CN105669890B - Anticorrosive metal paint polyvinylidene emulsions and preparation method and application - Google Patents
Anticorrosive metal paint polyvinylidene emulsions and preparation method and application Download PDFInfo
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- CN105669890B CN105669890B CN201610071159.1A CN201610071159A CN105669890B CN 105669890 B CN105669890 B CN 105669890B CN 201610071159 A CN201610071159 A CN 201610071159A CN 105669890 B CN105669890 B CN 105669890B
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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
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/02—Monomers containing chlorine
- C08F214/04—Monomers containing two carbon atoms
- C08F214/08—Vinylidene chloride
-
- 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
-
- 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
-
- 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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/04—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C09D127/08—Homopolymers or copolymers of vinylidene chloride
-
- 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 polyvinylidene emulsions for being used to prepare waterborne metal anti-corrosive paint and preparation method thereof, polyvinylidene chloride, acrylic ester monomer, hydroxyethyl meth acrylate phosphate, N NMAs, emulsifying agent and deionized water etc. are subjected to pre-emulsification, under initiator effect, using seeded emulsion polymerization method, polymerization obtains a kind of polyvinylidene emulsions of good emulsion stability.By introducing polar monomer, the adhesive force of emulsion and base material is added, the water-based anticorrosive paint of preparation is environment-protecting and non-poisonous without volatile organic solvent using water as main dispersing medium, is firmly bonded with metal base.
Description
Technical field
The present invention relates to a kind of preparation of polyvinylidene emulsions, applied specifically, being related to a kind of anti-corrosion of metal that is applied to
The preparation of the polyvinylidene emulsions of material.
Background technology
Polyvinylidene chloride（PVDC）Polymer is used as a small number of materials that there is height to hinder oxygen and height moisture barrier property simultaneously
One of, using quite varied in terms of packaging for foodstuff, pharmaceuticals packaging, precision instrument and electronic product packaging.Because poly-
The incomparable high barrier that vinylidene chloride film has, it can prevent steam from passing through in the separation layer that metal surface is formed
Film layer, so as to prevent steam from causing corrosion to metal.The metal works anti-corrosion used for applying in wet environment, use with
Polyvinylidene chloride is also a kind of effective means for the coating of material of main part.
Patent CN 101033276A disclose a kind of auto-deposition based on vinylidene chloride-acrylate copolymer latex and applied
Material and preparation method thereof, with vinylidene chloride and acrylic monomers, synthesis vinylidene chloride-acrylate copolymer latex, is added
Dispersible pigment color paste, hydrogen peroxide, iron powder, hydrofluoric acid and deionized water are configured to autodeposition coatings, available for the application of metal base, system
Standby autodeposition coatings are good to metal attachment fastness, antiseptic property is good, salt fog resistance up to 350h, impact resistance is good, and hardness can
Up to 4H.But the patent system is various for the acrylic ester monomer required for vinylidene chloride-acrylic ester copolymer latex, and with
The cementitiousness of base material not enough, compared with long time base material easily get rusty by use time.
Patent CN 101003706A disclose a kind of aqueous PVDC latex anti-corrosive primer, with PVDC copolymer emulsions, isopropyl
The aqueous PVDC anti-corrosive primers that alcohol, phosphoric acid and tannic acid etc. are prepared, which have, to block water, hinders oxygen, oil resistivity, self-extinguishment, chemically-resistant medicine
Moral character, it is mould proof to wait excellent properties.But use aqueous PVDC latexes anti-corrosive primer, the bonding with metal base made from the technology
Power is also inadequate.
The content of the invention
It is contemplated that overcoming the defect of above-mentioned prior art, there is provided a kind of stability is preferable, adhesive force is excellent, antirust effect
The really good polyvinylidene emulsions for being applied to prepare metal anti-corrosive paint.
It is a further object of the present invention to provide the preparation method of the polyvinylidene emulsions.
It is a further object of the present invention to provide the polyvinylidene emulsions in waterborne metal anti-corrosive paint is prepared
Using.
The present invention is achieved through the following technical solutions foregoing invention purpose.
