end is cooled to 30 DEG C and obtains seed culture based sols;Then, it will activate in step 1 Strain is connected to culture medium and obtains in seed culture fluid, 30 DEG C, 150r/min shaken cultivation 12h in total temperature shaken cultivation case, Obtain seed liquor;Wherein seed liquid culture medium w/v: glucose 2.0%, ammonium sulfate 0.6%, potassium dihydrogen phosphate 0.1%, magnesium sulfate 0.04%;Peptone 0.3%, yeast extract 0.225%, sodium carboxymethylcellulose 0.04%.
Further, it is added in the fermentation medium of Acetobacter xylinum NUST4.2 described in step 3 different The bamboo charcoal powder of mass volume ratio carries out static fermentation production, obtains bamboo charcoal/biology cellulose composite material, specific as follows:
Required ingredient is weighed according to fermentative medium formula and adds water constant volume, is adjusted to required pH, is 50% mounted in liquid measure is contained Triangular flask in, sterilize 30min at 121 DEG C, and sterilizing terminates to be cooled to 30 DEG C and obtain fermented and cultured based sols;It is by inoculum concentration 8% volume ratio accesses seed in fermented and cultured based sols, is then put in constant incubator and cultivates 7 days at 30 DEG C;Wherein Fermentation medium w/v: glucose 2.25%, sucrose 2.75%, ammonium sulfate 0.1%, potassium dihydrogen phosphate 0.5%, magnesium sulfate 0.07%, calcium lactate 0.02%, peptone 1.0%, yeast extract 0.75%, glacial acetic acid 0.15%, citric acid 0.06%, carboxylic first Base sodium cellulosate 0.04%, the bamboo charcoal powder of different quality volume ratio, pH=6.0;The wherein bamboo charcoal powder of different quality volume ratio point It Wei 0.01%, 0.1%, 0.2%, 0.5%, 1.0%, 2.0%.
Further, purification process is carried out to bamboo charcoal/biology cellulose composite material described in step 4, obtained spongiform Bamboo charcoal/biology cellulose composite material, specifically:
Step 3 gained bamboo charcoal/biology cellulose composite material is taken out, is rinsed for several times with tap water, then with 3 ‰ hydrogen Sodium hydroxide solution boils 2h at 80 DEG C, then is rinsed with deionized water to neutrality, and it is compound to obtain gelatinous bamboo charcoal/biology cellulose Material;The mode of bamboo charcoal/biology cellulose composite material gel freeze-drying is dry, obtain spongiform bamboo charcoal/life Fibres element composite material.
A kind of bamboo charcoal/the application of the biology cellulose composite material in facial treatment mask.
Compared with prior art, the present invention its remarkable advantage are as follows: (1) by biology compound method, in Acetobacter The bamboo charcoal powder that different quality volume fraction is added in the fermentation medium of xylinum NUST4.2 carries out life of fermenting of being association of activity and inertia It produces, has obtained the Modified Membrane of the excellent adsorption function of the good characteristic for having BC concurrently and bamboo charcoal powder;(2) to the optimal Modified Membrane of effect Spongiform film is obtained after being freeze-dried, and carries out correlated performance test to it, and porosity, gas permeability have to a certain degree Raising, and mechanical strength etc. does not decline, and meets its application as facial treatment mask.
Detailed description of the invention
Fig. 1 is moisture-vapor transmission experimental apparatus for testing schematic diagram.
Fig. 2 is scanning electron microscope (SEM) photograph, wherein (a) is BCP-BC low power SEM figure, (b) is schemed for BCP-BC high power SEM.
Specific embodiment
The invention will be further described with attached drawing with reference to embodiments.
The present invention is added in the fermentation medium of Acetobacter xylinum NUST4.2 by the compound method of biology Add the bamboo charcoal powder of different quality volume fraction to carry out fermenting and producing of being association of activity and inertia, and is existed by the compound method of biology The bamboo charcoal powder for adding different quality containing in the fermentation medium of Acetobacter xylinum NUST4.2 is association of activity and inertia Fermenting and producing has obtained having concurrently the Modified Membrane of BC good characteristic and the excellent adsorption function of bamboo charcoal powder.It is best to effect that (bamboo charcoal powder is dense Degree obtains spongiform film after being freeze-dried for Modified Membrane 1.0%), is carried out with scanning electron microscope to product morphology feature Characterization, and pair related physical performance such as porosity, hygroscopicity, penetrability test, its porosity and moisture-inhibiting as the result is shown Property has a certain upgrade relative to pure biology cellulose, and mechanical strength is not apparent from decline, can satisfy its as dressing or The application of facial mask.
