CN107974139A - A kind of preparation method of the highly-chlorinated polyethylene of the mica powder of coupling modifier containing dry method-anti-corrosive paint of epoxy resin paint - Google Patents
A kind of preparation method of the highly-chlorinated polyethylene of the mica powder of coupling modifier containing dry method-anti-corrosive paint of epoxy resin paint Download PDFInfo
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- CN107974139A CN107974139A CN201711162031.7A CN201711162031A CN107974139A CN 107974139 A CN107974139 A CN 107974139A CN 201711162031 A CN201711162031 A CN 201711162031A CN 107974139 A CN107974139 A CN 107974139A
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- toluene
- epoxy resin
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- 239000003973 paint Substances 0.000 title claims abstract description 38
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 33
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 33
- 239000000843 powder Substances 0.000 title claims abstract description 30
- 239000010445 mica Substances 0.000 title claims abstract description 28
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 28
- 239000004709 Chlorinated polyethylene Substances 0.000 title claims abstract description 21
- 230000008878 coupling Effects 0.000 title claims abstract description 16
- 238000010168 coupling process Methods 0.000 title claims abstract description 16
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 16
- 239000003607 modifier Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 89
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 230000004048 modification Effects 0.000 claims abstract description 14
- 238000012986 modification Methods 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 12
- 239000012948 isocyanate Substances 0.000 claims abstract description 10
- 239000000945 filler Substances 0.000 claims abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 9
- 239000004593 Epoxy Substances 0.000 claims abstract description 8
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000013019 agitation Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 229910000077 silane Inorganic materials 0.000 claims abstract description 8
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 6
- 239000002105 nanoparticle Substances 0.000 claims abstract description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 5
- 238000007599 discharging Methods 0.000 claims abstract description 5
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims abstract 2
- 238000010992 reflux Methods 0.000 claims abstract 2
- 239000011248 coating agent Substances 0.000 claims description 19
- 238000000576 coating method Methods 0.000 claims description 19
- 238000005260 corrosion Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 6
- 239000003085 diluting agent Substances 0.000 claims description 6
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 230000008595 infiltration Effects 0.000 claims description 3
- 238000001764 infiltration Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- -1 polyethylenes Polymers 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000009736 wetting Methods 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- QNYBOILAKBSWFG-UHFFFAOYSA-N 2-(phenylmethoxymethyl)oxirane Chemical group C1OC1COCC1=CC=CC=C1 QNYBOILAKBSWFG-UHFFFAOYSA-N 0.000 claims description 2
- APWQGZRMFPWDFZ-UHFFFAOYSA-N 3-phenylprop-2-enoic acid;tin Chemical compound [Sn].OC(=O)C=CC1=CC=CC=C1 APWQGZRMFPWDFZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000010426 asphalt Substances 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 claims description 2
- 239000008236 heating water Substances 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- 235000013980 iron oxide Nutrition 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- HSRJKNPTNIJEKV-UHFFFAOYSA-N Guaifenesin Chemical compound COC1=CC=CC=C1OCC(O)CO HSRJKNPTNIJEKV-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920006334 epoxy coating Polymers 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
Classifications
-
- 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
- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
- C09D123/26—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers modified by chemical after-treatment
- C09D123/28—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers modified by chemical after-treatment by reaction with halogens or compounds containing halogen
- C09D123/286—Chlorinated polyethylene
-
- 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
-
- 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
- C09D5/082—Anti-corrosive paints characterised by the anti-corrosive pigment
- C09D5/084—Inorganic compounds
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2272—Ferric oxide (Fe2O3)
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses the preparation method that a kind of highly-chlorinated polyethylene anti-corrosive paint of epoxy resin of mica powder of coupling modifier containing dry method paints, it is characterised in that silane coupler solution, ammonium hydroxide is added dropwise into mica powder, mechanical agitation is disperseed, and obtains dry method modification mica powder；Mixed after nano silicon dioxide is dried with polyethylene glycol, toluene, heating reflux reaction obtains polyethylene glycol Grafted Nano-scale particle；Into micaceous iron oxide plus toluene, stirring, ultrasonic component A；Toluene di-isocyanate(TDI), dibutyl tin dilaurate, toluene are mixed, are added drop-wise in component A, stirring reaction, then temperature reaction obtain toluene di-isocyanate(TDI) modified micaceous iron oxide filler；Highly-chlorinated polyethylene solution, epoxy compositions are added in dispersion tank, are uniformly dispersed, add curing agent, levelling agent, low speed disperses, filtering and discharging, and highly-chlorinated polyethylene anti-corrosive paint of epoxy resin paint is made.
