CN107200815A - A kind of SiO2The preparation technology of microcapsules modified aqueous acrylic acid anti-corrosion emulsion - Google Patents
A kind of SiO2The preparation technology of microcapsules modified aqueous acrylic acid anti-corrosion emulsion Download PDFInfo
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- CN107200815A CN107200815A CN201710311625.3A CN201710311625A CN107200815A CN 107200815 A CN107200815 A CN 107200815A CN 201710311625 A CN201710311625 A CN 201710311625A CN 107200815 A CN107200815 A CN 107200815A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
Abstract
The invention discloses a kind of SiO2The preparation technology of microcapsules modified aqueous acrylic acid anti-corrosion emulsion, technical scheme in turn includes the following steps:(1) polyethyleneimine and 95% ethanol are configured to certain density dispersion liquid;(2) in the above-mentioned alcohol dispersion liquid of polyethyleneimine 95% of mixed solution and dripping of tetraethyl orthosilicate (TEOS) and ethanol, the Nano-meter SiO_2 of parcel polyethyleneimine is made after ageing2Microcapsules;(3) by the monomers such as styrene, methyl methacrylate, butyl acrylate and the SiO of parcel polyethyleneimine2SiO is made in microcapsules copolymerization2Microcapsules modified aqueous acrylic acid anti-corrosion emulsion.This method can introduce cationic compound in anionic emulsion system;Microcapsule structure ruptures during film forming, is reacted by hydrophilic functional groups such as the imine groups and carboxyl of high reaction activity, increases substantially the water resistance of coating, adhesive force and salt spray resistance.
Description
Technical field
The present invention relates to water-based anticorrosive paint preparation field, and in particular to a kind of SiO2Microcapsules modified aqueous acrylic acid is prevented
The preparation technology of fermented bean curd liquid.
Background technology
The metal materials such as steel are exposed in outdoor environment, by the collective effect of oxygen, rainwater and atmosphere pollution,
Easy surface corrosion causes the heavy losses of property.Anticorrosive paint in metal surface by high-molecular organic material by forming physical isolation
Layer, hinders eroded elements infiltration to realize anti-corrosion purpose.In order to have after improving the antiseptic effect of coating, high polymer material film forming
There are good compactness, adhesive force and structural stability.At present, commercial anticorrosive coating is produced more than performance to improve using solvent-borne type
There is serious environmental pollution in product, work progress.
As national environmental protection regulation is further strict to the limitation of VOC content in coating, Water-borne modification is anticorrosive paint field
Development trend.Compared to solvent based coating, water paint is present in many birth defects, water paint preparation process, in order to carry
Dispersion stabilization of the high high-molecular organic material in water, it is necessary to introduce the hydroaropic substances such as a large amount of carboxyls, sulfonic group or hydroxyl,
There is the shortcomings of compactness is poor, water absorption rate is high, base material adhesive force is not enough after coating film forming.
In order to make up the drawbacks described above of water paint, generally improved by introducing functional monomer or two-component consolidated structures
The compactness and water resistance of system.For example:Coatings industry, 2016,46 (7), 40-45 discloses one kind with acrylate-epoxy
Hybridisation emulsion is film forming matter, and Dow Corning Z-6040 are adhesion promoter, and BACKOPOX VEH 2849W are curing agent,
40-50 μm of coating layer thickness, is resistant to neutral salt spray 300h.Chinese Patent Application No. CN201310293474.5 discloses one kind with water
Property fluorinated acrylate be film forming matter, non-ionic water polyurethane be curing agent water-based anticorrosive finish paint.With Jotun Barrier
80 be 95 ± 3 μm of anti-corrosion primer thickness, 45 ± 5 μm of finish paint thickness, salt-fog resistant time is more than 3500h.Shanghai coating, 2015,53
(3), 9-12, is disclosed with hydroxyethyl methacrylate, methyl methacrylate, butyl acrylate, phosphate ester monomer PAM-100
Phosphoric acid modification Acrylic hydroxyl emulsion is synthesized, then using the water-based isocyanates of Bayhydur 305 as curing agent, dual-component coating is resistance to
Salt fog time 192h.
