CN106752941B - A kind of construction timber transparent fire-resisting paint - Google Patents
A kind of construction timber transparent fire-resisting paint Download PDFInfo
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- CN106752941B CN106752941B CN201710027745.0A CN201710027745A CN106752941B CN 106752941 B CN106752941 B CN 106752941B CN 201710027745 A CN201710027745 A CN 201710027745A CN 106752941 B CN106752941 B CN 106752941B
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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
- C09D187/00—Coating compositions based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
- C09D187/005—Block or graft polymers not provided for in groups C09D101/00 - C09D185/04
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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
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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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
- C09D5/18—Fireproof paints including high temperature resistant paints
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
Abstract
The invention discloses a kind of construction timber transparent fire-resisting paints, are made of A, B, C, each component in the A are as follows: waterglass, deionized water, modified calcium carbonate, polyoxyethylene polyoxy propyl alcohol amidogen ether, sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer；Each component in the B are as follows: ethyl orthosilicate part, 2,2', 2 ", 2 " '-[1,2- ethanetetrayl four (4,1- phenylene methylene oxygen)] tetraoxane, bromo- 1, the 2- oxepane of 6-, ethyl alcohol；Each component in the C are as follows: modified manometer silicon dioxide, dimethyl sulfoxide, ethylene glycol, KH-550, N, N'- carbonyl dimidazoles.
Description
Technical field
The invention belongs to technical field of coatings, more particularly it relates to a kind of construction timber transparent fire-resisting paint.
Background technique
Currently, coating fireproof coating is best construction timber fire prevention means, extension wood can achieve when timber is by fire
The material resistance to combustion time, slow down the purpose of fire spreading, to there is time enough to save, is damaged caused by reduction fire as far as possible
It loses.In the prior art, in order to improve flame retardant effect, generally by inorganic fire auxiliary agent of the addition containing elements such as P, Si, B, N come real
Existing, the film transparency of fireproof coating can be weakened, or even destroy the original pattern of substrate, and for timber structure fireproof coating
For, dicoration exactly wants the factor of emphasis consideration: timber is generally used for building, historical relic's protection, building decoration and top grade
Furniture, and these building materials have very high requirement in terms of keeping original pattern, therefore also want to the dicoration of fire retarding wood protection coating
Ask very high.If but only consider that it is decorative and reduce the addition of fire proofing additive, the fire protecting performance of fireproof coating will be made to be not achieved
It is required that causing fire hazard that cannot effectively control.Therefore have both fire prevention and decoration functions transparent fire-resisting paint research and
Exploitation is by great concern both domestic and external.Currently, transparent finishing fire retardant paint both domestic and external is still at an early stage, market
Such coating of upper sale is fewer, can really put into the more rare of practical application.Limit transparent finishing fire retardant paint
The big factor of the one of practical application is that the flexibility, weatherability and anti-microbial property of film are too poor, and coating, which is coated on substrate, to be solidified
After phenomena such as being easy to appear film cracking, if film can be further exacerbated by order to improve if inorganic fire auxiliary agent is added in flame retardant effect
Cracking.
Hence it is highly desirable to obtain that flexibility is good, weatherability is strong, fire protecting performance is good by the improvement of formula and decorate function
The good transparent fire-resisting paint of energy.
