CN116920736A - MBT grafted microcapsule, preparation method and application thereof in coating - Google Patents
MBT grafted microcapsule, preparation method and application thereof in coating Download PDFInfo
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- CN116920736A CN116920736A CN202310886239.2A CN202310886239A CN116920736A CN 116920736 A CN116920736 A CN 116920736A CN 202310886239 A CN202310886239 A CN 202310886239A CN 116920736 A CN116920736 A CN 116920736A
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- mbt
- grafted
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- microcapsule
- resin
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 127
- 238000000576 coating method Methods 0.000 title claims abstract description 90
- 239000011248 coating agent Substances 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000011347 resin Substances 0.000 claims abstract description 49
- 229920005989 resin Polymers 0.000 claims abstract description 49
- 238000000016 photochemical curing Methods 0.000 claims abstract description 24
- 238000005260 corrosion Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000011162 core material Substances 0.000 claims abstract description 18
- 230000007797 corrosion Effects 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 12
- 239000003112 inhibitor Substances 0.000 claims abstract description 7
- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 6
- 239000000314 lubricant Substances 0.000 claims abstract description 6
- 230000007704 transition Effects 0.000 claims abstract description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 22
- 239000000839 emulsion Substances 0.000 claims description 19
- 239000004925 Acrylic resin Substances 0.000 claims description 17
- 229920000178 Acrylic resin Polymers 0.000 claims description 17
- 239000003921 oil Substances 0.000 claims description 17
- 235000019198 oils Nutrition 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000006185 dispersion Substances 0.000 claims description 13
- 238000003848 UV Light-Curing Methods 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- 229920000728 polyester Polymers 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 7
- 239000004593 Epoxy Substances 0.000 claims description 7
- 238000001723 curing Methods 0.000 claims description 7
- 230000001804 emulsifying effect Effects 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000003995 emulsifying agent Substances 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims description 4
- 239000000944 linseed oil Substances 0.000 claims description 4
- 235000021388 linseed oil Nutrition 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 3
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 229920005749 polyurethane resin Polymers 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 238000000935 solvent evaporation Methods 0.000 claims description 3
- QMMJWQMCMRUYTG-UHFFFAOYSA-N 1,2,4,5-tetrachloro-3-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=C(Cl)C(Cl)=CC(Cl)=C1Cl QMMJWQMCMRUYTG-UHFFFAOYSA-N 0.000 claims description 2
- 239000005725 8-Hydroxyquinoline Substances 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000005844 Thymol Substances 0.000 claims description 2
- 239000002199 base oil Substances 0.000 claims description 2
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 2
- 239000012964 benzotriazole Substances 0.000 claims description 2
- RECUKUPTGUEGMW-UHFFFAOYSA-N carvacrol Chemical compound CC(C)C1=CC=C(C)C(O)=C1 RECUKUPTGUEGMW-UHFFFAOYSA-N 0.000 claims description 2
- HHTWOMMSBMNRKP-UHFFFAOYSA-N carvacrol Natural products CC(=C)C1=CC=C(C)C(O)=C1 HHTWOMMSBMNRKP-UHFFFAOYSA-N 0.000 claims description 2
- 235000007746 carvacrol Nutrition 0.000 claims description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 2
- 238000005286 illumination Methods 0.000 claims description 2
- WYXXLXHHWYNKJF-UHFFFAOYSA-N isocarvacrol Natural products CC(C)C1=CC=C(O)C(C)=C1 WYXXLXHHWYNKJF-UHFFFAOYSA-N 0.000 claims description 2
- 239000012948 isocyanate Substances 0.000 claims description 2
- 150000002513 isocyanates Chemical class 0.000 claims description 2
- 239000010687 lubricating oil Substances 0.000 claims description 2
- 229940111617 oregano oil Drugs 0.000 claims description 2
- 239000010661 oregano oil Substances 0.000 claims description 2
- 229960003540 oxyquinoline Drugs 0.000 claims description 2
- 230000000379 polymerizing effect Effects 0.000 claims description 2
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims description 2
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 229920002050 silicone resin Polymers 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 229960000790 thymol Drugs 0.000 claims description 2
- 239000002383 tung oil Substances 0.000 claims description 2
- FAOSYNUKPVJLNZ-UHFFFAOYSA-N butylstannane Chemical compound CCCC[SnH3] FAOSYNUKPVJLNZ-UHFFFAOYSA-N 0.000 claims 1
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 abstract description 241
- 230000000694 effects Effects 0.000 abstract description 14
