CN105907261A - High heat-resistant and flame-retardant type modified epoxy resin based powder coating with intercalation polymerization of montmorillonite and preparation method of powder coating - Google Patents
High heat-resistant and flame-retardant type modified epoxy resin based powder coating with intercalation polymerization of montmorillonite and preparation method of powder coating Download PDFInfo
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- CN105907261A CN105907261A CN201610532588.4A CN201610532588A CN105907261A CN 105907261 A CN105907261 A CN 105907261A CN 201610532588 A CN201610532588 A CN 201610532588A CN 105907261 A CN105907261 A CN 105907261A
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- montmorillonite
- epoxy resin
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- modified epoxy
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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
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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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
- C09D5/18—Fireproof paints including high temperature resistant paints
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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
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The invention discloses high heat-resistant and flame-retardant type modified epoxy resin based powder coating with intercalation polymerization of montmorillonite. Montmorillonite is acidized with a dilute hydrochloric acid solution and then organically modified, thus the interlayer binding force of the montmorillonite is weakened, interlayer crystal lattices are split, surface high polarity is changed, interlayer hydrophilicity is changed into lipophilicity, surface energy is reduced, interlayer spacing is enlarged, and specific area and adsorptive capacity are remarkably increased; and finally, the treated montmorillonite is added at twice, thus the montmorillonite is fully intercalated and disbonded at the modification stage of the epoxy resin, the disbonded sheets and epoxy resin form chemical bonds and stably disperse in the resin system, so that the modified epoxy resin has superior high-temperature stability, heat storage stability and ageing resistance, and the boiling resistance and cathodic disbonding resistance of the coating are improved. Simultaneously, the modified epoxy resin based powder coating also is matched with compound modification filling and other effective additives, so that the prepared powder coating layer has good bond property, high temperature resistance to 300 DEG C and excellent flame retardant effect.
Description
Technical field
The present invention relates to powder coating technology field, particularly relate to a kind of high-temp resistant fire-retarding type montmorillonite intercalation polymeric modification epoxy resin based powder coating and preparation method thereof.
Background technology
Along with the enhancing of mankind's environmental consciousness, solvent based coating is gradually restricted, and it has been trend of the times that development meets the coating of environmental requirement, and Water-borne modification and solvent free coating are the directions of paint field development from now on.Powdery paints is a kind of novel without solvent 100% solid powdery coating, has the advantages such as high usage, easy application, corrosion-resistant, environmental protection, is widely applied in modern times spraying and corrosion-resistant field.
Epoxy powder coating is a kind of important new coating that development in recent years is got up, and occupies heavier status with its higher stock utilization, stronger adhesive force and antiseptic property coating industry the most at home.In recent years, the development of nano material opens the frontier of material science, and nanometer particle-modified corrosion-resistant epoxy paint also has vast potential for future development.Montmorillonite belongs to phyllosilicate, has the lattice arrangement of high-sequential.The research utilizing the montmorillonite with layer structure and epoxy resin intercalation synthesis to prepare a kind of high-performance epoxy resin based powder coatings receives much concern, epoxy resin based powder coating tradition modification is that modifying agent montmorillonite is disposably joined the twin-screw extrusion stage, when hot setting, make limellar stripping, the method montmorillonite intercalation in the epoxy and peel off insufficient, the antikathode affecting powdery paints is peeled off and water boiling resistance performance.
The research of epoxy resin and performance powder coating thereof " the montmorillonite intercalation polymerization prepare " utilizes low-molecular-weight epoxy resin (E-51) to insert stratiform organo montmorillonite (OMMT), by intercalation polymeric and bisphenol-A and the 3rd component 2,6-di-tert-butyl methyl phenol (BHT) reacts, and obtains a kind of powder coating epoxy resin.The test of X x ray diffraction shows, laminar nano montmorillonite layer is stripped completely, is dispersed in resin matrix.Controlling montmorillonite and add total amount and twice additional proportion, the antikathode that can be obviously improved this coating is peeled off and water boiling resistance performance.
But, montmorillonite belongs to inorganic mineral, by adding montmorillonite at twice, makes montmorillonite at epoxy resin preparatory phase by abundant intercalation and stripping, but both poor compatibility, certainly will affect the levelability of film, meanwhile, in literary composition, method of modifying is single, the powdery paints prepared only is peeled off at antikathode and makes moderate progress in water boiling resistance performance, and the aspects such as its comprcssive strength, scratch resistance, anti-corrosive properties are improved, accordingly, it would be desirable to improved existing technique and formula.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of high-temp resistant fire-retarding type montmorillonite intercalation polymeric modification epoxy resin based powder coating and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of high-temp resistant fire-retarding type montmorillonite intercalation polymeric modification epoxy resin based powder coating, is prepared by the raw materials in: bisphenol f type epoxy resin 68-71, montmorillonite 3.7-4.3, ethylenediamine 1.5-1.8, Oleum Brassicae campestris 8-9, vinyl three ('beta '-methoxy ethyoxyl) silane 3-4, Firebrake ZB 0.3-0.5, periclase powder 16-18, Folium Artemisiae Argyi 17-20, rosin milk 10-12, firming agent 2-4, pigment 5-7.