The above method, by grafted-organosilicon, fluorochemical monomer, phosphate ester monomer functional group on macromolecular chain, make its
Hydrophilic radical is shielded on space structure;And the form solidified by two-component further forms IPN between macromolecular chain
Network, so as to considerably reduce influence of the hydrophilic functional groups to coating performance.But the above method does not change fundamentally
The hydrophilic birth defect of macromolecular chain, its antiseptic property still has larger gap with solvent based coating.
Polyethyleneimine is the part branch chain polymerization that one kind that polymerization of ethyleneimine is produced includes primary amine, secondary amine and tertiary amine
Thing.Polyethyleneimine is due to that with reactivity very strong primary amine and secondary amine, can be easy to and epoxy, carboxylic acid, isocyanation esterification
Compound reacts, and the attachment in base materials such as metal, film, plastics, glass can be increased substantially by adding it in high polymer material
Power.Chemical barrier layer can be formed simultaneously, carbon dioxide, nitrogen oxides, oxysulfide, ozone, aldehyde, ketone and other chemicals are prevented
Matter is penetrated into.Polyethyleneimine can be applied to the ink of dicyandiamide solution, coating, the field such as binding agent.Because polyethyleneimine is water-soluble
High-cation characteristic is presented in liquid, is easily mutually adsorbed with the anionic emulsifier in water paint and causes system to be demulsified, there is no
Method is applied to aqueous coating system.
The content of the invention
The invention aims to overcome the deficiencies in the prior art, there is provided a kind of SiO2Microcapsules modified aqueous acrylic acid is prevented
The preparation technology of fermented bean curd liquid, increases substantially the water resistance and salt spray resistance of waterborne anti-corrosive coatings.
The technical solution adopted by the present invention is in turn include the following steps:
(1) it is 95 that the polyethyleneimine for being 4000-60000 by number-average molecular weight, which is scattered in ethanol and water quality ratio,:5
In solution (hereinafter referred to as 95% ethanol), 95% ethanol of regulation is (3-8) with polyethyleneimine mass ratio:1, poly- second is made
The alcohol dispersion liquid of alkene imines -95%;
(2) mass ratio of tetraethyl orthosilicate (TEOS) and absolute ethyl alcohol, TEOS and absolute ethyl alcohol is added in the reactor
For (0.1-0.5):At 1,20~40 DEG C, the alcohol dispersion liquid of polyethyleneimine -95% obtained by step (1) is slowly added dropwise, is aged
10 hours, centrifugation, dry it must wrap up the SiO of polyethyleneimine2Microcapsules (hereinafter referred to as SiO2Microcapsules);
(3) by the SiO obtained by step (2)2Microcapsules, SiO is made by following process2Microcapsules modified aqueous acrylic acid
Anti-corrosion emulsion:
A. under stirring condition, emulsifying agent is dissolved in deionized water, nuclear layer monomer mixture is then added, continues to stir
Mix, stratum nucleare pre-emulsion be made,
B. under stirring condition, emulsifying agent is dissolved in deionized water, shell monomers mixture and step (2) is then added
The SiO of gained2Microcapsules, continue to stir, shell pre-emulsion are made,
C. under stirring condition, emulsifying agent and sodium acid carbonate are dissolved in deionized water, then the synchronous, difference at 80 DEG C
Stratum nucleare pre-emulsion and initiator solution is added dropwise, completion of dropping is incubated 0.5 hour, continue it is synchronous, be added dropwise respectively shell pre-emulsion and
Initiator solution, completion of dropping is warming up to 90 DEG C and is incubated 2 hours, reaction is cooled to 40 DEG C, the pH of ammoniacal liquor regulation system after terminating
Value is to 8, and filtering produces SiO2Microcapsules modified aqueous acrylic acid anti-corrosion emulsion.
