CN106336802A - Ship heavy anticorrosive coating - Google Patents
Ship heavy anticorrosive coating Download PDFInfo
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- CN106336802A CN106336802A CN201610703524.6A CN201610703524A CN106336802A CN 106336802 A CN106336802 A CN 106336802A CN 201610703524 A CN201610703524 A CN 201610703524A CN 106336802 A CN106336802 A CN 106336802A
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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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/10—Block or graft copolymers containing polysiloxane sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/452—Block-or graft-polymers containing polysiloxane sequences containing nitrogen-containing sequences
- C08G77/455—Block-or graft-polymers containing polysiloxane sequences containing nitrogen-containing sequences containing polyamide, polyesteramide or polyimide sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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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
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/106—Anti-corrosive paints containing metal dust containing Zn
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
The invention discloses a ship heavy anticorrosive coating comprising a component A and a component B in the weight ratio of 15: 5-1; the component A comprises the following preparation raw materials by weight: 15-20 parts of zinc powder, 10-15 parts of titanium dioxide, 10-15 parts of molybdenum sesquioxide, 15-30 parts of octaphenyl polyhedral oligomeric silsesquioxane-modified sulfonated polyimide, 0.5-3 parts of polyoxyethylene polyoxypropylene ether, 1-5 parts of N, N-dimethyl piperazine, 1-10 parts of KH-550, 1-5 parts of graphene oxide, 30-50 parts of tetraethoxysilane and 10-20 parts of dimethyl sulfoxide; the component B comprises the following preparation raw materials by weight: 5-10 parts of beta-cyclodextrin-modified amino terminated sulfonated polybenzimidazole, 30-50 parts of nano titanium dioxide, 15-20 parts of quartz powder, 40-50 parts of epoxy resin E51, 1-10 parts of KH-560, 5-10 parts of 1,12-dodecamethylene dibromide, 5-10 parts of glycol and 1-10 parts of pentaerythritol.
Description
Technical field
A kind of the invention belongs to technical field of coatings, more particularly it relates to Heavy-Duty Marine Paints.
Background technology
In marine ship industry, sea marine organism pollution and marine corrosion is prevented to be always a larger difficult problem.Traditional
Antifouling anticorrosive coating suppresses attachment and the growth of marine growth using the toxicant such as Red copper oxide or stannum class, but these toxicity
Material causes severe contamination to sea water.Therefore, find new nontoxic, high anticorrosive property energy antifouling anticorrosive coating to become
A direction for people's research.
Due to being limited by own material property and technique, the corrosion protection to parent metal acts on not traditional coating for watercraft
Very preferable, and have quite a few coating because of harmful toxic matters such as leaded or chromate, exist dirty during preparation and use
The danger of dye environment, this is incompatible with the requirement of Sustainable Socioeconomic Development strategy.More universal anti-corrosion of at present application
Erosion coating is mostly epoxy zinc-rich paint, but in the prior art, dry film metal Zn content based on epoxy zinc rich primer is 80%
More than, the adhesive force of coating, impact-resistant mechanical performance can reduce with the raising of Zn content, and salt spray resistance also can be
Reduce, so easily destroyed by external force in work progress floating coat and affect the Corrosion Protection of coating.And, existing ship applies
Material generally uses Lauxite, melmac, acrylic resin or phenolic resin as filmogen, and these polymer are tough
Property poor, low intensity, weatherability difference and salt spray resistance is also bad, leverage the combination property of coating.
Hence it is highly desirable to by the improvement of formula, obtain the ship that pliability is good, weatherability is strong and salt spray resistance is good
Anticorrosive paint.
Content of the invention
In order to solve the above problems, one aspect of the present invention provides a kind of Heavy-Duty Marine Paints, by component a and component
B forms, and by weight, the weight of described component a and component b ratio is for 15: 5～1；The preparing raw material of each component by weight,
As follows:
15～20 parts of component a: zinc powder, 10～15 parts of titanium dioxide, 10～15 parts of molybdenum sesquioxide, the poly- sesquialter of octaphenyl cage modle
15～30 parts of silicone-modified sulfonated polyimide, 0.5～3 part of polyoxyethylene polyoxy propanol amidogen ether, n, n- lupetazin 1～
5 parts, 1～10 part of kh-550,1～5 part of graphene oxide, 30～50 parts of tetraethyl orthosilicate and 10～20 parts of dimethyl sulfoxide；
Component b: beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole 5-10 part, 30～50 parts of nano titanium oxide,
Silica flour 15～20,40～50 parts of epoxy resin e51,1～10 part of kh-560,5～10 parts of 1,12- dibromo-dodecane, second two
5～10 parts of alcohol and 1～10 part of tetramethylolmethane.
