CN106147540A - A kind of tough and tensile montmorillonite intercalation polymeric modification epoxy resin based powder coating and preparation method thereof - Google Patents

A kind of tough and tensile montmorillonite intercalation polymeric modification epoxy resin based powder coating and preparation method thereof Download PDF

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Publication number
CN106147540A
CN106147540A CN201610532559.8A CN201610532559A CN106147540A CN 106147540 A CN106147540 A CN 106147540A CN 201610532559 A CN201610532559 A CN 201610532559A CN 106147540 A CN106147540 A CN 106147540A
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China
Prior art keywords
montmorillonite
epoxy resin
tough
tensile
powder coating
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CN201610532559.8A
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Chinese (zh)
Inventor
陈俊
刘学涛
赵遵刚
霍柏林
李正
孙红兴
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Yan Mei Powdery Paints Co Ltd Of Hefei City
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Yan Mei Powdery Paints Co Ltd Of Hefei City
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Priority to CN201610532559.8A priority Critical patent/CN106147540A/en
Publication of CN106147540A publication Critical patent/CN106147540A/en
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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
    • C09D163/04—Epoxynovolacs
    • 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
    • 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
    • C09D5/08—Anti-corrosive paints
    • 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
    • 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
    • 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
    • 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
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • 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

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

nullThe invention discloses a kind of tough and tensile montmorillonite intercalation polymeric modification epoxy resin based powder coating，Montmorillonite dilute hydrochloric acid solution acidification is carried out organically-modified 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，Interlamellar spacing is made to expand，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 prepared is applied to pipeline corrosion protection field，There is good toughness、The advantage that shock resistance is high.