Described emulsifying agent is the composite emulsifier being made up of anion emulsifier and nonionic emulsifier, the anion
The mass ratio of emulsifying agent and nonionic emulsifier is (1-2):1;Described anion emulsifier is lauryl sodium sulfate, ten
One kind in dialkyl diphenyl ether sodium disulfonate, allyloxy nonyl phenol propyl alcohol polyoxyethylene ether ammonium sulfate;Described nonionic
Emulsifying agent is one kind in AEO, NPE.
Described initiator solution is that ammonium persulfate and deionized water are 1 according to mass ratio:9 10wt% being configured to
Ammonium persulfate aqueous solution.
Described nuclear layer monomer is styrene, methyl methacrylate, butyl acrylate, methacrylic acid, divinyl
Two or more in benzene, Triallyl isocyanurate, trimethylol-propane trimethacrylate.
Described shell monomers are styrene, methyl methacrylate, dodecafluorhe-ptylacrylate, Solvay
Two kinds in SIPOMER PAM-200, butyl acrylate, methacrylic acid, acrylamide, hydroxyethyl methacrylate or two kinds
More than.
The beneficial effect of invention
1st, by SiO2Microcapsule structure introduces cationic polyethylene imines in anionic emulsion system, it is ensured that breast
The stability of liquid.
2nd, by emulsion polymerization, the SiO of parcel polyethyleneimine is introduced in styrene-acrylic system2Microcapsules.Emulsion is dried
Microcapsule structure ruptures during film forming, and polyethyleneimine in the paramount intramolecule space of release, reacts inside microcapsules by height
The functional group reactionses such as the imine group and carboxyl of activity, on the one hand can make the increase of system consistency, on the other hand reduce free
Hydrophilic carboxylic acid's group, the water resistance of coating, adhesive force and salt spray resistance can be increased substantially.
Brief description of the drawings
Accompanying drawing 1 is the SiO of parcel polyethyleneimine2Microcapsules TEM electron microscopes, accompanying drawing 2 is the horse after 720h neutral salt spray
Mouth iron test plate (panel) corrosion condition figure.
Embodiment
Technical scheme is further described with reference to embodiments.
Embodiment 1
1kg number-average molecular weights are scattered in the ethanol of 3kg 95% for 4000 polyethyleneimine, obtained polyethyleneimine-
95% alcohol dispersion liquid.Add at 0.5kg tetraethyl orthosilicates (TEOS) and 5kg absolute ethyl alcohols, 20 DEG C, delay in another reactor
It is slow that the above-mentioned alcohol dispersion liquids of polyethyleneimine -95% of 0.2kg are added dropwise, it is aged 10 hours, centrifugation, dry must wraps up polyethyleneimine
SiO2Microcapsules (hereinafter referred to as SiO2Microcapsules).
By 2.5g lauryl sodium sulfate, 2.5g NPEs, 0.3kg deionized waters, rotating speed 1000rpm is stirred
Mix to being completely dissolved, add 0.25kg styrene, 0.3kg butyl acrylates, 0.05kg Triallyl isocyanurates, continue to stir
Mix 0.5 hour, stratum nucleare pre-emulsion is made.
5g lauryl sodium sulfate, 5g AEOs (AEO-9), 1.2kg deionizations are added in the reactor
Water, rotating speed 1000rpm is stirred to being completely dissolved, add 1.5kg styrene, 1.3kg butyl acrylates, 0.1kg methacrylic acids,
0.1kg dodecafluorhe-ptylacrylates, 0.05kg SiO2Microcapsules, 0.05kgPAM-200 continues to stir 0.5 hour, shell is made
Layer pre-emulsion.
