CN106318198A - Water-based nano-resin outdoor ultrathin fireproof coating for steel structure - Google Patents
Water-based nano-resin outdoor ultrathin fireproof coating for steel structure Download PDFInfo
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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
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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Abstract
The invention discloses water-based nano-resin outdoor ultrathin fireproof coating for a steel structure. The water-based nano-resin outdoor ultrathin fireproof coating comprises a component A and a component B, wherein the weight ratio of the component A to the component B is 15:(5-1); the component A comprises, by weight, 15-20 parts of zinc powder, 10-15 parts of talcum powder, 10-15 parts of vanadium dioxide, 15-30 parts of water-based nano-resin 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 tetraethyl orthosilicate and 10-20 parts of N, N-dimethyl formamide; the component B comprises, by weight, beta-cyclodextrin modified amino terminated sulfonated polybenzimidazole, 15-30 parts of epoxy terminated polyether amine, 30-50 parts of nano silicon 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-dibromo dodecane, 5-10 parts of ethylene glycol and 1-10 parts of pentaerythritol.
Description
Technical field
The invention belongs to technical field of coatings, more particularly it relates to an water nano resin outdoor is ultrathin
Fire-resistant coating for steel structure.
Background technology
In marine ship industry, sea marine organism pollution and marine corrosion is prevented to be always a bigger difficult problem.Traditional
Antifouling anticorrosive coating utilize the toxicant such as Red copper oxide or stannum class to suppress attachment and the growth of marine growth, but these toxicity
Material causes severe contamination to sea water.Therefore, the antifouling anticorrosive coating finding novel Corrosion Protection nontoxic, high becomes
A direction for people's research.
Tradition coating for watercraft is owing to being limited by own material character and technique, to the corrosion protection effect of parent metal not
Very preferable, and have quite a few coating because of harmful toxic matters such as leaded or chromate, there is dirt in preparation and during using
The danger of dye environment, this is incompatible with the requirement of Sustainable Socioeconomic Development strategy.Apply the most universal anticorrosion at present
Erosion coating is mostly epoxy zinc-rich paint, but in the prior art, dry film metallic zinc content based on epoxy zinc rich primer is 80%
Above, the adhesive force of coating, impact-resistant mechanical performance can reduce along with the raising of Zn content, and salt spray resistance also can be
Reduce, so easily destroyed by external force at work progress floating coat and affect the Corrosion Protection of coating.And, existing boats and ships are coated with
Material generally uses Lauxite, melmac, acrylic resin or phenolic resin as filmogen, and these polymer are tough
Property is poor, intensity is low, weatherability is poor and salt spray resistance is the most bad, leverages the combination property of coating.
Hence it is highly desirable to by the improvement of formula, obtain the aqueous that pliability is good, weatherability is strong and salt spray resistance is good
Nano-resin outdoor super-thin steel structure fire-proof paint.
Summary of the invention
In order to solve the problems referred to above, one aspect of the present invention provides a kind of water nano resin outdoor ultra-thin steel structure
Fireproof coating, is made up of component A and component B, and by weight, described component A is 15: 5～1 with the weight ratio of component B；Each component
Prepare raw material by weight, as follows:
Component A: zinc powder 15～20 parts, Pulvis Talci 10～15 parts, vanadium dioxide 10～15 parts, water nano resin octaphenyl
Cage modle polysilsesquioxane modification sulphonation polyimides 15～30 parts, polyoxyethylene polyoxy propanol amidogen ether 0.5～3 parts, N, N-bis-
Methyl piperazine 1～5 parts, KH-550 1～10 parts, graphene oxide 1～5 parts, tetraethyl orthosilicate 30～50 parts and N, N-diformazan
Base Methanamide 10～20 parts；
Component B: beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole 5-10 part, epoxy-capped polyetheramine 15～30
Part, nano silicon 30～50 parts, silica flour 15～20, epoxy resin E51 40～50 parts, KH-560 1～10 parts, 1,
12-dibromo-dodecane 5～10 parts, ethylene glycol 5～10 parts and tetramethylolmethane 1～10 parts.
In one embodiment, described water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyamides is sub-
Amine is prepared from by following methods:
In the three-necked bottle that 100mL is dried, it is sequentially added into 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 anhydrides, 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 precipitation；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C are dried 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, then in described amino-terminated sulfonated polyimide pre-polymer solution, add poly-times of octaphenyl cage modle
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, in precipitating to water, filters and collect product,
It is vacuum dried 10 hours at 60 DEG C, obtains water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyamides sub-
Amine.
