CN105997573A - Marine polysaccharide in-situ coated nano-iron composite material and preparation method thereof - Google Patents
Marine polysaccharide in-situ coated nano-iron composite material and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
- A61K8/86—Polyethers
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/20—Halogens; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/23—Sulfur; Selenium; Tellurium; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/65—Collagen; Gelatin; Keratin; Derivatives or degradation products thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/736—Chitin; Chitosan; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
- C11D9/22—Organic compounds, e.g. vitamins
- C11D9/26—Organic compounds, e.g. vitamins containing oxygen
- C11D9/262—Organic compounds, e.g. vitamins containing oxygen containing carbohydrates
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/10—General cosmetic use
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Abstract
The invention discloses a marine polysaccharide in-situ coated nano-iron composite material and a preparation method thereof. The method includes the following steps that firstly, a ferrite aqueous solution is prepared from ferrite; secondly, marine polysaccharide is dissolved in a 0.05-0.5% nitric acid solution to obtain a marine polysaccharide nitric acid solution; thirdly, the marine polysaccharide nitric acid solution is added into the ferrite aqueous solution, and then polyethylene glycol is added to be evenly stirred; fourthly, a sodium borohydride aqueous solution is added and stirred to obtain the marine polysaccharide coated nano-iron composite material. The preparation method of the marine polysaccharide in-situ coated nano-iron composite material is mild in reaction condition and easy to operate, raw materials are obtained from natural marine polysaccharide, rich and easy to obtain, and the prepared marine polysaccharide in-situ coated nano-iron composite material is free of toxicity, good in safety and capable of being used in the field of cosmetics.
Description
Technical field
The present invention relates to field of nano material preparation, particularly to a kind of marine polysaccharide in-stiu coating Nanoscale Iron
Composite and preparation method thereof.
Background technology
Nanoscale Iron has the strongest reproducibility, and the surface area that compares is big, applies more in terms of water purification.So
And nano-iron particle is very easy under the effect of water occur oxidation reaction, generates ferrum oxide, not only lose
Original effectiveness, and the rust of redness can have a strong impact on the outward appearance of product.Therefore must protect
Process.Cladding document about Nanoscale Iron mainly has carbon cladding and coated with silica two kinds, but all makes
By inorganic material, Nanoscale Iron is coated with, and inorganic material coating nano-iron particle is generally not capable of preventing completely
Only Nanoscale Iron oxidation.
The method using organic material to be coated with Nanoscale Iron is typically with polymer such as polyethylene
(PE)-polyisobutylene-TEPA cladding, polystyrene (PS)-TEPA cladding etc..But, these methods have
Following defect: use macromolecule organic, itself be difficult to degrade, or it is easily sedimentation, and may
There is unknowable bio-toxicity, if applying to cosmetic field, it is possible to create hazardness.
Summary of the invention
Present invention aim to address the defect of organic material cladding Nanoscale Iron in prior art, it is provided that a kind of
The preparation method of marine polysaccharide in-stiu coating Nanoscale Iron composite, its reaction condition is gentle, low cost,
The coating formed is stable, had good sustained release effect.
In order to achieve the above object, the invention provides a kind of marine polysaccharide in-stiu coating Nanoscale Iron composite wood
The preparation method of material, the method includes:
Step 1, uses ferrous salt to prepare perferrite solution；
Step 2, is dissolved in marine polysaccharide in the salpeter solution of 0.05%-0.5%, obtains marine polysaccharide nitre
Acid solution；
Step 3, joins in perferrite solution by described marine polysaccharide salpeter solution, adds poly-
Ethylene glycol, stirs；
Step 4, adds sodium borohydride aqueous solution, stirring, obtains the Nanoscale Iron of marine polysaccharide cladding；
Described marine polysaccharide at least contains any one coordinating group in hydroxyl, amino or carboxyl.
The preparation method of above-mentioned marine polysaccharide in-stiu coating Nanoscale Iron composite, wherein, described Asia
Iron salt selects ferrous sulfate or ferrous chloride or the mixture of the two.
The preparation method of above-mentioned marine polysaccharide in-stiu coating Nanoscale Iron composite, wherein, described sea
Ocean polysaccharide is natural marine polysaccharide.
The preparation method of above-mentioned marine polysaccharide in-stiu coating Nanoscale Iron composite, wherein, described sea
Ocean polysaccharide selects at least one in chitosan, gelatin, carrageenan, agar.
The mixing time of step 4 is 30-120min.
The preparation method of above-mentioned marine polysaccharide in-stiu coating Nanoscale Iron composite, wherein, described step
Rapid 4 post-processing steps also comprising routine.