Summary of the invention
To solve the above-mentioned problems, one aspect of the present invention provides a kind of construction timber transparent fire-resisting paint, special
Sign is, is made of A, B, C, and the mass ratio of described A, B, C are 1:(0.1~0.5): (0.1~0.5)；
The mass fraction of each component in the A are as follows: 50~80 parts of waterglass, 10~30 parts of deionized water, modified calcium carbonate
15~50 parts, 1~3 part of amidogen ether of polyoxyethylene polyoxy propyl alcohol, sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat ternary is total
15~30 parts of polymers；
The mass fraction of each component in the B are as follows: 60~80 parts of ethyl orthosilicate, 2,2', 2 ", 2 " '-[1,2- union II Asias
Methyl four (4,1- phenylene methylene oxygen)] 15~30 parts of tetraoxane, 5~10 parts of bromo- 1, the 2- oxepane of 6-, ethyl alcohol 5-10
Part；
The mass fraction of each component in the C are as follows: 30~50 parts of modified manometer silicon dioxide, dimethyl sulfoxide 10~20
Part, 5~10 parts of ethylene glycol, 5~10 parts of KH-550, N, 1~5 part of N'- carbonyl dimidazoles；
Wherein, the modified calcium carbonate the preparation method comprises the following steps:
(1) bromine sealing end polyquaternium is prepared
In 1000ml dry three-necked bottle, 1,12- dibromo-dodecane 0.1mol, Isosorbide-5-Nitrae-lupetazin is added
0.092mol and solvent dimethyl sulfoxide 80ml, after reacting 5 hours at 50 DEG C, add N- methylimidazole 0.0025mol with
And N-methylmorpholine 0.0025mol, after reacting 5 hours at 50 DEG C, vacuum distillation removal solvent obtains bromine sealing end polyquaternium；
(2) amino-terminated polyetheramine is prepared
In 1000mL dry three-necked bottle, sequentially add 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams
Dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to room
Temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water, take out
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain amino-terminated polyetheramine；
(3) modified calcium carbonate is prepared
In 100ml three-necked bottle, the ammonia that bromine sealing end 0.4 gram of polyquaternium, the step (2) that step (1) obtains obtain is added
1.3 grams of base end capped polyether amine and dimethyl sulfoxide 50ml, are stirred to polymer at room temperature after being completely dissolved, and are sequentially added average
3 grams of the calcium carbonate of 2000 mesh of partial size, 3 grams of the calcium carbonate of 2500 mesh of average grain diameter, 3000 mesh of average grain diameter 2 grams of calcium carbonate, flat
2 grams of the calcium carbonate of equal 800 mesh of partial size and 1 gram of cylite, after stirring 5 hours at 60 DEG C of heating, are down to room temperature, filter and collect
Solid product, in vacuum drying oven, 50 DEG C drying 24 hours, obtain modified calcium carbonate；
The modified manometer silicon dioxide the preparation method comprises the following steps:
(1) epoxy-capped polyetheramine is prepared
In 1000mL dry three-necked bottle, the benzylamine and 700 of 100 grams epoxy resin E51,0.25mol are sequentially added
Gram dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to
Room temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water,
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain epoxy-capped polyetheramine；
(2) modified manometer silicon dioxide is prepared
In 100ml three-necked bottle, 0.5 gram of epoxy-capped polyetheramine and dimethyl sulfoxide that step (1) obtains is added
20ml is stirred to polymer at room temperature after being completely dissolved, and 5 grams of silica of 300 nanometers of average grain diameter is added, at 60 DEG C of heating
Stirring 5 hours after, be down to room temperature, filter and collect solid product, in vacuum drying oven, 50 DEG C drying 24 hours, be modified
Nano silica.
In one embodiment, the system of the sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer
Preparation Method are as follows:
(1) amino-terminated polyetheramine is prepared
In 1000mL dry three-necked bottle, sequentially add 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams
Dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to room
Temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water, take out
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain amino-terminated polyetheramine；
(2) amino-terminated polybenzimidazoles is prepared
By the 3 of 0.1mol, 3 ', 4,4 '-tetramino benzophenone, 0.03mol 5- sulfonic acid M-phthalic acid and
The adipic acid of 0.065mol is dissolved in 300g polyphosphoric acids, leads to nitrogen protection after 0.5 hour, is warming up to 180 DEG C of reactions for 24 hours