- 230000005764 inhibitory process Effects 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 description 23
- 238000007792 addition Methods 0.000 description 16
- 238000011068 loading method Methods 0.000 description 10
- 150000003839 salts Chemical class 0.000 description 9
- 230000004048 modification Effects 0.000 description 8
- 238000012986 modification Methods 0.000 description 8
- -1 4-methylthiophenyl Chemical group 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 239000002318 adhesion promoter Substances 0.000 description 4
- 239000003085 diluting agent Substances 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- XMLYCEVDHLAQEL-UHFFFAOYSA-N 2-hydroxy-2-methyl-1-phenylpropan-1-one Chemical group CC(C)(O)C(=O)C1=CC=CC=C1 XMLYCEVDHLAQEL-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 239000004814 polyurethane Substances 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002715 modification method Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012782 phase change material Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/025—Applications of microcapsules not provided for in other subclasses
-
- 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
-
- 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
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plant Pathology (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention relates to an MBT (2-mercaptobenzothiazole) grafted microcapsule, a preparation method and application thereof in a coating, and belongs to the field of microcapsules. The MBT grafted microcapsule consists of a shell layer and a core material, wherein the shell layer wraps the core material; the core material is a corrosion inhibitor, a self-repairing agent, an antibacterial agent, a self-lubricating agent, a phase transition agent and other functional substances; the shell layer is MBT modified photo-curing resin; the functional substance is one or a combination of the functional substances. MBT is introduced into the microcapsule shell layer by a one-step method, and the shell layer modified MBT grafted microcapsule is prepared. The dispersibility of the microcapsule in the coating can be effectively improved, and the problem of reduced basic performance of the coating caused by the addition of the microcapsule is avoided. Meanwhile, the MBT has good corrosion inhibition effect, and can effectively improve the corrosion resistance effect of the coating. The MBT grafted microcapsules with different functions are added into the coating to obtain the functional coating with excellent performance.
Description
Technical Field
The invention relates to an MBT (2-mercaptobenzothiazole) grafted microcapsule, a preparation method and application thereof in a coating, and belongs to the field of microcapsules.
Background
Functional coatings have been widely used in various fields due to their specific functionality. The filler is added into the coating, so that the method is a simple and effective method for endowing the coating with functions and improving the coating performance, and has good development trend in the field of coating research. At present, the use of microcapsules encapsulating different core materials as fillers in coating systems to impart specific functions to the coating has become a focus of research. The common core materials in the microcapsule mainly comprise medicines, dyes, bactericides, repairing agents, corrosion inhibitors, phase change materials and the like.
Microcapsules are an important prerequisite for their function in achieving good dispersion of the coating when added to the coating. If the dispersion is poor, the compactness of the coating is affected, defects are formed in the coating and become stress concentration points, so that the mechanical property of the coating is reduced. 2-Mercaptobenzothiazole (MBT) is a heterocyclic compound that is widely used as a metal type ionic corrosion inhibitor. MBT in MBT microcapsule is usually used as core material, and the active ingredient 2-mercaptobenzothiazole is gradually released after the MBT microcapsule is added in the coating. These active ingredients can react with oxygen and water on the metal surface to form insoluble metal sulfide precipitates, thereby forming a protective film to prevent further corrosion. Microencapsulation can delay the release rate of MBT, so that the durability and stability of the corrosion inhibition effect can be maintained. However, due to the poor dispersibility, the application of the MBT microcapsule is limited, and MBT microcapsule added into the coating is easy to agglomerate to form defects, so that the performance of the coating is affected.
One direction to solve this problem is to modify MBT microcapsules to improve their dispersibility, but the modification method in the prior art is relatively complex, and generally needs to modify the microcapsule wall material first and then perform microencapsulation, or modify the wall material after preparing microcapsules, and the preparation process of modified microcapsules is relatively complex.
