A kind of timber structure transparent fire-resisting paint
Technical field
The invention belongs to technical field of coatings, more particularly it relates to an timber structure transparent fire-resisting paint.
Background technology
Coating fireproof coating is the most best fire retarding wood protection means, can reach the resistance to combustion of prolonging wood when timber is by fire
Time, slow down the purpose of fire spreading, in order to have time enough to put out a fire to save life and property, reduce the loss that fire causes as far as possible.Existing
Have in technology, in order to improve flame retardant effect, typically realized containing the inorganic fire auxiliary agent of the elements such as P, Si, B, N by interpolation, anti-
The film transparency of fire coating can weaken, and even destroys the pattern that base material is original, and for timber structure fireproof coating,
Its dicoration wants the factor that emphasis considers exactly: timber is generally used for building, historical relic's protection, building decoration and top-grade furniture,
And these building materials have the highest requirement in terms of keeping original pattern, therefore the dicoration of fire retarding wood protection coating is also required that very
High.If but only consider it ornamental and reduce the addition of fire proofing additive, the fire protecting performance of fireproof coating will be made not reach requirement,
Cause fire hazard to can not get effectively to control.The research and development of the transparent fire-resisting paint therefore having fire prevention and decoration functions concurrently is subject to
To great concern both domestic and external.At present, transparent finishing fire retardant paint both domestic and external is still at an early stage, sells on the market
This type of coating fewer, it is possible to real put into the most rare of reality application.Limit transparent finishing fire retardant paint actual should
A big factor be the pliability of film and weatherability the poorest, easily there is film cracking after being coated on base material solidification in coating
Etc. phenomenon, if adding inorganic fire auxiliary agent to improve flame retardant effect, the cracking of film can be further exacerbated by.
Hence it is highly desirable to by the improvement of formula, obtain that pliability is good, weatherability is strong, fire protecting performance good and decoration merit
The transparent fire-resisting paint that energy is good.
Summary of the invention
In order to solve the problems referred to above, one aspect of the present invention provides a kind of timber structure transparent fire-resisting paint, by A, B, C group
Becoming, the mass ratio of described A, B, C is 1:(0.1~0.5): (0.1~0.4);
In described A, the mass fraction of each component is: waterglass 50~70 parts, deionized water 15~25 parts, kieselguhr 15~
50 parts, polyoxyethylene polyoxy propanol amidogen ether 0.5~3 parts, N, N-lupetazin 1~5 parts, octaphenyl cage modle polysilsesquioxane
Modification sulphonation polyimides 15~30 parts;
In described B, the mass fraction of each component is: tetraethyl orthosilicate 60~80 parts, KH-560 15~30 parts, 1,12-bis-
Bromo-dodecane 5~10 parts, dimethyl sulfoxide 5-10 part, beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole 5-10 part;
In described C, the mass fraction of each component is: nano titanium oxide 30~50 parts, graphene oxide 1~5 parts, diformazan
Base sulfoxide 10~20 parts, ethylene glycol 5~10 parts, sodium hydroxide 0.01~0.1 part, KH-550 5~10 parts.
In one embodiment, described 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 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
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 dimethyl sulfoxide, nitrogen
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, in precipitating to acetone, filter and collect product, being vacuum dried at 60 DEG C
20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
The preparation method of the timber structure transparent fire-resisting paint described in another aspect of the present invention offer, comprises the following steps:
(1) by waterglass 50~70 parts, kieselguhr 15~50 parts, polyoxyethylene polyoxy propanol amidogen ether 0.5~3 parts, N, N-
Lupetazin 1~5 parts and octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides 15~30 parts mix with mixer
After closing uniformly, join in 15~25 parts of deionized waters, be component A, stand-by;
(2) by tetraethyl orthosilicate 60~80 parts, KH-560 15~30 parts, 1,12-dibromo-dodecane 5~10 parts, dimethyl
Sulfoxide 5-10 part, beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole 5-10 part is used mixer mix homogeneously, is B group
Point, stand-by;
(3) by nano titanium oxide 30~50 parts, graphene oxide 1~5 parts, ethylene glycol 5~10 parts, sodium hydroxide 0.01
~0.1 part, KH-550 5~10 parts, with after mixer mix homogeneously, join in 10~20 parts of dimethyl sulfoxide, are C group
Point, stand-by;
(4) A, B, C mix homogeneously is i.e. obtained a kind of timber structure transparent fire-resisting paint.