In one embodiment, described octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides are by following methods
It is prepared from:
In the three-necked bottle that 100ml is dried, sequentially add 1.6mmol 2,2 '-bis- (4- sulfonic benzo epoxide) biphenyl two
Amine, 12.5ml m-creso1 and 0.8ml triethylamine, logical nitrogen protection magnetic agitation；Treat 2,2 '-bis- (4- sulfonic benzo oxygen
Base) after benzidine is completely dissolved, sequentially add 1.55mmol 3,4,9,10- tetracarboxylic anhydride, 3.0mmol benzoic acid with
And 0.6ml isoquinolin；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, 180 DEG C of reaction 20h；After reaction terminates, it is down to room temperature, and
Pour into rapidly in 150ml methanol, obtain a large amount of solid precipitations；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C of dryings 20 hours, obtain amino-terminated sulfonated polyimide prepolymer；
100 grams of described amino-terminated sulfonated polyimide prepolymers are first dissolved in containing 86wt% phosphorus pentoxide
In 1000 grams of polyphosphoric acids, octaphenyl cage modle is then added to gather again toward in described amino-terminated sulfonated polyimide pre-polymer solution
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, precipitating, in water, filters and collects product,
It is vacuum dried 10 hours at 60 DEG C, obtain octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides.
In one embodiment, described beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole is by following methods system
Standby form:
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxide
In phosphoric acid, then the 5- sulfonic group M-phthalic acid of 0.02 mole of 5- amino isophthalic acid and 0.08 mole is added to
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, and precipitating, in water, is then neutralized with ammonia, mistake
Filter and collect product, be vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, sequentially add 1.2 grams of beta-schardinger dextrin -s, 0.2 gram of sodium hydroxide, 0.5 gram of epoxy chloropropionate
Alkane, 13 grams of amino-terminated sulfonate polybenzimidazole obtained above, 100 milliliters of ethanol and 200 milliliters of dimethyl sulfoxide, nitrogen
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, precipitating, in acetone, filters and collects product, be vacuum dried at 60 DEG C
20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
Another aspect of the present invention provides the preparation method of described Heavy-Duty Marine Paints, comprises the following steps:
By 15～20 parts of zinc powder, 10～15 parts of titanium dioxide, 10～15 parts of molybdenum sesquioxide, the poly- silsesquioxane of octaphenyl cage modle
15～30 parts of alkane modification sulphonation polyimides, 0.5～3 part of polyoxyethylene polyoxy propanol amidogen ether, n, 1～5 part of n- lupetazin,
1～10 part of kh-550,1～5 part of graphene oxide, 30～50 parts of tetraethyl orthosilicate and 10～20 parts of dimethyl sulfoxide are poured into
In pill tank, it is stirred by dispersator, mixing speed controls at 300 revs/min -500 revs/min, mixing time is 15 points
Clock, obtains component a；
Beta-schardinger dextrin-modified amido is blocked sulfonate polybenzimidazole 5-10 part, 30～50 parts of nano titanium oxide, quartz
Powder 15～20,40～50 parts of epoxy resin e51,1～10 part of kh-560,5～10 parts of 1,12- dibromo-dodecane, ethylene glycol 5～
10 parts and 1～10 part of tetramethylolmethane are poured in pill tank, are stirred by dispersator, mixing speed control 800 turns/
Divide -1000 revs/min, mixing time is 30 minutes, obtains component b；
By described component a with component b by weight mixing for 15: 5～1, obtain final product Heavy-Duty Marine Paints.
Compared with prior art, the invention has the benefit that
1st, cage modle polysilsesquioxane is a kind of extraordinary nano sized inorganic fillers, can be effectively improved the strong of system
Degree, wearability and salt spray resistance, studies have found that, in the system of the present invention, its can not disperse well it is easy to
Reunite, effective effect can not be played.By being modified with sulfonated polyimide, can be greatly improved it in system
Dispersibility.Further, since cage modle polysilsesquioxane is located at side chain and rigidity is strong, considerably increase the distance of strand, and
Match with the polyimides of good weatherability, the weatherability of system can be greatly improved.Additionally, introducing phenylate structure in side chain,
Both wearability can have been improved, sulfonic presence in a large number can significantly reduce the content of free calcium hydroxide in material, plays suppression
The generation of the accumulation of salt in the surface soil phenomenon on cement mortar surface, sulfonic water absorption, the system that is also prevented from is excessively crisp, thus providing this
Bright Advantageous Effects.