In view of the above problems, it is necessary to develop a microcapsule which is simple in modification method, can make full use of MBT corrosion inhibition performance, and imparts specific functions to the coating while improving dispersibility of the microcapsule.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a method for preparing MBT grafted microcapsules by a one-step method. Preparing microcapsules by adopting a solvent volatilization method, wherein a shell layer adopts photo-curing resin; MBT is added into the oil phase, and in the process of volatilizing the solvent, the MBT can be subjected to phase separation along with the photo-curing resin prepolymer and migrate to an oil-water interface. The photo-curing resin is subjected to UV curing to form a microcapsule shell layer, and the MBT reacts with double bonds in the photo-curing resin to realize shell modification of the microcapsule, so that the MBT grafted microcapsule is obtained. Simultaneously, MBT grafted microcapsules coated with different core materials are added into the coating.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a first object of the present invention is to provide an MBT grafted microcapsule, comprising a shell layer and a core material, characterized in that the shell layer encapsulates the core material; the core material is a functional substance; the shell layer is MBT modified photo-curing resin;
the MBT modified light-cured resin is formed by polymerizing light-cured resin prepolymer and MBT under illumination;
the functional substance is one or a combination of corrosion inhibitor, self-repairing agent, antibacterial agent, self-lubricant and phase transition agent.
MBT-modified photocurable resins i.e. photocurable resins that have been graft modified with MBT.
In one embodiment, the photocurable resin prepolymer is one or a combination of urethane acrylate, polyester acrylate and epoxy acrylate.
The corrosion inhibitor is selected from one of MBT, benzotriazole and 8-hydroxyquinoline;
the self-repairing agent is selected from one of drying oil such as linseed oil, tung oil and the like;
the antibacterial agent is selected from one of carvacrol, thymol and oregano oil;
the self-lubricant is selected from one of lubricating oil base oil, silicone oil, siloxane and isocyanate;
the phase transition agent is selected from one of paraffin, butyl stearate and n-hexadecane;
the photoinitiator is selected from one of 2-hydroxy-2-methyl-1-phenyl-1-acetone, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone and 2-methyl-1- (4-methylthiophenyl) -2-morpholino-1-acetone.
The second object of the present invention is to provide a method for preparing MBT grafted microcapsules, characterized by comprising the steps of:
s1: dissolving MBT, functional substances, a photo-curing resin prepolymer and a photoinitiator in an organic solvent to obtain an oil phase, and using an aqueous dispersion liquid of an emulsifier as a water phase; mixing and emulsifying the water phase and the oil phase to obtain emulsion A;
s2: and (3) stirring the emulsion A to volatilize the solvent, and then placing the emulsion A under a light source for photo-curing to obtain the MBT grafted microcapsule.
The MBT grafted microcapsule is prepared by a one-step method, and the microcapsule preparation and the shell modification are completed in one step.
In one embodiment, the emulsification mode of the water phase and the oil phase in the step S1 adopts a cell pulverizer, and emulsion is prepared after the emulsification of the cell pulverizer;
in one embodiment, the cell disruptor emulsifying time is from 10 minutes to 20 minutes.
In one embodiment, in step S1: the oil phase comprises the following components in percentage by mass: 35-65 parts of organic solvent, 15-25 parts of photo-curing resin prepolymer, 15-25 parts of core material and 1-4 parts of photoinitiator.
Further, the added amount of the MBT is 2.5-10 wt% of the photo-curing resin prepolymer;
in one embodiment, in step S1: the emulsifier is one or a combination of polyvinyl alcohol, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and cetyltrimethylammonium bromide;
in one embodiment, the aqueous emulsifier dispersion has a concentration of 0.5wt% to 2.0wt%;
in one embodiment, the organic solvent is selected from one or a combination of dichloromethane, chloroform, ethyl acetate and toluene;
in one embodiment, the volume ratio of the oil phase to the water phase is from 1:4 to 1:10.