Description
Technical field
The present invention relates to paint field, and in particular to a kind of highly-chlorinated polyethylene-ring of the mica powder of coupling modifier containing dry method
The preparation method of oxygen resin anti-corrosive paint paint.
Background technology
Coating protection method is to prevent that metal erosion is most effective, most widely used method, and epoxy resin is to apply at present
Widest anticorrosive paint, but due to epoxy coating itself property it is crisp, easy to aging the shortcomings of, epoxy resin coating is that important have
One of machine coating, but its toughness and resistance to elevated temperatures are bad, it usually needs it is modified.Micaceous iron oxide is the master of rust resisting pigment
One of kind is wanted, is crystallized in flake, heat resistance is high.There is good formation film, excellent with coating made of micaceous iron oxide
Adhesive force and connection performance, anti-atmosphere pollution and radiationless, the splendid durability of ultraviolet light and easily apply that to dress up thick film etc. special
Point.It is main film forming substance to select the excellent highly-chlorinated polyethylene of Corrosion Protection and the strong epoxy resin of caking property.
The content of the invention
The invention mainly solves the technical problem of providing a kind of highly-chlorinated polyethylene of the mica powder of coupling modifier containing dry method-
The preparation method of anti-corrosive paint of epoxy resin paint, it is resistance to good anticorrosive wear-resistant according to paint of coating prepared by this method
Water-based energy.
The technical problems to be solved by the invention are realized using following technical solution：
A kind of preparation method of the highly-chlorinated polyethylene of the mica powder of coupling modifier containing dry method-anti-corrosive paint of epoxy resin paint, its
It is characterized in that, carries out according to the following steps：
（1）Mica powder dry method coupling modifier technique：
Into 0.1-0.12 parts by weight silane coupling agents KH570 1:18-20 adds ethanol water, is 4-6 with vinegar acid for adjusting pH,
Stirring hydrolysis 2-3h at room temperature, is made silane coupler solution；
9-11 parts by weight mica powder is put into 115-120 DEG C of Constant Temp. Oven dry 2-3h, after cooling, it is even that silane is added dropwise
Join agent solution, add 0.08-0.1 parts by weight auxiliary agent ammonium hydroxide, it is 98-102 DEG C to control modification temperature, and mechanical agitation disperses 60-
80min, obtains dry method modification product；
（2）It is grafted polyethylene glycol method modified manometer silicon dioxide：
4-6 parts by weight nano silicon dioxides are dried into 2-3h in 115-120 DEG C of vacuum drying oven, then with the poly- second of 14-16 parts by weight
Glycol, 85-90 parts by weight of toluene mix, sonic oscillation 30-35min, and 108-112 DEG C of back flow reaction 2- is heated under magnetic agitation
3h, centrifuges, is washed 3-5 times with ethanol, 1-2h is dried in 120-125 DEG C of vacuum drying oven, obtains polyethylene glycol Grafted Nano-scale
Particle；
（3）The modification of micaceous iron oxide：
80-90 parts by weight of toluene is added into 4-6 parts by weight mica iron oxide, 20- is ultrasonically treated after stirring 30-35min
25min, obtains component A；Under nitrogen protection, by 2-4 parts by weight of toluene diisocyanate, 0.05-0.1 parts by weight dibutyl tins
Cinnamic acid tin, 40-45 parts by weight of toluene mix, and are then added drop-wise in component A, after high-speed stirred reaction 1-2h, are warming up to 88-92 DEG C
The reaction was continued 5-6h, filtering, toluene wash 3-5 time, obtain the micaceous iron oxide filler that toluene di-isocyanate(TDI) is modified；
（4）The preparation of highly-chlorinated polyethylene/anti-corrosive paint of epoxy resin：
By solvent xylene, toluene in mass ratio 7:3 are uniformly mixed, and stir lower addition 30-40 parts by weight highly-chlorinated polyethylenes,
60-65 DEG C of heating water bath dissolving, is made the highly-chlorinated polyethylene solution that mass concentration is 34-36%；
By in 30-40 parts by weight epoxy resin, 30-35 parts by weight diluent input homogenizer dispersion tank, it is uniformly dispersed, adds
Enter 1-2 parts by weight wetting dispersing agent and 0.5-1 parts by weight defoamers, disperse 20-30min, be slowly added to institute in (1), (2), (3)
Material, stirring infiltration filler powder are obtained, epoxy compositions are made in scattered 1-2h；
Highly-chlorinated polyethylene solution, epoxy compositions are added in dispersion tank, are uniformly dispersed, addition 10-15 parts by weight curing agent,
1-2 parts by weight levelling agents, low speed disperse 1-2h, and filtering and discharging, is made highly-chlorinated polyethylene-asphalt mixtures modified by epoxy resin that solid content is 60-65%
Fat anticorrosive paint paints.