In one embodiment, described beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole is by following methods system
For forming:
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-amino isophthalic acid of 0.02 mole and the 5-sulfonic group M-phthalic acid of 0.08 mole are joined
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, in precipitating to water, then neutralizes with ammonia, mistake
Filter and collect product, being vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, it is sequentially added into 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 N, N-dimethyl formyls
Amine, nitrogen is protected and after 80 DEG C of reactions 2 hours, is down to room temperature, in precipitating to acetone, filters and collect product, at 60 DEG C
It is vacuum dried 20 hours, obtains beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
In one embodiment, described epoxy-capped polyetheramine is prepared from by following methods:
In the three-necked bottle that 100mL is dried, it is sequentially added into the benzylamine of epoxy resin E51,0.24mol of 100 grams and 500 grams
Propylene glycol monomethyl ether, logical nitrogen protection magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to room
Temperature, and pour into rapidly in 150mL deionized water, obtain a large amount of solid precipitation；After this product of deionized water cyclic washing, sucking filtration
And collected polymer, in vacuum drying oven, 60 DEG C are dried 20 hours, obtain epoxy-capped polyetheramine.
The preparation of the water nano resin outdoor super-thin steel structure fire-proof paint described in another aspect of the present invention offer
Method, comprises the following steps:
By zinc powder 15～20 parts, Pulvis Talci 10～15 parts, vanadium dioxide 10～15 parts, water nano resin octaphenyl cage modle
Polysilsesquioxane modification sulphonation polyimides 15～30 parts, polyoxyethylene polyoxy propanol amidogen ether 0.5～3 parts, N, N-dimethyl
Piperazine 1～5 parts, KH-550 1～10 parts, graphene oxide 1～5 parts, tetraethyl orthosilicate 30～50 parts and N, N-dimethyl methyl
Amide 10～20 parts are poured in pill tank, dispersator be stirred, mixing speed control 300 revs/min-500 turns/
Point, mixing time is 15 minutes, obtains component A；
By beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole 5-10 part, epoxy-capped polyetheramine 15～30 parts, receive
Rice silicon dioxide 30～50 parts, silica flour 15～20, epoxy resin E51 40～50 parts, KH-5601～10 parts, 1,12-dibromo
Dodecane 5～10 parts, ethylene glycol 5～10 parts and tetramethylolmethane 1～10 parts are poured in pill tank, dispersator stir
Mixing, mixing speed controls at 800 revs/min-1000 revs/min, and mixing time is 30 minutes, obtains component B；
It is 15: 5～1 to mix by weight with component B by described component A, obtains the outdoor ultra-thin shaped steel of water nano resin
Structure fire coating.
Compared with prior art, the invention have the benefit that
1, 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, it can not well disperse, 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.Additionally, due to cage modle polysilsesquioxane is positioned 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, introduce phenylate structure at side chain,
Both can improve wearability, a large amount of sulfonic existence can significantly reduce the content of free calcium hydroxide in material, play suppression
The generation of accumulation of salt in the surface soil phenomenon, sulfonic water absorption, it is also possible to prevent system the most crisp, thus provide the Advantageous effect of the present invention
Really.
2, polybenzimidazoles has the ageing-resistant ability of excellence, both can significantly be carried by sulfonation and beta-schardinger dextrin-modification
High its with the compatibility of system, the crosslink density of system can be greatly improved again, improve cohesion and intensity, thus provide this
The Advantageous Effects of invention.
3, N, N-lupetazin can be with 1, and the reaction of 12-dibromo-dodecane obtains polyquaternary ammonium salt, and 1,12-dibromo 12
Alkane can also react with amino, is greatly improved the crosslinking rate of system, shortens hardening time, thus provides the useful of the present invention
Technique effect.
4, epoxy-capped polyetheramine contains great amount of hydroxy group, can be greatly improved the cohesive force of coating and base material, improves coating
Ageing-resistant ability, additionally, it also can react with amino, improve crosslink density and solidification rate, a large amount of rigidity on this outside chain
The introducing of phenyl ring, can improve the distance of strand, improves flame retardant effect.
Detailed description of the invention
Raw material:
All tetramines, diacid are purchased from CTI, SigmaAldrich, AlfaAesar or SCRC, and directly use, it is not necessary to
It is further purified.Graphene oxide is purchased from Hunan richization, and model is FH-661.Other raw materials are purchased from the limited public affairs of Aladdin reagent
Department.Epoxy silane coupling agent KH-560 and amino silicane coupling agent KH-550 is purchased from Chemical Reagent Co., Ltd., Sinopharm Group.