In one embodiment, the solvent evaporation temperature in step S2 is 20-60 ℃;
in one embodiment, the solvent evaporation time in step S2 is 2-10 hours;
in one embodiment, the photo-curing in step S2 is performed by UV curing, wherein the UV curing wavelength is 230-420nm and the curing time is 1-10min.
In one embodiment, the solvent volatilization is accelerated by adopting a stirring mode, and the stirring time is 2-10 hours;
in one embodiment, the light source for photocuring employs an ultraviolet lamp;
in one embodiment, the photoinitiator is 2-hydroxy-2-methyl-1-phenyl-1-propanone;
it is a third object of the present invention to provide the use of MBT grafted microcapsules in a coating formed by curing a film-forming resin coating system to which 2-10wt% MBT modified microcapsules have been added.
In one embodiment, the film-forming resin is one or more of polyurethane resin, epoxy resin, acrylic resin, fluorocarbon resin, silicone resin, urethane acrylic resin, epoxy acrylic resin, polyester acrylate.
The beneficial effects are that:
(1) MBT is introduced into a shell layer in the microcapsule preparation process by a one-step method, so that the shell layer modified MBT grafted microcapsule is successfully prepared.
(2) The MBT grafted microcapsule is added into the coating, so that the dispersibility of the microcapsule in the coating is obviously improved, and the problem of reduced basic performance of the coating caused by agglomeration of the microcapsule is effectively avoided.
(3) The dispersibility of the grafted microcapsule in the coating is obviously improved, and the MBT has good corrosion inhibition effect, so that the corrosion resistance effect of the coating can be effectively improved.
(4) The self-repairing agent, the antibacterial agent, the self-lubricating agent, the phase transition agent and other substances are coated in the grafted microcapsule, and the microcapsule is added into the coating, so that the functional coating with excellent performances can be successfully prepared.
Drawings
FIG. 1 is a scanning electron microscope characterization diagram of MBT grafted microcapsules prepared in example 1;
FIG. 2 is a scanning electron microscope characterization diagram and a microcapsule surface element energy spectrum diagram of MBT grafted microcapsules with different MBT addition amounts prepared in example 2, wherein the graphs (a), (b) and (c) are respectively a scanning electron microscope characterization diagram and a surface element energy spectrum diagram of 10MBT-PUA MCs, 30MBT-PUA MCs and 50MBT PUA MCs;
FIG. 3 is a scanning electron microscope image of a cross section of a sample bar prepared in example 5, and graphs (a), (b), (c) and (d) are scanning electron microscope characterization images of the dispersion of unmodified microcapsules, 10MBT-PUA MCs, 30MBT-PUA MCs and 50MBT PUA MCs, respectively;
FIG. 4 is a photograph of a salt spray test of the pure resin coating prepared in example 7 and a composite coating with MBT grafted microcapsules of varying degrees of modification within 500 hours.
Detailed Description
The preparation method of the invention comprises the following steps: mixing the photo-curing resin prepolymer, an organic solvent, a core material and MBT as an oil phase, taking a polyvinyl alcohol aqueous dispersion liquid as a water phase, and emulsifying by using a cell pulverizer to obtain an emulsion. After the emulsion volatilizes the solvent, the emulsion is placed under an ultraviolet lamp for photo-curing to obtain MBT grafted microcapsules, and the MBT grafted microcapsules are added into the coating to explore the influence of the MBT grafted microcapsules on each performance of the coating. The method specifically comprises the following steps:
1. preparation of MBT grafted microcapsules: mixing the photo-curing resin prepolymer, the organic solvent, the core material and the MBT to prepare an oil phase, adding the oil phase into a polyvinyl alcohol aqueous dispersion liquid serving as a water phase, and emulsifying the mixture by a cell pulverizer to obtain an emulsion. The resulting emulsion was stirred at room temperature to volatilize the solvent, and the photo-curable resin prepolymer was phase-separated to migrate to the oil-water interface. And (3) placing the emulsion after volatilizing the solvent under an ultraviolet lamp for curing to obtain the MBT grafted microcapsule.
2. Preparation of the composite coating: MBT grafted microcapsules are added to the coating system. The film-forming resin is one or more of polyurethane resin, epoxy resin, acrylic resin, fluorocarbon resin, organic silicon resin, polyurethane acrylic resin, epoxy acrylic resin and polyester acrylic ester.