Afterwards, reaction solution is poured into ice water, then neutralizing the aqueous solution to PH with sodium hydroxide is 5, then filters and uses deionized water
This is finally deposited in vacuum drying oven 80 DEG C of dry l0h to get amino-terminated polyphenyl and miaow by the precipitating washed repeatedly
Azoles；
(3) hyperbranched poly pyrrole throat is prepared
In 100mL dry three-necked bottle, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) benzene are sequentially added
Three acid anhydrides and 25ml metacresol, are stirred under nitrogen protection, and after three acid anhydrides are completely dissolved, 0.006 mole of 3,3 '-diamino are added
Benzidine after 60min is stirred at room temperature, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction,
It is down to room temperature, and is poured into rapidly in 2000mL methanol, a large amount of solid precipitatings are obtained；After washing the product repeatedly with methanol, filter
And collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours to get the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
(4) polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer is prepared
In 100mL dry three-necked bottle, 1 gram of the amino-terminated polyetheramine, 0.4 gram of the naphthalene anhydride are sequentially added
Terminated hyperbranched poly- pyrrole throat, 0.2 gram of the amino-terminated polybenzimidazoles, 10mL dimethyl sulfoxide and 10mL between first
Phenol after stirring 60min under nitrogen protection, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction,
It is down to room temperature, and is poured into rapidly in 2000mL methanol, a large amount of solid precipitatings are obtained；After washing the product repeatedly with methanol, filter
And collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours to get polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat three
Membered copolymer；
(5) sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer is prepared
In 100mL dry three-necked bottle, 1 gram of the polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat is sequentially added
The concentrated sulfuric acid of the mass fraction 98% of terpolymer and 10mL after stirring 180min at 40 DEG C, pours under nitrogen protection
In ice water, after washing the product repeatedly with ice water, filter and collected polymer, in vacuum drying oven, 60 DEG C drying 24 hours be
Obtain sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer.
Compared with prior art, the invention has the benefit that
1, the addition of sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer, can provide it is excellent at
Film properties, improve the weatherability, intensity and flame retardant property of coating, to provide advantageous effects of the invention.
2, the addition of modified calcium carbonate and modified manometer silicon dioxide can be improved the rigidity of system, crosslink density, fill out
Material dispersibility, anti-microbial property and fire resistance, to provide advantageous effects of the invention.
3,2,2', 2 ", 2 " '-[1,2- ethanetetrayl four (4,1- phenylene methylene oxygen)] tetraoxanes, 6- bromo- 1,
2- oxepane and N, the addition of N'- carbonyl dimidazoles can further effectively improve the crosslink density of system, when shortening surface drying
Between, enhance the intensity and water resistance of coating, to provide advantageous effects of the invention.
Specific embodiment
Raw material:
Waterglass (300 mesh of granularity) is purchased from Jinan Te Xing Chemical Co., Ltd..The calcium carbonate of 2000 mesh of average grain diameter is averaged
The calcium carbonate of 2500 mesh of partial size, the calcium carbonate of 800 mesh of calcium carbonate and average grain diameter of 3000 mesh of average grain diameter are contained purchased from Jiangxi
Safe chemical industry.The silica that 300 nanometers of average grain diameter is purchased from win wound Degussa.(BAPE is nitrogenous for polyoxyethylene polyoxy propyl alcohol amidogen ether
Polyether antifoam agent) it is purchased from Shanghai De Mao, model K12.3,3 '-diaminobenzidines are purchased from CTI, and directly use, and are not necessarily to
It is further purified.Epoxy silane coupling agent KH-560 is purchased from Sinopharm Chemical Reagent Co., Ltd..1,3,5- tri- (4- naphthalene oxygen
Base -1,8- diacid) benzene three acid anhydride according to method disclosed in patent CN101270111B prepare.Other raw materials are purchased from Aladdin reagent
Co., Ltd.