The preparation method of above-mentioned marine polysaccharide in-stiu coating Nanoscale Iron composite, wherein, described step
Rapid 4 also comprise: centrifugal treating, be filtered, washed and dried step.
The preparation method of above-mentioned marine polysaccharide in-stiu coating Nanoscale Iron composite, wherein, described washes
Wash that solvent selects in water, ethanol or ethanol water any one more than.
The preparation method of above-mentioned marine polysaccharide in-stiu coating Nanoscale Iron composite, wherein, step 1,
All use protective atmosphere during step 3 and step 4, keep anaerobic state.
The preparation method of above-mentioned marine polysaccharide in-stiu coating Nanoscale Iron composite, wherein, described guarantor
Protect atmosphere and refer to nitrogen or argon.
Present invention also offers a kind of system using above-mentioned marine polysaccharide in-stiu coating Nanoscale Iron composite
Marine polysaccharide in-stiu coating Nanoscale Iron composite prepared by Preparation Method, its particle diameter is nanoscale
Chitosan (chitosan), also known as chitosan, is the chitin being widely present by nature
(chitin) obtaining through deacetylation, chemical name is Chitosan (1-4)-2-amino-B-D Fructus Vitis viniferae
Sugar, molecular formula is as follows:
Its odorless, tasteless, avirulence.Because of in chitosan molecule with active hydroxyl and amino, have stronger
Chemical reaction ability.Under given conditions, chitosan can hydrolyze, alkylation, acylation,
Carboxy methylation, sulfonation, nitrification, halogenation, aoxidize, reduce, be condensed and the chemical reaction such as complexation, can give birth to
Become the various chitosan derivatives with different performance, and there is good water-retaining property and chemical stability.
It has been investigated that, Chitosan-phospholipid complex has good antibiotic property, non-oxidizability, electrolyte absorption
Ability.Chitosan with in its molecule containing the increasing of amino quantity, its amino characteristic is the most notable, this just its
The place of peculiar property, has thus established many biological characteristicses and the basis of processing characteristics of chitosan.
Gelatin mainly comprise the mixing of peptide molecule that molecular weight distribution is the widest for aminoacid composition is identical
Thing, molecular weight is typically several ten thousand to tens0000.Being the natural macromolecule amylose of a kind of nature, gelatin is
Hydrophilic colloid, belongs to ampholyte, has foaming and the effect of steady bubble, and has retentiveness,
The functional characteristic that film property and emulsibility etc. are excellent.
The polysaccharide sulfuric ester that the chemical constitution of carrageenan is made up of galactose and Anhydrogalactose.
Calcium, potassium, magnesium, ammonium salt.Molecular formula is (C12H18O9) n, white or light brown granule or powder,
Odorless or micro-smelly, mouthfeel stick-slip.It is dissolved in 80 DEG C water, forms viscosity, transparent or slight milky
Easy fluent solution.It has thickening property, potassium ion exist can generate heat-convertible gel, can with Konjac glucomannan,
Xanthan gum isocolloid produces synergism, improves elasticity and the water-retaining property of gel.
Agar is colourless, amorphous solid, is dissolved in hot water.It is usually used in food industry, it is possible to substantially change
Become the quality of food, improve the class of food.There is coagulability, stability, can be formed with some materials
The physicochemical properties such as complex, stability, as thickening agent, coagulator, suspending agent, emulsifying agent,
Antistaling agent and stabilizer.
Polyethylene Glycol has another name called the polymer of α-hydrogen-ω-hydroxyl.Progressively added with water or ethylene glycol by oxirane
One-tenth is polymerized.Nontoxic, nonirritant, mildly bitter flavor, there is good water solublity, excellent lubricity,
Moisture retention, dispersibility, bonding agent, antistatic behaviour also have good intermiscibility etc. with many organic matter components.
Nontoxic, and to skin eyes without obvious stimulation.
The present invention uses and at least contains the marine polysaccharide of any one coordinating group in hydroxyl, amino or carboxyl
Carry out cladding protection.Because those marine polysaccharide macromolecular structures are joined containing hydroxyl, amino or carboxyl etc.
Position group, and marine polysaccharide itself has good tunicle, gelling, stability, can be with nanometer
Ferrum forms stronger coordination combination, forms tight clad on Nanoscale Iron surface, can be preferably
Protection Nanoscale Iron, plays the effect of inhibition.