Other raw materials are purchased from Aladdin reagent company limited.
Embodiment 1
By zinc powder 20 parts, Pulvis Talci 15 parts, vanadium dioxide 15 parts, water nano resin octaphenyl cage modle polysilsesquioxane
Modification sulphonation polyimides 30 parts, polyoxyethylene polyoxy propanol amidogen ether 3 parts, N, N-lupetazin 3 parts, KH-550 8 parts, oxygen
Functionalized graphene 4 parts, tetraethyl orthosilicate 40 parts and DMF 15 parts are poured in pill tank, dispersator enter
Row stirring, mixing speed controls at 400 revs/min, and mixing time is 15 minutes, obtains component A；
Beta-schardinger dextrin-modified amido is blocked sulfonate polybenzimidazole 8 parts, epoxy-capped polyetheramine 20 parts, nanometer titanium dioxide
Silicon 40 parts, silica flour 18, epoxy resin E51 45 parts, KH-560 8 parts, 1,12-dibromo-dodecane 8 parts, ethylene glycol 8 parts and
Tetramethylolmethane 8 parts is poured in pill tank, dispersator be stirred, and mixing speed controls at 1000 revs/min, mixing time
It is 30 minutes, obtains component B；
It is to mix at 15: 3 by weight with component B by described component A, obtains water nano resin outdoor ultra-thin steel structure
Fireproof coating；
Wherein said water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides is by following methods
It is prepared from:
In the three-necked bottle that 100mL is dried, it is sequentially added into 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 anhydrides, 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 precipitation；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C are dried 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, then in described amino-terminated sulfonated polyimide pre-polymer solution, add poly-times of octaphenyl cage modle
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, in precipitating to water, filters and collect product,
It is vacuum dried 10 hours at 60 DEG C, obtains water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyamides sub-
Amine；
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-amino isophthalic acid of 0.02 mole and the 5-sulfonic group M-phthalic acid of 0.08 mole are joined
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, in precipitating to water, then neutralizes with ammonia, mistake
Filter and collect product, being vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, it is sequentially added into 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 N, N-dimethyl formyls
Amine, nitrogen is protected and after 80 DEG C of reactions 2 hours, is down to room temperature, in precipitating to acetone, filters and collect product, at 60 DEG C
It is vacuum dried 20 hours, obtains beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole；
Described epoxy-capped polyetheramine is prepared from by following methods:
In the three-necked bottle that 100mL is dried, it is sequentially added into the benzylamine of epoxy resin E51,0.24mol of 100 grams and 500 grams
Propylene glycol monomethyl ether, logical nitrogen protection magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to room
Temperature, and pour into rapidly in 150mL deionized water, obtain a large amount of solid precipitation；After this product of deionized water cyclic washing, sucking filtration
And collected polymer, in vacuum drying oven, 60 DEG C are dried 20 hours, obtain epoxy-capped polyetheramine.
Embodiment 2
By zinc powder 20 parts, Pulvis Talci 15 parts, vanadium dioxide 15 parts, water nano resin octaphenyl cage modle polysilsesquioxane
Modification sulphonation polyimides 30 parts, polyoxyethylene polyoxy propanol amidogen ether 3 parts, N, N-lupetazin 3 parts, KH-550 8 parts, oxygen
Functionalized graphene 4 parts, tetraethyl orthosilicate 40 parts and DMF 15 parts are poured in pill tank, dispersator enter
Row stirring, mixing speed controls at 400 revs/min, and mixing time is 15 minutes, obtains component A；
Beta-schardinger dextrin-modified amido is blocked sulfonate polybenzimidazole 8 parts, epoxy-capped polyetheramine 20 parts, nanometer titanium dioxide
Silicon 40 parts, silica flour 18, epoxy resin E51 45 parts, KH-560 8 parts, 1,12-dibromo-dodecane 8 parts, ethylene glycol 8 parts and
Tetramethylolmethane 8 parts is poured in pill tank, dispersator be stirred, and mixing speed controls at 1000 revs/min, mixing time
It is 30 minutes, obtains component B；
It is to mix at 15: 3 by weight with component B by described component A, obtains water nano resin outdoor ultra-thin steel structure
Fireproof coating；
Wherein, described water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides is by following methods
It is prepared from:
In the three-necked bottle that 100mL is dried, it is sequentially added into 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 1.55mmol 3,4,9,10-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, obtain a large amount of solid precipitation；After this product of methanol cyclic washing,
Sucking filtration collected polymer, in vacuum drying oven, 60 DEG C are dried 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, then in described amino-terminated sulfonated polyimide pre-polymer solution, add poly-times of octaphenyl cage modle
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, in precipitating to water, filters and collect product,
It is vacuum dried 10 hours at 60 DEG C, obtains water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyamides sub-
Amine；
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-amino isophthalic acid of 0.02 mole and the 5-sulfonic group M-phthalic acid of 0.08 mole are joined
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, in precipitating to water, then neutralizes with ammonia, mistake
Filter and collect product, being vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, it is sequentially added into 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 N, N-dimethyl formyls
Amine, nitrogen is protected and after 80 DEG C of reactions 2 hours, is down to room temperature, in precipitating to acetone, filters and collect product, at 60 DEG C
It is vacuum dried 20 hours, obtains beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole；
Described epoxy-capped polyetheramine is prepared from by following methods:
In the three-necked bottle that 100mL is dried, it is sequentially added into the benzylamine of epoxy resin E51,0.24mol of 100 grams and 500 grams
Propylene glycol monomethyl ether, logical nitrogen protection magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to room
Temperature, and pour into rapidly in 150mL deionized water, obtain a large amount of solid precipitation；After this product of deionized water cyclic washing, sucking filtration
And collected polymer, in vacuum drying oven, 60 DEG C are dried 20 hours, obtain epoxy-capped polyetheramine.