The manufacture method of described a kind of high-temp resistant fire-retarding type montmorillonite intercalation polymeric modification epoxy resin based powder coating, comprises the following steps:
(1) montmorillonite is put in the dilute hydrochloric acid solution that mass fraction is 5-8% and stir 3-5 hour at 50 DEG C-90 DEG C, filtering, washing, to neutral, is dried, it is dispersed in EtOH-DI water solution, add ethylenediamine at 60 DEG C of stirred in water bath 2-4 hour, ultrasonic disperse 20-30 minute, sucking filtration, washing, being dried under vacuum to constant weight, grind, sieve to obtain modified nano montmorillonite；
(2) dried by Folium Artemisiae Argyi, attrition grinding crosses 200 mesh sieves; addition rosin milk, periclase powder, Firebrake ZB stirring and evenly mixing stand 12-14 hour; pelletize; sinter 20-30 minute in 800-1000 DEG C under nitrogen protection, add vinyl three ('beta '-methoxy ethyoxyl) silane and grind 20-30 minute to obtain composite modified filler；
(3) by bisphenol f type epoxy resin, Oleum Brassicae campestris stirring and evenly mixing, add the modified nano montmorillonite of half quality, take out after reacting by heating 2-3 hour at 130-150 DEG C, obtain modified epoxy；
(4) modified epoxy, step (2) material, the modified nano montmorillonite of second half quality remaining and other residual componentss that step (3) prepares are put into stirring and evenly mixing in high mixer, melt extrude through double screw extruder, cooling pulverizing, crosses 250-300 mesh sieve, discharging.
nullThe invention have the advantage that montmorillonite dilute hydrochloric acid solution acidification is carried out organically-modified by the present invention again，Weaken the adhesion between cheating engaging layer，Interlayer lattice is made to split，Change the highly polar of surface，Interlayer is made to be changed into lipophile by hydrophilic，Reduce its surface energy，Make interlamellar spacing expand simultaneously，Specific surface area and absorbability dramatically increase，Finally it is added at twice，Make montmorillonite in the epoxy resin modification stage by abundant intercalation and stripping，The lamella peeled off forms chemical bond with epoxy resin and is stably scattered in resin system，Modified epoxy is made to have superior high-temperature stability、Hot storage stability and ageing resistance，Improve water boiling resistance and the antikathode stripping performance of coating，The present invention goes back the composite modified filler of compatibility and other effective auxiliary agents simultaneously，The powdery paints coating adhesion prepared is good，It is resistant to the high temperature of 300 DEG C，Flame retardant effect is excellent，It it is the powdery paints of a kind of excellent performance.
Detailed description of the invention
A kind of high-temp resistant fire-retarding type montmorillonite intercalation polymeric modification epoxy resin based powder coating, is prepared by the raw materials in: bisphenol f type epoxy resin 68, montmorillonite 3.7, ethylenediamine 1.5, Oleum Brassicae campestris 8, vinyl three ('beta '-methoxy ethyoxyl) silane 3, Firebrake ZB 0.3, periclase powder 16, Folium Artemisiae Argyi 17, rosin milk 10, firming agent 2, pigment 5.
The manufacture method of described a kind of high-temp resistant fire-retarding type montmorillonite intercalation polymeric modification epoxy resin based powder coating, comprises the following steps:
(1) montmorillonite is put in the dilute hydrochloric acid solution that mass fraction is 5-8% and stir 3-5 hour at 50 DEG C-90 DEG C, filtering, washing, to neutral, is dried, it is dispersed in EtOH-DI water solution, add ethylenediamine at 60 DEG C of stirred in water bath 2-4 hour, ultrasonic disperse 20-30 minute, sucking filtration, washing, being dried under vacuum to constant weight, grind, sieve to obtain modified nano montmorillonite；
(2) dried by Folium Artemisiae Argyi, attrition grinding crosses 200 mesh sieves; addition rosin milk, periclase powder, Firebrake ZB stirring and evenly mixing stand 12-14 hour; pelletize; sinter 20-30 minute in 800-1000 DEG C under nitrogen protection, add vinyl three ('beta '-methoxy ethyoxyl) silane and grind 20-30 minute to obtain composite modified filler；
(3) by bisphenol f type epoxy resin, Oleum Brassicae campestris stirring and evenly mixing, add the modified nano montmorillonite of half quality, take out after reacting by heating 2-3 hour at 130-150 DEG C, obtain modified epoxy；
(4) modified epoxy, step (2) material, the modified nano montmorillonite of second half quality remaining and other residual componentss that step (3) prepares are put into stirring and evenly mixing in high mixer, melt extrude through double screw extruder, cooling pulverizing, crosses 250-300 mesh sieve, discharging.