Embodiment 1
(1) by 65 grams of waterglass, 35 grams of modified calcium carbonate, 2 grams of polyoxyethylene polyoxy propyl alcohol amidogen ether and sulfonated polyether amine-
Polybenzimidazoles -26 grams of terpolymer of hyperbranched poly pyrrole throat after mixing, is added in 20 grams of deionized waters with mixing machine,
As component A, for use；
(2) by 70 grams of ethyl orthosilicate, 2,2', 2 ", 2 " '-[1,2- ethanetetrayls four (4,1- phenylene methylene oxygen)]
20 grams of tetraoxane, 9 grams of 8 grams of bromo- 1, the 2- oxepane of 6- and ethyl alcohol are uniformly mixed with mixing machine, as B component, to
With；
(3) by 35 grams of modified manometer silicon dioxide, 7 grams of ethylene glycol, 8 grams of KH-550 and 3 grams of N, N'- carbonyl dimidazoles
After mixing with mixing machine, it is added in 15 grams of dimethyl sulfoxides, as component C, for use；
(4) A, B, C are uniformly mixed up to a kind of timber structure transparent fire-resisting paint；
Wherein, the modified calcium carbonate the preparation method comprises the following steps:
(1) bromine sealing end polyquaternium is prepared
In 1000ml dry three-necked bottle, 1,12- dibromo-dodecane 0.1mol, Isosorbide-5-Nitrae-lupetazin is added
0.092mol and solvent dimethyl sulfoxide 80ml, after reacting 5 hours at 50 DEG C, add N- methylimidazole 0.0025mol with
And N-methylmorpholine 0.0025mol, after reacting 5 hours at 50 DEG C, vacuum distillation removal solvent obtains bromine sealing end polyquaternium；
(2) amino-terminated polyetheramine is prepared
In 1000mL dry three-necked bottle, sequentially add 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams
Dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to room
Temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water, take out
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain amino-terminated polyetheramine；
(3) modified calcium carbonate is prepared
In 100ml three-necked bottle, the ammonia that bromine sealing end 0.4 gram of polyquaternium, the step (2) that step (1) obtains obtain is added
1.3 grams of base end capped polyether amine and dimethyl sulfoxide 50ml, are stirred to polymer at room temperature after being completely dissolved, and are sequentially added average
3 grams of the calcium carbonate of 2000 mesh of partial size, 3 grams of the calcium carbonate of 2500 mesh of average grain diameter, 3000 mesh of average grain diameter 2 grams of calcium carbonate, flat
2 grams of the calcium carbonate of equal 800 mesh of partial size and 1 gram of cylite, after stirring 5 hours at 60 DEG C of heating, are down to room temperature, filter and collect
Solid product, in vacuum drying oven, 50 DEG C drying 24 hours, obtain modified calcium carbonate；
The modified manometer silicon dioxide the preparation method comprises the following steps:
(1) epoxy-capped polyetheramine is prepared
In 1000mL dry three-necked bottle, the benzylamine and 700 of 100 grams epoxy resin E51,0.25mol are sequentially added
Gram dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to
Room temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water,
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain epoxy-capped polyetheramine；
(2) modified manometer silicon dioxide is prepared
In 100ml three-necked bottle, 0.5 gram of epoxy-capped polyetheramine and dimethyl sulfoxide that step (1) obtains is added
20ml is stirred to polymer at room temperature after being completely dissolved, and 5 grams of silica of 300 nanometers of average grain diameter is added, at 60 DEG C of heating
Stirring 5 hours after, be down to room temperature, filter and collect solid product, in vacuum drying oven, 50 DEG C drying 24 hours, be modified
Nano silica；
Sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat the terpolymer the preparation method comprises the following steps:
(1) amino-terminated polyetheramine is prepared
In 1000mL dry three-necked bottle, sequentially add 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams
Dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to room
Temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water, take out
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain amino-terminated polyetheramine；
(2) amino-terminated polybenzimidazoles is prepared
By the 3 of 0.1mol, 3 ', 4,4 '-tetramino benzophenone, 0.03mol 5- sulfonic acid M-phthalic acid and
The adipic acid of 0.065mol is dissolved in 300g polyphosphoric acids, leads to nitrogen protection after 0.5 hour, is warming up to 180 DEG C of reactions for 24 hours
Afterwards, reaction solution is poured into ice water, then neutralizing the aqueous solution to PH with sodium hydroxide is 5, then filters and uses deionized water
This is finally deposited in vacuum drying oven 80 DEG C of dry l0h to get amino-terminated polyphenyl and miaow by the precipitating washed repeatedly
Azoles；
(3) hyperbranched poly pyrrole throat is prepared
In 100mL dry three-necked bottle, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) benzene are sequentially added
Three acid anhydrides and 25ml metacresol, are stirred under nitrogen protection, and after three acid anhydrides are completely dissolved, 0.006 mole of 3,3 '-diamino are added
Benzidine after 60min is stirred at room temperature, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction,
It is down to room temperature, and is poured into rapidly in 2000mL methanol, a large amount of solid precipitatings are obtained；After washing the product repeatedly with methanol, filter
And collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours to get the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
(4) polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer is prepared
In 100mL dry three-necked bottle, 1 gram of the amino-terminated polyetheramine, 0.4 gram of the naphthalene anhydride are sequentially added
Terminated hyperbranched poly- pyrrole throat, 0.2 gram of the amino-terminated polybenzimidazoles, 10mL dimethyl sulfoxide and 10mL between first
Phenol after stirring 60min under nitrogen protection, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction,
It is down to room temperature, and is poured into rapidly in 2000mL methanol, a large amount of solid precipitatings are obtained；After washing the product repeatedly with methanol, filter
And collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours to get polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat three
Membered copolymer；
(5) sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer is prepared
In 100mL dry three-necked bottle, 1 gram of the polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat is sequentially added
The concentrated sulfuric acid of the mass fraction 98% of terpolymer and 10mL after stirring 180min at 40 DEG C, pours under nitrogen protection
In ice water, after washing the product repeatedly with ice water, filter and collected polymer, in vacuum drying oven, 60 DEG C drying 24 hours be
Obtain sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer.