Embodiment 3
By zinc powder 20 parts, Pulvis Talci 15 parts, vanadium dioxide 15 parts, water nano resin octaphenyl cage modle polysilsesquioxane
Modification sulphonation polyimides 30 parts, polyoxyethylene polyoxy propanol amidogen ether 3 parts, N, N-lupetazin 3 parts, KH-550 8 parts, oxygen
Functionalized graphene 4 parts, tetraethyl orthosilicate 40 parts and DMF 15 parts are poured in pill tank, dispersator enter
Row stirring, mixing speed controls at 400 revs/min, and mixing time is 15 minutes, obtains component A；
Beta-schardinger dextrin-modified amido is blocked sulfonate polybenzimidazole 8 parts, epoxy-capped polyetheramine 20 parts, nanometer titanium dioxide
Silicon 40 parts, silica flour 18, epoxy resin E51 45 parts, KH-560 8 parts, 1,12-dibromo-dodecane 8 parts, ethylene glycol 8 parts and
Tetramethylolmethane 8 parts is poured in pill tank, dispersator be stirred, and mixing speed controls at 1000 revs/min, mixing time
It is 30 minutes, obtains component B；
It is to mix at 15: 3 by weight with component B by described component A, obtains water nano resin outdoor ultra-thin steel structure
Fireproof coating；
Wherein, described water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides is by following methods
It is prepared from:
In the three-necked bottle that 100mL is dried, it is sequentially added into 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 anhydrides, 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 precipitation；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C are dried 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, then in described amino-terminated sulfonated polyimide pre-polymer solution, add poly-times of octaphenyl cage modle
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, in precipitating to water, filters and collect product,
It is vacuum dried 10 hours at 60 DEG C, obtains water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyamides sub-
Amine；
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 joining in reactant liquor by the 5-sulfonic group M-phthalic acid of 0.1 mole, nitrogen is protected and 210 DEG C of reactions
After 15 hours, it is down to room temperature, in precipitating to water, then neutralizes with ammonia, filter and collect product, be vacuum dried at 120 DEG C
10 hours, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, it is sequentially added into 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 N, N-dimethyl formyls
Amine, nitrogen is protected and after 80 DEG C of reactions 2 hours, is down to room temperature, in precipitating to acetone, filters and collect product, at 60 DEG C
It is vacuum dried 20 hours, obtains beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole；
Described epoxy-capped polyetheramine is prepared from by following methods:
In the three-necked bottle that 100mL is dried, it is sequentially added into the benzylamine of epoxy resin E51,0.24mol of 100 grams and 500 grams
Propylene glycol monomethyl ether, logical nitrogen protection magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to room
Temperature, and pour into rapidly in 150mL deionized water, obtain a large amount of solid precipitation；After this product of deionized water cyclic washing, sucking filtration
And collected polymer, in vacuum drying oven, 60 DEG C are dried 20 hours, obtain epoxy-capped polyetheramine.