Firstly, the present invention provides a kind of bamboo charcoal/biology cellulose composite materials, which is characterized in that by In the fermentation medium of Acetobacter xylinum NUST4.2, the bamboo charcoal powder of addition different quality volume ratio carries out static Fermenting and producing forms, and bamboo charcoal particle is wrapped in the reticular fiber structure of biology cellulose.The different quality volume ratio Bamboo charcoal powder, respectively 0.1%, 0.25%, 0.5%, 1.0%, 5.0%.
The present invention provides a kind of bamboo charcoal/biology cellulose composite material preparation methods, the specific steps are as follows:
Step 1, strain Acetobacter xylinum NUST4.2 is activated;
The activation of strain: weighing required ingredient according to solid culture based formulas and add water constant volume, and be adjusted to required pH, and 121 DEG C Lower sterilizing 30min.After sterilizing, liquid is poured into sterilized culture dish be cooled to room temperature to obtain solid culture while hot Base.Strain Acetobacter xylinum NUST4.2 is connected in solid medium, and puts it into constant incubator in 30 Stationary culture 3-5 days at DEG C finally obtain activation bacterium.Wherein solid medium (w/v): glucose 2.0%, sucrose 1.0%, egg White peptone 1.0%, yeast extract 0.1%, agar 1.8%, sodium dihydrogen phosphate 0.25%, citric acid 0.11%, magnesium sulfate 0.04%; PH=6.0.
Step 2, the seed liquor of strain Acetobacter xylinum NUST4.2 is prepared;
The preparation of seed liquor: weighing required ingredient according to seed culture based formulas and add water constant volume, and being placed on and containing liquid measure is 25% Triangular flask in, sterilize 30min at 121 DEG C, and sterilizing terminates to be cooled to 30 DEG C and obtain seed culture based sols.Then, in purification The strain activated is connected to obtain in seed culture fluid in workbench, 30 DEG C, 150r/min is in total temperature shaken cultivation case Shaken cultivation 12h or so, obtains seed liquor.Wherein seed liquid culture medium (w/v): glucose 2.0%, ammonium sulfate 0.6%, phosphoric acid Potassium dihydrogen 0.1%, magnesium sulfate 0.04%;Peptone 0.3%, yeast extract 0.225%, sodium carboxymethylcellulose 0.04%.
Step 3, different quality volume fraction is added in the fermentation medium of Acetobacter xylinum NUST4.2 Bamboo charcoal powder carry out fermenting and producing of being association of activity and inertia, obtain bamboo charcoal biology cellulose composite membrane;
The preparation of bamboo charcoal biology cellulose composite membrane: weighing required ingredient according to fermentative medium formula and add water constant volume, and It is adjusted to required pH, mounted in containing in the triangular flask that liquid measure is 50%, sterilize 30min at 121 DEG C, and sterilizing end is cooled to 30 DEG C and obtains Fermented and cultured based sols.It is 10% (volume ratio) by seed access fermented and cultured based sols by inoculum concentration, is then put in It is cultivated 7 days at 30 DEG C in constant incubator.Wherein glucose fermentation 2.25%, sucrose 2.75%, ammonium sulfate 0.1%, phosphoric acid Potassium dihydrogen 0.5%, magnesium sulfate 0.07%, calcium lactate 0.02%, peptone 1.0%, yeast extract 0.75%, glacial acetic acid 0.15%, citric acid 0.06%, sodium carboxymethylcellulose 0.04%, the bamboo charcoal powder of different quality volume fraction, pH=6.0.Its The bamboo charcoal powder of middle different quality volume fraction is respectively 0.1%, 0.25%, 0.5%, 1.0%, 5.0%.