Embodiment 2
(1) by 65 grams of waterglass, 35 grams of the calcium carbonate of 2000 mesh of average grain diameter, 2 grams of polyoxyethylene polyoxy propyl alcohol amidogen ether with
And 26 grams of terpolymer of hyperbranched poly pyrrole throat of sulfonated polyether amine-polybenzimidazoles-with mixing machine after mixing, be added to 20
In gram deionized water, as component A, for use；
(2) by 70 grams of ethyl orthosilicate, 2,2', 2 ", 2 " '-[1,2- ethanetetrayl four (4,1- phenylene methylene oxygen)]
20 grams of tetraoxane, 9 grams of 8 grams of bromo- 1, the 2- oxepane of 6- and ethyl alcohol are uniformly mixed with mixing machine, as B component, to
With；
(3) by 35 grams of modified manometer silicon dioxide, 7 grams of ethylene glycol, 8 grams of KH-550 and 3 grams of N, N'- carbonyl dimidazoles
After mixing with mixing machine, it is added in 15 grams of dimethyl sulfoxides, as component C, for use；
(4) A, B, C are uniformly mixed up to a kind of timber structure transparent fire-resisting paint；
Wherein, the modified manometer silicon dioxide the preparation method comprises the following steps:
(1) epoxy-capped polyetheramine is prepared
In 1000mL dry three-necked bottle, the benzylamine and 700 of 100 grams epoxy resin E51,0.25mol are sequentially added
Gram dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to
Room temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water,
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain epoxy-capped polyetheramine；
(2) modified manometer silicon dioxide is prepared
In 100ml three-necked bottle, 0.5 gram of epoxy-capped polyetheramine and dimethyl sulfoxide that step (1) obtains is added
20ml is stirred to polymer at room temperature after being completely dissolved, and 5 grams of silica of 300 nanometers of average grain diameter is added, at 60 DEG C of heating
Stirring 5 hours after, be down to room temperature, filter and collect solid product, in vacuum drying oven, 50 DEG C drying 24 hours, be modified
Nano silica；
Sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat the terpolymer the preparation method comprises the following steps:
(1) amino-terminated polyetheramine is prepared
In 1000mL dry three-necked bottle, sequentially add 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams
Dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to room
Temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water, take out
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain amino-terminated polyetheramine；
(2) amino-terminated polybenzimidazoles is prepared
By the 3 of 0.1mol, 3 ', 4,4 '-tetramino benzophenone, 0.03mol 5- sulfonic acid M-phthalic acid and
The adipic acid of 0.065mol is dissolved in 300g polyphosphoric acids, leads to nitrogen protection after 0.5 hour, is warming up to 180 DEG C of reactions for 24 hours
Afterwards, reaction solution is poured into ice water, then neutralizing the aqueous solution to PH with sodium hydroxide is 5, then filters and uses deionized water
This is finally deposited in vacuum drying oven 80 DEG C of dry l0h to get amino-terminated polyphenyl and miaow by the precipitating washed repeatedly
Azoles；
(3) hyperbranched poly pyrrole throat is prepared
In 100mL dry three-necked bottle, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) benzene are sequentially added
Three acid anhydrides and 25ml metacresol, are stirred under nitrogen protection, and after three acid anhydrides are completely dissolved, 0.006 mole of 3,3 '-diamino are added
Benzidine after 60min is stirred at room temperature, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction,
It is down to room temperature, and is poured into rapidly in 2000mL methanol, a large amount of solid precipitatings are obtained；After washing the product repeatedly with methanol, filter
And collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours to get the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
(4) polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer is prepared
In 100mL dry three-necked bottle, 1 gram of the amino-terminated polyetheramine, 0.4 gram of the naphthalene anhydride are sequentially added
Terminated hyperbranched poly- pyrrole throat, 0.2 gram of the amino-terminated polybenzimidazoles, 10mL dimethyl sulfoxide and 10mL between first