Embodiment 4
By zinc powder 20 parts, Pulvis Talci 15 parts, vanadium dioxide 15 parts, water nano resin octaphenyl cage modle polysilsesquioxane
Modification sulphonation polyimides 30 parts, polyoxyethylene polyoxy propanol amidogen ether 3 parts, N, N-lupetazin 3 parts, KH-550 8 parts, oxygen
Functionalized graphene 4 parts, tetraethyl orthosilicate 40 parts and DMF 15 parts are poured in pill tank, dispersator enter
Row stirring, mixing speed controls at 400 revs/min, and mixing time is 15 minutes, obtains component A；
By amino-terminated sulfonate polybenzimidazole 8 parts, epoxy-capped polyetheramine 20 parts, nano silicon 40 parts, quartz
Powder 18, epoxy resin E51 45 parts, KH-560 8 parts, 1,12-dibromo-dodecane 8 parts, ethylene glycol 8 parts and tetramethylolmethane 8 parts
Pouring in pill tank, dispersator be stirred, mixing speed controls at 1000 revs/min, and mixing time is 30 minutes,
To component B；
It is to mix at 15: 3 by weight with component B by described component A, obtains water nano resin outdoor ultra-thin steel structure
Fireproof coating；
Wherein said water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides is by following methods
It is prepared from:
In the three-necked bottle that 100mL is dried, it is sequentially added into 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 anhydrides, 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 precipitation；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C are dried 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, then in described amino-terminated sulfonated polyimide pre-polymer solution, add poly-times of octaphenyl cage modle
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, in precipitating to water, filters and collect product,
It is vacuum dried 10 hours at 60 DEG C, obtains water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyamides sub-
Amine；
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-amino isophthalic acid of 0.02 mole and the 5-sulfonic group M-phthalic acid of 0.08 mole are joined
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, in precipitating to water, then neutralizes with ammonia, mistake
Filter and collect product, being vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
Described epoxy-capped polyetheramine is prepared from by following methods:
In the three-necked bottle that 100mL is dried, it is sequentially added into the benzylamine of epoxy resin E51,0.24mol of 100 grams and 500 grams
Propylene glycol monomethyl ether, logical nitrogen protection magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to room
Temperature, and pour into rapidly in 150mL deionized water, obtain a large amount of solid precipitation；After this product of deionized water cyclic washing, sucking filtration
And collected polymer, in vacuum drying oven, 60 DEG C are dried 20 hours, obtain epoxy-capped polyetheramine.
Embodiment 5
By zinc powder 20 parts, Pulvis Talci 15 parts, vanadium dioxide 15 parts, water nano resin octaphenyl cage modle polysilsesquioxane
Modification sulphonation polyimides 30 parts, polyoxyethylene polyoxy propanol amidogen ether 3 parts, N, N-lupetazin 3 parts, KH-550 8 parts, oxygen
Functionalized graphene 4 parts, tetraethyl orthosilicate 40 parts and DMF 15 parts are poured in pill tank, dispersator enter
Row stirring, mixing speed controls at 400 revs/min, and mixing time is 15 minutes, obtains component A；
By nano silicon 40 parts, silica flour 18, epoxy resin E51 45 parts, KH-560 8 parts, 1,12-dibromo 12
8 parts of alkane, ethylene glycol 8 parts and tetramethylolmethane 8 parts are poured in pill tank, dispersator be stirred, and mixing speed controls
At 1000 revs/min, mixing time is 30 minutes, obtains component B；
It is to mix at 15: 3 by weight with component B by described component A, obtains water nano resin outdoor ultra-thin steel structure
Fireproof coating；
Wherein, described water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides is by following methods
It is prepared from:
In the three-necked bottle that 100mL is dried, it is sequentially added into 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 anhydrides, 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 precipitation；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C are dried 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, then in described amino-terminated sulfonated polyimide pre-polymer solution, add poly-times of octaphenyl cage modle
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, in precipitating to water, filters and collect product,
It is vacuum dried 10 hours at 60 DEG C, obtains water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyamides sub-
Amine.
