CN107383435A - A kind of fresh-keeping preparation method for carrying medicine sponge of Cellulose/Chitosan base nanometer - Google Patents
A kind of fresh-keeping preparation method for carrying medicine sponge of Cellulose/Chitosan base nanometer Download PDFInfo
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- CN107383435A CN107383435A CN201710657428.7A CN201710657428A CN107383435A CN 107383435 A CN107383435 A CN 107383435A CN 201710657428 A CN201710657428 A CN 201710657428A CN 107383435 A CN107383435 A CN 107383435A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
- C08L1/26—Cellulose ethers
- C08L1/28—Alkyl ethers
- C08L1/286—Alkyl ethers substituted with acid radicals, e.g. carboxymethyl cellulose [CMC]
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0482—Elimination of a frozen liquid phase the liquid phase being organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
The present invention relates to a kind of fresh-keeping preparation method for carrying medicine sponge of Cellulose/Chitosan base nanometer, belong to packaging material for food technical field.The present invention is using sodium carboxymethylcellulose and chitosan as main base material.The step of its preparation method, includes：First by sodium carboxymethylcellulose and chitosan in certain mass ratio dissolve respectively with distilled water and acetic acid solution, then two kinds of solution are blended, the use of salt acid for adjusting pH value is 1.0, add antibacterial factor nano titanium oxide, ethylene absorption factor bentonite and plasticizer glycerine, it is sufficiently stirred, defoaming is stood, finally pours into mould, sponge products are formed through vacuum freeze-drying.The product is nontoxic, biodegradable, is environmentally friendly product；The product adds the nano-antibacterial factor and the ethylene absorption factor, while possessing filling sponge basic mechanical damping performance, has had excellent bacteriostasis, preservation effect concurrently.
Description
Technical field
The invention belongs to packaging material for food technical field, is related to a kind of preparation method of sponginess material, more particularly to
A kind of preparation method of the biodegradable packaging filling sponge with bacteriostasis, preservation effect.
Background technology
With problem of environmental pollution getting worse, nonhazardous, degradable, green packaging material turn into current and ground
Study carefully focus.All the time, the preservation technology of traditional tropical fruit (tree) is relied primarily on to the medicament immersion of fruit and petroleum source plastics
The use of product.Although the method for medicament immersion is simple efficiently, there is harm of the medicament residual to health and risk；
It is plastics packed that caused food-safety problem is migrated to food using on the one hand there is small organic molecule, on the other hand
It also result in the consumption of the energy and the pollution of environment.
Sodium carboxymethylcellulose（CMC）It is a kind of cellulose derivative using natural fiber mass as raw material, has good
Biocompatibility, wetability, dispersiveness, cementability, thickening property, emulsibility, water-retaining property and film forming, it is and nontoxic, it is raw
Biodegradable；CMC aquogel system is that a kind of covalent bond, hydrogen bond, Van der Waals force and physics by between macromolecule twines
The spacial framework that the crosslinked actions such as knot are formed, therefore have using CMC as polymer composite prepared by base material excellent
Mechanical performance.Chitosan（Chitosan, CS）Also known as chitosan, poly glucosamine, it is to be widely present by nature
Chitin obtained by deacetylation.The chemical name of chitosan is β-(1,4) -2- amino -2- deoxidation-D- grapes
Sugar, simultaneously containing hydroxyl and carboxyl, therefore the two can pass through phenolate, carboxylated, esterification, alkanisation, halogenation, oxidation, hydrolysis, chela
The reactions such as conjunction, grafting and crosslinking generate a series of different structures and the derivative of performance.Meanwhile as natural biological polysaccharide crust
There is free amino group in the deacetylation derivative of matter, chitosan, physicochemical property is very active, have have no toxic side effect, biofacies
Capacitive is good, biodegradation is controllable and the characteristic such as no antigen.Therefore, chitosan delays in biomedicine, organizational project, medicine
Release, all many-sides such as cell and enzyme immobilizatio suffer from quite varied application.In recent years, the good processing of chitosan is utilized
Property and antibacterial activity, it is relatively broad to prepare the correlative study of degradable sponge material using chitosan as raw material, such as Chinese patent
The chitosan sponge for clinical medicine purpose that CN200610036069 and CN200710031328 is announced, but such material
The biocidal property of material is only having the situation for going deep into brought into interactive contact just to have good embodiment with biosystem, for food packaging applications
Speech, although chitosan-based degradable package material can be effectively increased CO in fruits and vegetables tissue2Content, reduce O2Content, suppress breathing
Effect and moisture loss, slow down fruits and vegetables tissue and mechanism aging, but its antiseptic and inhibiting bacteria function characteristic can not but give full play to so that this
The excellent specific property of one potential packaging material for food is had a greatly reduced quality.
