CN110256604A - A kind of chitosan-based fluorescent material, preparation method and the purposes for being used to prepare aqueous epoxide resin paint - Google Patents
A kind of chitosan-based fluorescent material, preparation method and the purposes for being used to prepare aqueous epoxide resin paint Download PDFInfo
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- CN110256604A CN110256604A CN201910540969.0A CN201910540969A CN110256604A CN 110256604 A CN110256604 A CN 110256604A CN 201910540969 A CN201910540969 A CN 201910540969A CN 110256604 A CN110256604 A CN 110256604A
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- chitosan
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/22—Luminous paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1018—Heterocyclic compounds
- C09K2211/1025—Heterocyclic compounds characterised by ligands
- C09K2211/1088—Heterocyclic compounds characterised by ligands containing oxygen as the only heteroatom
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- Paints Or Removers (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a kind of chitosan-based fluorescent material, preparation method and the purposes for being used to prepare aqueous epoxide resin paint, which is prepared by chitosan with hydrogen peroxide and hypochlorite oxidation.The present invention uses environmental type oxidant hydrogen peroxide and sodium hypochlorite etc. to aoxidize chitosan under acidic environment as oxidant, obtains a kind of substance with fluorescent characteristic, is configured to fluorescence epoxy coating with fluorescent material, solidification effect is good, and fluorescence is stronger.Fluorescent material is produced with the extensive natural products chitosan in source, low in cost, process contamination is few, therefore the invention has the potentiality of industrialization amplification.
Description
Technical field
The invention belongs to chemical fields, are related to the preparation and application of fluorescent material, and in particular to a kind of chitosan-based fluorescence
Material, preparation method and the purposes for being used to prepare aqueous epoxide resin paint.
Background technique
Chitosan is made by chitin deacetylate, chitin be widely present in crustacean shell and fungi it is thin
In cell wall, raw material sources are abundant, and yield is huge, environmentally protective.The application field of chitosan includes water process, medicine, chemical industry etc..
The application of chitosan-based material is developed, there is at low cost, degradable, advantages of environment protection.Chemical degradation is carried out to it, is reduced
Molecular weight, increasing solubility etc. is current research emphasis, but is developed into fluorescent material and be not yet seen in document.
Fluorescent chemicals in analytical chemistry as ligand be used to detect and identify metal ion and quantitative analysis metal from
The content of son, can issue the coating of visible light, therefore painting can be enhanced when derivative fluorescent paint is irradiated with ultraviolet radiation
Expect the brightness on surface.Fluorescent paint is to assign fluorescent functional by the fluorescent pigment in its component, in traffic route marker, is built
The fields such as object surface colouring and biomarker are built to be widely used, epoxy resin have extraordinary mechanics effect, electrical insulating property,
Chemicals-resistant and binding function, research fluorescence epoxy coating have a extensive future.
However, common formulation for coating material on the market all contains more organic solvent at present, environmental pollution, greenhouse will cause
Effect, and jeopardize the health of people.The hydrotropic trend of the development of environment-friendly type coating is more and more obvious.Develop water-base epoxy
Coating is the effective way for solving the high VOCs discharge of coating.
Summary of the invention
For overcome the deficiencies in the prior art, an object of the present disclosure is to provide a kind of chitosan-based fluorescent material, the
Two are designed to provide the preparation method of the chitosan-based fluorescent material, and third is designed to provide the chitosan-based fluorescent material
It is used to prepare the purposes of aqueous epoxide resin paint.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
Chitosan is prepared a kind of chitosan-based fluorescent material with hydrogen peroxide and hypochlorite oxidation.
A method of preparing above-mentioned chitosan-based fluorescent material, step are as follows: dissolve chitosan in acetum, add
Enter hydrogen peroxide and sodium hypochlorite, oxidation reaction for a period of time after, obtain a kind of fluorescent solutions, adjusted with saturated sodium bicarbonate solution
To neutrality, precipitating, drying are collected in filtering.
A method of preparing above-mentioned chitosan-based fluorescent material, step are as follows: dissolve chitosan in acetum, add
Enter hydrogen peroxide and sodium hypochlorite, oxidation reaction for a period of time after, obtain a kind of fluorescent solutions, dry.
A method of preparing above-mentioned chitosan-based fluorescent material, step are as follows: dissolve chitosan in acetum, add
Enter hydrogen peroxide and sodium hypochlorite, oxidation reaction for a period of time after, obtain a kind of fluorescent solutions, naturally dry.
Chitosan-based fluorescent material described above is used to prepare the purposes of aqueous epoxide resin paint.
A kind of aqueous epoxide resin paint, is prepared by the following raw material and method: will be described above chitosan-based
It after fluorescent material is mixed with suitable epoxy resin E-44, emulsifier and ethanol amine, heats, suitable quantity of water is added dropwise under stirring condition,
It is cooling up to homogeneous coating after reaction.
Further, the emulsifier is obtained by epoxy resin and polyethylene glycol heating reaction.