Embodiment 6
By zinc powder 20 parts, Pulvis Talci 15 parts, vanadium dioxide 15 parts, acrylic resin 30 parts, polyoxyethylene polyoxy Propanolamine
3 parts of ether, N, N-lupetazin 3 parts, KH-550 8 parts, graphene oxide 4 parts, tetraethyl orthosilicate 40 parts and N, N-dimethyl
Methanamide 15 parts is poured in pill tank, dispersator be stirred, and mixing speed controls at 400 revs/min, and mixing time is
15 minutes, obtain component A；
Beta-schardinger dextrin-modified amido is blocked sulfonate polybenzimidazole 8 parts, epoxy-capped polyetheramine 20 parts, nanometer titanium dioxide
Silicon 40 parts, silica flour 18, epoxy resin E51 45 parts, KH-560 8 parts, 1,12-dibromo-dodecane 8 parts, ethylene glycol 8 parts and
Tetramethylolmethane 8 parts is poured in pill tank, dispersator be stirred, and mixing speed controls at 1000 revs/min, mixing time
It is 30 minutes, obtains component B；
It is to mix at 15: 3 by weight with component B by described component A, obtains water nano resin outdoor ultra-thin steel structure
Fireproof coating；
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-amino isophthalic acid of 0.02 mole and the 5-sulfonic group M-phthalic acid of 0.08 mole are joined
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, in precipitating to water, then neutralizes with ammonia, mistake
Filter and collect product, being vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, it is sequentially added into 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 N, N-dimethyl formyls
Amine, nitrogen is protected and after 80 DEG C of reactions 2 hours, is down to room temperature, in precipitating to acetone, filters and collect product, at 60 DEG C
It is vacuum dried 20 hours, obtains beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole；
Described epoxy-capped polyetheramine is prepared from by following methods:
In the three-necked bottle that 100mL is dried, it is sequentially added into the benzylamine of epoxy resin E51,0.24mol of 100 grams and 500 grams
Propylene glycol monomethyl ether, logical nitrogen protection magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to room
Temperature, and pour into rapidly in 150mL deionized water, obtain a large amount of solid precipitation；After this product of deionized water cyclic washing, sucking filtration
And collected polymer, in vacuum drying oven, 60 DEG C are dried 20 hours, obtain epoxy-capped polyetheramine.
Embodiment 7
By zinc powder 20 parts, Pulvis Talci 15 parts, vanadium dioxide 15 parts, water nano resin octaphenyl cage modle polysilsesquioxane
Modification sulphonation polyimides 30 parts, polyoxyethylene polyoxy propanol amidogen ether 3 parts, KH-550 8 parts, graphene oxide 4 parts, positive silicic acid
Ethyl ester 40 parts and DMF 15 parts are poured in pill tank, dispersator be stirred, mixing speed control
System is at 400 revs/min, and mixing time is 15 minutes, obtains component A；
Beta-schardinger dextrin-modified amido is blocked sulfonate polybenzimidazole 8 parts, epoxy-capped polyetheramine 20 parts, nanometer titanium dioxide
Silicon 40 parts, silica flour 18, epoxy resin E51 45 parts, KH-560 8 parts, ethylene glycol 8 parts and tetramethylolmethane 8 parts pour dispensing into
In cylinder, dispersator being stirred, mixing speed controls at 1000 revs/min, and mixing time is 30 minutes, obtains component B；
It is to mix at 15: 3 by weight with component B by described component A, obtains water nano resin outdoor ultra-thin steel structure
Fireproof coating；
Wherein said water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides is by following methods
It is prepared from:
In the three-necked bottle that 100mL is dried, it is sequentially added into 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 anhydrides, 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 precipitation；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C are dried 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, then in described amino-terminated sulfonated polyimide pre-polymer solution, add poly-times of octaphenyl cage modle
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, in precipitating to water, filters and collect product,
It is vacuum dried 10 hours at 60 DEG C, obtains water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyamides sub-
Amine；
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-amino isophthalic acid of 0.02 mole and the 5-sulfonic group M-phthalic acid of 0.08 mole are joined
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, in precipitating to water, then neutralizes with ammonia, mistake
Filter and collect product, being vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, it is sequentially added into 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 N, N-dimethyl formyls
Amine, nitrogen is protected and after 80 DEG C of reactions 2 hours, is down to room temperature, in precipitating to acetone, filters and collect product, at 60 DEG C
It is vacuum dried 20 hours, obtains beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole；
Described epoxy-capped polyetheramine is prepared from by following methods:
In the three-necked bottle that 100mL is dried, it is sequentially added into the benzylamine of epoxy resin E51,0.24mol of 100 grams and 500 grams
Propylene glycol monomethyl ether, logical nitrogen protection magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to room
Temperature, and pour into rapidly in 150mL deionized water, obtain a large amount of solid precipitation；After this product of deionized water cyclic washing, sucking filtration
And collected polymer, in vacuum drying oven, 60 DEG C are dried 20 hours, obtain epoxy-capped polyetheramine.