A kind of polyvinylidene emulsions, are prepared by pre-emulsion, kettle material and initiator solution, by weight, described pre-
Emulsion includes：
75~86 parts of vinylidene chloride；
6~15 parts of A classes reaction monomers, wherein A classes reaction monomers are butyl acrylate, methyl methacrylate, acrylic acid
One or more in ethyl ester, methyl methacrylate；
1~2 part of B classes reaction monomers, wherein B classes reaction monomers refer to one kind in acrylic acid, methacrylic acid, itaconic acid or
It is a variety of；
2~4 parts of hydroxyethyl meth acrylate phosphate；
3~5 parts of N hydroxymethyl acrylamide；
1.0~2.0 parts of anionic emulsifier；
1.0~2.0 parts of response type nonionic emulsifier；
0.1~2 part of molecular weight regulator；
0.2~1 part of polyvinylpyrrolidone；
40~50 parts of deionized water；
The kettle material includes：
0.4~0.5 part of emulsifying agent；
40~50 parts of deionized water；
NaHCO3 And/or Na2CO3 0.3~0.9 part；
0.01~0.1 part of EDTA；
The initiator solution includes：
0.3~0.4 part of oxidizing initiators；
Reduce 0.15~0.2 part of initiator；
10~20 parts of deionized water.
The present invention by emulsion simultaneously introduce N hydroxymethyl acrylamide, hydroxyethyl meth acrylate phosphate this
Two kinds of monomers containing polar group, utilize-NCH2The collective effect of both polar groups of OH ,-OH, significantly improves breast
The cohesive force of liquid and matrix；Bound phosphate groups are introduced in the molecular structure of emulsion, bound phosphate groups can be with film forming procedure
Ground metal forms the phosphate coating of densification, is passivated metal surface, and itself will not corrode base material, and emulsion has
Good antirust function；Using the combination of anionic emulsifier and response type nonionic emulsifier, the chemistry of emulsion is improved
Stability.
Preferably, the anionic emulsifier is lauryl sodium sulfate（SDS）.
Preferably, the response type nonionic emulsifier is allyloxy NPE（ANPEO-10）.
Preferably, the oxidizing initiators are sodium peroxydisulfate.
Preferably, the reduction initiator is sodium hydrogensulfite.
Preferably, the molecular weight regulator is 3- isooctyl mercaptopropionates（IOPM）.
The preparation method of the polyvinylidene emulsions, comprises the following steps：
S1. pre- emulsified material is mixed respectively by formula, with high-speed stirred 30~60min of pre-emulsification, prepares pre-emulsion standby；
S2. by formula by kettle material it is well mixed after, mixing speed is 200~300rpm, is warming up to 55 DEG C~65 DEG C, plus
Enter in the 10~15% of pre-emulsion and the 20~40% of initiator solution to reactor, react 30~60min, form seed breast
Liquid.
S3. remaining 85~90% pre-emulsions, 50~70% initiator solutions are added into seed emulsion, in 4~6 hours
Add.Continue to be incubated after 0.5~1.5h, add remaining initiator solution, be cooled to less than 40 DEG C, discharging.
Preferably, the S2. and S3. are carried out under inert gas atmosphere.
Preferably, the S2 is after by formula, kettle material is well mixed, to pour into reactor, reactor is sealed, to reaction
Kettle fills N2And vacuumize, in triplicate, finally fill N2It is normal pressure to make the pressure in kettle.Reactor opens stirring, and mixing speed is
200~300rpm, is warming up to 55 DEG C, adds the 30% of 10~15% and initiator solution of pre-emulsion, reacts 30~60min,
Form seed emulsion.
Preferably, the S3 is that remaining 85~90% pre-emulsions, 60% initiator solution are added into seed emulsion, small 5
When interior add.Continue to be incubated after 1h, then be continuously added to remaining 10% initiator solution, vacuumize, cool, be cooled to less than 40 DEG C,
Filtering, discharging.
