CN104327233A - Synthesis method of anti-dazzle polyurethane coating - Google Patents
Synthesis method of anti-dazzle polyurethane coating Download PDFInfo
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- CN104327233A CN104327233A CN201410579747.7A CN201410579747A CN104327233A CN 104327233 A CN104327233 A CN 104327233A CN 201410579747 A CN201410579747 A CN 201410579747A CN 104327233 A CN104327233 A CN 104327233A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
Abstract
The invention relates to a synthesis method of an anti-dazzle polyurethane coating. The synthesis method comprises the following steps: adding a monomer, dropwise adding polyether glycol to a three-neck flask containing MDI-100 to react by using a constant pressure funnel; weighing DMPA, dissolving into acetone, and adding to the three-neck flask; enabling the DMPA to react with a prepolymer, so as to obtain an anionic hydrophilic-modified polyurethane prepolymer containing carboxyl; adding excessive diethylene glycol, carrying out chain-expanding reaction, carrying out neutral reaction on triethylamine and DMPA to obtain a waterborne polyurethane dispersion; taking ethanediamine and distilled water to prepare a dispersion solution; adding the dispersion solution by the dispersion under the mechanical stirring condition; mechanically dispersing, thereby obtaining a semi-transparent water-borne emulsion with blue light; and vacuumizing the water-borne emulsion in a vacuum pump, so as to obtain the water-borne PU emulsion which can be stably stored. The method disclosed by the invention is simple and low in cost, and the synthesized polyurethane coating is good in stability and excellent in anti-dazzle property.
Description
Technical field
The present invention relates to a kind of synthetic technology of organic coating, particularly relate to a kind of anti-dazzle polyurethane coating synthetic method.
Background technology
Based on this problem existed in actual life, in the urgent need to preparing a kind of transparent Anti Glare Coatings, being mainly applied in the light fixture of interior lighting, lampshade and automobile lamp etc., playing the effect of anti-dazzle.Domestic before the standard mesh of anti-dazzle do not have ready-made quantizating index, and the anti-dazzle standard of special Japanese Hakawa Paper-making Co., Ltd., obtains different performance index.Solve the coating of current glare phenomenon, need the advantages such as anti-dazzle performance is good, the transparency is good, sticking power is high, good weatherability, hardness are high, safety and environmental protection.Intend adopting aqueous polyurethane emulsion as the filmogen preparing transparent anti-glare coating, using the Nano microsphere of nucleocapsid structure as anti-dazzle modified additive and by adding the coatings additive(s)s such as flow agent, dispersion agent, wetting agent defoamer.
Summary of the invention
It is simple that technical problem to be solved by this invention is to provide a kind of method, with low cost, the polyurethane coating good stability of synthesis, the synthetic method of anti-dazzle excellent performance.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of anti-dazzle polyurethane coating synthetic method, is characterized in that, comprise the steps:
Add monomer, in the there-necked flask that MDI-100 is housed, drip polyether Glycols reaction by constant pressure funnel;
Take DMPA, be dissolved in acetone, join in there-necked flask, DMPA and prepolymer react, and obtain the polyurethane prepolymer of carboxylic anionic hydrophilic modification;
Add glycol ether excessive, chain extending reaction;
By triethylamine, DMPA, neutralization reaction obtains the dispersion of aqueous polyurethane;
Get quadrol and distilled water preparation dispersion liquid, dispersion is added dispersion liquid under mechanical agitation, after mechanical dispersion, obtains the water-based emulsion of translucent blueing light;
Aqueous polyurethane emulsion is at vacuum pump evacuation, and obtaining can the water-based PU emulsion of stably stored.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described interpolation monomer, drips being implemented as follows of polyether Glycols reactions steps by constant pressure funnel in the there-necked flask that MDI-100 is housed:
Monomer is added, at N in isocyanate index R (NCO/OH)=2:2 ~ 2:3 ratio
2under protecting 50 ~ 70 DEG C of conditions, in the there-necked flask that MDI-100 is housed, drip polyether Glycols 1 ~ 2h by constant pressure funnel and react 2 ~ 4h.
Further, described in take DMPA, be dissolved in acetone, join in there-necked flask, DMPA and prepolymer react, and obtain being implemented as follows of the polyurethane prepolymer step of carboxylic anionic hydrophilic modification:
Take the DMPA accounting for total component mass ratio 3 ~ 6%, be dissolved in acetone, join in there-necked flask, DMPA and prepolymer react 2 ~ 3h, obtain the polyurethane prepolymer of carboxylic anionic hydrophilic modification.
Further, described interpolation glycol ether is excessive, being implemented as follows of chain extending reaction step:
Add the excessive 15 ~ 20ml of glycol ether, chain extending reaction 0.5 ~ 1h.
Further, described by triethylamine, DMPA, neutralization reaction obtains being implemented as follows of the dispersion step of aqueous polyurethane:
Triethylamine/DMPA=0.58:1 in mass ratio, neutralization reaction 10 ~ 30min, obtain the dispersion of aqueous polyurethane.