2nd, polybenzimidazoles has excellent ageing-resistant ability, both can significantly be carried by sulfonation and beta-schardinger dextrin-modification
Its compatibility with system high, can greatly improve the crosslink density of system again, improve cohesion and intensity, thus providing this
The Advantageous Effects of invention.
3rd, n, n- lupetazin can obtain polyquaternary ammonium salt with the reaction of 1,12- dibromo-dodecane, and 1,12- dibromo 12
Alkane can also be reacted with amino, greatly improves the crosslinking rate of system, shortens hardening time, thus providing the beneficial of the present invention
Technique effect.
Specific embodiment
Raw material:
All tetramines, diacid are purchased from cti, sigmaaldrich, alfaaesar or scrc, and directly use, need not
It is further purified.Epoxy silane coupling agent kh-560 and kh-550 is purchased from Chemical Reagent Co., Ltd., Sinopharm Group.Other are former
Material is purchased from Aladdin reagent company limited.
Embodiment 1
20 parts of zinc powder, 15 parts of titanium dioxide, 15 parts of molybdenum sesquioxide, octaphenyl cage modle polysilsesquioxane modification sulphonation are gathered
30 parts of acid imide, 3 parts of polyoxyethylene polyoxy propanol amidogen ether, n, 3 parts of n- lupetazin, 8 parts of kh-550, graphene oxide 4
Part, 40 parts of tetraethyl orthosilicate and 15 parts of dimethyl sulfoxide are poured in pill tank, are stirred by dispersator, mixing speed
Control at 400 revs/min, mixing time is 15 minutes, obtains component a；
Beta-schardinger dextrin-modified amido is blocked 8 parts of sulfonate polybenzimidazole, 40 parts of nano titanium oxide, silica flour 18, ring
45 parts of oxygen tree fat e51,8 parts of kh-560,8 parts of 1,12- dibromo-dodecane, 8 parts of ethylene glycol and 8 parts of tetramethylolmethane pour dispensing into
In cylinder, it is stirred by dispersator, mixing speed controls at 1000 revs/min, mixing time is 30 minutes, obtains component b；
By described component a with component b by weight mixing for 15: 3, obtain final product Heavy-Duty Marine Paints；
Wherein said octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides are prepared from by following methods:
In the three-necked bottle that 100ml is dried, sequentially add 1.6mmol 2,2 '-bis- (4- sulfonic benzo epoxide) biphenyl two
Amine, 12.5ml m-creso1 and 0.8ml triethylamine, logical nitrogen protection magnetic agitation；Treat 2,2 '-bis- (4- sulfonic benzo oxygen
Base) after benzidine is completely dissolved, sequentially add 1.55mmol 3,4,9,10- tetracarboxylic anhydride, 3.0mmol benzoic acid with
And 0.6ml isoquinolin；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, 180 DEG C of reaction 20h；After reaction terminates, it is down to room temperature, and
Pour into rapidly in 150ml methanol, obtain a large amount of solid precipitations；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C of dryings 20 hours, obtain amino-terminated sulfonated polyimide prepolymer；
100 grams of described amino-terminated sulfonated polyimide prepolymers are first dissolved in containing 86wt% phosphorus pentoxide
In 1000 grams of polyphosphoric acids, octaphenyl cage modle is then added to gather again toward in described amino-terminated sulfonated polyimide pre-polymer solution
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, precipitating, in water, filters and collects product,
It is vacuum dried 10 hours at 60 DEG C, obtain octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides；
Described beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole is prepared from by following methods:
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxide
In phosphoric acid, then the 5- sulfonic group M-phthalic acid of 0.02 mole of 5- amino isophthalic acid and 0.08 mole is added to
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, and precipitating, in water, is then neutralized with ammonia, mistake
Filter and collect product, be vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, sequentially add 1.2 grams of beta-schardinger dextrin -s, 0.2 gram of sodium hydroxide, 0.5 gram of epoxy chloropropionate
Alkane, 13 grams of amino-terminated sulfonate polybenzimidazole obtained above, 100 milliliters of ethanol and 200 milliliters of dimethyl sulfoxide, nitrogen
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, precipitating, in acetone, filters and collects product, be vacuum dried at 60 DEG C
20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
Embodiment 2
20 parts of zinc powder, 15 parts of titanium dioxide, 15 parts of molybdenum sesquioxide, octaphenyl cage modle polysilsesquioxane modification sulphonation are gathered
30 parts of acid imide, 3 parts of polyoxyethylene polyoxy propanol amidogen ether, n, 3 parts of n- lupetazin, 8 parts of kh-550, graphene oxide 4