The invention discloses application of the polyvinylidene emulsions in waterborne metal anti-corrosive paint is prepared.It will prepare
Vinylidene chloride emulsion and a certain amount of mill base, ammoniacal liquor, Alkali-soluble acrylic's emulsion, propane diols, thickener, defoamer etc. it is mixed
Allotment is closed, metal anti-corrosive paint can be prepared.
Specifically, the metal anti-corrosive paint preparation process is as follows：With 100 parts of vinylidene chloride emulsion, mill base 20~30
Part, 1~2 part of ammoniacal liquor, 1 part of Alkali-soluble acrylic's emulsion, 5~10 parts of propane diols, 0.2 part of thickener, 0.4 part of defoamer, go from
Sub- appropriate amount of water, the metal anti-corrosive paint that configuration solid content is 40%, film forming, spray gun bore are carried out using spraying process：1.7~2.0
Mm, air pressure：3~4 bar, prepare 30~40 microns of wet films.
Compared with prior art, innovative point of the invention is：The present invention in emulsion by introducing N- methylols simultaneously
Both contain the monomer of polar group for acrylamide, hydroxyethyl meth acrylate phosphate, utilize-NCH2OH ,-OH this two
The collective effect of polar group is planted, emulsion and the cohesive force of matrix is significantly improved；Phosphorus is introduced in the molecular structure of emulsion
Acid esters group, bound phosphate groups can form the phosphate coating of densification with ground metal in film forming procedure, make metal surface
It is passivated, while phosphate is compared to inorganic acids such as phosphoric acid, it is acid weaker, it itself will not corrode base material, emulsion has good
Antirust function；Using the combination of anionic emulsifier and response type nonionic emulsifier, the chemically stable of emulsion is improved
Property；Select each monomeric species and consumption, find best joint, be maximally maintained the excellent waterproof of vinylidene chloride material every
Gas performance, while compensate for the problem of stability of emulsion is bad when VOC content is high in metachloroethylene copolymer.
Embodiment
Embodiment 1
The emulsion synthesizing formula of table 1
S1. pre-emulsification：
It is formulated by table 1 by SDS, ANPEO-10, vinylidene chloride, butyl acrylate, hydroxyethyl meth acrylate phosphoric acid
Ester, N hydroxymethyl acrylamide, acrylic acid, IOPM, PVK homogenizer pre-emulsification 30min, prepare pre-emulsion standby；
S2. seeded emulsion polymerization
By table 1 be formulated by SDS, NaHCO3, EDTA, deionized water magnetic stirrer it is uniform after, pour into reactor
In, sealing reactor rushes nitrogen to reactor and vacuumized, continuous three times, air in exclusion system.Finally filling N2 makes in kettle
Pressure is normal pressure.Reactor opens stirring, and mixing speed is 200 ~ 300rpm, is warming up to 55 DEG C, disposable addition pre-emulsion
15% and initiator solution 30% in reactor, react 60min, form seed emulsion.
S3. emulsion polymerization
Remaining 85% pre-emulsion and 60% initiator solution are at the uniform velocity added, control was added in 5 hours.Continue to be incubated after 1h,
Remaining 10% initiator solution is continuously added in reactor, treats that pressure stability is constant（About 1h）, defoamer is added, gas phase is opened and goes out
Mouth valve, vacuumizes, then opens cooling water temperature, is cooled to less than 40 DEG C, filtering, discharging.
Embodiment 2
Repeat embodiment 1, from embodiment 1 formula unlike, the consumption of mix monomer is：Vinylidene chloride 85g, propylene
Acid butyl ester 8g, hydroxyethyl meth acrylate phosphate 2g, N hydroxymethyl acrylamide 3g, acrylic acid 2g compositions.
Embodiment 3
Repeat embodiment 1, from embodiment 1 formula unlike, the consumption of mix monomer is：Vinylidene chloride 75g, propylene
Acid butyl ester 14g, hydroxyethyl meth acrylate phosphate 4g, N hydroxymethyl acrylamide 5g, acrylic acid 2g compositions.