3. Testing of coating properties:
(1) Basic properties of the coating: the steel plate is used as a coating film base material, and the thickness, pencil hardness, adhesive force, impact resistance and other basic properties of the coating are tested.
(2) Coating corrosion resistance: the corrosion resistance of the coating was tested by electrochemical and salt spray tests.
(3) Coating self-repairing performance: scratches were made on the surface of the coating, and repair of the scratches was observed to test the self-repair properties of the coating.
The present invention will be described in further detail with reference to examples.
Example 1: preparation of MBT grafted microcapsules
(1) Preparing emulsion: MBT (0.025 parts), methylene dichloride (2.5 parts) and linseed oil (functional substances, 1 part) which are prepared by taking certain mass, polyurethane acrylic ester (photo-curing resin prepolymer, 1 part) and 2-hydroxy-2-methyl-1-phenyl-1-acetone (photoinitiator 1173,0.02 parts) as oil phases and 1.5 weight percent polyvinyl alcohol aqueous dispersion liquid as water phases; emulsifying under the condition that the oil-water ratio is 1:6 to obtain emulsion;
(2) Preparation of MBT grafted microcapsules: the emulsion obtained in the previous step is stirred for 10 hours at 20 ℃ to volatilize dichloromethane, and then the dichloromethane is placed under an ultraviolet lamp to be subjected to photo-curing for 15 minutes to obtain the MBT grafted microcapsule.
From the scanning electron microscope characterization of MBT grafted microcapsules prepared in example 1 of FIG. 1, it can be seen that MBT grafted microcapsules were successfully prepared, and that the particle size of the microcapsules was about 5-10. Mu.m.
Example 2: preparation of MBT grafted microcapsules with different MBT addition amounts
(1) Preparing emulsion: MBT (0.025 parts, 0.075 parts, 0.125 parts), methylene dichloride (organic solvent, 2.5 parts), linseed oil (functional substance, 1 part), polyurethane acrylic ester (photo-curing resin prepolymer, 1 part), 2-hydroxy-2-methyl-1-phenyl-1-acetone (photo-initiator 1173,0.02 parts) which are used as oil phases, and 1.5wt% polyvinyl alcohol aqueous dispersion liquid which is used as water phases; emulsifying under the condition that the oil-water ratio is 1:6 to obtain emulsion;
(2) Preparation of MBT grafted microcapsules: the emulsion obtained in the previous step was stirred at 20℃for 10 hours to volatilize methylene chloride, which was then subjected to photo-curing under an ultraviolet lamp for 15 minutes to obtain MBT graft microcapsules with different MBT addition amounts of 0.025 parts, 0.075 parts and 0.125 parts, and the microcapsules obtained were 10MBT-PUA MCs, 30MBT-PUA MCs and 50MBT PUA MCs, respectively.
(3) MBT grafting test: and testing surface elements of the MBT grafted microcapsule by an EDS (electron beam ionization) spectrometer, and observing the grafting condition of the MBT on the surface of the microcapsule.
FIG. 2 is a scanning electron microscope characterization diagram of MBT grafted microcapsules with different MBT addition amounts prepared in example 2 of the invention and a microcapsule surface element energy spectrum; the successful preparation of MBT grafted microcapsules can be seen from the scanning electron microscope image in fig. 2. In addition, since the MBT contains sulfur element, as can be seen from the energy spectrum of the element on the surface of the microcapsule, the atomic percent of the sulfur element on the surface of the microcapsule gradually increases with the increase of the added amount of the MBT, which indicates that the MBT is successfully grafted on the surface of the microcapsule, and the grafting amount of the MBT on the surface of the microcapsule gradually increases with the increase of the added amount of the MBT.
Example 3: effect of MBT addition on MBT loading in microcapsules
And weighing 1g of each MBT microcapsule prepared under different MBT addition amounts, respectively soaking the MBT microcapsules in 50ml of absolute ethyl alcohol after wrapping the MBT microcapsules by using weighing paper, and testing the concentration of the MBT in the absolute ethyl alcohol by using an ultraviolet-visible spectrophotometer after soaking the MBT microcapsules for 24 hours, thereby calculating and obtaining the loading rate and the loading efficiency of the MBT in the MBT microcapsules under different MBT addition amounts. The effect of MBT addition on the loading rate and loading efficiency of MBT in microcapsules is shown in table 1.