The decocting in water performance and the antikathode fissility that utilize the powdery paints that the present invention prepares all reach Primary plateaus；Impact resistance is 37.9kg cm.
Claims (2)
1. a high-temp resistant fire-retarding type montmorillonite intercalation polymeric modification epoxy resin based powder coating, it is characterized in that, be prepared by the raw materials in: bisphenol f type epoxy resin 68-71, montmorillonite 3.7-4.3, ethylenediamine 1.5-1.8, Oleum Brassicae campestris 8-9, vinyl three ('beta '-methoxy ethyoxyl) silane 3-4, Firebrake ZB 0.3-0.5, periclase powder 16-18, Folium Artemisiae Argyi 17-20, rosin milk 10-12, firming agent 2-4, pigment 5-7.
The manufacture method of a kind of high-temp resistant fire-retarding type montmorillonite intercalation polymeric modification epoxy resin based powder coating the most according to claim 1, it is characterised in that comprise the following steps:
(1) montmorillonite is put in the dilute hydrochloric acid solution that mass fraction is 5-8% and stir 3-5 hour at 50 DEG C-90 DEG C, filtering, washing, to neutral, is dried, it is dispersed in EtOH-DI water solution, add ethylenediamine at 60 DEG C of stirred in water bath 2-4 hour, ultrasonic disperse 20-30 minute, sucking filtration, washing, being dried under vacuum to constant weight, grind, sieve to obtain modified nano montmorillonite；
(2) dried by Folium Artemisiae Argyi, attrition grinding crosses 200 mesh sieves; addition rosin milk, periclase powder, Firebrake ZB stirring and evenly mixing stand 12-14 hour; pelletize; sinter 20-30 minute in 800-1000 DEG C under nitrogen protection, add vinyl three ('beta '-methoxy ethyoxyl) silane and grind 20-30 minute to obtain composite modified filler；
(3) by bisphenol f type epoxy resin, Oleum Brassicae campestris stirring and evenly mixing, add the modified nano montmorillonite of half quality, take out after reacting by heating 2-3 hour at 130-150 DEG C, obtain modified epoxy；
(4) modified epoxy, step (2) material, the modified nano montmorillonite of second half quality remaining and other residual componentss that step (3) prepares are put into stirring and evenly mixing in high mixer, melt extrude through double screw extruder, cooling pulverizing, crosses 250-300 mesh sieve, discharging.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610532588.4A CN105907261A (en) | 2016-07-07 | 2016-07-07 | High heat-resistant and flame-retardant type modified epoxy resin based powder coating with intercalation polymerization of montmorillonite and preparation method of powder coating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610532588.4A CN105907261A (en) | 2016-07-07 | 2016-07-07 | High heat-resistant and flame-retardant type modified epoxy resin based powder coating with intercalation polymerization of montmorillonite and preparation method of powder coating |
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| CN105907261A true CN105907261A (en) | 2016-08-31 |
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| CN201610532588.4A Withdrawn CN105907261A (en) | 2016-07-07 | 2016-07-07 | High heat-resistant and flame-retardant type modified epoxy resin based powder coating with intercalation polymerization of montmorillonite and preparation method of powder coating |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109487358A (en) * | 2018-11-16 | 2019-03-19 | 安徽碧深高纤有限公司 | A kind of high strength fibre and preparation method thereof |
| CN111171671A (en) * | 2019-12-26 | 2020-05-19 | 中南林业科技大学 | Fireproof super-hydrophobic coating, super-hydrophobic material and preparation method thereof |
| CN115403989A (en) * | 2022-10-17 | 2022-11-29 | 浙江绿环新材料科技有限公司 | Preparation process of epoxy resin-based low-temperature curing powder coating |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709894A (en) * | 2013-12-02 | 2014-04-09 | 江苏科技大学 | Modified montmorillonite/epoxy resin composite material and preparation method thereof |
-
2016
- 2016-07-07 CN CN201610532588.4A patent/CN105907261A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709894A (en) * | 2013-12-02 | 2014-04-09 | 江苏科技大学 | Modified montmorillonite/epoxy resin composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 高阔等: "蒙脱土插层聚合制备环氧树脂及其粉末涂料性能的研究", 《胶体与聚合物》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109487358A (en) * | 2018-11-16 | 2019-03-19 | 安徽碧深高纤有限公司 | A kind of high strength fibre and preparation method thereof |
| CN111171671A (en) * | 2019-12-26 | 2020-05-19 | 中南林业科技大学 | Fireproof super-hydrophobic coating, super-hydrophobic material and preparation method thereof |
| CN115403989A (en) * | 2022-10-17 | 2022-11-29 | 浙江绿环新材料科技有限公司 | Preparation process of epoxy resin-based low-temperature curing powder coating |
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