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, thermostability and fire resistance, studies have found that, in the system of the present invention, it can not well disperse, it is easy to group
Poly-, 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 to be positioned at side chain and rigidity strong, considerably increase the distance of strand, and with
The polyimides of good weatherability matches, and can be greatly improved fire protecting performance and the weatherability of system.Additionally, introduce at side chain
Phenylate structure, both can improve wearability, and a large amount of sulfonic existence can significantly reduce the content of free calcium hydroxide in material,
Play the generation of the accumulation of salt in the surface soil phenomenon on suppression cement mortar surface, sulfonic water absorption, it is also possible to prevent system the most crisp, thus put forward
Supply the Advantageous Effects of the present invention.
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.
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.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
(1) by waterglass 60 parts, 40 parts of kieselguhr, polyoxyethylene polyoxy propanol amidogen ether 2 parts, N, N-lupetazin 3 parts
And octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides 20 parts is with after mixer mix homogeneously, joins 20 parts and goes
In ionized water, it is component A, stand-by;
(2) by tetraethyl orthosilicate 70 parts, KH-560 18 parts, 1,12-dibromo-dodecane 8 parts, dimethyl sulfoxide 8 parts, β-ring
Dextrin modified amino-terminated sulfonate polybenzimidazole 8 parts uses mixer mix homogeneously, is B component, stand-by;
(3) by nano titanium oxide 40 parts, graphene oxide 3 parts, ethylene glycol 8 parts, sodium hydroxide 0.08 part, KH-550 8
Part, with after mixer mix homogeneously, joins in 15 parts of dimethyl sulfoxide, is component C, stand-by;
(4) A, B, C mix homogeneously is i.e. obtained a kind of timber structure transparent fire-resisting paint;
Wherein, described 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) 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 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-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 dimethyl sulfoxide, nitrogen
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, in precipitating to acetone, filter and collect product, being vacuum dried at 60 DEG C
20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
Described timber structure transparent fire-resisting paint is coated on timber structure, completes construction.
Embodiment 2
(1) by waterglass 60 parts, 40 parts of kieselguhr, polyoxyethylene polyoxy propanol amidogen ether 2 parts, N, N-lupetazin 3 parts
And octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides 20 parts is with after mixer mix homogeneously, joins 20 parts and goes
In ionized water, it is component A, stand-by;
(2) by tetraethyl orthosilicate 70 parts, KH-560 18 parts, 1,12-dibromo-dodecane 8 parts, dimethyl sulfoxide 8 parts, β-ring
Dextrin modified amino-terminated sulfonate polybenzimidazole 8 parts uses mixer mix homogeneously, is B component, stand-by;
(3) by nano titanium oxide 40 parts, graphene oxide 3 parts, ethylene glycol 8 parts, sodium hydroxide 0.08 part, KH-550 8
Part, with after mixer mix homogeneously, joins in 15 parts of dimethyl sulfoxide, is component C, stand-by;
(4) A, B, C mix homogeneously is i.e. obtained a kind of timber structure transparent fire-resisting paint;
Wherein, described 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 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, 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 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-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 dimethyl sulfoxide, nitrogen
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, in precipitating to acetone, filter and collect product, being vacuum dried at 60 DEG C
20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
Described timber structure transparent fire-resisting paint is coated on timber structure, completes construction.