Step 4, purification process is carried out to bamboo charcoal biology cellulose composite membrane;
The purifying of bamboo charcoal biology cellulose composite membrane: the optimal gel film of ferment effect is taken out, is rinsed with tap water For several times, 2h is then boiled at 80 DEG C with 3 ‰ sodium hydroxide solution, then rinsed with deionized water to neutrality, obtain gelatinous Bamboo charcoal biological cellulose membrane.It is fine that the mode that bamboo charcoal biological fiber gel is freeze-dried is dried to obtain spongiform bamboo charcoal biology Tie up plain film.
Step 5, to the shape characteristic of bamboo charcoal biology cellulose composite membrane, it is scanned electron microscope observation;
The characterization of bamboo charcoal biological composite membrane: by step 4 by dry bamboo charcoal biology cellulose membrane sample to its pattern spy Sign is scanned electron microscope observation.
Step 6, correlated performance test is carried out to bamboo charcoal biology cellulose composite membrane.
The performance test of bamboo charcoal biology cellulose composite membrane: obtained Modified Membrane BCP-BC is subjected to a series of correlation It can be such as the test of porosity, penetrability.
The specific implementation process of step 6 is as follows:
Porosity is measured by medium saturation, and bamboo charcoal biology cellulose membrane sample is cut into 2 × 1cm2Size, then It is dipped in dehydrated alcohol, after sample adsorption saturation, the ethyl alcohol on its surface is sucked with filter paper, its quality is claimed to be denoted as rapidly m.Then sample is put into drying box, until its quality no longer changes, and remembers that its quality is m1, hole is carried out according to formula (1) Gap rate.
Wherein, ε is porosity, %;D is thickness of sample, cm;ρ is the density of dehydrated alcohol, g.cm-3.
Water vapour permeability is surveyed by the transmitance (Water VBCPor Transmission Rates, WVTR) of vapor Fixed, referring in particular to the method for ASTME96/E96M-05, test device is as shown in Figure 1, including closed container 1, electronic balance 2, surveying Measuring cup 3, temperature & relative humidity indicator 4, the solution of potassium carbonate 5 being saturated.It is specific to calculate such as formula (2).
Wherein △ m is of poor quality, the g of the measuring cup of certain time interval;A is the effective area of sample film, m2;T is to survey Measure time, d.
The present invention is described in further details combined with specific embodiments below.
Embodiment 1
Step 1, the activation of strain: according to solid medium (w/v): glucose 2.0%, sucrose 1.0%, peptone 1.0%, yeast extract 0.1%, agar 1.8%, sodium dihydrogen phosphate 0.25%, citric acid 0.11%, magnesium sulfate 0.04%;PH= 6.0, it weighs required substance and water constant volume is added to prepare 200ml solution, be inoculated with, be put at 30 DEG C in clean bench after sterilizing packing is cooling Stationary culture 3-5 days, finally obtain activation bacterium.
Step 2, the preparation of seed liquor: according to seed culture based formulas: glucose 2.0%, ammonium sulfate 0.6%, di(2-ethylhexyl)phosphate Hydrogen potassium 0.1%, magnesium sulfate 0.04%;Peptone 0.3%, yeast extract 0.225%, sodium carboxymethylcellulose 0.04% weigh institute It needs ingredient to add water constant volume 50ml, is placed on and contains in the triangular flask that liquid measure is 25%, sterilize 30min at 121 DEG C, and sterilizing terminates to be cooled to 30 DEG C obtain seed culture based sols.Then, the strain activated is connected to obtain in seed culture fluid in clean work station, 30 DEG C, 150r/min shaken cultivation 12h or so in total temperature shaken cultivation case obtains seed liquor.
Step 3, the preparation of bamboo charcoal biology cellulose composite membrane: according to fermentative medium formula: glucose 2.25%, sucrose 2.75%, ammonium sulfate 0.1%, potassium dihydrogen phosphate 0.5%, magnesium sulfate 0.07%, calcium lactate 0.02%, peptone 1.0%, yeast Leaching powder 0.75%, glacial acetic acid 0.15%, citric acid 0.06%, sodium carboxymethylcellulose 0.04%, 0.01% bamboo charcoal powder weigh institute It needs ingredient to add water constant volume 50ml, and is adjusted to required pH, mounted in containing in the triangular flask that liquid measure is 50%, sterilize 20min at 121 DEG C, Sterilizing end is cooled to 30 DEG C and obtains fermented and cultured based sols.Seed is accessed into fermented and cultured for 10% (volume ratio) by inoculum concentration In based sols, then it is put in constant incubator and cultivates suitable time at 30 DEG C.