Description

A kind of tough and tensile montmorillonite intercalation polymeric modification epoxy resin based powder coating and making thereof Method
Technical field
The present invention relates to powder coating technology field, particularly relate to a kind of tough and tensile montmorillonite intercalation polymeric modification epoxy resin Based powder coatings and preparation method thereof.
Background technology
Along with the enhancing of mankind's environmental consciousness, solvent based coating is gradually restricted, and development meets the coating of environmental requirement Being trend of the times, 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, there is the advantages such as high usage, easy application, corrosion-resistant, environmental protection, the modern times spray It is widely applied with in corrosion-resistant field.
Epoxy powder coating is a kind of important new coating that development in recent years is got up, with the material profit that it is higher Heavier status is occupied with rate, stronger adhesive force and antiseptic property coating industry the most at home.In recent years, nanometer material The development of 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.Utilize montmorillonite and the asphalt mixtures modified by epoxy resin with layer structure Fat intercalation synthesis is prepared the research of a kind of high-performance epoxy resin based powder coatings and is received much concern, and epoxy resin based powder coating passes System modification is that modifying agent montmorillonite is disposably joined the twin-screw extrusion stage, when hot setting, makes limellar stripping, this side 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 tree Fat (E-51) inserts stratiform organo montmorillonite (OMMT), by intercalation polymeric and bisphenol-A and the 3rd component 2,6-di-t-butyl P-methyl phenol (BHT) reacts, and obtains a kind of powder coating epoxy resin.The test of X x ray diffraction shows, stratiform is received Rice montmorillonite layer is stripped completely, is dispersed in resin matrix.Control 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 prepare rank at epoxy resin Section is by abundant intercalation and stripping, but both poor compatibility, the levelability of film certainly will be affected, 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 its comprcssive strength, scratch resistance, anti-corrosive properties Etc. aspect improved, accordingly, it would be desirable to existing technique and formula are improved.
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 tough and tensile montmorillonite intercalation polymeric modification ring Epoxy resin-based powdery paints and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of tough and tensile montmorillonite intercalation polymeric modification epoxy resin based powder coating, is prepared by the raw materials in: phenolic aldehyde Epoxy resin 65-69, montmorillonite 3.2-3.7, polylactic acid 8-10, polyester resin emulsion 12-14, CNT 1.1-1.2, three second Amine 0.9-1.3, aluminium silicate 0.8-1.2, mullite powder 19-24, Semen Ziziphi Spinosae 18-23, aluminate coupling agent DL-411 3.7-4.3, Casein 0.2-0.4, firming agent 3-5, pigment 4-6.
The manufacture method of described a kind of tough and tensile montmorillonite intercalation polymeric modification epoxy resin based powder coating, including following Step:
(1) montmorillonite is put in the dilute hydrochloric acid solution that mass fraction is 5-8% and stirs 3-5 hour at 50 DEG C-90 DEG C, filter, Washing, to neutral, dried, is dispersed in EtOH-DI water solution, adds triethylamine, casein 60 DEG C of stirred in water bath 2- 4 hours, ultrasonic disperse 20-30 minute, sucking filtration, washing, it is dried under vacuum to constant weight, grinds, sieve to obtain modified nano montmorillonite；
(2) dried by Semen Ziziphi Spinosae, attrition grinding crosses 200 mesh sieves, adds polyester resin emulsion, mullite powder stirring and evenly mixing standing 12-14 hour, pelletize, sinter 20-30 minute in 800-1000 DEG C under nitrogen protection, addition aluminate coupling agent DL-411, CNT grinds 20-30 minute to obtain composite modified filler；
(3) by novolac epoxy resin, polylactic acid stirring and evenly mixing, the modified nano montmorillonite of half quality is added, in 130-150 DEG C Take out after lower reacting by heating 2-3 hour, obtain modified epoxy；
(4) modified epoxy prepared for step (3), step (2) material, the modified Nano of second half quality remaining are covered de- Soil and other residual componentss put into stirring and evenly mixing in high mixer, melt extrude through double screw extruder, cool down pulverizing, cross 250- 300 mesh sieves, discharging.
The invention have the advantage that montmorillonite dilute hydrochloric acid solution acidification is carried out organically-modified by the present invention again, weaken Adhesion between cheating engaging layer, makes interlayer lattice split, changes the highly polar of surface, make interlayer be changed into parent by hydrophilic Oiliness, reduces its surface energy, makes interlamellar spacing expand, and specific surface area and absorbability dramatically increase, and finally it are added at twice, Make montmorillonite steady by abundant intercalation and stripping, the lamella of stripping and epoxy resin formation chemical bond in the epoxy resin modification stage Surely it is scattered in resin system, makes modified epoxy have superior high-temperature stability, hot storage stability and aging resistance Property, improve water boiling resistance and the antikathode stripping performance of coating, the present invention goes back the composite modified filler of compatibility and other have simultaneously Effect auxiliary agent, prepared powdery paints is applied to pipeline corrosion protection field, has good toughness, an advantage that shock resistance is high, and preparation Technique is simple, is suitable to large-scale production.
Detailed description of the invention
A kind of tough and tensile montmorillonite intercalation polymeric modification epoxy resin based powder coating, is prepared by the raw materials in: Novolac epoxy resin 65, montmorillonite 3.2, polylactic acid 8, polyester resin emulsion 12, CNT 1.1, triethylamine 0.9, aluminium silicate 0.8, mullite powder 19, Semen Ziziphi Spinosae 18, aluminate coupling agent DL-411, casein 0.2, firming agent 3, pigment 4.
The manufacture method of described a kind of tough and tensile montmorillonite intercalation polymeric modification epoxy resin based powder coating, including following Step:
(1) montmorillonite is put in the dilute hydrochloric acid solution that mass fraction is 5-8% and stirs 3-5 hour at 50 DEG C-90 DEG C, filter, Washing, to neutral, dried, is dispersed in EtOH-DI water solution, adds triethylamine, casein 60 DEG C of stirred in water bath 2- 4 hours, ultrasonic disperse 20-30 minute, sucking filtration, washing, it is dried under vacuum to constant weight, grinds, sieve to obtain modified nano montmorillonite；
(2) dried by Semen Ziziphi Spinosae, attrition grinding crosses 200 mesh sieves, adds polyester resin emulsion, mullite powder stirring and evenly mixing standing 12-14 hour, pelletize, sinter 20-30 minute in 800-1000 DEG C under nitrogen protection, addition aluminate coupling agent DL-411, CNT grinds 20-30 minute to obtain composite modified filler；
(3) by novolac epoxy resin, polylactic acid stirring and evenly mixing, the modified nano montmorillonite of half quality is added, in 130-150 DEG C Take out after lower reacting by heating 2-3 hour, obtain modified epoxy；
(4) modified epoxy prepared for step (3), step (2) material, the modified Nano of second half quality remaining are covered de- Soil and other residual componentss put into stirring and evenly mixing in high mixer, melt extrude through double screw extruder, cool down pulverizing, cross 250- 300 mesh sieves, discharging.
The decocting in water performance and the antikathode fissility that utilize the powdery paints that the present invention prepares all reach Primary plateaus；Shock resistance Ability is 39.9kg cm.