Embodiment 3
(1) by waterglass 60 parts, 40 parts of kieselguhr, polyoxyethylene polyoxy propanol amidogen ether 2 parts, N, N-lupetazin 3 parts
And octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides 20 parts is with after mixer mix homogeneously, joins 20 parts and goes
In ionized water, it is component A, stand-by;
(2) by tetraethyl orthosilicate 70 parts, KH-560 18 parts, 1,12-dibromo-dodecane 8 parts, dimethyl sulfoxide 8 parts, β-ring
Dextrin modified amino-terminated sulfonate polybenzimidazole 8 parts uses mixer mix homogeneously, is B component, stand-by;
(3) by nano titanium oxide 40 parts, graphene oxide 3 parts, ethylene glycol 8 parts, sodium hydroxide 0.08 part, KH-550 8
Part, with after mixer mix homogeneously, joins in 15 parts of dimethyl sulfoxide, is component C, stand-by;
(4) A, B, C mix homogeneously is i.e. obtained a kind of timber structure transparent fire-resisting paint;
Wherein, described 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) 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 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 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 dimethyl sulfoxide, nitrogen
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, in precipitating to acetone, filter and collect product, being vacuum dried at 60 DEG C
20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
Described timber structure transparent fire-resisting paint is coated on timber structure, completes construction.
Embodiment 4
(1) by waterglass 60 parts, 40 parts of kieselguhr, polyoxyethylene polyoxy propanol amidogen ether 2 parts, N, N-lupetazin 3 parts
And octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides 20 parts is with after mixer mix homogeneously, joins 20 parts and goes
In ionized water, it is component A, stand-by;
(2) by tetraethyl orthosilicate 70 parts, KH-560 18 parts, 1,12-dibromo-dodecane 8 parts, 8 parts of use of dimethyl sulfoxide are mixed
Conjunction machine mix homogeneously, is B component, stand-by;
(3) by nano titanium oxide 40 parts, graphene oxide 3 parts, ethylene glycol 8 parts, sodium hydroxide 0.08 part, KH-550 8
Part, with after mixer mix homogeneously, joins in 15 parts of dimethyl sulfoxide, is component C, stand-by;
(4) A, B, C mix homogeneously is i.e. obtained a kind of timber structure transparent fire-resisting paint;
Wherein, described 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) 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 octaphenyl cage modle polysilsesquioxane modification sulphonation polyimides.
Described timber structure transparent fire-resisting paint is coated on timber structure, completes construction.
Embodiment 5
(1) by waterglass 60 parts, 40 parts of kieselguhr, polyoxyethylene polyoxy propanol amidogen ether 2 parts, N, N-lupetazin 3 parts
And polyvinyl alcohol 20 parts is with after mixer mix homogeneously, joins in 20 parts of deionized waters, is component A, stand-by;
(2) by tetraethyl orthosilicate 70 parts, KH-560 18 parts, 1,12-dibromo-dodecane 8 parts, dimethyl sulfoxide 8 parts, β-ring
Dextrin modified amino-terminated sulfonate polybenzimidazole 8 parts uses mixer mix homogeneously, is B component, stand-by;
(3) by nano titanium oxide 40 parts, graphene oxide 3 parts, ethylene glycol 8 parts, sodium hydroxide 0.08 part, KH-550 8
Part, with after mixer mix homogeneously, joins in 15 parts of dimethyl sulfoxide, is component C, stand-by;
(4) A, B, C mix homogeneously is i.e. obtained a kind of timber structure transparent fire-resisting paint;
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 dimethyl sulfoxide, nitrogen
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, in precipitating to acetone, filter and collect product, being vacuum dried at 60 DEG C
20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
Described timber structure transparent fire-resisting paint is coated on timber structure, completes construction.