Add in the reactor 17.5g lauryl sodium sulfate, 17.5g NPEs, 20g sodium acid carbonates,
1.9kg deionized water rotating speeds 200rpm is stirred to being completely dissolved.Be warming up to 80 DEG C, it is synchronous, be added dropwise respectively stratum nucleare pre-emulsion and
0.18kg initiator solutions, drop Bi Baowen 0.5 hour.Continuation is synchronous, shell pre-emulsion and 0.24kg initiators are added dropwise respectively
The aqueous solution, treats that shell pre-emulsion drop finishes, is warming up to 90 DEG C and is incubated 2 hours, is cooled to 40 DEG C, ammoniacal liquor adjusts pH to 8, filters out
Material, obtains SiO2Microcapsules modified aqueous acrylic acid anti-corrosion emulsion.
By obtained anti-corrosion emulsion even application in the tinplate test plate (panel) after surface treatment, drying at room temperature 24 hours or 80 DEG C
Baking 10 minutes, thickness of dry film controls 30-50 μm, and test plate (panel) carries out performance test after being labeled as 1#, edge sealing.
Embodiment 2
1kg number-average molecular weights are scattered in the ethanol of 5kg 95% for 20000 polyethyleneimine, polyethyleneimine is made
The alcohol dispersion liquid of amine -95%.0.5kg tetraethyl orthosilicates (TEOS) and 1.5kg absolute ethyl alcohols in another reactor, at 30 DEG C,
It is slowly added dropwise the above-mentioned alcohol dispersion liquids of polyethyleneimine -95% of 0.2kg, is aged 10 hours, centrifugation, dry must wraps up polyethyleneimine
The SiO of amine2Microcapsules (hereinafter referred to as SiO2Microcapsules).
By 14g disodium 4-dodecyl-2,4 '-oxydibenzenesulfonates, 7g AEOs (AEO-9), 0.6kg deionized waters,
Rotating speed 1000rpm is stirred to being completely dissolved, and adds 0.3kg methyl methacrylates, 0.7kg butyl acrylates, 0.06kg diethyls
Alkenyl benzene, 0.16kg trimethylol-propane trimethacrylates, continue to stir 0.5 hour, stratum nucleare pre-emulsion are made.
24g disodium 4-dodecyl-2,4 '-oxydibenzenesulfonates, 12g AEOs (AEO-9), 1.6kg deionized waters, turn
Fast 1000rpm is stirred to being completely dissolved, add 1.0kg styrene, 1.4kg butyl acrylates, 0.1kg methacrylic acids,
0.03kg dodecafluorhe-ptylacrylates, 0.06kg SiO2Microcapsules, 0.1kg hydroxyethyl methacrylates continue stirring 0.5 small
When, shell pre-emulsion is made.
30g lauryl sodium sulfate, 15g NPEs, 45g sodium acid carbonates, 2.5kg are added in the reactor
Deionized water rotating speed 200rpm is stirred to being completely dissolved.80 DEG C are warming up to, stratum nucleare pre-emulsion is added dropwise synchronously, respectively and 0.18kg draws
Send out the agent aqueous solution, drop Bi Baowen 0.5 hour.Continuation is synchronous, shell pre-emulsion and 0.24kg initiator solutions are added dropwise respectively, treats
Shell pre-emulsion drop finishes, and is warming up to 90 DEG C of insulation 2h, is cooled to 40 DEG C, ammoniacal liquor regulation pH to 8, filtering and discharging obtains SiO2Micro- glue
Capsule modified aqueous acrylic acid anti-corrosion emulsion.
By obtained anti-corrosion emulsion even application in the tinplate test plate (panel) after surface treatment, drying at room temperature 24 hours or 80 DEG C
Baking 10 minutes, thickness of dry film controls 30-50 μm, and test plate (panel) carries out performance test after being labeled as 2#, edge sealing.