The content of the invention
The present invention is directed to the existing issue for the chitosan fresh preservation material mentioned in background technology, in order to give full play to shell
The good antiseptic and inhibiting bacteria function characteristic of poly- saccharide material, there is provided a kind of Cellulose/Chitosan base nanometer is fresh-keeping to carry medicine sponge and its preparation
Method, it is characterized mainly in that and adds nano titanium oxide as antimicrobial factorses, this outstanding food preservative can be with
Acted synergistically with glycan substrate, extend the freshness date of packaged food.
The purpose of the present invention can be achieved through the following technical solutions：A kind of fresh-keeping load medicine of Cellulose/Chitosan base nanometer
The preparation method of the preparation method of sponge, it is characterised in that this method comprises the following steps：
（1）Sodium carboxymethylcellulose is dissolved in distilled water, carboxymethylcellulose sodium solution is formed, it is molten that chitosan is dissolved in acetic acid
Liquid, the pH value of two kinds of solution is adjusted using hydrochloric acid；
（2）By step（1）In two kinds of solution blendings, and add nano titanium oxide, bentonite, glycerine, stir, stand
Defoaming；
（3）By step（2）Obtained mixed liquor is poured into mould, and the sponge products of the present invention are obtained through vacuum freeze drying.
Step（1）Described in the substitution value of sodium carboxymethylcellulose be 0.7 ~ 1.2, the deacetylation of chitosan for 50 ~
95%.Described mass ratio is carboxymethyl cellulose：Chitosan is 2 ~ 5:1；
Step（1）Described in solution ph scope be 1.0-4.0；
Step（2）Described in nano titanium oxide granularity be 50-400 nm, addition is the 1 ~ 10% of total solid yield, swelling
Native density is 2 ~ 3 g/cm3, addition is the 1 ~ 6% of total solid yield, and glycerine input is the 1 ~ 8% of total solid yield；
Step（3）Described in mould be polystyrene material prepare mould.
The present invention compared with prior art, has the advantage that：
（1）The base material sodium carboxymethylcellulose and chitosan that the present invention uses are biomass polymer substance, are had well
Filming performance is crosslinked, the sponge of formation has uniform spacial framework, not only possesses excellent buffer capacity, resist simultaneously
Bacteria factor nano titanium oxide and ethylene absorption factor bentonite also have good load and controlled release ability.
（2）One of the base material of present invention chitosan has natural bacteriostatic activity, the function factor nanometer titanium dioxide of addition
Titanium also has excellent bacteriostasis, and bentonite is excellent ethene adsorbent.Therefore the sponge products are possessing mechanical damping
While function, have anti-bacterial refreshing concurrently, delay the effect of corruption.Following table experimental result shows that part Common Fruits are Celsius 15
Spend under environment using general sponge net, chitosan sponge, the freshness date of nano titanium oxide chitosan sponge packaging（Sample size：
20, average in table）：
（3）Biomass polymer composite and medicament slow release technology are applied to packaging for foodstuff packing material field by the present invention,
Meet the developing direction of green material, there is important social and economic benefit.
Embodiment
Embodiment 1：
（1）In mass ratio 2:1 weighs sodium carboxymethylcellulose and Chitosan powder；The substitution value of wherein sodium carboxymethylcellulose is
0.7, the deacetylation of chitosan is 50%, and sodium carboxymethylcellulose is dissolved in distilled water, forms 2% sodium carboxymethylcellulose
Solution, chitosan is dissolved in acetic acid solution, forms the chitosan solution that concentration is 1.5%, the pH of two kinds of solution is adjusted using hydrochloric acid
It is worth to 1.0；
（2）By step（1）In two kinds of solution blendings, and add nano titanium oxide, bentonite, glycerine, stir, stand
Defoaming；Wherein, nano titanium oxide granularity is 60 nm, and addition is the 1% of total solid yield, and bentonite density is 2 ~ 3 g/
Cm3, addition are the 6% of total solid yield, and glycerine input is the 4% of total solid yield；
（3）By step（2）Obtained mixed liquor is poured into mould, and the sponge products of the present invention are obtained through vacuum freeze drying.
Embodiment 2：
（1）In mass ratio 3:1 weighs sodium carboxymethylcellulose and Chitosan powder；The substitution value of wherein sodium carboxymethylcellulose is
0.8, the deacetylation of chitosan is 60%, and sodium carboxymethylcellulose is dissolved in distilled water, forms 2% sodium carboxymethylcellulose
Solution, chitosan is dissolved in acetic acid solution, forms the chitosan solution that concentration is 1.5%, the pH of two kinds of solution is adjusted using hydrochloric acid
It is worth to 1.0；
（2）By step（1）In two kinds of solution blendings, and add nano titanium oxide, bentonite, glycerine, stir, stand
Defoaming；Wherein, nano titanium oxide granularity is 150 nm, and addition is the 4% of total solid yield, and bentonite density is 2 ~ 3 g/
Cm3, addition are the 4% of total solid yield, and glycerine input is the 4% of total solid yield；
（3）By step（2）Obtained mixed liquor is poured into mould, and the sponge products of the present invention are obtained through vacuum freeze drying.