Embodiment 4
Repeat embodiment 1, from embodiment 1 formula unlike, emulsifier is in pre-emulsion：SDS 1.0g,
ANPEO-10 2.0g。
Comparative example 1
Embodiment 1 is repeated, as different from Example 1, hydroxyethyl meth acrylate phosphate is free of in pre-emulsion.
Comparative example 2
Embodiment 1 is repeated, as different from Example 1, N hydroxymethyl acrylamide is free of in pre-emulsion.
Comparative example 3
Embodiment 1 is repeated, as different from Example 1, the hydroxyethyl meth acrylate phosphate in pre-emulsion is replaced
Change the phosphoric acid of equivalent into.
The polyvinylidene emulsions that by more than prepared by four embodiments and three comparative examples, are applied for preparing anti-corrosion of metal
Material, preparation process is as follows：100 parts of dichloroethylene emulsion, 30.0 parts of mill base, 1.5 parts of ammoniacal liquor, 1.2 parts of Alkali-soluble acrylic's emulsion,
8.0 parts of propane diols, 0.2 part of thickener, 0.4 part of defoamer, deionized water configure the anti-corrosion of metal that solid content is 40% and applied in right amount
Material, film forming, spray gun bore are carried out using spraying process：2.0 mm, air pressure：4 bar, prepare 30 microns of wet films.
The performance indications of embodiment and comparative example are shown in Table 2,3.
The emulsion property index of the embodiment of table 2 and comparative example
The primer performance index of the embodiment of table 3 and comparative example
It was found from embodiment 1~4, the anticorrosive metal paint polyvinylidene emulsions prepared by the present invention have good
Good heat endurance and ordinary temperature stability, is had well based on metal anti-corrosive paint prepared by the polyvinylidene emulsions
Salt fog resistance（Corrosion resistance）, there is higher adhesive force to metal base, and do not corrode metal.According to comparative example 1 and contrast
The contrast of example 2 and embodiment 1 is understood, only when hydroxyethyl meth acrylate phosphate and N hydroxymethyl acrylamide are made jointly
Used time, prepared anticorrosive paint just has good tack to metal base.According to the contrast of comparative example 3 and embodiment 1
Understand, the anti-corrosive properties of coating can be effectively improved from hydroxyethyl meth acrylate phosphate, are avoided that base material by coating again
Component itself is corroded.
Embodiment described above only expresses embodiments of the present invention, and it describes more specific and detailed, but can not
Therefore the limitation to the scope of the claims of the present invention is interpreted as, as long as the skill obtained using the form of equivalent substitution or equivalent transformation
Art scheme, all should be included within the protection domain of the claims in the present invention.
Claims (10)
1. a kind of polyvinylidene emulsions, are prepared, it is characterised in that by weight by pre-emulsion, kettle material and initiator solution
Meter,
The pre-emulsion includes：
75~86 parts of vinylidene chloride；
6~15 parts of A classes reaction monomers, wherein A classes reaction monomers are butyl acrylate, methyl methacrylate, ethyl acrylate
In one or more；
1~2 part of B classes reaction monomers, wherein B classes reaction monomers refer to one kind or many in acrylic acid, methacrylic acid, itaconic acid
Kind；
2~4 parts of hydroxyethyl meth acrylate phosphate；
3~5 parts of N hydroxymethyl acrylamide；
1.0~2.0 parts of anionic emulsifier；
1.0~2.0 parts of response type nonionic emulsifier；
0.1~2 part of molecular weight regulator；
0.2~1 part of polyvinylpyrrolidone；
40~50 parts of deionized water；
The kettle material includes：
0.4~0.5 part of emulsifying agent；
40~50 parts of deionized water；
NaHCO3 And/or Na2CO3 0.3~0.9 part；
0.01~0.1 part of EDTA；
The initiator solution includes：
0.3~0.4 part of oxidizing initiators；
Reduce 0.15~0.2 part of initiator；
10~20 parts of deionized water.
2. polyvinylidene emulsions according to claim 1, it is characterised in that the anionic emulsifier is dodecane
Base sodium sulphate.
3. polyvinylidene emulsions according to claim 1, it is characterised in that the response type nonionic emulsifier is alkene
Propoxyl group NPE.