Part, 40 parts of tetraethyl orthosilicate and 15 parts of dimethyl sulfoxide are poured in pill tank, are stirred by dispersator, mixing speed
Control at 400 revs/min, mixing time is 15 minutes, obtains component a；
Beta-schardinger dextrin-modified amido is blocked 8 parts of sulfonate polybenzimidazole, 40 parts of nano titanium oxide, silica flour 18, ring
45 parts of oxygen tree fat e51,8 parts of kh-560,8 parts of 1,12- dibromo-dodecane, 8 parts of ethylene glycol and 8 parts of tetramethylolmethane pour dispensing into
In cylinder, it is stirred by dispersator, mixing speed controls at 1000 revs/min, mixing time is 30 minutes, obtains component b；
By described component a with component b by weight mixing for 15: 3, obtain final product Heavy-Duty Marine Paints；
Wherein, described octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides are prepared from by following methods:
In the three-necked bottle that 100ml is dried, sequentially add 1.6mmol 4,4 '-two (4- amino-benzene oxygen) biphenyl -3,3 '
Disulfonic acid aniline, 12.5ml m-creso1 and 0.8ml triethylamine, logical nitrogen protection magnetic agitation；Treat 4,4 '-two (4- amino
Phenoxy group) biphenyl -3, after 3 ' disulfonic acid aniline are completely dissolved, sequentially add 1.55mmol3,4,9,10- tetracarboxylic anhydrides,
3.0mmol benzoic acid and 0.6ml isoquinolin；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, 180 DEG C of reaction 20h；Reaction knot
Shu Hou, is down to room temperature, and pours into rapidly in 150ml methanol, obtains a large amount of solid precipitations；After this product of methanol cyclic washing,
Sucking filtration collected polymer, in vacuum drying oven, 60 DEG C of dryings 20 hours, obtain amino-terminated sulfonated polyimide prepolymer；
100 grams of described amino-terminated sulfonated polyimide prepolymers are first dissolved in containing 86wt% phosphorus pentoxide
In 1000 grams of polyphosphoric acids, octaphenyl cage modle is then added to gather again toward in described amino-terminated sulfonated polyimide pre-polymer solution
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, precipitating, in water, filters and collects product,
It is vacuum dried 10 hours at 60 DEG C, obtain octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides；
Described beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole is prepared from by following methods:
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxide
In phosphoric acid, then the 5- sulfonic group M-phthalic acid of 0.02 mole of 5- amino isophthalic acid and 0.08 mole is added to
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, and precipitating, in water, is then neutralized with ammonia, mistake
Filter and collect product, be vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, sequentially add 1.2 grams of beta-schardinger dextrin -s, 0.2 gram of sodium hydroxide, 0.5 gram of epoxy chloropropionate
Alkane, 13 grams of amino-terminated sulfonate polybenzimidazole obtained above, 100 milliliters of ethanol and 200 milliliters of dimethyl sulfoxide, nitrogen
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, precipitating, in acetone, filters and collects product, be vacuum dried at 60 DEG C
20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
Embodiment 3
20 parts of zinc powder, 15 parts of titanium dioxide, 15 parts of molybdenum sesquioxide, octaphenyl cage modle polysilsesquioxane modification sulphonation are gathered
30 parts of acid imide, 3 parts of polyoxyethylene polyoxy propanol amidogen ether, n, 3 parts of n- lupetazin, 8 parts of kh-550, graphene oxide 4
Part, 40 parts of tetraethyl orthosilicate and 15 parts of dimethyl sulfoxide are poured in pill tank, are stirred by dispersator, mixing speed
Control at 400 revs/min, mixing time is 15 minutes, obtains component a；
Beta-schardinger dextrin-modified amido is blocked 8 parts of sulfonate polybenzimidazole, 40 parts of nano titanium oxide, silica flour 18, ring
45 parts of oxygen tree fat e51,8 parts of kh-560,8 parts of 1,12- dibromo-dodecane, 8 parts of ethylene glycol and 8 parts of tetramethylolmethane pour dispensing into
In cylinder, it is stirred by dispersator, mixing speed controls at 1000 revs/min, mixing time is 30 minutes, obtains component b；
By described component a with component b by weight mixing for 15: 3, obtain final product Heavy-Duty Marine Paints；
Wherein, described octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides are prepared from by following methods:
In the three-necked bottle that 100ml is dried, sequentially add 1.6mmol 2,2 '-bis- (4- sulfonic benzo epoxide) biphenyl two
Amine, 12.5ml m-creso1 and 0.8ml triethylamine, logical nitrogen protection magnetic agitation；Treat 2,2 '-bis- (4- sulfonic benzo oxygen
Base) after benzidine is completely dissolved, sequentially add 1.55mmol 3,4,9,10- tetracarboxylic anhydride, 3.0mmol benzoic acid with