Wherein, step（1）Middle ethanol water concentration is 94-96%.Step（2）Middle molecular weight polyethylene glycol is 1000.Step
Suddenly（3）Middle rate of addition is 10-15 drops/min.Step（4）Epoxy resin is bisphenol A type epoxy resin E-51, and diluent is
Benzyl glycidyl ether 692, rate of dispersion 500-800rpm, curing agent are curing agent NX-2003, and levelling agent is levelling agent
835。
The present invention reaction mechanism and have the beneficial effect that：
Dry method coating modification is carried out to mica powder using silane coupling agent as modifying agent, the alkoxy in KH570 hydrolyzes to form silanol,
Covalent bond can be formed with the hydroxyl reaction of powder surface, coupling agent is adsorbed on the surface of mica powder by chemically reacting, and improves it
Dispersiveness, can improve the corrosion resistance of coating；It is that modifying agent is carried out with nano-silicon dioxide particle surface hydroxyl with polyethylene glycol
Alcohol esterification is reacted, and nano-particle good dispersion in a solvent, is added to the adhesive force that can improve coating in coating after graft modification,
It is good to be grafted the wear-resisting property of polyethylene glycol method modified manometer silicon dioxide composite coating, can also improve the water resistance of coating；With
Micaceous iron oxide is rust resisting pigment, it is modified with toluene di-isocyanate(TDI), improves its dispersiveness in the coating, and flat
Lamella of the row in metal surface increases, and can reduce the water absorption rate of coating；Obtained dry method modification mica powder, polyethylene glycol are connect
The micaceous iron oxide filler that branch modified Nano particle, toluene di-isocyanate(TDI) are modified is added to highly-chlorinated polyethylene/epoxy resin
In anticorrosive paint, a kind of anticorrosive wear-resistant water-resistant type coating can obtain.
Embodiment
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention easy to understand, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment
A kind of preparation side of the highly-chlorinated polyethylene of the mica powder of coupling modifier containing dry method-anti-corrosive paint of epoxy resin paint
Method, it is characterised in that carry out according to the following steps：
（1）Mica powder dry method coupling modifier technique：
Into 0.1kg silane coupling agents KH570 1:20 add ethanol water, are 4-6 with vinegar acid for adjusting pH, stir water at room temperature
2.5h is solved, silane coupler solution is made；
9kg mica powders are put into 115-120 DEG C of Constant Temp. Oven dry 2h, after cooling, silane coupler solution is added dropwise,
0.08kg auxiliary agent ammonium hydroxide is added, it is 98-102 DEG C to control modification temperature, and mechanical agitation disperses 70min, obtains dry method modification production
Product；
（2）It is grafted polyethylene glycol method modified manometer silicon dioxide：
4kg nano silicon dioxides are dried into 2h in 115-120 DEG C of vacuum drying oven, then with 14kg polyethylene glycol, 85-90kg toluene
Mixing, sonic oscillation 35min, 108-112 DEG C of back flow reaction 3h is heated under magnetic agitation, centrifugation, washed 3 times with ethanol,
2h is dried in 120-125 DEG C of vacuum drying oven, obtains polyethylene glycol Grafted Nano-scale particle；
（3）The modification of micaceous iron oxide：
80kg toluene is added into 4kg micaceous iron oxides, 25min is ultrasonically treated after stirring 35min, obtains component A；Protected in nitrogen
Under, 2kg toluene di-isocyanate(TDI)s, 0.05kg dibutyl tin dilaurates, 40kg toluene are mixed, are then added drop-wise in component A,
After high-speed stirred reaction 1h, 88-92 DEG C is warming up to the reaction was continued 5h, filtering, toluene wash 3 times, obtain toluene di-isocyanate(TDI)
Modified micaceous iron oxide filler；
（4）The preparation of highly-chlorinated polyethylene/anti-corrosive paint of epoxy resin：
By solvent xylene, toluene in mass ratio 7:3 are uniformly mixed, and stir lower addition 40kg highly-chlorinated polyethylenes, 60-65 DEG C of water
Bath dissolves by heating, and the highly-chlorinated polyethylene solution that mass concentration is 34% is made；
By in 40kg epoxy resin, 30kg diluents input homogenizer dispersion tank, it is uniformly dispersed, adds 1kg wetting and dispersings
Agent and 0.5kg defoamers, disperse 30min, are slowly added to resulting material in (1), (2), (3), stirring infiltration filler powder, disperses
Epoxy compositions are made in 1h；
Highly-chlorinated polyethylene solution, epoxy compositions are added in dispersion tank, are uniformly dispersed, add 10kg curing agent, 1kg levellings
Agent, low speed disperse 1h, and filtering and discharging, is made highly-chlorinated polyethylene-anti-corrosive paint of epoxy resin paint that solid content is 60%.