Embodiment 3
1kg number-average molecular weights are scattered in the ethanol of 8kg 95% for 60000 polyethyleneimine, polyethyleneimine is made
The alcohol dispersion liquid of amine -95%.0.5kg tetraethyl orthosilicates (TEOS) and 1kg absolute ethyl alcohols in another reactor, at 40 DEG C, delay
It is slow that the above-mentioned alcohol dispersion liquids of polyethyleneimine -95% of 0.2kg are added dropwise, it is aged 10 hours, centrifugation, dry must wraps up polyethyleneimine
SiO2Microcapsules (hereinafter referred to as SiO2Microcapsules).
4.5g allyloxy nonyl phenol propyl alcohol polyoxyethylene ether ammonium sulfate, 2.8g NPEs, 0.4kg go from
Sub- water, rotating speed 1000rpm is stirred to being completely dissolved, and adds 0.6kg styrene, 0.3kg butyl acrylates, 0.1kg metering systems
Acid, continues to stir 0.5 hour, stratum nucleare pre-emulsion is made.
20g allyloxy nonyl phenol propyl alcohol polyoxyethylene ether ammonium sulfate, 12.5g NPEs, 1.6kg go from
Sub- water, rotating speed 1000rpm is stirred to being completely dissolved, and adds 1.5kg methyl methacrylates, 1.7kg butyl acrylates, 0.1kg
Methacrylic acid, 0.2kg acrylamides, 0.02kg dodecafluorhe-ptylacrylates, 0.02kgSiO2Microcapsules, 0.1kg PAM-
200, continue to stir 0.5 hour, shell pre-emulsion is made.
25g allyloxy nonyl phenol propyl alcohol polyoxyethylene ether ammonium sulfate, 15.7g NPEs, 25g bicarbonates
Sodium, 1.9kg deionized water rotating speeds 200rpm are stirred to being completely dissolved.Be warming up to 80 DEG C, it is synchronous, be added dropwise respectively stratum nucleare pre-emulsion and
0.18kg initiator solutions, drop Bi Baowen 0.5 hour.Continuation is synchronous, shell pre-emulsion and 0.24kg initiators are added dropwise respectively
The aqueous solution, treats that shell pre-emulsion drop finishes, and is warming up to 90 DEG C of insulation 2h, is cooled to 40 DEG C, ammoniacal liquor regulation pH to 8, filtering and discharging is obtained
SiO2Microcapsules modified aqueous acrylic acid anti-corrosion emulsion.
By obtained anti-corrosion emulsion even application in the tinplate test plate (panel) after surface treatment, drying at room temperature 24 hours or 80 DEG C
Baking 10 minutes, thickness of dry film controls 30-50 μm, and test plate (panel) carries out performance test after being labeled as 3#, edge sealing.
Sample tests of the embodiment of the present invention are shown in Table 1.
The sample tests of table 1
Claims (5)
1. a kind of SiO2The preparation technology of microcapsules modified aqueous acrylic acid anti-corrosion emulsion, it is characterized in that in turn including the following steps:
(1) it is 95 that the polyethyleneimine for being 4000-60000 by number-average molecular weight, which is scattered in ethanol and water quality ratio,:5 solution
In (hereinafter referred to as 95% ethanol), 95% ethanol of regulation is (3-8) with polyethyleneimine mass ratio:1, polyethyleneimine is made
The alcohol dispersion liquid of amine -95%;
(2) tetraethyl orthosilicate (TEOS) and absolute ethyl alcohol is added in the reactor, the mass ratio of TEOS and absolute ethyl alcohol is
(0.1-0.5):At 1,20~40 DEG C, the alcohol dispersion liquid of polyethyleneimine -95% obtained by step (1), ageing 10 is slowly added dropwise
Hour, centrifugation, dry it must wrap up the SiO of polyethyleneimine2Microcapsules (hereinafter referred to as SiO2Microcapsules);
(3) by the SiO obtained by step (2)2Microcapsules, SiO is made by following process2Microcapsules modified aqueous acrylic acid anti-corrosion
Emulsion:
A. under stirring condition, emulsifying agent is dissolved in deionized water, nuclear layer monomer mixture is then added, continues to stir 0.5
Hour, stratum nucleare pre-emulsion is made,
B. under stirring condition, emulsifying agent is dissolved in deionized water, then added obtained by shell monomers mixture and step (2)
SiO2Microcapsules, continue to stir 0.5 hour, shell pre-emulsion are made,
C. under stirring condition, emulsifying agent and sodium acid carbonate are dissolved in deionized water, then synchronously, are respectively added dropwise at 80 DEG C
Stratum nucleare pre-emulsion and initiator solution, completion of dropping are incubated 0.5 hour, continue that shell pre-emulsion is added dropwise synchronously, respectively and draw
The agent aqueous solution is sent out, completion of dropping is warming up to 90 DEG C and is incubated 2 hours, reaction is cooled to 40 DEG C, the pH of ammoniacal liquor regulation system after terminating
Value is to 8, and filtering produces SiO2Microcapsules modified aqueous acrylic acid anti-corrosion emulsion.