And 0.6ml isoquinolin；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, 180 DEG C of reaction 20h；After reaction terminates, it is down to room temperature, and
Pour into rapidly in 150ml methanol, obtain a large amount of solid precipitations；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C of dryings 20 hours, obtain amino-terminated sulfonated polyimide prepolymer；
100 grams of described amino-terminated sulfonated polyimide prepolymers are first dissolved in containing 86wt% phosphorus pentoxide
In 1000 grams of polyphosphoric acids, octaphenyl cage modle is then added to gather again toward in described amino-terminated sulfonated polyimide pre-polymer solution
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, precipitating, in water, filters and collects product,
It is vacuum dried 10 hours at 60 DEG C, obtain octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides；
Described beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole is prepared from by following methods:
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxide
In phosphoric acid, then 0.1 mole of 5- sulfonic group M-phthalic acid is added in reactant liquor, nitrogen protection is simultaneously reacted at 210 DEG C
After 15 hours, it is down to room temperature, precipitating, in water, is then neutralized with ammonia, filters and collect product, be vacuum dried at 120 DEG C
10 hours, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, sequentially add 1.2 grams of beta-schardinger dextrin -s, 0.2 gram of sodium hydroxide, 0.5 gram of epoxy chloropropionate
Alkane, 13 grams of amino-terminated sulfonate polybenzimidazole obtained above, 100 milliliters of ethanol and 200 milliliters of dimethyl sulfoxide, nitrogen
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, precipitating, in acetone, filters and collects product, be vacuum dried at 60 DEG C
20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
Embodiment 4
20 parts of zinc powder, 15 parts of titanium dioxide, 15 parts of molybdenum sesquioxide, octaphenyl cage modle polysilsesquioxane modification sulphonation are gathered
30 parts of acid imide, 3 parts of polyoxyethylene polyoxy propanol amidogen ether, n, 3 parts of n- lupetazin, 8 parts of kh-550, graphene oxide 4
Part, 40 parts of tetraethyl orthosilicate and 15 parts of dimethyl sulfoxide are poured in pill tank, are stirred by dispersator, mixing speed
Control at 400 revs/min, mixing time is 15 minutes, obtains component a；
By 8 parts of amino-terminated sulfonate polybenzimidazole, 40 parts of nano titanium oxide, silica flour 18, epoxy resin e51 45
Part, 8 parts of kh-560,8 parts of 1,12- dibromo-dodecane, 8 parts of ethylene glycol and 8 parts of tetramethylolmethane are poured in pill tank, by disperseing
Blender is stirred, and mixing speed controls at 1000 revs/min, and mixing time is 30 minutes, obtains component b；
By described component a with component b by weight mixing for 15: 3, obtain final product Heavy-Duty Marine Paints；
Wherein said octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides are prepared from by following methods:
In the three-necked bottle that 100ml is dried, sequentially add 1.6mmol 2,2 '-bis- (4- sulfonic benzo epoxide) biphenyl two
Amine, 12.5ml m-creso1 and 0.8ml triethylamine, logical nitrogen protection magnetic agitation；Treat 2,2 '-bis- (4- sulfonic benzo oxygen
Base) after benzidine is completely dissolved, sequentially add 1.55mmol 3,4,9,10- tetracarboxylic anhydride, 3.0mmol benzoic acid with
And 0.6ml isoquinolin；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, 180 DEG C of reaction 20h；After reaction terminates, it is down to room temperature, and
Pour into rapidly in 150ml methanol, obtain a large amount of solid precipitations；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C of dryings 20 hours, obtain amino-terminated sulfonated polyimide prepolymer；
100 grams of described amino-terminated sulfonated polyimide prepolymers are first dissolved in containing 86wt% phosphorus pentoxide
In 1000 grams of polyphosphoric acids, octaphenyl cage modle is then added to gather again toward in described amino-terminated sulfonated polyimide pre-polymer solution
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, precipitating, in water, filters and collects product,
It is vacuum dried 10 hours at 60 DEG C, obtain octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides；
Described amino-terminated sulfonate polybenzimidazole is prepared from by following methods:
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxide
In phosphoric acid, then the 5- sulfonic group M-phthalic acid of 0.02 mole of 5- amino isophthalic acid and 0.08 mole is added to
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, and precipitating, in water, is then neutralized with ammonia, mistake
Filter and collect product, be vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole.