Embodiment 8
By zinc powder 20 parts, Pulvis Talci 15 parts, vanadium dioxide 15 parts, water nano resin octaphenyl cage modle polysilsesquioxane
Modification sulphonation polyimides 30 parts, polyoxyethylene polyoxy propanol amidogen ether 3 parts, N, N-lupetazin 3 parts, KH-550 8 parts, oxygen
Functionalized graphene 4 parts, tetraethyl orthosilicate 40 parts and DMF 15 parts are poured in pill tank, dispersator enter
Row stirring, mixing speed controls at 400 revs/min, and mixing time is 15 minutes, obtains component A；
Beta-schardinger dextrin-modified amido is blocked sulfonate polybenzimidazole 8 parts, nano silicon 40 parts, silica flour 18, ring
Epoxy resins E51 45 parts, KH-560 8 parts, 1,12-dibromo-dodecane 8 parts, ethylene glycol 8 parts and tetramethylolmethane 8 parts pour dispensing into
In cylinder, dispersator being stirred, mixing speed controls at 1000 revs/min, and mixing time is 30 minutes, obtains component B；
It is to mix at 15: 3 by weight with component B by described component A, obtains water nano resin outdoor ultra-thin steel structure
Fireproof coating；
Wherein said water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides is by following methods
It is prepared from:
In the three-necked bottle that 100mL is dried, it is sequentially added into 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 anhydrides, 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 precipitation；After this product of methanol cyclic washing, sucking filtration collected polymer,
In vacuum drying oven, 60 DEG C are dried 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, then in described amino-terminated sulfonated polyimide pre-polymer solution, add poly-times of octaphenyl cage modle
Half siloxanes 5g, after nitrogen is protected and heated up 210 DEG C and react 5 hours, is down to room temperature, in precipitating to water, filters and collect product,
It is vacuum dried 10 hours at 60 DEG C, obtains water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyamides sub-
Amine；
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-amino isophthalic acid of 0.02 mole and the 5-sulfonic group M-phthalic acid of 0.08 mole are joined
In reactant liquor, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, in precipitating to water, then neutralizes with ammonia, mistake
Filter and collect product, being vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, it is sequentially added into 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 N, N-dimethyl formyls
Amine, nitrogen is protected and after 80 DEG C of reactions 2 hours, is down to room temperature, in precipitating to acetone, filters and collect product, at 60 DEG C
It is vacuum dried 20 hours, obtains beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
Test condition
Embodiment 1-8 gained water nano resin outdoor super-thin steel structure fire-proof paint is coated in outdoor steel structure
On, and test performance, to test by GB14907-2002 " fire-resistant coating for steel structure ", test result is shown in Table 1.
According to GB/14907-2002 standard testing, particularly as follows:
1, surface drying time answers≤8h
2, crack resistance: occur without crackle
3, adhesion strength >=0.2Mpa
4, resistance to water: after 24h, coating does not ftractures, aliquation, obscission
5, cold-hot cyclicity/number of times: after 15 times, coating does not ftractures, aliquation, obscission
6, fire endurance: coating layer thickness is 2mm, and fire endurance is not less than 1h
Test result is shown in Table 1.
Table 1
Data above is it can be seen that gather with not using epoxy-capped polyetheramine and the end-blocking sulfonation of beta-schardinger dextrin-modified amido
The coating of benzimidazole is compared, and the coating of the present invention has obvious better performance, is thus provided that the Advantageous of the present invention
Effect.
Claims (5)
1. a water nano resin outdoor super-thin steel structure fire-proof paint, it is characterised in that be made up of component A and component B,
By weight, described component A is 15: 5～1 with the weight ratio of component B；Each component prepare raw material by weight, as follows:
Component A: zinc powder 15～20 parts, Pulvis Talci 10～15 parts, vanadium dioxide 10～15 parts, water nano resin octaphenyl cage modle
Polysilsesquioxane modification sulphonation polyimides 15～30 parts, polyoxyethylene polyoxy propanol amidogen ether 0.5～3 parts, N, N-dimethyl
Piperazine 1～5 parts, KH-550 1～10 parts, graphene oxide 1～5 parts, tetraethyl orthosilicate 30～50 parts and N, N-dimethyl methyl
Amide 10～20 parts；
Component B: beta-schardinger dextrin-modified amido blocks sulfonate polybenzimidazole 5-10 part, epoxy-capped polyetheramine 15～30 parts, receives
Rice silicon dioxide 30～50 parts, silica flour 15～20, epoxy resin E51 40～50 parts, KH-560 1～10 parts, 1,12-dibromo
Dodecane 5～10 parts, ethylene glycol 5～10 parts and tetramethylolmethane 1～10 parts.