Phenol after stirring 60min under nitrogen protection, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction,
It is down to room temperature, and is poured into rapidly in 2000mL methanol, a large amount of solid precipitatings are obtained；After washing the product repeatedly with methanol, filter
And collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours to get polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat three
Membered copolymer；
(5) sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer is prepared
In 100mL dry three-necked bottle, 1 gram of the polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat is sequentially added
The concentrated sulfuric acid of the mass fraction 98% of terpolymer and 10mL after stirring 180min at 40 DEG C, pours under nitrogen protection
In ice water, after washing the product repeatedly with ice water, filter and collected polymer, in vacuum drying oven, 60 DEG C drying 24 hours be
Obtain sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer.
Embodiment 3
(1) by 65 grams of waterglass, 35 grams of modified calcium carbonate, 2 grams of polyoxyethylene polyoxy propyl alcohol amidogen ether and sulfonated polyether amine-
Polybenzimidazoles -26 grams of terpolymer of hyperbranched poly pyrrole throat after mixing, is added in 20 grams of deionized waters with mixing machine,
As component A, for use；
(2) by 70 grams of ethyl orthosilicate, 2,2', 2 ", 2 " '-[1,2- ethanetetrayls four (4,1- phenylene methylene oxygen)]
20 grams of tetraoxane, 9 grams of 8 grams of bromo- 1, the 2- oxepane of 6- and ethyl alcohol are uniformly mixed with mixing machine, as B component, to
With；
(3) by 35 grams of silica of 300 nanometers of average grain diameter, 7 grams of ethylene glycol, 8 grams of KH-550 and N, N'- carbonyl
3 grams of diimidazole with mixing machine after mixing, be added in 15 grams of dimethyl sulfoxides, as component C, for use；
(4) A, B, C are uniformly mixed up to a kind of timber structure transparent fire-resisting paint；
Wherein, the modified calcium carbonate the preparation method comprises the following steps:
(1) bromine sealing end polyquaternium is prepared
In 1000ml dry three-necked bottle, 1,12- dibromo-dodecane 0.1mol, Isosorbide-5-Nitrae-lupetazin is added
0.092mol and solvent dimethyl sulfoxide 80ml, after reacting 5 hours at 50 DEG C, add N- methylimidazole 0.0025mol with
And N-methylmorpholine 0.0025mol, after reacting 5 hours at 50 DEG C, vacuum distillation removal solvent obtains bromine sealing end polyquaternium；
(2) amino-terminated polyetheramine is prepared
In 1000mL dry three-necked bottle, sequentially add 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams
Dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to room
Temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water, take out
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain amino-terminated polyetheramine；
(3) modified calcium carbonate is prepared
In 100ml three-necked bottle, the ammonia that bromine sealing end 0.4 gram of polyquaternium, the step (2) that step (1) obtains obtain is added
1.3 grams of base end capped polyether amine and dimethyl sulfoxide 50ml, are stirred to polymer at room temperature after being completely dissolved, and are sequentially added average
3 grams of the calcium carbonate of 2000 mesh of partial size, 3 grams of the calcium carbonate of 2500 mesh of average grain diameter, 3000 mesh of average grain diameter 2 grams of calcium carbonate, flat
2 grams of the calcium carbonate of equal 800 mesh of partial size and 1 gram of cylite, after stirring 5 hours at 60 DEG C of heating, are down to room temperature, filter and collect
Solid product, in vacuum drying oven, 50 DEG C drying 24 hours, obtain modified calcium carbonate；
Sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat the terpolymer the preparation method comprises the following steps:
(1) amino-terminated polyetheramine is prepared
In 1000mL dry three-necked bottle, sequentially add 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams
Dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to room
Temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water, take out
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain amino-terminated polyetheramine；