The utility model has the advantages that
The present invention uses environmental type oxidant hydrogen peroxide and sodium hypochlorite etc. to aoxidize under acidic environment as oxidant
Chitosan, obtains a kind of substance with fluorescent characteristic, is configured to fluorescence epoxy coating with fluorescent material, solidification effect is good
Good, fluorescence is stronger.Fluorescent material is produced with the extensive natural products chitosan in source, low in cost, pollution is few, industrial prospect
It is good.
Detailed description of the invention
Fig. 1 is the hydrogen nuclear magnetic resonance spectrogram of the chitosan-based fluorescent material of embodiment 1, and fluorescent characteristic may be believed with δ 8.25
It is number related；
Fig. 2 is the infrared spectrogram of the chitosan-based fluorescent material of embodiment 1；
Fig. 3 is fluorescence detection figure of the fluorescent solutions at 365nm in the chitosan-based fluorescent material preparation process of embodiment 1；
Fig. 4 is to be coated with embodiment 4 fluorescence detection figure of the smear of coating at 365nm is made.
Specific embodiment
It is specific with reference to the accompanying drawings and examples to introduce essentiality content of the present invention, but guarantor of the invention is not limited with this
Protect range.
Embodiment 1: chitosan-based fluorescent material is prepared
It takes 1.58g chitosan that round-bottomed flask is added, weighs 1.60g glacial acetic acid, be diluted to 25mL with distilled water and round bottom is added
In flask, stirring is slowly added to hydrogen peroxide and the 1.5mL liquor natrii hypochloritis that 4mL mass fraction is 30%, in 37 DEG C of water-bath items
50h is reacted under part, being adjusted to PH with saturated sodium bicarbonate solution is 7, filtering precipitating, obtains white admittedly after being put into drying in oven
Body has stronger tackness, has blue-fluorescence at 365nm.Fig. 1 is the nuclear magnetic resonance of the chitosan-based fluorescent material of embodiment 1
Hydrogen spectrogram, fluorescent characteristic may be related with 8.25 signal of δ；Fig. 2 is the infrared spectroscopy of the chitosan-based fluorescent material of embodiment 1
Figure；Fig. 3 is fluorescence detection figure of the fluorescent solutions at 365nm in the chitosan-based fluorescent material preparation process of embodiment 1.
Embodiment 2: chitosan-based fluorescent material is prepared
It takes 1.58g chitosan that round-bottomed flask is added, weighs 1.60g glacial acetic acid, be diluted to 25mL with distilled water and round bottom is added
In flask, stirring is slowly added to hydrogen peroxide and the 1.5mL liquor natrii hypochloritis that 4mL mass fraction is 30%, in 37 DEG C of water-bath items
50h is reacted under part, reaction solution directly in drying in oven, obtains faint yellow granular disintegration, has blue-fluorescence under 365nm.
Embodiment 3: chitosan-based fluorescent material is prepared
It takes 1.58g chitosan that round-bottomed flask is added, weighs 1.60g glacial acetic acid, be diluted to 25mL with distilled water and round bottom is added
In flask, stirring is slowly added to hydrogen peroxide and the 1.5mL liquor natrii hypochloritis that 4mL mass fraction is 30%.In 37 DEG C of water-bath items
50h is reacted under part, obtains light yellow viscous liquid, naturally dry in air is stood, obtains one layer of firm film, 365nm
Under have a blue-fluorescence, stand the very stable no moisture absorption phenomenon of 48h in air.
Embodiment 4: aqueous epoxide resin paint is prepared
Chitosan-based fluorescent material solid, 0.7g self-control emulsifier prepared by 4.8g epoxy resin E-44,1g embodiment 1
(being obtained by epoxy resin and polyethylene glycol heating reaction, see patent CN105505132A) and 0.4g ethanol amine are added to three-necked flask
In, for heating water bath to 60 DEG C, simultaneously 2ml water is added dropwise in mechanical stirring, is terminated after stirring 20min, is obtained homogeneous coating.Coating is coated onto
On the iron sheet of polishing, room temperature is dried.Coating is securely uniform, and surface is smooth, transparency is higher, and hardness is big, scrapes, under 365nm
There is blue-fluorescence, as shown in Figure 4.
Without significant change after tap water 2h, fluorescence does not weaken coating bubble.Be added dropwise 1% solution of potassium carbonate to coating surface without
Significant change, also without significant change after 2h inside solution of potassium carbonate, fluorescence does not weaken bubble.
To sum up, the present invention uses environmental type oxidant hydrogen peroxide and sodium hypochlorite etc. as oxidant in acyclic acidic
Chitosan is aoxidized under border, obtains a kind of substance with fluorescent characteristic, fluorescence epoxy coating is configured to fluorescent material, Gu
Change works well, and fluorescence is stronger, resistance to bubble, alkaline-resisting.Fluorescent material is produced with the extensive natural products chitosan in source, it is at low cost
Honest and clean, process contamination is few, therefore the invention has the potentiality of industrialization amplification.