Wherein, step（1）Middle ethanol water concentration is 94%.Step（2）Middle molecular weight polyethylene glycol is 1000.Step
（3）Middle rate of addition is 15 drops/min.Step（4）Epoxy resin is bisphenol A type epoxy resin E-51, and diluent contracts for benzyl
Water glycerin ether 692, rate of dispersion 500rpm, curing agent are curing agent NX-2003, and levelling agent is levelling agent 835.
Claims (6)
1. a kind of preparation method of highly-chlorinated polyethylene of the mica powder of coupling modifier containing dry method-anti-corrosive paint of epoxy resin paint,
It is characterized in that：Silane coupler solution, ammonium hydroxide are added dropwise into mica powder, mechanical agitation is disperseed, and obtains dry method modification mica powder；
Mixed after nano silicon dioxide is dried with polyethylene glycol, toluene, heating reflux reaction obtains polyethylene glycol Grafted Nano-scale grain
Son；Into micaceous iron oxide plus toluene, stirring, ultrasonic component A；By toluene di-isocyanate(TDI), dibutyl tin dilaurate, first
Benzene mixes, and is added drop-wise in component A, and stirring reaction, then temperature reaction obtain toluene di-isocyanate(TDI) modified micaceous iron oxide filler；Will
Highly-chlorinated polyethylene solution, epoxy compositions are added in dispersion tank, are uniformly dispersed, and add curing agent, levelling agent, and low speed disperses,
Filtering and discharging, is made highly-chlorinated polyethylene-anti-corrosive paint of epoxy resin paint.
2. a kind of preparation method of highly-chlorinated polyethylene of the mica powder of coupling modifier containing dry method-anti-corrosive paint of epoxy resin paint,
It is characterized in that, carry out according to the following steps：
（1）Mica powder dry method coupling modifier technique：
Into 0.1-0.12 parts by weight silane coupling agents KH570 1:18-20 adds ethanol water, is 4-6 with vinegar acid for adjusting pH,
Stirring hydrolysis 2-3h at room temperature, is made silane coupler solution；
9-11 parts by weight mica powder is put into 115-120 DEG C of Constant Temp. Oven dry 2-3h, after cooling, it is even that silane is added dropwise
Join agent solution, add 0.08-0.1 parts by weight auxiliary agent ammonium hydroxide, it is 98-102 DEG C to control modification temperature, and mechanical agitation disperses 60-
80min, obtains dry method modification product；
（2）It is grafted polyethylene glycol method modified manometer silicon dioxide：
4-6 parts by weight nano silicon dioxides are dried into 2-3h in 115-120 DEG C of vacuum drying oven, then with the poly- second of 14-16 parts by weight
Glycol, 85-90 parts by weight of toluene mix, sonic oscillation 30-35min, and 108-112 DEG C of back flow reaction 2- is heated under magnetic agitation
3h, centrifuges, is washed 3-5 times with ethanol, 1-2h is dried in 120-125 DEG C of vacuum drying oven, obtains polyethylene glycol Grafted Nano-scale
Particle；
（3）The modification of micaceous iron oxide：
80-90 parts by weight of toluene is added into 4-6 parts by weight mica iron oxide, 20- is ultrasonically treated after stirring 30-35min
25min, obtains component A；Under nitrogen protection, by 2-4 parts by weight of toluene diisocyanate, 0.05-0.1 parts by weight dibutyl tins
Cinnamic acid tin, 40-45 parts by weight of toluene mix, and are then added drop-wise in component A, after high-speed stirred reaction 1-2h, are warming up to 88-92 DEG C
The reaction was continued 5-6h, filtering, toluene wash 3-5 time, obtain the micaceous iron oxide filler that toluene di-isocyanate(TDI) is modified；
（4）The preparation of highly-chlorinated polyethylene/anti-corrosive paint of epoxy resin：
By solvent xylene, toluene in mass ratio 7:3 are uniformly mixed, and stir lower addition 30-40 parts by weight highly-chlorinated polyethylenes,
60-65 DEG C of heating water bath dissolving, is made the highly-chlorinated polyethylene solution that mass concentration is 34-36%；
By in 30-40 parts by weight epoxy resin, 30-35 parts by weight diluent input homogenizer dispersion tank, it is uniformly dispersed, adds
Enter 1-2 parts by weight wetting dispersing agent and 0.5-1 parts by weight defoamers, disperse 20-30min, be slowly added to institute in (1), (2), (3)
Material, stirring infiltration filler powder are obtained, epoxy compositions are made in scattered 1-2h；
Highly-chlorinated polyethylene solution, epoxy compositions are added in dispersion tank, are uniformly dispersed, addition 10-15 parts by weight curing agent,
1-2 parts by weight levelling agents, low speed disperse 1-2h, and filtering and discharging, is made highly-chlorinated polyethylene-asphalt mixtures modified by epoxy resin that solid content is 60-65%
Fat anticorrosive paint paints.