The preparation method reaction condition that the present invention provides is gentle, and easy and simple to handle, raw material comes from marine natural
Polysaccharide, rich and easy to get, and prepare marine polysaccharide in-stiu coating Nanoscale Iron composite there is no toxicity, peace
Good perfection.Use natural marine Polysaccharide-coated Nanoscale Iron, be easily formed stable coordination compound, prevent Nanoscale Iron
Ineffective because reuniting or aoxidize, and chitosan has good sterilizing ability, in conjunction with Nanoscale Iron also
The ability of former fishy smell material, is used in cosmetic field (such as soap), can play sterilization, except raw meat etc.
Excellent results.
Accompanying drawing explanation
Fig. 1 a is the scanning of the Nanoscale Iron composite of the marine polysaccharide cladding that embodiments of the invention 1 prepare
Electronic Speculum figure, Fig. 1 b is its energy spectrum analysis figure.
Fig. 2 is the scanning of the Nanoscale Iron composite of the marine polysaccharide cladding that embodiments of the invention 2 prepare
Electronic Speculum figure.
Fig. 3 is the scanning of the Nanoscale Iron composite of the marine polysaccharide cladding that embodiments of the invention 3 prepare
Electronic Speculum figure.
Detailed description of the invention
The invention provides the preparation method of a kind of marine polysaccharide in-stiu coating Nanoscale Iron composite, the party
Method includes:
Step 1, uses ferrous salt to prepare perferrite solution；
Step 2, is dissolved in marine polysaccharide in the salpeter solution of 0.05%-0.5%, obtains marine polysaccharide nitre
Acid solution；
Step 3, joins in perferrite solution by described marine polysaccharide salpeter solution, adds poly-
Ethylene glycol, stirs；
Step 4, adds sodium borohydride aqueous solution, stirring, obtains the Nanoscale Iron of marine polysaccharide cladding；
Described marine polysaccharide at least contains any one coordinating group in hydroxyl, amino or carboxyl.
Wherein, the consumption of above-mentioned each raw material is: on the basis of ferrous salt, 0.1mol ferrous salt, adds
0.2-1mol sodium borohydride, adds polysaccharide mixture 5-10g, adds Polyethylene Glycol 0.05-5g.
With embodiment, technical scheme is described further below in conjunction with the accompanying drawings.
Embodiment 1: chitosan in situ cladding Nanoscale Iron
Step 1, weighs the ferrous sulfate heptahydrate of 0.278g in there-necked flask, is subsequently adding 20mL's
Deionized water, is continually fed into argon shield, it is thus achieved that perferrite solution；
Step 2, weighs 0.05g chitosan and joins in the salpeter solution that concentration is 0.05%, obtain ocean
Polysaccharide salpeter solution；
Step 3, by water-soluble for the ferrous salt that the marine polysaccharide salpeter solution prepared in step 2 adds step 1
In liquid, adding 0.01g Polyethylene Glycol, mechanical agitation is until mix homogeneously；
Step 4, weighs 0.378g sodium borohydride and is placed in beaker, adds 20ml deionized water, has treated
Slowly instill in there-necked flask by constant pressure funnel after CL；
Step 5, whole process all uses argon shield, and it is many that mechanic whirl-nett reaction 2h obtains nanoscale ocean
The Nanoscale Iron composite of sugar cladding, is centrifuged and is washed with deionized 3 times, is dried, and stores.
The scanning electron microscope (SEM) photograph of the Nanoscale Iron composite of the nanoscale marine polysaccharide cladding that the present embodiment obtains
As it is shown in figure 1, particle size range is between 100-500nm.Fig. 1 b is that the power spectrum of this scanning electron microscope (SEM) photograph is divided
Analysis figure and EDAX results, can be seen that from this energy spectrum analysis figure, receiving of this nanoscale marine polysaccharide cladding
Elementary composition C, O of being mainly composed of Fe and covering material of rice iron composite material.
Embodiment 2: chitosan/carrageenan mixed solution in-stiu coating Nanoscale Iron
Difference from Example 1 is in step 2 to use the chitosan/carrageenan mixing of mass ratio 2: 1
Solution.
The scanning electron microscope (SEM) photograph of the Nanoscale Iron composite of the nanoscale marine polysaccharide cladding that the present embodiment obtains is such as
Shown in Fig. 2, particle size range is between 100-500nm.
Embodiment 3: chitosan/agar mixed solution in-stiu coating Nanoscale Iron
Difference from Example 1 is in step 2 that the chitosan/agar mixing using mass ratio 2: 1 is molten
Liquid.
The scanning electron microscope (SEM) photograph of the Nanoscale Iron composite of the nanoscale marine polysaccharide cladding that the present embodiment obtains is such as
Shown in Fig. 3, particle size range is between 100-500nm.