Embodiment 5
20 parts of zinc powder, 15 parts of titanium dioxide, 15 parts of molybdenum sesquioxide, octaphenyl cage modle polysilsesquioxane modification sulphonation are gathered
30 parts of acid imide, 3 parts of polyoxyethylene polyoxy propanol amidogen ether, n, 3 parts of n- lupetazin, 8 parts of kh-550, graphene oxide 4
Part, 40 parts of tetraethyl orthosilicate and 15 parts of dimethyl sulfoxide are poured in pill tank, are stirred by dispersator, mixing speed
Control at 400 revs/min, mixing time is 15 minutes, obtains component a；
By 40 parts of nano titanium oxide, silica flour 18,45 parts of epoxy resin e51,8 parts of kh-560,1,12- dibromo 12
8 parts of alkane, 8 parts of ethylene glycol and 8 parts of tetramethylolmethane are poured in pill tank, are stirred by dispersator, and mixing speed controls
At 1000 revs/min, mixing time is 30 minutes, obtains component b；
By described component a with component b by weight mixing for 15: 3, obtain final product Heavy-Duty Marine Paints；
Wherein, described octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides are prepared from by following methods:
In the three-necked bottle that 100ml is dried, sequentially add 1.6mmol 2,2 '-bis- (4- sulfonic benzo epoxide) biphenyl two
Amine, 12.5ml m-creso1 and 0.8ml triethylamine, logical nitrogen protection magnetic agitation；Treat 2,2 '-bis- (4- sulfonic benzo oxygen
Base) after benzidine is completely dissolved, sequentially add 1.55mmol 3,4,9,10- tetracarboxylic anhydride, 3.0mmol benzoic acid with
And 0.6ml isoquinolin；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, 180 DEG C of reaction 20h；After reaction terminates, it is down to room temperature, and
Pour into rapidly in 150ml methanol, obtain a large amount of solid precipitations；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C of dryings 20 hours, obtain amino-terminated sulfonated polyimide prepolymer；
100 grams of described amino-terminated sulfonated polyimide prepolymers are first dissolved in containing 86wt% phosphorus pentoxide
In 1000 grams of polyphosphoric acids, octaphenyl cage modle is then added to gather again toward in described amino-terminated sulfonated polyimide pre-polymer solution
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, precipitating, in water, filters and collects product,
It is vacuum dried 10 hours at 60 DEG C, obtain octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides.
Embodiment 6
By 20 parts of zinc powder, 15 parts of titanium dioxide, 15 parts of molybdenum sesquioxide, 30 parts of acrylic resin, polyoxyethylene polyoxy propanol
3 parts of amidogen ether, n, 3 parts of n- lupetazin, 8 parts of kh-550,4 parts of graphene oxide, 40 parts of tetraethyl orthosilicate and dimethyl are sub-
15 parts of sulfone is poured in pill tank, is stirred by dispersator, and mixing speed controls at 400 revs/min, and mixing time is 15 points
Clock, obtains component a；
Beta-schardinger dextrin-modified amido is blocked 8 parts of sulfonate polybenzimidazole, 40 parts of nano titanium oxide, silica flour 18, ring
45 parts of oxygen tree fat e51,8 parts of kh-560,8 parts of 1,12- dibromo-dodecane, 8 parts of ethylene glycol and 8 parts of tetramethylolmethane pour dispensing into
In cylinder, it is stirred by dispersator, mixing speed controls at 1000 revs/min, mixing time is 30 minutes, obtains component b；
By described component a with component b by weight mixing for 15: 3, obtain final product Heavy-Duty Marine Paints；
Wherein, described beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole is prepared from by following methods:
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxide
In phosphoric acid, then the 5- sulfonic group M-phthalic acid of 0.02 mole of 5- amino isophthalic acid and 0.08 mole is added to
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, and precipitating, in water, is then neutralized with ammonia, mistake
Filter and collect product, be vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, sequentially add 1.2 grams of beta-schardinger dextrin -s, 0.2 gram of sodium hydroxide, 0.5 gram of epoxy chloropropionate
Alkane, 13 grams of amino-terminated sulfonate polybenzimidazole obtained above, 100 milliliters of ethanol and 200 milliliters of dimethyl sulfoxide, nitrogen
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, precipitating, in acetone, filters and collects product, be vacuum dried at 60 DEG C
20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
Embodiment 7
20 parts of zinc powder, 15 parts of titanium dioxide, 15 parts of molybdenum sesquioxide, octaphenyl cage modle polysilsesquioxane modification sulphonation are gathered