Further, described in get quadrol and distilled water preparation dispersion liquid, dispersion is added dispersion liquid under mechanical agitation, after mechanical dispersion, obtains being implemented as follows of the water-based emulsion step of translucent blueing light:
Get 10 ~ 15ml quadrol and 200 ~ 300ml distilled water preparation dispersion liquid, dispersion is added dispersion liquid under mechanical stirring 2500r/min velocity conditions, after mechanical dispersion 0.5 ~ 1h, obtains the water-based emulsion of translucent blueing light.
The invention has the beneficial effects as follows: method is simple, with low cost, the polyurethane coating good stability of synthesis, anti-dazzle excellent performance.
Embodiment
Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.
A kind of anti-dazzle polyurethane coating synthetic method, is characterized in that, comprise the steps:
Add monomer, in the there-necked flask that MDI-100 is housed, drip polyether Glycols reaction by constant pressure funnel;
Take DMPA, be dissolved in acetone, join in there-necked flask, DMPA and prepolymer react, and obtain the polyurethane prepolymer of carboxylic anionic hydrophilic modification;
Add glycol ether excessive, chain extending reaction;
By triethylamine, DMPA, neutralization reaction obtains the dispersion of aqueous polyurethane;
Get quadrol and distilled water preparation dispersion liquid, dispersion is added dispersion liquid under mechanical agitation, after mechanical dispersion, obtains the water-based emulsion of translucent blueing light;
Aqueous polyurethane emulsion is at vacuum pump evacuation, and obtaining can the water-based PU emulsion of stably stored.
Embodiment 1:
Monomer is added, at N in isocyanate index R (NCO/OH)=2:2 ratio
2under protecting 50 DEG C of conditions, in the there-necked flask that MDI-100 is housed, drip polyether Glycols 1h by constant pressure funnel and react 2h; Take the DMPA accounting for total component mass ratio 3%, be dissolved in acetone, join in there-necked flask, DMPA and prepolymer react 2h, obtain the polyurethane prepolymer of carboxylic anionic hydrophilic modification; Add the excessive 15ml of glycol ether, chain extending reaction 0.5h; Triethylamine/DMPA=0.58:1, neutralization reaction 10min in mass ratio, obtains the dispersion of aqueous polyurethane; Get 10ml quadrol and 200ml distilled water preparation dispersion liquid, dispersion is added dispersion liquid under mechanical stirring 2500r/min velocity conditions, after mechanical dispersion 0.5h, obtains the water-based emulsion of translucent blueing light; Aqueous polyurethane emulsion is at vacuum pump evacuation, and obtaining can the water-based PU emulsion of stably stored.
Embodiment 2:
Monomer is added, at N in isocyanate index R (NCO/OH)=2:2.5 ratio
2under protecting 60 DEG C of conditions, in the there-necked flask that MDI-100 is housed, drip polyether Glycols 1.5h by constant pressure funnel and react 3h; Take the DMPA accounting for total component mass ratio 5%, be dissolved in acetone, join in there-necked flask, DMPA and prepolymer react 2.5h, obtain the polyurethane prepolymer of carboxylic anionic hydrophilic modification; Add the excessive 18ml of glycol ether, chain extending reaction 0.8h; Triethylamine/DMPA=0.58:1, neutralization reaction 20min in mass ratio, obtains the dispersion of aqueous polyurethane; Get 12ml quadrol and 240ml distilled water preparation dispersion liquid, dispersion is added dispersion liquid under mechanical stirring 2500r/min velocity conditions, after mechanical dispersion 0.6h, obtains the water-based emulsion of translucent blueing light; Aqueous polyurethane emulsion is at vacuum pump evacuation, and obtaining can the water-based PU emulsion of stably stored.
Embodiment 3:
Monomer is added, at N in isocyanate index R (NCO/OH)=2:3 ratio
2under protecting 70 DEG C of conditions, in the there-necked flask that MDI-100 is housed, drip polyether Glycols 2h by constant pressure funnel and react 4h; Take the DMPA accounting for total component mass ratio 6%, be dissolved in acetone, join in there-necked flask, DMPA and prepolymer react 3h, obtain the polyurethane prepolymer of carboxylic anionic hydrophilic modification; Add the excessive 20ml of glycol ether, chain extending reaction 1h; Triethylamine/DMPA=0.58:1, neutralization reaction 30min in mass ratio, obtains the dispersion of aqueous polyurethane; Get 15ml quadrol and 300ml distilled water preparation dispersion liquid, dispersion is added dispersion liquid under mechanical stirring 2500r/min velocity conditions, after mechanical dispersion 1h, obtains the water-based emulsion of translucent blueing light; Aqueous polyurethane emulsion is at vacuum pump evacuation, and obtaining can the water-based PU emulsion of stably stored.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. an anti-dazzle polyurethane coating synthetic method, is characterized in that, comprise the steps:
Add monomer, in the there-necked flask that MDI-100 is housed, drip polyether Glycols reaction by constant pressure funnel;
Take DMPA, be dissolved in acetone, join in there-necked flask, DMPA and prepolymer react, and obtain the polyurethane prepolymer of carboxylic anionic hydrophilic modification;
Add glycol ether excessive, chain extending reaction;
By triethylamine, DMPA, neutralization reaction obtains the dispersion of aqueous polyurethane;
Get quadrol and distilled water preparation dispersion liquid, dispersion is added dispersion liquid under mechanical agitation, after mechanical dispersion, obtains the water-based emulsion of translucent blueing light;
Aqueous polyurethane emulsion is at vacuum pump evacuation, and obtaining can the water-based PU emulsion of stably stored.