Step 4, the purifying of bamboo charcoal biology cellulose composite membrane: the gel film of fermenting and producing is taken out, is rushed with tap water It washes for several times, then boils 2h at 80 DEG C with 3 ‰ sodium hydroxide solution, then rinsed to neutrality with deionized water, obtain gel Bamboo charcoal biological cellulose membrane.It is raw that the mode that bamboo charcoal biological cellulose gel is freeze-dried is dried to obtain spongiform bamboo charcoal Fibres element film.
Embodiment 2
Steps 1 and 2 are as above.
Step 3, the preparation of bamboo charcoal biology cellulose composite membrane: according to fermentative medium formula: glucose 2.25%, sucrose 2.75%, ammonium sulfate 0.1%, potassium dihydrogen phosphate 0.5%, magnesium sulfate 0.07%, calcium lactate 0.02%, peptone 1.0%, yeast Soak powder 0.75%, glacial acetic acid 0.15%, citric acid 0.06%, sodium carboxymethylcellulose 0.04%, needed for 0.1% bamboo charcoal powder weighs Ingredient adds water constant volume 50ml, and is adjusted to required pH, and mounted in containing in the triangular flask that liquid measure is 50%, sterilize 30min at 121 DEG C, goes out Bacterium, which terminates to be cooled to 30 DEG C, obtains fermented and cultured based sols.Seed is accessed into fermentation medium for 10% (volume ratio) by inoculum concentration In solution, then it is put in constant incubator and cultivates suitable time at 30 DEG C.
Step 4, the purifying of bamboo charcoal biology cellulose composite membrane: the gel film of fermenting and producing is taken out, is rushed with tap water It washes for several times, then boils 2h at 80 DEG C with 3 ‰ sodium hydroxide solution, then rinsed to neutrality with deionized water, obtain gel Bamboo charcoal biological cellulose membrane.It is raw that the mode that bamboo charcoal biological cellulose gel is freeze-dried is dried to obtain spongiform bamboo charcoal Fibres element film.
Embodiment 3
Steps 1 and 2 are as above.
Step 3, the preparation of bamboo charcoal biological composite membrane: according to fermentative medium formula: glucose 2.25%, sucrose 2.75%, ammonium sulfate 0.1%, potassium dihydrogen phosphate 0.5%, magnesium sulfate 0.07%, calcium lactate 0.02%, peptone 1.0%, yeast Soak powder 0.75%, glacial acetic acid 0.15%, citric acid 0.06%, sodium carboxymethylcellulose 0.04%, needed for 0.2% bamboo charcoal powder weighs Ingredient adds water constant volume 50ml, and is adjusted to required pH, and mounted in containing in the triangular flask that liquid measure is 50%, sterilize 20min at 121 DEG C, goes out Bacterium, which terminates to be cooled to 30 DEG C, obtains fermented and cultured based sols.Seed is accessed into fermentation medium for 10% (volume ratio) by inoculum concentration In solution, then it is put in constant incubator and is cultivated 7 days at 30 DEG C.
Step 4, the purifying of bamboo charcoal biology cellulose composite membrane: the gel film of fermenting and producing is taken out, is rushed with tap water It washes for several times, then boils 2h at 80 DEG C with 3 ‰ sodium hydroxide solution, then rinsed to neutrality with deionized water, obtain gel Bamboo charcoal biological cellulose membrane.It is raw that the mode that bamboo charcoal biological cellulose gel is freeze-dried is dried to obtain spongiform bamboo charcoal Fibres element film.
Embodiment 4
Steps 1 and 2 are as above.
Step 3, the preparation of bamboo charcoal biological composite membrane: according to fermentative medium formula: glucose 2.25%, sucrose 2.75%, ammonium sulfate 0.1%, potassium dihydrogen phosphate 0.5%, magnesium sulfate 0.07%, calcium lactate 0.02%, peptone 1.0%, yeast Soak powder 0.75%, glacial acetic acid 0.15%, citric acid 0.06%, sodium carboxymethylcellulose 0.04%, needed for 0.5% bamboo charcoal powder weighs Ingredient adds water constant volume 50ml, and is adjusted to required pH, and mounted in containing in the triangular flask that liquid measure is 50%, sterilize 20min at 121 DEG C, goes out Bacterium, which terminates to be cooled to 30 DEG C, obtains fermented and cultured based sols.Seed is accessed into fermentation medium for 10% (volume ratio) by inoculum concentration In solution, then it is put in constant incubator and is cultivated 7 days at 30 DEG C.