30 parts of acid imide, 3 parts of polyoxyethylene polyoxy propanol amidogen ether, 8 parts of kh-550,4 parts of graphene oxide, 40 parts of tetraethyl orthosilicate with
And 15 parts of dimethyl sulfoxide pours in pill tank, it is stirred by dispersator, mixing speed controls at 400 revs/min, stirring
Time is 15 minutes, obtains component a；
Beta-schardinger dextrin-modified amido is blocked 8 parts of sulfonate polybenzimidazole, 40 parts of nano titanium oxide, silica flour 18, ring
45 parts of oxygen tree fat e51,8 parts of kh-560,8 parts of ethylene glycol and 8 parts of tetramethylolmethane are poured in pill tank, are entered by dispersator
Row stirring, mixing speed controls at 1000 revs/min, and mixing time is 30 minutes, obtains component b；
By described component a with component b by weight mixing for 15: 3, obtain final product Heavy-Duty Marine Paints；
Wherein said octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides are prepared from by following methods:
In the three-necked bottle that 100ml is dried, sequentially add 1.6mmol 2,2 '-bis- (4- sulfonic benzo epoxide) biphenyl two
Amine, 12.5ml m-creso1 and 0.8ml triethylamine, logical nitrogen protection magnetic agitation；Treat 2,2 '-bis- (4- sulfonic benzo oxygen
Base) after benzidine is completely dissolved, sequentially add 1.55mmol 3,4,9,10- tetracarboxylic anhydride, 3.0mmol benzoic acid with
And 0.6ml isoquinolin；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, 180 DEG C of reaction 20h；After reaction terminates, it is down to room temperature, and
Pour into rapidly in 150ml methanol, obtain a large amount of solid precipitations；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C of dryings 20 hours, obtain amino-terminated sulfonated polyimide prepolymer；
100 grams of described amino-terminated sulfonated polyimide prepolymers are first dissolved in containing 86wt% phosphorus pentoxide
In 1000 grams of polyphosphoric acids, octaphenyl cage modle is then added to gather again toward in described amino-terminated sulfonated polyimide pre-polymer solution
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, precipitating, in water, filters and collects product,
It is vacuum dried 10 hours at 60 DEG C, obtain octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides；
Described beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole is prepared from by following methods:
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxide
In phosphoric acid, then the 5- sulfonic group M-phthalic acid of 0.02 mole of 5- amino isophthalic acid and 0.08 mole is added to
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, and precipitating, in water, is then neutralized with ammonia, mistake
Filter and collect product, be vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, sequentially add 1.2 grams of beta-schardinger dextrin -s, 0.2 gram of sodium hydroxide, 0.5 gram of epoxy chloropropionate
Alkane, 13 grams of amino-terminated sulfonate polybenzimidazole obtained above, 100 milliliters of ethanol and 200 milliliters of dimethyl sulfoxide, nitrogen
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, precipitating, in acetone, filters and collects product, be vacuum dried at 60 DEG C
20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
Test condition
Embodiment 1-7 gained coating is coated on ship, and test performance, test result is shown in Table 1.
Table 1
Data above can be seen that with do not use octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides and β-
The coating of the amino-terminated sulfonate polybenzimidazole of cyclo-dextrin-modified is compared, and the coating of the present invention has obvious better performance, because
This provides the Advantageous Effects of the present invention.
Claims (4)
1. a kind of Heavy-Duty Marine Paints are it is characterised in that form, by weight, described component a and group by component a and component b
The weight of point b ratio is for 15: 5～1；The preparing raw material of each component is by weight, as follows:
15～20 parts of component a: zinc powder, 10～15 parts of titanium dioxide, 10～15 parts of molybdenum sesquioxide, the poly- silsesquioxane of octaphenyl cage modle
15～30 parts of alkane modification sulphonation polyimides, 0.5～3 part of polyoxyethylene polyoxy propanol amidogen ether, n, 1～5 part of n- lupetazin,
1～10 part of kh-550,1～5 part of graphene oxide, 30～50 parts of tetraethyl orthosilicate and 10～20 parts of dimethyl sulfoxide；
Component b: beta-schardinger dextrin-modified amido blocks sulfonate polybenzimidazole 5-10 part, 30～50 parts of nano titanium oxide, quartz
Powder 15～20,40～50 parts of epoxy resin e51,1～10 part of kh-560,5～10 parts of 1,12- dibromo-dodecane, ethylene glycol 5～
10 parts and 1～10 part of tetramethylolmethane.