A kind of 3. highly-chlorinated polyethylene-epoxy resin anti-corrosion of mica powder of coupling modifier containing dry method according to claim 2
The preparation method of paint of coating, it is characterised in that step（1）Middle ethanol water concentration is 94-96%.
A kind of 4. highly-chlorinated polyethylene-epoxy resin anti-corrosion of mica powder of coupling modifier containing dry method according to claim 2
The preparation method of paint of coating, it is characterised in that step（2）Middle molecular weight polyethylene glycol is 1000.
A kind of 5. highly-chlorinated polyethylene-epoxy resin anti-corrosion of mica powder of coupling modifier containing dry method according to claim 2
The preparation method of paint of coating, it is characterised in that step（3）Middle rate of addition is 10-15 drops/min.
A kind of 6. highly-chlorinated polyethylene-epoxy resin anti-corrosion of mica powder of coupling modifier containing dry method according to claim 2
The preparation method of paint of coating, it is characterised in that step（4）Epoxy resin is bisphenol A type epoxy resin E-51, and diluent is
Benzyl glycidyl ether 692, rate of dispersion 500-800rpm, curing agent are curing agent NX-2003, and levelling agent is levelling agent
835。
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| CN108929622A (en) * | 2018-06-15 | 2018-12-04 | 汪国亮 | A kind of preparation method of the acrylic acid insulated heat powdery paints for anti-corrosion of metal |
| WO2020118746A1 (en) * | 2018-12-13 | 2020-06-18 | 安徽安利材料科技股份有限公司 | Soft solvent-free flame-retardant polyurethane synthetic leather and preparation method therefor |
| CN117602908A (en) * | 2024-01-19 | 2024-02-27 | 佛山市南海联兴得利装饰材料有限公司 | Sound-insulation heat-preservation fireproof plate and preparation method and application thereof |
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| CN102796439A (en) * | 2012-07-11 | 2012-11-28 | 常州大学 | Solvent-free nanometer modified epoxy weather-resistant type anticorrosive paint and preparation method thereof |
| CN103275596A (en) * | 2013-03-29 | 2013-09-04 | 厦门双瑞船舶涂料有限公司 | Light-color modified epoxy static conductive anticorrosion coating and preparation method thereof |
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| CN102796439A (en) * | 2012-07-11 | 2012-11-28 | 常州大学 | Solvent-free nanometer modified epoxy weather-resistant type anticorrosive paint and preparation method thereof |
| CN103275596A (en) * | 2013-03-29 | 2013-09-04 | 厦门双瑞船舶涂料有限公司 | Light-color modified epoxy static conductive anticorrosion coating and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108929622A (en) * | 2018-06-15 | 2018-12-04 | 汪国亮 | A kind of preparation method of the acrylic acid insulated heat powdery paints for anti-corrosion of metal |
| WO2020118746A1 (en) * | 2018-12-13 | 2020-06-18 | 安徽安利材料科技股份有限公司 | Soft solvent-free flame-retardant polyurethane synthetic leather and preparation method therefor |
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| CN117602908A (en) * | 2024-01-19 | 2024-02-27 | 佛山市南海联兴得利装饰材料有限公司 | Sound-insulation heat-preservation fireproof plate and preparation method and application thereof |
| CN117602908B (en) * | 2024-01-19 | 2024-04-30 | 佛山市南海联兴得利装饰材料有限公司 | Sound-insulation heat-preservation fireproof plate and preparation method and application thereof |
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