As can be seen from the data in table 1, as the MBT addition increases, the MBT loading rate in the microcapsules increases gradually, and the loading efficiency increases and decreases. This shows that when the added amount of MBT in the microcapsule is increased from 10mg/g (MBT/methylene chloride) to 30mg/g, the effective loading amount of MBT in the core material is increased with the increase of the added amount of MBT, and when the added amount of MBT is further increased to 50mg/g, more MBT is grafted to the surface of the microcapsule shell layer, resulting in a decrease in the loading efficiency of MBT. In combination with the results of example 2, it was demonstrated that MBT moieties were grafted onto the microcapsule surface, and that further moieties were encapsulated in microcapsules.
TABLE 1 loading of MBT in microcapsules at different MBT additions
| 10MBT-PUA MCs | 30MBT-PUAMCs | 50MBT-PUAMCs | |
| Load factor (%) | 1.24 | 3.19 | 5.17 |
| Load efficiency (%) | 18.37 | 21.29 | 20.68 |
Example 4: preparation of coatings with MBT grafted microcapsules
(1) Preparation of a resin System A certain mass of epoxy acrylic resin (prepolymer, 30 parts), polyester acrylic resin (prepolymer, 40 parts), isobornene acrylate (reactive diluent, 30 parts), 2-methyl-2-acrylic acid-2-hydroxyethyl phosphate (adhesion promoter, 2 parts), 2-hydroxy-2-methyl-1-phenyl-1-propanone (photoinitiator, 1173,2 parts) was weighed, 5 parts of MBT grafted microcapsules were added, ball milling was performed at 2500rpm, and the resin system with MBT grafted microcapsules was obtained after 3min of dispersion.
(2) Preparation of the coating: and coating the prepared resin system on the surface of a low-carbon steel plate by using a frame type film scraping device, and curing by using a crawler-type UV curing machine to obtain the composite coating added with the MBT grafted microcapsule.
Example 5: effect of MBT addition on the dispersibility of microcapsules in coatings
(1) Preparation of the resin System: the epoxy acrylic resin (prepolymer, 30 parts), the polyester acrylic resin (prepolymer, 40 parts), the isobornene acrylate (reactive diluent, 30 parts), the 2-methyl-2-acrylic acid-2-hydroxyethyl phosphate (adhesion promoter, 2 parts), the 2-hydroxy-2-methyl-1-phenyl-1-propanone (photoinitiator 1173,2 parts) were weighed into each of 5 parts of unmodified microcapsules, 10MBT-PUA MCs, 30MBT-PUAMCs and 50MBT PUA MCs, ball-milled at 2500rpm, and dispersed for 3 minutes to obtain a mixed resin system added with MBT grafted microcapsules of different modification degrees.
(2) Preparing a spline: and (3) adding the resin mixture obtained in the steps into a dumbbell-shaped mold, and placing under a crawler-type UV curing machine for curing to obtain a spline.
(3) Dispersibility test: and (3) placing the sample strips obtained in the steps in liquid nitrogen for brittle fracture, and observing the section of the sample strips by using a scanning electron microscope, so as to compare the dispersion conditions of the unmodified microcapsules and the microcapsules prepared under different MBT addition amounts in the coating.
From fig. 3, a scanning electron microscope image of a section of a spline was prepared in example 5, wherein (a) unmodified microcapsules were added, and it can be seen that agglomeration occurred in the section; (b) After the modified microcapsule is added in the steps (c) and (d), the dispersibility of the microcapsule is obviously improved, and the agglomeration phenomenon is obviously reduced. In addition, it can be seen that the dispersibility of the MBT grafted microcapsules in the coating gradually increases as the amount of MBT added increases.