(2) amino-terminated polybenzimidazoles is prepared
By the 3 of 0.1mol, 3 ', 4,4 '-tetramino benzophenone, 0.03mol 5- sulfonic acid M-phthalic acid and
The adipic acid of 0.065mol is dissolved in 300g polyphosphoric acids, leads to nitrogen protection after 0.5 hour, is warming up to 180 DEG C of reactions for 24 hours
Afterwards, reaction solution is poured into ice water, then neutralizing the aqueous solution to PH with sodium hydroxide is 5, then filters and uses deionized water
This is finally deposited in vacuum drying oven 80 DEG C of dry l0h to get amino-terminated polyphenyl and miaow by the precipitating washed repeatedly
Azoles；
(3) hyperbranched poly pyrrole throat is prepared
In 100mL dry three-necked bottle, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) benzene are sequentially added
Three acid anhydrides and 25ml metacresol, are stirred under nitrogen protection, and after three acid anhydrides are completely dissolved, 0.006 mole of 3,3 '-diamino are added
Benzidine after 60min is stirred at room temperature, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction,
It is down to room temperature, and is poured into rapidly in 2000mL methanol, a large amount of solid precipitatings are obtained；After washing the product repeatedly with methanol, filter
And collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours to get the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
(4) polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer is prepared
In 100mL dry three-necked bottle, 1 gram of the amino-terminated polyetheramine, 0.4 gram of the naphthalene anhydride are sequentially added
Terminated hyperbranched poly- pyrrole throat, 0.2 gram of the amino-terminated polybenzimidazoles, 10mL dimethyl sulfoxide and 10mL between first
Phenol after stirring 60min under nitrogen protection, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction,
It is down to room temperature, and is poured into rapidly in 2000mL methanol, a large amount of solid precipitatings are obtained；After washing the product repeatedly with methanol, filter
And collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours to get polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat three
Membered copolymer；
(5) sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer is prepared
In 100mL dry three-necked bottle, 1 gram of the polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat is sequentially added
The concentrated sulfuric acid of the mass fraction 98% of terpolymer and 10mL after stirring 180min at 40 DEG C, pours under nitrogen protection
In ice water, after washing the product repeatedly with ice water, filter and collected polymer, in vacuum drying oven, 60 DEG C drying 24 hours be
Obtain sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer.
Embodiment 4
(1) by 65 grams of waterglass, 35 grams of modified calcium carbonate, 2 grams of polyoxyethylene polyoxy propyl alcohol amidogen ether and sulfonated polyether amine-
26 grams of copolymer of hyperbranched poly pyrrole throat with mixing machine after mixing, be added in 20 grams of deionized waters, as component A, for use；
(2) by 70 grams of ethyl orthosilicate, 2,2', 2 ", 2 " '-[1,2- ethanetetrayls four (4,1- phenylene methylene oxygen)]
20 grams of tetraoxane, 9 grams of 8 grams of bromo- 1, the 2- oxepane of 6- and ethyl alcohol are uniformly mixed with mixing machine, as B component, to
With；
(3) by 35 grams of modified manometer silicon dioxide, 7 grams of ethylene glycol, 8 grams of KH-550 and 3 grams of N, N'- carbonyl dimidazoles
After mixing with mixing machine, it is added in 15 grams of dimethyl sulfoxides, as component C, for use；
(4) A, B, C are uniformly mixed up to a kind of timber structure transparent fire-resisting paint；
Wherein, the modified calcium carbonate the preparation method comprises the following steps:
(1) bromine sealing end polyquaternium is prepared
In 1000ml dry three-necked bottle, 1,12- dibromo-dodecane 0.1mol, Isosorbide-5-Nitrae-lupetazin is added
0.092mol and solvent dimethyl sulfoxide 80ml, after reacting 5 hours at 50 DEG C, add N- methylimidazole 0.0025mol with
And N-methylmorpholine 0.0025mol, after reacting 5 hours at 50 DEG C, vacuum distillation removal solvent obtains bromine sealing end polyquaternium；