2. technique according to claim 1, it is characterised in that described emulsifying agent is by anion emulsifier and nonionic
The composite emulsifier of emulsifying agent composition, the mass ratio of the anion emulsifier and nonionic emulsifier is (1-2):1;It is described
Anion emulsifier be lauryl sodium sulfate, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, allyloxy nonyl phenol propyl alcohol polyoxy
One kind in ethene ether ammonium sulfate;Described nonionic emulsifier is AEO (AEO-9), polyoxyethylene nonyl phenyl second
One kind in alkene ether.
3. technique according to claim 1, it is characterised in that described initiator solution is ammonium persulfate and deionization
Water is 1 according to mass ratio:The 9 10wt% ammonium persulfate aqueous solutions being configured to.
4. technique according to claim 1, it is characterised in that described nuclear layer monomer is styrene, methyl methacrylate
Ester, butyl acrylate, methacrylic acid, divinylbenzene, Triallyl isocyanurate, trimethylol propane trimethyl propylene
Two or more in acid esters.
5. technique according to claim 1, it is characterised in that described shell monomers are styrene, methyl methacrylate
Ester, dodecafluorhe-ptylacrylate, Solvay SIPOMER PAM-200, butyl acrylate, methacrylic acid, acrylamide,
Two or more in hydroxyethyl methacrylate.
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Cited By (3)
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CN108855831A (en) * | 2018-07-10 | 2018-11-23 | 陕西科技大学 | A kind of construction method of anticorrosion type metal coating |
CN109161051A (en) * | 2018-08-07 | 2019-01-08 | 深圳先进技术研究院 | Modified hexagonal boron nitride and its preparation method and application |
CN114307028A (en) * | 2021-12-31 | 2022-04-12 | 广东粤港澳大湾区黄埔材料研究院 | Fire-extinguishing microcapsule core material, fire-extinguishing microcapsule and preparation method thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0847426B1 (en) * | 1996-06-24 | 2003-07-30 | Borealis Technology Oy | Antifouling coating |
CN102030990A (en) * | 2009-09-28 | 2011-04-27 | 复旦大学 | Silicone oil microcapsule with slow-release characteristics and preparation method thereof |
CN104710555A (en) * | 2015-04-01 | 2015-06-17 | 海安索菲亚生态环境新材料科技有限公司 | Method for preparing water-based hybrid anti-corrosive emulsion with self-repairing function |
-
2017
- 2017-05-05 CN CN201710311625.3A patent/CN107200815B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0847426B1 (en) * | 1996-06-24 | 2003-07-30 | Borealis Technology Oy | Antifouling coating |
CN102030990A (en) * | 2009-09-28 | 2011-04-27 | 复旦大学 | Silicone oil microcapsule with slow-release characteristics and preparation method thereof |
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