2. a kind of Heavy-Duty Marine Paints according to claim 1 are it is characterised in that the poly- sesquialter silicon of described octaphenyl cage modle
Siloxane modified sulfonated polyimide is prepared from by following methods:
100ml be dried three-necked bottle in, sequentially add 1.6mmol 2,2 '-bis- (4- sulfonic benzo epoxide) benzidine,
12.5ml m-creso1 and 0.8ml triethylamine, logical nitrogen protection magnetic agitation；Treat that 2,2 '-bis- (4- sulfonic benzo epoxide) joins
After phenylenediamine is completely dissolved, sequentially add 1.55mmol 3,4,9,10- tetracarboxylic anhydride, 3.0mmol benzoic acid and
0.6ml isoquinolin；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, 180 DEG C of reaction 20h；After reaction terminates, it is down to room temperature, and fast
Speed is poured in 150ml methanol, obtains a large amount of solid precipitations；After this product of methanol cyclic washing, sucking filtration collected polymer, in
In vacuum drying oven, 60 DEG C of dryings 20 hours, obtain amino-terminated sulfonated polyimide prepolymer；
100 grams of described amino-terminated sulfonated polyimide prepolymers are first dissolved in 1000 grams containing 86wt% phosphorus pentoxide
In polyphosphoric acids, toward in described amino-terminated sulfonated polyimide pre-polymer solution, then add the poly- silsesquioxane of octaphenyl cage modle
Alkane 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, precipitating, in water, filters and collects product, in 60 DEG C
Lower vacuum drying 10 hours, obtains octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides.
3. a kind of Heavy-Duty Marine Paints according to claim 1 are it is characterised in that described beta-schardinger dextrin-modified amido
End-blocking sulfonate polybenzimidazole is prepared from by following methods:
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polyphosphoric acids containing 86wt% phosphorus pentoxide
In, then the 5- sulfonic group M-phthalic acid of 0.02 mole of 5- amino isophthalic acid and 0.08 mole is added to reaction
In liquid, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, and precipitating, in water, is then neutralized with ammonia, filters simultaneously
Collect product, be vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, sequentially add 1.2 grams of beta-schardinger dextrin -s, 0.2 gram of sodium hydroxide, 0.5 gram of epoxychloropropane, 13
Gram amino-terminated sulfonate polybenzimidazole obtained above, 100 milliliters of ethanol and 200 milliliters of dimethyl sulfoxide, nitrogen is protected
And after 80 DEG C of reactions 2 hours, it is down to room temperature, precipitating, in acetone, filters and collects product, at 60 DEG C, vacuum drying 20 is little
When, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
4. the preparation method of the Heavy-Duty Marine Paints as any one of claim 1-3 is it is characterised in that include following
Step:
15～20 parts of zinc powder, 10～15 parts of titanium dioxide, 10～15 parts of molybdenum sesquioxide, octaphenyl cage modle polysilsesquioxane are changed
15～30 parts of sulfonated polyimide of property, 0.5～3 part of polyoxyethylene polyoxy propanol amidogen ether, n, 1～5 part of n- lupetazin, kh-
550 1～10 parts, 1～5 part of graphene oxide, 30～50 parts of tetraethyl orthosilicate and 10～20 parts of dimethyl sulfoxide pour dispensing into
In cylinder, it is stirred by dispersator, mixing speed controls at 300 revs/min -500 revs/min, mixing time is 15 minutes, obtains
To component a；
Beta-schardinger dextrin-modified amido is blocked sulfonate polybenzimidazole 5-10 part, 30～50 parts of nano titanium oxide, silica flour 15
～20,40～50 parts of epoxy resin e51,1～10 part of kh-560,5～10 parts of 1,12- dibromo-dodecane, 5～10 parts of ethylene glycol
And 1～10 part of tetramethylolmethane pours in pill tank, be stirred by dispersator, mixing speed control 800 revs/min-
1000 revs/min, mixing time is 30 minutes, obtains component b；
By described component a with component b by weight mixing for 15: 5～1, obtain final product Heavy-Duty Marine Paints.
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| CN107603296A (en) * | 2017-10-13 | 2018-01-19 | 重庆晋豪美耐皿制品有限公司 | A kind of stalk is modified wall powdery paints |
| CN108977059A (en) * | 2018-06-07 | 2018-12-11 | 河南万工环保材料有限公司 | A kind of novel anticorrosive paint and its preparation process |
| CN110373083A (en) * | 2019-02-22 | 2019-10-25 | 福建科华中盈新材料有限公司 | A kind of apply requires low anticorrosive paint and preparation method thereof to preceding processing on ship |
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