Claims (2)

1. a tough and tensile montmorillonite intercalation polymeric modification epoxy resin based powder coating, it is characterised in that by following weight portion Raw material is made: novolac epoxy resin 65-69, montmorillonite 3.2-3.7, polylactic acid 8-10, polyester resin emulsion 12-14, carbon nanometer Pipe 1.1-1.2, triethylamine 0.9-1.3, aluminium silicate 0.8-1.2, mullite powder 19-24, Semen Ziziphi Spinosae 18-23, aluminate coupling agent DL-411 3.7-4.3, casein 0.2-0.4, firming agent 3-5, pigment 4-6.
The making side of a kind of tough and tensile montmorillonite intercalation polymeric modification epoxy resin based powder coating the most according to claim 1 Method, 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 stirs 3-5 hour at 50 DEG C-90 DEG C, filter, Washing, to neutral, dried, is dispersed in EtOH-DI water solution, adds triethylamine, casein 60 DEG C of stirred in water bath 2- 4 hours, ultrasonic disperse 20-30 minute, sucking filtration, washing, it is dried under vacuum to constant weight, grinds, sieve to obtain modified nano montmorillonite；
(2) dried by Semen Ziziphi Spinosae, attrition grinding crosses 200 mesh sieves, adds polyester resin emulsion, mullite powder stirring and evenly mixing standing 12-14 hour, pelletize, sinter 20-30 minute in 800-1000 DEG C under nitrogen protection, addition aluminate coupling agent DL-411, CNT grinds 20-30 minute to obtain composite modified filler；
(3) by novolac epoxy resin, polylactic acid stirring and evenly mixing, the modified nano montmorillonite of half quality is added, in 130-150 DEG C Take out after lower reacting by heating 2-3 hour, obtain modified epoxy；
(4) modified epoxy prepared for step (3), step (2) material, the modified Nano of second half quality remaining are covered de- Soil and other residual componentss put into stirring and evenly mixing in high mixer, melt extrude through double screw extruder, cool down pulverizing, cross 250- 300 mesh sieves, discharging.
CN201610532559.8A 2016-07-07 2016-07-07 A kind of tough and tensile montmorillonite intercalation polymeric modification epoxy resin based powder coating and preparation method thereof Withdrawn CN106147540A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108610900A (en) * 2018-04-08 2018-10-02 苏州聚康新材料科技有限公司 A kind of thermosetting powder coating preparation method and applications
CN113321861A (en) * 2021-05-20 2021-08-31 苏州赛荣建筑装饰工程有限公司 Antifouling flame-retardant high-density resin and preparation method thereof
CN117701112A (en) * 2024-01-23 2024-03-15 中建国际工程有限公司 Water-based building anti-corrosion coating and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
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

Patent Citations (1)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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 (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108610900A (en) * 2018-04-08 2018-10-02 苏州聚康新材料科技有限公司 A kind of thermosetting powder coating preparation method and applications
CN113321861A (en) * 2021-05-20 2021-08-31 苏州赛荣建筑装饰工程有限公司 Antifouling flame-retardant high-density resin and preparation method thereof
CN113321861B (en) * 2021-05-20 2023-09-08 贵州联创管业有限公司 Antifouling flame-retardant high-density resin and preparation method thereof
CN117701112A (en) * 2024-01-23 2024-03-15 中建国际工程有限公司 Water-based building anti-corrosion coating and preparation method thereof
CN117701112B (en) * 2024-01-23 2024-05-07 中建国际工程有限公司 Water-based building anti-corrosion coating and preparation method thereof

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