2. a kind of anti-dazzle polyurethane coating synthetic method according to claim 1, is characterized in that, described interpolation monomer, drips being implemented as follows of polyether Glycols reactions steps by constant pressure funnel in the there-necked flask that MDI-100 is housed:
Monomer is added, at N in isocyanate index R (NCO/OH)=2:2 ~ 2:3 ratio
2under protecting 50 ~ 70 DEG C of conditions, in the there-necked flask that MDI-100 is housed, drip polyether Glycols 1 ~ 2h by constant pressure funnel and react 2 ~ 4h.
3. a kind of anti-dazzle polyurethane coating synthetic method according to claim 1, is characterized in that, described in take DMPA, be dissolved in acetone, join in there-necked flask, DMPA and prepolymer react, and obtain being implemented as follows of the polyurethane prepolymer step of carboxylic anionic hydrophilic modification:
Take the DMPA accounting for total component mass ratio 3 ~ 6%, be dissolved in acetone, join in there-necked flask, DMPA and prepolymer react 2 ~ 3h, obtain the polyurethane prepolymer of carboxylic anionic hydrophilic modification.
4. a kind of anti-dazzle polyurethane coating synthetic method according to claim 1, it is characterized in that, described interpolation glycol ether is excessive, being implemented as follows of chain extending reaction step:
Add the excessive 15 ~ 20ml of glycol ether, chain extending reaction 0.5 ~ 1h.
5. a kind of anti-dazzle polyurethane coating synthetic method according to claim 1, it is characterized in that, described by triethylamine, DMPA, neutralization reaction obtains being implemented as follows of the dispersion step of aqueous polyurethane:
Triethylamine/DMPA=0.58:1 in mass ratio, neutralization reaction 10 ~ 30min, obtain the dispersion of aqueous polyurethane.
6. a kind of anti-dazzle polyurethane coating synthetic method according to claim 1, it is characterized in that, described get quadrol and distilled water preparation dispersion liquid, dispersion is added dispersion liquid under mechanical agitation, after mechanical dispersion, obtains being implemented as follows of the water-based emulsion step of translucent blueing light:
Get 10 ~ 15ml quadrol and 200 ~ 300ml distilled water preparation dispersion liquid, dispersion is added dispersion liquid under mechanical stirring 2500r/min velocity conditions, after mechanical dispersion 0.5 ~ 1h, obtains the water-based emulsion of translucent blueing light.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105348484A (en) * | 2015-12-04 | 2016-02-24 | 成都印钞有限公司 | Method for preparing waterborne polyurethane-polyurea paper surface sizing agent |
CN106380569A (en) * | 2016-09-27 | 2017-02-08 | 华南理工大学 | Water-based polyurethane anti-glare coating material and preparation method thereof |
CN110531447A (en) * | 2019-08-16 | 2019-12-03 | 深圳市摩码科技有限公司 | A kind of anti-dazzle protective film and preparation method thereof |
CN117624692A (en) * | 2024-01-25 | 2024-03-01 | 广东工业大学 | Low-carbon biodegradable composite membrane and preparation method and application thereof |
-
2014
- 2014-10-26 CN CN201410579747.7A patent/CN104327233A/en active Pending
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105348484A (en) * | 2015-12-04 | 2016-02-24 | 成都印钞有限公司 | Method for preparing waterborne polyurethane-polyurea paper surface sizing agent |
CN106380569A (en) * | 2016-09-27 | 2017-02-08 | 华南理工大学 | Water-based polyurethane anti-glare coating material and preparation method thereof |
CN106380569B (en) * | 2016-09-27 | 2019-01-15 | 华南理工大学 | A kind of aqueous polyurethane Anti Glare Coatings material and preparation method thereof |
CN110531447A (en) * | 2019-08-16 | 2019-12-03 | 深圳市摩码科技有限公司 | A kind of anti-dazzle protective film and preparation method thereof |
CN117624692A (en) * | 2024-01-25 | 2024-03-01 | 广东工业大学 | Low-carbon biodegradable composite membrane and preparation method and application thereof |
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