Embodiment 3：
（1）In mass ratio 4:1 weighs sodium carboxymethylcellulose and Chitosan powder；The substitution value of wherein sodium carboxymethylcellulose is
0.7, the deacetylation of chitosan is 50%, and sodium carboxymethylcellulose is dissolved in distilled water, forms 2% sodium carboxymethylcellulose
Solution, chitosan is dissolved in acetic acid solution, forms the chitosan solution that concentration is 1.5%, the pH of two kinds of solution is adjusted using hydrochloric acid
It is worth to 1.0；
（2）By step（1）In two kinds of solution blendings, and add nano titanium oxide, bentonite, glycerine, stir, stand
Defoaming；Wherein, nano titanium oxide granularity is 60 nm, and addition is the 7% of total solid yield, and bentonite density is 2 ~ 3 g/
Cm3, addition are the 2% of total solid yield, and glycerine input is the 4% of total solid yield；
（3）By step（2）Obtained mixed liquor is poured into mould, and the sponge products of the present invention are obtained through vacuum freeze drying.
Embodiment 4：
（1）In mass ratio 5:1 weighs sodium carboxymethylcellulose and Chitosan powder；The substitution value of wherein sodium carboxymethylcellulose is
0.7, the deacetylation of chitosan is 50%, and sodium carboxymethylcellulose is dissolved in distilled water, forms 2% sodium carboxymethylcellulose
Solution, chitosan is dissolved in acetic acid solution, forms the chitosan solution that concentration is 1.5%, the pH of two kinds of solution is adjusted using hydrochloric acid
It is worth to 1.0；
（2）By step（1）In two kinds of solution blendings, and add nano titanium oxide, bentonite, glycerine, stir, stand
Defoaming；Wherein, nano titanium oxide granularity is 200 nm, and addition is the 10% of total solid yield, and bentonite density is 2 ~ 3 g/
Cm3, addition are the 1% of total solid yield, and glycerine input is the 4% of total solid yield；
（3）By step（2）Obtained mixed liquor is poured into mould, and the sponge products of the present invention are obtained through vacuum freeze drying.
Embodiment 5：
（1）In mass ratio 2:1 weighs sodium carboxymethylcellulose and Chitosan powder；The substitution value of wherein sodium carboxymethylcellulose is
0.7, the deacetylation of chitosan is 50%, and sodium carboxymethylcellulose is dissolved in distilled water, forms 2% sodium carboxymethylcellulose
Solution, chitosan is dissolved in acetic acid solution, forms the chitosan solution that concentration is 1.5%, the pH of two kinds of solution is adjusted using hydrochloric acid
It is worth to 2.0；
（2）By step（1）In two kinds of solution blendings, and add nano titanium oxide, bentonite, glycerine, stir, stand
Defoaming；Wherein, nano titanium oxide granularity is 170 nm, and addition is the 1% of total solid yield, and bentonite density is 2 ~ 3 g/
Cm3, addition are the 6% of total solid yield, and glycerine input is the 8% of total solid yield；
（3）By step（2）Obtained mixed liquor is poured into mould, and the sponge products of the present invention are obtained through vacuum freeze drying.
Embodiment 6：
（1）In mass ratio 3:1 weighs sodium carboxymethylcellulose and Chitosan powder；The substitution value of wherein sodium carboxymethylcellulose is
0.8, the deacetylation of chitosan is 60%, and sodium carboxymethylcellulose is dissolved in distilled water, forms 2% sodium carboxymethylcellulose
Solution, chitosan is dissolved in acetic acid solution, forms the chitosan solution that concentration is 1.5%, the pH of two kinds of solution is adjusted using hydrochloric acid
It is worth to 4.0；
（2）By step（1）In two kinds of solution blendings, and add nano titanium oxide, bentonite, glycerine, stir, stand
Defoaming；Wherein, nano titanium oxide granularity is 80 nm, and addition is the 4% of total solid yield, and bentonite density is 2 ~ 3 g/
Cm3, addition are the 4% of total solid yield, and glycerine input is the 8% of total solid yield；
（3）By step（2）Obtained mixed liquor is poured into mould, and the sponge products of the present invention are obtained through vacuum freeze drying.