Embodiment 6
(1) by waterglass 60 parts, 40 parts of kieselguhr, polyoxyethylene polyoxy propanol amidogen ether 2 parts, N, N-lupetazin 3 parts
And polyvinyl alcohol 20 parts is with after mixer mix homogeneously, joins in 20 parts of deionized waters, is component A, stand-by;
(2) by tetraethyl orthosilicate 70 parts, KH-560 18 parts, 1,12-dibromo-dodecane 8 parts, 8 parts of use of dimethyl sulfoxide are mixed
Conjunction machine mix homogeneously, is B component, stand-by;
(3) by nano titanium oxide 40 parts, graphene oxide 3 parts, ethylene glycol 8 parts, sodium hydroxide 0.08 part, KH-550 8
Part, with after mixer mix homogeneously, joins in 15 parts of dimethyl sulfoxide, is component C, stand-by;
(4) A, B, C mix homogeneously is i.e. obtained a kind of timber structure transparent fire-resisting paint.
Described timber structure transparent fire-resisting paint is coated on timber structure, completes construction.
Embodiment 7
(1) by waterglass 60 parts, 40 parts of kieselguhr, polyoxyethylene polyoxy propanol amidogen ether 2 parts and poly-times of octaphenyl cage modle
Half silicone-modified sulfonated polyimide 20 parts, with after mixer mix homogeneously, joins in 20 parts of deionized waters, is A group
Point, stand-by;
(2) by tetraethyl orthosilicate 70 parts, KH-560 18 parts, dimethyl sulfoxide 8 parts, beta-schardinger dextrin-modified amido end-blocking sulphur
Change polybenzimidazoles 8 parts and use mixer mix homogeneously, be B component, stand-by;
(3) by nano titanium oxide 40 parts, graphene oxide 3 parts, ethylene glycol 8 parts, sodium hydroxide 0.08 part, KH-550 8
Part, with after mixer mix homogeneously, joins in 15 parts of dimethyl sulfoxide, is component C, stand-by;
(4) A, B, C mix homogeneously is i.e. obtained a kind of timber structure transparent fire-resisting paint;
Wherein, described 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) 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 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-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 dimethyl sulfoxide, nitrogen
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, in precipitating to acetone, filter and collect product, being vacuum dried at 60 DEG C
20 hours, obtain beta-schardinger dextrin-modified amido end-blocking sulfonate polybenzimidazole.
Described timber structure transparent fire-resisting paint is coated on timber structure, completes construction.
Method of testing
According to GB 12441-2005 standard testing, particularly as follows:
1, surface drying time answers≤5h
2, adhesive force/level :≤3
3, resistance to impact/cm: >=20
4, after resistance to water/h:24h, coating is wrinkle resistant, does not falls off
5, after humidity resistance/h:48h, coating is non-foaming, does not falls off
6, resistance to combustion time/min: >=15
Antifriction performance: (89, method of testing is to use ethanol wear-resistant tester, adds 500g weight by standard GB/T1768 79
Counterweight, infiltrates the ethanol of 99.7% concentration, rubs back and forth with white cotton, and recording ink starts number of times when destroying.
Test result is shown in Table 1.
Table 1
Test event |
Embodiment 1 |
Embodiment 2 |
Embodiment 3 |
Embodiment 4 |
Embodiment 5 |
Embodiment 6 |
Embodiment 7 |
Surface drying time/h |
1.5 |
1.6 |
1.4 |
2.8 |
3.0 |
6.1 |
2.0 |
Adhesive force/level |
1 |
1 |
1 |
1 |
1 |
2 |
1 |
Resistance to impact/cm |
27 |
27 |
27 |
24 |
21 |
15 |
24 |
Resistance to water/h |
108 |
99 |
97 |
57 |
43 |
20 |
72 |
Humidity resistance/h |
211 |
193 |
185 |
77 |
69 |
35 |
92 |
Resistance to combustion time/min |
41 |
35 |
37 |
26 |
20 |
10 |
39 |
Antifriction performance/number of times |
1662 |
1467 |
1521 |
834 |
705 |
138 |
1009 |
Data above it 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 of
This provides the Advantageous Effects of the present invention.