Example 6: effect of MBT grafted microcapsules on basic coating Properties
(1) Preparation of the coating: weighing epoxy acrylic resin (prepolymer, 30 parts), polyester acrylic resin (prepolymer, 40 parts), isobornene acrylic ester (active diluent, 30 parts), 2-methyl-2-acrylic acid-2-hydroxyethyl phosphate (adhesion promoter, 2 parts) and 2-hydroxy-2-methyl-1-phenyl-1-acetone (photoinitiator, 1173,2 parts), adding 5 parts of MBT grafted microcapsules, ball milling at 2500rpm, and dispersing for 3min to obtain a mixed resin system added with MBT grafted microcapsules with different modification degrees. The resin mixture was coated on the surface of a low carbon steel plate using a frame type film wiper, and cured using a crawler type UV curing machine to obtain a coated sample.
(2) Testing of basic properties of the coating:
thickness: the coating is horizontally placed on a tabletop, a 1500-type coating thickness meter of Germany Qnix company is used for testing according to GB/T13452.2-2008, the same coating is measured for three times at different positions, and the final result is obtained as a data average value;
pencil hardness test: horizontally placing the coating on a tabletop, scraping the surface of the coating by using a pencil at an angle of 45 degrees, evaluating the pencil hardness of the coating according to the GB/T6739-2006 standard, measuring the same coating at different positions for three times, and taking a data average value of the final result;
and (3) testing adhesive force by a cross-hatch method: the coating is horizontally placed on a tabletop, the test is carried out according to national standard GB/T9286-1998 by a hundred grid method, the same coating is measured for three times at different positions, and the final result is obtained as a data average value;
impact strength test: using an impact strength tester to test the impact strength of the coating, testing according to GB 1943-2007, measuring the same coating at different positions for three times, and taking a data average value as a final result;
the results obtained are shown in Table 2 below, and it can be seen from the table that the film thickness, pencil hardness and adhesion of the composite coating to which the MBT grafted microcapsule was added were not significantly changed, but the impact strength was slightly lowered, as compared with the pure resin coating. This is mainly due to the fact that the addition of microcapsules has an effect on the compactness of the coating, resulting in a decrease of the impact strength.
TABLE 2 basic Properties of coating
Example 7: effect of MBT grafted microcapsules on coating anti-corrosive Properties
(1) Preparation of the coating: weighing epoxy acrylic resin (prepolymer, 30 parts), polyester acrylic resin (prepolymer, 40 parts), isobornene acrylate (reactive diluent, 30 parts), 2-methyl-2-acrylic acid-2-hydroxyethyl phosphate (adhesion promoter, 2 parts), 2-hydroxy-2-methyl-1-phenyl-1-acetone (photoinitiator 1173,2 parts), respectively adding 5 parts of 10MBT-PUAMCs, 30MBT-PUAMCs and 50MBT PUA MCs, ball milling at 2500rpm, dispersing for 3min, and obtaining a mixed resin system added with MBT grafted microcapsules with different modification degrees. The resin mixture was coated on the surface of a low carbon steel plate using a frame type film wiper, and cured using a crawler type UV curing machine to obtain a coated sample. Pure resin coated samples without MBT grafted microcapsules were prepared by the same procedure.
(2) And (3) testing the corrosion resistance of the coating: the anti-corrosion performance of the coating is tested by a neutral salt spray resistance test. Sealing the back and edge parts of the low-carbon steel plate coated with the coating by using a waterproof adhesive tape, and sealing the gaps by using a mixture of paraffin and rosin. The salt FOG resistance test is carried out by using a Q-FOG SSP-600 type circulating corrosion salt FOG box of Q-Lab company according to the standard GB/T1771-2007 determination of neutral salt FOG resistance of color paint and varnish, the concentration of NaCl solution used by salt FOG is 5wt%, the test temperature is 35 ℃, and the pressure in the salt FOG box is 10KPa.