Embodiment 4: chitosan/gelatin mixed solution cladding Nanoscale Iron
Difference from Example 1 is in step 2 that the chitosan/gelatin mixing using mass ratio 2: 1 is molten
Liquid.
The present invention uses natural marine polysaccharide to be coated with, and the coating of formation is sufficiently stable, and dispersibility is more
Good, it is difficult to reunite, and there is good bioaffinity, be coated with raw material sources Yu Haiyang, the most any
Biohazardous, can be used for Cosmetic Manufacture.
Although present disclosure has been made to be discussed in detail by above preferred embodiment, but it should understanding
It is not considered as limitation of the present invention to the description above.Read above-mentioned those skilled in the art
After content, multiple amendment and replacement for the present invention all will be apparent from.Therefore, the present invention
Protection domain should be limited to the appended claims.
Claims (10)
1. the preparation method of a marine polysaccharide in-stiu coating Nanoscale Iron composite, it is characterised in that the method includes:
Step 1, uses ferrous salt to prepare perferrite solution；
Step 2, is dissolved in marine polysaccharide in the salpeter solution of 0.05% 0.5%, obtains marine polysaccharide salpeter solution；
Step 3, joins in perferrite solution by described marine polysaccharide salpeter solution, adds Polyethylene Glycol, stir；
Step 4, adds sodium borohydride aqueous solution, stirring, obtains the Nanoscale Iron of marine polysaccharide cladding；
Described marine polysaccharide at least contains any one coordinating group in hydroxyl, amino or carboxyl.
2. the preparation method of marine polysaccharide in-stiu coating Nanoscale Iron composite as claimed in claim 1, it is characterised in that described ferrous salt selects ferrous sulfate or ferrous chloride or the mixture of the two.
3. the preparation method of marine polysaccharide in-stiu coating Nanoscale Iron composite as claimed in claim 1, it is characterised in that described marine polysaccharide is natural marine polysaccharide.
4. the preparation method of marine polysaccharide in-stiu coating Nanoscale Iron composite as claimed in claim 1, it is characterised in that described marine polysaccharide selects at least one in chitosan, gelatin, carrageenan, agar.
5. the preparation method of marine polysaccharide in-stiu coating Nanoscale Iron composite as claimed in claim 1, it is characterised in that described sodium borohydride is (2-10) with the mol ratio of ferrous salt: 1.
6. the preparation method of marine polysaccharide in-stiu coating Nanoscale Iron composite as claimed in claim 1, it is characterised in that the mixing time of step 4 is 30-120min.
7. the preparation method of marine polysaccharide in-stiu coating Nanoscale Iron composite as claimed in claim 1, it is characterised in that described step 4 also comprises post-processing step, and it comprises: centrifugal treating, be filtered, washed and dried step.
8. the preparation method of marine polysaccharide in-stiu coating Nanoscale Iron composite as claimed in claim 1, it is characterised in that
All use protective atmosphere during step 1, step 3 and step 4, keep anaerobic state.
9. the preparation method of marine polysaccharide in-stiu coating Nanoscale Iron composite as claimed in claim 1, it is characterised in that described protective atmosphere refers to nitrogen or argon.
10. using a marine polysaccharide in-stiu coating Nanoscale Iron composite prepared by the preparation method of the marine polysaccharide in-stiu coating Nanoscale Iron composite described in claim 1, its particle diameter is nanoscale.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109172541A (en) * | 2018-07-18 | 2019-01-11 | 湖北工业大学 | A kind of preparation method of stable nanogel polyferose |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101537489A (en) * | 2008-03-20 | 2009-09-23 | 南开大学 | Nanometer zero-valent iron particle capable of stably existing in air, and preparation method thereof |
| CN104877148A (en) * | 2015-05-27 | 2015-09-02 | 成都理工大学 | Preparation method of carboxymethyl chitosan gel beads coated with nano iron |
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2016
- 2016-06-15 CN CN201610423881.7A patent/CN105997573A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101537489A (en) * | 2008-03-20 | 2009-09-23 | 南开大学 | Nanometer zero-valent iron particle capable of stably existing in air, and preparation method thereof |
| CN104877148A (en) * | 2015-05-27 | 2015-09-02 | 成都理工大学 | Preparation method of carboxymethyl chitosan gel beads coated with nano iron |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109172541A (en) * | 2018-07-18 | 2019-01-11 | 湖北工业大学 | A kind of preparation method of stable nanogel polyferose |
| CN109172541B (en) * | 2018-07-18 | 2020-12-29 | 湖北工业大学 | Preparation method of stable nano gel polysaccharide iron |
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Application publication date: 20161012 |