4. polyvinylidene emulsions according to claim 1, it is characterised in that the oxidizing initiators are sodium peroxydisulfate.
5. polyvinylidene emulsions according to claim 1, it is characterised in that the reduction initiator is bisulfite
Sodium.
6. the preparation method of polyvinylidene emulsions as described in Claims 1 to 5 any claim, it is characterised in that bag
Include following steps：
S1. pre- emulsified material is mixed respectively by formula, high-speed stirred 30~60min of pre-emulsification prepares pre-emulsion standby；
S2. after kettle material is well mixed by formula, mixing speed is 200~300rpm, is warming up to 55 DEG C~65 DEG C, is added pre-
The 10~15% of emulsion and the 20~40% of initiator solution to reactor in, react 30~60min, formed seed emulsion；
S3. remaining 85~90% pre-emulsions, 50~70% initiator solutions are added into seed emulsion, were added in 4~6 hours；
Continue to be incubated after 0.5~1.5h, add remaining initiator solution, be cooled to less than 40 DEG C, discharging.
7. the preparation method of polyvinylidene emulsions according to claim 6, it is characterised in that the S2. and S3. be
Carried out under inert gas atmosphere.
8. the preparation method of polyvinylidene emulsions according to claim 6 or 7, it is characterised in that the S2 is by formula
After kettle material is well mixed, pour into reactor, seal reactor, N is filled to reactor2And vacuumize, in triplicate, finally fill
N2It is normal pressure to make the pressure in kettle;Reactor opens stirring, and mixing speed is 200~300rpm, is warming up to 55 DEG C, adds pre- breast
The 10~15% of liquid and the 30% of initiator solution, 30~60min is reacted, seed emulsion is formed.
9. the preparation method of polyvinylidene emulsions according to claim 6 or 7, it is characterised in that the S3 is to seed
Remaining 85~90% pre-emulsions, 60% initiator solution are added in emulsion, was added in 5 hours；Continue to be incubated after 1h, then continuously add
Enter remaining 10% initiator solution, vacuumize, cool, be cooled to less than 40 DEG C, filter, discharging.
10. polyvinylidene emulsions are in waterborne metal anti-corrosive paint is prepared described in Claims 1 to 5 any claim
Using.
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| CN106279515B (en) * | 2016-08-16 | 2018-08-28 | 衡水新光新材料科技有限公司 | A kind of preparation process of anticorrosion water-soluble acrylic emulsion |
| CN106280745A (en) * | 2016-09-14 | 2017-01-04 | 四川力久云智知识产权运营有限公司 | A kind of anticorrosive coating of improvement |
| CN106752947A (en) * | 2016-11-30 | 2017-05-31 | 湖州练市双龙木业有限公司 | A kind of mould proof protective agent for wood products and preparation method thereof |
| CN107964292A (en) * | 2017-08-28 | 2018-04-27 | 河北晨阳工贸集团有限公司 | A kind of track machine road spring paint and preparation method thereof |
| CN110205030A (en) * | 2019-05-29 | 2019-09-06 | 张家港市天源制漆涂装有限公司 | A kind of aqueous bottom surface unification coating and preparation method thereof |
| CN111269347A (en) * | 2020-03-23 | 2020-06-12 | 泰安聚仁新材料有限公司 | Dichloroethylene-acrylic ester copolymer emulsion and preparation method thereof |
| CN111518235A (en) * | 2020-06-29 | 2020-08-11 | 天津城建大学 | Water-based vinylidene chloride copolymer resin and preparation method thereof |
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| JP4128376B2 (en) * | 2002-02-26 | 2008-07-30 | 旭化成ケミカルズ株式会社 | Vinylidene chloride copolymer latex |
| CN100569880C (en) * | 2007-01-15 | 2009-12-16 | 浙江野风塑胶有限公司 | Rustproofing primer of aqueous polyvinylidene chloride and preparation method thereof |
| CN100497408C (en) * | 2007-03-27 | 2009-06-10 | 中山大学 | Self-deposition coating based on vinylidene chloride-acrylate copolymer latex and preparing method |
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