As shown in the salt spray test photograph of fig. 4, it can be seen from the figure that at a test time of 100 hours, a clear pitting phenomenon appears on the surface of the pure resin coating, whereas no pitting is observed on the surface of the composite coating added with the MBT grafted microcapsules. When the test time reaches 300 hours, the pitting phenomenon of the surface of the pure resin coating is aggravated, the surface of the coating added with 10MBT-PUA MCs and 30MBT-PUA MCs is slightly pitted, and the surface of the coating added with 50MBT-PUA MCs is still unchanged obviously, which indicates that the addition of the MBT grafted microcapsule can improve the anti-corrosion effect of the coating, and the 50MBT-PUA MCs have the best effect of improving the anti-corrosion performance of the coating. The addition of the MBT grafted microcapsule can effectively improve the anti-corrosion performance of the coating, and the anti-corrosion effect is obviously improved along with the increase of the MBT addition in the microcapsule preparation process.
The foregoing is only a preferred embodiment of the invention, it being noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (10)
1. An MBT grafted microcapsule comprises a shell layer and a core material, and is characterized in that the shell layer wraps the core material; the core material is a functional substance; the shell layer is MBT modified photo-curing resin;
the MBT modified light-cured resin is formed by polymerizing light-cured resin prepolymer and MBT under illumination;
the functional substance is one or a combination of corrosion inhibitor, self-repairing agent, antibacterial agent, self-lubricant and phase transition agent.
2. The MBT grafted microcapsule according to claim 1, wherein the photocurable resin prepolymer is one or a combination of urethane acrylate, polyester acrylate and epoxy acrylate.
3. The MBT grafted microcapsule of claim 1,
the corrosion inhibitor is selected from one of MBT, benzotriazole and 8-hydroxyquinoline;
the self-repairing agent is selected from one of drying oil such as linseed oil, tung oil and the like;
the antibacterial agent is selected from one of carvacrol, thymol and oregano oil;
the self-lubricant is selected from one of lubricating oil base oil, silicone oil, siloxane and isocyanate;
the phase transition agent is selected from one of paraffin, butyl stearate and n-hexadecane.
4. A process for the preparation of MBT grafted microcapsules according to any of claims 1-3, comprising the steps of:
s1: dissolving MBT, functional substances, a photo-curing resin prepolymer and a photoinitiator in an organic solvent to obtain an oil phase, and using an aqueous dispersion liquid of an emulsifier as a water phase; mixing and emulsifying the water phase and the oil phase to obtain emulsion A;
s2: and (3) stirring the emulsion A to volatilize the solvent, and then placing the emulsion A under a light source for photo-curing to obtain the MBT grafted microcapsule.
5. The method of preparing MBT grafted microcapsules according to claim 4, wherein in step S1:
the oil phase comprises the following components in percentage by mass: 35-65 parts of organic solvent, 15-25 parts of photo-curing resin prepolymer, 15-25 parts of core material and 1-4 parts of photoinitiator.
6. The method of preparing MBT grafted microcapsules according to claim 4, wherein in step S1:
the emulsifier is one or a combination of polyvinyl alcohol, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and cetyltrimethylammonium bromide; the concentration of the emulsifier aqueous dispersion is 0.5wt% to 2.0wt%.
7. The method for preparing MBT grafted microcapsules according to claim 4, wherein the organic solvent is selected from one or a combination of dichloromethane, chloroform, ethyl acetate, toluene;
the volume ratio of the oil phase to the water phase is 1:4-1:10.
8. The method for preparing MBT grafted microcapsules according to claim 4, wherein the solvent evaporation temperature is 20-60 ℃; the solvent volatilizing time is 2-10h;
the photo-curing adopts UV curing, wherein the wavelength of the UV curing is 230-420nm, and the curing time is 1-10min.
9. Use of MBT grafted microcapsules according to any of claims 1-3 or MBT grafted microcapsules obtainable by the process according to any of claims 4-8, characterized in that it is applied in a coating formed by curing a film-forming resin coating system to which 2-10wt% of MBT modified microcapsules are added.
10. The use of MBT grafted microcapsules according to claim 9, wherein the film-forming resin is one or more of polyurethane resin, epoxy resin, acrylic resin, fluorocarbon resin, silicone resin, urethane acrylic resin, epoxy acrylic resin, polyester acrylate.
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| CN117165135B (en) * | 2023-11-02 | 2024-01-02 | 江苏新福乐威涂料有限公司 | Preparation method of anti-corrosion and anti-scale fluorocarbon coating material |
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