The effect of above-described embodiment is specifically to introduce essentiality content of the invention, but those skilled in the art should know
Protection scope of the present invention should not be confined to the specific embodiment by road.
Claims (7)
1. a kind of chitosan-based fluorescent material, it is characterised in that: chitosan to be prepared with hydrogen peroxide and hypochlorite oxidation.
2. the preparation method of chitosan-based fluorescent material described in a kind of claim 1, it is characterised in that: dissolve chitosan in vinegar
In acid solution, be added hydrogen peroxide and sodium hypochlorite, oxidation reaction for a period of time after, obtain a kind of fluorescent solutions, use unsaturated carbonate
Hydrogen sodium solution is adjusted to neutrality, filtering, collects precipitating, drying.
3. the preparation method of chitosan-based fluorescent material described in a kind of claim 1, it is characterised in that: dissolve chitosan in vinegar
In acid solution, be added hydrogen peroxide and sodium hypochlorite, oxidation reaction for a period of time after, obtain a kind of fluorescent solutions, dry.
4. the preparation method of chitosan-based fluorescent material described in a kind of claim 1, it is characterised in that: dissolve chitosan in vinegar
In acid solution, be added hydrogen peroxide and sodium hypochlorite, oxidation reaction for a period of time after, obtain a kind of fluorescent solutions, naturally dry.
5. chitosan-based fluorescent material described in claim 1 is used to prepare the purposes of aqueous epoxide resin paint.
6. a kind of aqueous epoxide resin paint, which is characterized in that be prepared by the following raw material and method: by claim 1
After the chitosan-based fluorescent material is mixed with suitable epoxy resin E-44, emulsifier and ethanol amine, heating, stirring condition
Lower dropwise addition suitable quantity of water, it is cooling up to homogeneous coating after reaction.
7. aqueous epoxide resin paint according to claim 6, it is characterised in that: the emulsifier is by epoxy resin and gathers
Ethylene glycol heating reaction obtains.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910540969.0A CN110256604B (en) | 2019-06-21 | 2019-06-21 | Chitosan-based fluorescent material, preparation method and application of chitosan-based fluorescent material in preparation of waterborne epoxy resin coating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910540969.0A CN110256604B (en) | 2019-06-21 | 2019-06-21 | Chitosan-based fluorescent material, preparation method and application of chitosan-based fluorescent material in preparation of waterborne epoxy resin coating |
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| CN110256604A true CN110256604A (en) | 2019-09-20 |
| CN110256604B CN110256604B (en) | 2021-08-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113265245A (en) * | 2021-03-18 | 2021-08-17 | 中国科学院苏州生物医学工程技术研究所 | Nano fluorescent probe, preparation method and application thereof |
Citations (4)
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| CN1389477A (en) * | 2002-07-18 | 2003-01-08 | 上海交通大学 | Prepn. of water soluble chitosan with controllable molecular weight |
| CN104592856A (en) * | 2014-12-11 | 2015-05-06 | 青岛佰众化工技术有限公司 | Waterborne epoxy anti-corrosion coating added with chitosan |
| CN105255262A (en) * | 2015-11-20 | 2016-01-20 | 天津美士邦涂料化工有限公司 | Aqueous antibacterial coating |
| CN109181478A (en) * | 2018-08-24 | 2019-01-11 | 河北晨阳工贸集团有限公司 | A kind of aqueous fluorescent epoxide terrace paint and preparation method thereof |
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2019
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| CN1389477A (en) * | 2002-07-18 | 2003-01-08 | 上海交通大学 | Prepn. of water soluble chitosan with controllable molecular weight |
| CN104592856A (en) * | 2014-12-11 | 2015-05-06 | 青岛佰众化工技术有限公司 | Waterborne epoxy anti-corrosion coating added with chitosan |
| CN105255262A (en) * | 2015-11-20 | 2016-01-20 | 天津美士邦涂料化工有限公司 | Aqueous antibacterial coating |
| CN109181478A (en) * | 2018-08-24 | 2019-01-11 | 河北晨阳工贸集团有限公司 | A kind of aqueous fluorescent epoxide terrace paint and preparation method thereof |
Non-Patent Citations (5)
| Title |
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| JENNIFER L. WEIST ET AL.: ""Development of a Fluorescence Sensor to Monitor Lipid Oxidation. 1. Fluorescence Spectra of Chitosan Powder and Polyamide Powder after Exposure to Volatile Lipid Oxidation Products"", 《J. AGRIC. FOOD CHEM.》 * |
| M. ABD EL-FATTAH ET AL,.: ""Improvement of corrosion resistance, antimicrobial activity, mechanical and chemical properties of epoxy coating by loading chitosan as a natural renewable resource"", 《PROGRESS IN ORGANIC COATINGS》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113265245A (en) * | 2021-03-18 | 2021-08-17 | 中国科学院苏州生物医学工程技术研究所 | Nano fluorescent probe, preparation method and application thereof |
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