Step 4, the purifying of bamboo charcoal biology cellulose composite membrane: the gel film of fermenting and producing is taken out, is rushed with tap water It washes for several times, then boils 2h at 80 DEG C with 3 ‰ sodium hydroxide solution, then rinsed to neutrality with deionized water, obtain gel Bamboo charcoal biological cellulose membrane.It is raw that the mode that bamboo charcoal biological cellulose gel is freeze-dried is dried to obtain spongiform bamboo charcoal Fibres element film.
Embodiment 5
Steps 1 and 2 are as above.
Step 3, the preparation of bamboo charcoal biology cellulose composite membrane: according to fermentative medium formula: glucose 2.25%, sucrose 2.75%, ammonium sulfate 0.1%, potassium dihydrogen phosphate 0.5%, magnesium sulfate 0.07%, calcium lactate 0.02%, peptone 1.0%, yeast Soak powder 0.75%, glacial acetic acid 0.15%, citric acid 0.06%, sodium carboxymethylcellulose 0.04%, needed for 1.0% bamboo charcoal powder weighs Ingredient adds water constant volume 50ml, and is adjusted to required pH, and mounted in containing in the triangular flask that liquid measure is 50%, sterilize 20min at 121 DEG C, goes out Bacterium, which terminates to be cooled to 30 DEG C, obtains fermented and cultured based sols.Seed is accessed into fermentation medium for 10% (volume ratio) by inoculum concentration In solution, then it is put in constant incubator and is cultivated 7 days at 30 DEG C.
Step 4, the purifying of bamboo charcoal biology cellulose composite membrane: the gel film of fermenting and producing is taken out, is rushed with tap water It washes for several times, then boils 2h at 80 DEG C with 3 ‰ sodium hydroxide solution, then rinsed to neutrality with deionized water, obtain gel Bamboo charcoal biological cellulose membrane.It is raw that the mode that bamboo charcoal biological cellulose gel is freeze-dried is dried to obtain spongiform bamboo charcoal Fibres element film.
Embodiment 6
Steps 1 and 2 are as above.
Step 3, the preparation of bamboo charcoal biology cellulose composite membrane: according to fermentative medium formula: glucose 2.25%, sucrose 2.75%, ammonium sulfate 0.1%, potassium dihydrogen phosphate 0.5%, magnesium sulfate 0.07%, calcium lactate 0.02%, peptone 1.0%, yeast Soak powder 0.75%, glacial acetic acid 0.15%, citric acid 0.06%, sodium carboxymethylcellulose 0.04%, needed for 2.0% bamboo charcoal powder weighs Ingredient adds water constant volume 50ml, and is adjusted to required pH, and mounted in containing in the triangular flask that liquid measure is 50%, sterilize 20min at 121 DEG C, goes out Bacterium, which terminates to be cooled to 30 DEG C, obtains fermented and cultured based sols.Seed is accessed into fermentation medium for 10% (volume ratio) by inoculum concentration In solution, then it is put in constant incubator and is cultivated 7 days at 30 DEG C.
Step 4, the purifying of bamboo charcoal biology cellulose composite membrane: the gel film of fermenting and producing is taken out, is rushed with tap water It washes for several times, then boils 2h at 80 DEG C with 3 ‰ sodium hydroxide solution, then rinsed to neutrality with deionized water, obtain gel Bamboo charcoal biological cellulose membrane.It is raw that the mode that bamboo charcoal biological cellulose gel is freeze-dried is dried to obtain spongiform bamboo charcoal Fibres element film.
Embodiment 6
Through the multiple above experimental verification bamboo charcoal powder at 1.0%, effect is best, therefore to bamboo charcoal powder quality volume fraction A series of characterizations and test have been done when being 1.0%.It is specific as follows:
Step 1, the bamboo charcoal biology cellulose composite membrane obtained by embodiment 5 is cut into the sample of 2mm × 2mm, in its table Face metal spraying is placed under scanning electron microscope JSM-6380LV type and observes its pattern, acceleration voltage 30KV.