A kind of water nano resin outdoor the most according to claim 1 super-thin steel structure fire-proof paint, it is characterised in that
Described water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides is prepared from by following methods:
In the three-necked bottle that 100mL is dried, it is sequentially added into 1.6mmol 2,2 '-bis-(4-sulfonic benzo epoxide) benzidines,
12.5mL m-creso1 and 0.8mL triethylamine, logical nitrogen protection magnetic agitation；Treat that 2,2 '-bis-(4-sulfonic benzo epoxides) join
After phenylenediamine is completely dissolved, sequentially add 1.55mmol 3,4,9,10-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；After reaction terminates, it is down to room temperature, and fast
Speed is poured in 150mL methanol, obtains a large amount of solid precipitation；After this product of methanol cyclic washing, sucking filtration collected polymer, in
In vacuum drying oven, 60 DEG C are dried 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, then in described amino-terminated sulfonated polyimide pre-polymer solution, 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, in precipitating to water, filters and collect product, in 60 DEG C
Lower vacuum drying 10 hours, obtains water nano resin octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides.
A kind of water nano resin outdoor the most according to claim 1 super-thin steel structure fire-proof paint, 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-amino isophthalic acid of 0.02 mole and the 5-sulfonic group M-phthalic acid of 0.08 mole are joined reaction
In liquid, nitrogen is protected and after 210 DEG C of reactions 15 hours, is down to room temperature, in precipitating to water, then neutralizes with ammonia, filters also
Collect product, be vacuum dried 10 hours at 120 DEG C, obtain amino-terminated sulfonate polybenzimidazole；
In 500 milliliters of three-necked bottles, be sequentially added into 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 DMFs, nitrogen
Gas shielded and 80 DEG C reaction 2 hours after, be down to room temperature, in precipitating to acetone, filter and collect product, at 60 DEG C vacuum do
Dry 20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
A kind of water nano resin outdoor the most according to claim 1 super-thin steel structure fire-proof paint, it is characterised in that
Described epoxy-capped polyetheramine is prepared from by following methods:
In the three-necked bottle that 100mL is dried, it is sequentially added into the benzylamine of epoxy resin E51,0.24mol of 100 grams and 500 grams the third two
Alcohol methyl ether, logical nitrogen protection magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to room temperature,
And pour into rapidly in 150mL deionized water, obtain a large amount of solid precipitation；After this product of deionized water cyclic washing, sucking filtration is also
Collected polymer, in vacuum drying oven, 60 DEG C are dried 20 hours, obtain epoxy-capped polyetheramine.
5. according to the preparation of the water nano resin outdoor super-thin steel structure fire-proof paint according to any one of claim 1-4
Method, it is characterised in that comprise the following steps:
By zinc powder 15～20 parts, Pulvis Talci 10～15 parts, vanadium dioxide 10～15 parts, poly-times of water nano resin octaphenyl cage modle
Half silicone-modified sulfonated polyimide 15～30 parts, polyoxyethylene polyoxy propanol amidogen ether 0.5～3 parts, N, N-lupetazin 1
～5 parts, KH-550 1～10 parts, graphene oxide 1～5 parts, tetraethyl orthosilicate 30～50 parts and N,N-dimethylformamide
Pouring in pill tank, dispersator be stirred for 10～20 parts, mixing speed controls, at 300 revs/min-500 revs/min, to stir
The time of mixing is 15 minutes, obtains component A；
By beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole 5-10 part, epoxy-capped polyetheramine 15～30 parts, nanometer two
Silicon oxide 30～50 parts, silica flour 15～20, epoxy resin E51 40～50 parts, KH-560 1～10 parts, 1,12-dibromo 12
Alkane 5～10 parts, ethylene glycol 5～10 parts and tetramethylolmethane 1～10 parts are poured in pill tank, dispersator be stirred,
Mixing speed controls at 800 revs/min-1000 revs/min, and mixing time is 30 minutes, obtains component B；
It is 15: 5～1 to mix by weight with component B by described component A, obtains water nano resin outdoor ultra-thin steel structure
Fireproof coating.
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Effective date of registration: 20181119 Address after: 675000 Chuxiong Small and Medium-sized Enterprise Center, Chuxiong, east of Chufeng Court, Sunshine Avenue, Lucheng Town, Chuxiong City, Chuxiong Yi Autonomous Prefecture, Yunnan Province, 6-5 Applicant after: Chuxiong Youlin Sheng Technology Co., Ltd. Address before: 100024 Beijing Chaoyang District Wuliqiao 1st Street Courtyard Non-Center 7th Floor, 3rd Floor Applicant before: Beijing you Linsheng Technology Co. Ltd. |
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