Embodiment 7：
（1）In mass ratio 4:1 weighs sodium carboxymethylcellulose and Chitosan powder；The substitution value of wherein sodium carboxymethylcellulose is
0.7, the deacetylation of chitosan is 50%, and sodium carboxymethylcellulose is dissolved in distilled water, forms 2% sodium carboxymethylcellulose
Solution, chitosan is dissolved in acetic acid solution, forms the chitosan solution that concentration is 1.5%, the pH of two kinds of solution is adjusted using hydrochloric acid
It is worth to 3.0；
（2）By step（1）In two kinds of solution blendings, and add nano titanium oxide, bentonite, glycerine, stir, stand
Defoaming；Wherein, nano titanium oxide granularity is 120 nm, and addition is the 7% of total solid yield, and bentonite density is 2 ~ 3 g/
Cm3, addition are the 2% of total solid yield, and glycerine input is the 8% of total solid yield；
（3）By step（2）Obtained mixed liquor is poured into mould, and the sponge products of the present invention are obtained through vacuum freeze drying.
Embodiment 8：
（1）In mass ratio 5:1 weighs sodium carboxymethylcellulose and Chitosan powder；The substitution value of wherein sodium carboxymethylcellulose is
0.7, the deacetylation of chitosan is 50%, and sodium carboxymethylcellulose is dissolved in distilled water, forms 2% sodium carboxymethylcellulose
Solution, chitosan is dissolved in acetic acid solution, forms the chitosan solution that concentration is 1.5%, the pH of two kinds of solution is adjusted using hydrochloric acid
It is worth to 2.0；
（2）By step（1）Two kinds of solution blendings, and add nano titanium oxide, bentonite, glycerine, stir, standing disappears
Bubble；Wherein, nano titanium oxide granularity is 70 nm, and addition is the 10% of total solid yield, and bentonite density is 2 ~ 3 g/
Cm3, addition are the 1% of total solid yield, and glycerine input is the 8% of total solid yield；
（3）By step（2）Obtained mixed liquor is poured into mould, and the sponge products of the present invention are obtained through vacuum freeze drying.
Claims (5)
1. the fresh-keeping preparation method for carrying medicine sponge of a kind of Cellulose/Chitosan base nanometer, it is characterised in that this method includes following
Step：
（1）Sodium carboxymethylcellulose is dissolved in distilled water, carboxymethylcellulose sodium solution is formed, it is molten that chitosan is dissolved in acetic acid
Liquid, the pH value of two kinds of solution is adjusted using hydrochloric acid；
（2）By step（1）In two kinds of solution blendings, and add nano titanium oxide, bentonite, glycerine, stir, stand
Defoaming；
（3）By step（2）Obtained mixed liquor is poured into mould, and the sponge products of the present invention are obtained through vacuum freeze drying.
2. according to the method for claim 1, it is characterised in that step（1）Described in sodium carboxymethylcellulose substitution value
For 0.7 ~ 1.2, the deacetylation of chitosan is 50 ~ 95%；Described mass ratio is carboxymethyl cellulose：Chitosan is 2 ~ 5:
1。
3. according to the method for claim 1, it is characterised in that step（2）Described in solution ph scope be 1.0-4.0.
4. according to the method for claim 1, it is characterised in that step（3）Described in nano titanium oxide particle size range be
50-400 nm, addition are the 1 ~ 10% of total solid yield, and bentonite density is 2 ~ 3 g/cm3, and addition is total solid yield
1 ~ 6%, glycerine input be total solid yield 1 ~ 8%.
5. according to the method for claim 1, it is characterised in that step（4）Described in mould be polystyrene material prepare
Mould.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710657428.7A CN107383435B (en) | 2017-08-03 | 2017-08-03 | Preparation method of cellulose/chitosan-based nano fresh-keeping drug-loaded sponge |
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| CN201710657428.7A CN107383435B (en) | 2017-08-03 | 2017-08-03 | Preparation method of cellulose/chitosan-based nano fresh-keeping drug-loaded sponge |
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| CN107383435B CN107383435B (en) | 2020-07-24 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109880181A (en) * | 2019-03-26 | 2019-06-14 | 宋海军 | A kind of mould proof hydrophobic type sponge and preparation method thereof |
| CN111357767A (en) * | 2020-04-03 | 2020-07-03 | 祁海强 | Preparation method of high-dispersion anti-discoloration nano-silver antibacterial agent material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109880181A (en) * | 2019-03-26 | 2019-06-14 | 宋海军 | A kind of mould proof hydrophobic type sponge and preparation method thereof |
| CN111357767A (en) * | 2020-04-03 | 2020-07-03 | 祁海强 | Preparation method of high-dispersion anti-discoloration nano-silver antibacterial agent material |
| CN111357767B (en) * | 2020-04-03 | 2021-02-23 | 李建勋 | Preparation method of high-dispersion anti-discoloration nano-silver antibacterial agent material |
| CN112438274A (en) * | 2020-04-03 | 2021-03-05 | 祁海强 | Preparation method of high-dispersion anti-discoloration nano-silver antibacterial agent material |
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| CN107383435B (en) | 2020-07-24 |
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