Step 2, porosity is surveyed by medium saturation, bamboo charcoal biology cellulose composite membrane sample is cut into 1 × 2cm2Greatly It is small, it is then immersed in dehydrated alcohol, after sample adsorption saturation, is drawn off, the ethyl alcohol on surface is sucked with filter paper, it is fast Speed claims its quality to be denoted as m.Then sample is put into drying box, until its quality no longer changes, and remembers that its quality is m1, according to Formula (1) carries out porosity.
Embodiment 7
Step 1, multiple groups measurement water is carried out to bamboo charcoal biology cellulose composite membrane referring to the method for ASTME96/E96M-05 to steam Vapor permeability experiment, is finally averaged, as last evaluation result.Device figure is added into measuring cup appropriate as shown in Figure 1: Distilled water, then seals rim of a cup with certain thickness sample film, and the effective area of sample film is 66.58cm2.Cup is put into one In closed container, same measuring cup is open, as control.Suitable unsaturated carbonate potassium solution is placed in closed container to tie up Certain relative humidity is held, while putting a temperature & relative humidity indicator (test temperature is to measure the temperature and humidity in closed container 30 ± 1 DEG C, relative humidity is about 50 ± 5%).Vapor can be determined by the variable quantity of the gross mass of measurement measuring cup Transit dose, specific calculate press formula (2).
Interpretation of result is as follows: by Fig. 2 (a) it can be seen that, the upper uniform load of BC bamboo charcoal powder, and have a certain number of holes Hole.It can be seen that bamboo charcoal particle and fiber have good combination from Fig. 2 (b), and remain as three-dimensional mesh structural porous knot Structure, fiber winding is close, mesh-structured intensive, illustrates that the incorporation of bamboo charcoal powder does not have an impact the reticular structure of BC.
The test result of step 6 porosity is as shown in table 1
Table 1.BC-Foam, BCP-BC-Foam porosity test result
From table 1 it follows that modified bamboo charcoal biology cellulose composite membrane has preferable porosity, as dressing And facial mask, can have good hygroscopicity, be conducive to liquid infiltration and nutriment and metabolic waste fully absorb and Discharge etc..
The test result of step 6 penetrability is as shown in table 2
2 biology cellulose composite membrane of table, bamboo charcoal biology cellulose composite membrane penetrability test result
Good penetrability allows skin absorbing the breathing that can guarantee skin while nutrition, while reasonable penetrability Nutrient solution can be prevented excessively to be lost and cause wasting phenomenon.Modified bamboo charcoal biology cellulose is compound as can be seen from Table 2 The penetrability of film increases, but as facial mask, can also make moderate progress.

Claims (8)

1. a kind of bamboo charcoal/biology cellulose composite material, which is characterized in that by Acetobacter xylinum In the fermentation medium of NUST4.2, the bamboo charcoal powder of addition different quality volume ratio carries out static fermentation and produces, bamboo charcoal particle It is wrapped in the reticular fiber structure of biology cellulose.
2. bamboo charcoal according to claim 1/biology cellulose composite material, which is characterized in that the different quality volume The bamboo charcoal powder of ratio, respectively 0.1%, 0.25%, 0.5%, 1.0%, 5.0%.
3. a kind of preparation method of bamboo charcoal of any of claims 1 or 2/biology cellulose composite material, which is characterized in that including Following steps:
Step 1, activated spawn Acetobacter xylinum NUST4.2;
Step 2, strain Acetobacter xylinum NUST4.2 seed liquor is prepared;
Step 3, the bamboo charcoal of different quality volume ratio is added in the fermentation medium of Acetobacter xylinum NUST4.2 Powder carries out static fermentation production, obtains bamboo charcoal/biology cellulose composite material;
Step 4, purification process is carried out to bamboo charcoal/biology cellulose composite material, it is multiple obtains spongiform bamboo charcoal/biology cellulose Condensation material.
4. bamboo charcoal according to claim 3/biology cellulose composite material preparation method, which is characterized in that step 1 institute Activated spawn Acetobacter xylinum NUST4.2 is stated, specific as follows:
Required ingredient is weighed according to solid culture based formulas and adds water constant volume, is adjusted to required pH, sterilize 30min at 121 DEG C;Sterilizing After, it is cooled to room temperature to obtain solid medium;Strain Acetobacter xylinum NUST4.2 is connected to solid culture In base, and constant incubator is put it into stationary culture 5-7 days at 30 DEG C, finally obtain activation bacterium;Wherein solid medium W/v: glucose 2.0%, sucrose 1.0%, peptone 1.0%, yeast extract 0.1%, agar 1.8%, sodium dihydrogen phosphate 0.25%, citric acid 0.11%, magnesium sulfate 0.04%;PH=6.0.
5. bamboo charcoal according to claim 3/biology cellulose composite material preparation method, which is characterized in that step 2 institute It states and prepares strain Acetobacter xylinum NUST4.2 seed liquor, specific as follows:
Required ingredient is weighed according to seed culture based formulas and adds water constant volume, is placed on and is contained in the triangular flask that liquid measure is 25%, 121 DEG C Lower sterilizing 30min, sterilizing end are cooled to 30 DEG C and obtain seed culture based sols;Then, the strain activated in step 1 is connect It is obtained in seed culture fluid to culture medium, 30 DEG C, 150r/min shaken cultivation 12h in total temperature shaken cultivation case are planted Sub- liquid;Wherein seed liquid culture medium w/v: glucose 2.0%, ammonium sulfate 0.6%, potassium dihydrogen phosphate 0.1%, magnesium sulfate 0.04%;Peptone 0.3%, yeast extract 0.225%, sodium carboxymethylcellulose 0.04%.
6. bamboo charcoal according to claim 3/biology cellulose composite material preparation method, which is characterized in that step 3 institute The bamboo charcoal powder progress for stating the addition different quality volume ratio in the fermentation medium of Acetobacter xylinum NUST4.2 is quiet State fermenting and producing obtains bamboo charcoal/biology cellulose composite material, specific as follows:
Required ingredient is weighed according to fermentative medium formula and adds water constant volume, is adjusted to required pH, mounted in three that Sheng liquid measure is 50% In the bottle of angle, sterilize 30min at 121 DEG C, and sterilizing end is cooled to 30 DEG C and obtains fermented and cultured based sols;It is 8% body by inoculum concentration Then product is put in constant incubator and cultivates 7 days at 30 DEG C than accessing seed in fermented and cultured based sols;Wherein fermentation training Support base w/v: glucose 2.25%, sucrose 2.75%, ammonium sulfate 0.1%, potassium dihydrogen phosphate 0.5%, magnesium sulfate 0.07%, lactic acid Calcium 0.02%, peptone 1.0%, yeast extract 0.75%, glacial acetic acid 0.15%, citric acid 0.06%, sodium carboxymethylcellulose 0.04%, the bamboo charcoal powder of different quality volume ratio, pH=6.0;Wherein the bamboo charcoal powder of different quality volume ratio be respectively 0.01%, 0.1%, 0.2%, 0.5%, 1.0%, 2.0%.
7. bamboo charcoal according to claim 1/biology cellulose composite material preparation method, which is characterized in that step 4 institute It states and purification process is carried out to bamboo charcoal/biology cellulose composite material, obtain spongiform bamboo charcoal/biology cellulose composite material, Specifically:
Step 3 gained bamboo charcoal/biology cellulose composite material is taken out, is rinsed for several times with tap water, then with 3 ‰ hydroxide Sodium solution boils 2h at 80 DEG C, then is rinsed with deionized water to neutrality, obtains gelatinous bamboo charcoal/biology cellulose composite wood Material;The mode of bamboo charcoal/biology cellulose composite material gel freeze-drying is dry, obtain spongiform bamboo charcoal/biology Cellulose composite material.
8. a kind of bamboo charcoal as claimed in claim 1 or 2/application of the biology cellulose composite material in facial treatment mask.
CN201710428104.6A 2017-06-08 2017-06-08 A kind of bamboo charcoal/biology cellulose composite material and preparation method and application Pending CN109021296A (en)

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CN110960470A (en) * 2019-12-20 2020-04-07 北京致成生物医学科技有限公司 Mask with photo-thermal effect and preparation method thereof
CN112754944A (en) * 2019-11-05 2021-05-07 钟春燕 Bio-cellulose-based skin cleaning product and preparation method and application thereof
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Application publication date: 20181218