(2) amino-terminated polyetheramine is prepared
In 1000mL dry three-necked bottle, sequentially add 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams
Dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to room
Temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water, take out
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain amino-terminated polyetheramine；
(3) modified calcium carbonate is prepared
In 100ml three-necked bottle, the ammonia that bromine sealing end 0.4 gram of polyquaternium, the step (2) that step (1) obtains obtain is added
1.3 grams of base end capped polyether amine and dimethyl sulfoxide 50ml, are stirred to polymer at room temperature after being completely dissolved, and are sequentially added average
3 grams of the calcium carbonate of 2000 mesh of partial size, 3 grams of the calcium carbonate of 2500 mesh of average grain diameter, 3000 mesh of average grain diameter 2 grams of calcium carbonate, flat
2 grams of the calcium carbonate of equal 800 mesh of partial size and 1 gram of cylite, after stirring 5 hours at 60 DEG C of heating, are down to room temperature, filter and collect
Solid product, in vacuum drying oven, 50 DEG C drying 24 hours, obtain modified calcium carbonate；
The modified manometer silicon dioxide the preparation method comprises the following steps:
(1) epoxy-capped polyetheramine is prepared
In 1000mL dry three-necked bottle, the benzylamine and 700 of 100 grams epoxy resin E51,0.25mol are sequentially added
Gram dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to
Room temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water,
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain epoxy-capped polyetheramine；
(2) modified manometer silicon dioxide is prepared
In 100ml three-necked bottle, 0.5 gram of epoxy-capped polyetheramine and dimethyl sulfoxide that step (1) obtains is added
20ml is stirred to polymer at room temperature after being completely dissolved, and 5 grams of silica of 300 nanometers of average grain diameter is added, at 60 DEG C of heating
Stirring 5 hours after, be down to room temperature, filter and collect solid product, in vacuum drying oven, 50 DEG C drying 24 hours, be modified
Nano silica；
The sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer the preparation method comprises the following steps:
(1) amino-terminated polyetheramine is prepared
In 1000mL dry three-necked bottle, sequentially add 95 grams epoxy resin E51,0.26mol benzylamine and 700 grams
Dimethyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to room
Temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water, take out
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain amino-terminated polyetheramine；
(2) hyperbranched poly pyrrole throat is prepared
In 100mL dry three-necked bottle, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) benzene are sequentially added
Three acid anhydrides and 25ml metacresol, are stirred under nitrogen protection, after three acid anhydrides are completely dissolved, 0.006 mole of tetramine are added, in room temperature
After lower stirring 60min, 80 DEG C are heated to, reacts 4h, then at 185 DEG C, reacts 10h；After reaction, it is down to room temperature, and fast
Speed is poured into 2000mL methanol, and a large amount of solid precipitatings are obtained；After washing the product repeatedly with methanol, simultaneously collected polymer is filtered,
In vacuum drying oven, 50 DEG C drying 24 hours to get the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
(3) polyetheramine-hyperbranched poly pyrrole throat copolymer is prepared
In 100mL dry three-necked bottle, 1 gram of the amino-terminated polyetheramine, 0.6 gram of the naphthalene anhydride are sequentially added
Terminated hyperbranched poly- pyrrole throat, the dimethyl sulfoxide of 10mL and the metacresol of 10mL add after stirring 60min under nitrogen protection
Heat reacts 4h to 80 DEG C, then at 185 DEG C, reacts 10h；After reaction, it is down to room temperature, and pours into 2000mL methanol rapidly
In, obtain a large amount of solid precipitatings；After washing the product repeatedly with methanol, simultaneously collected polymer, in vacuum drying oven, 50 DEG C are filtered
Dry 24 hours to get polyetheramine-hyperbranched poly pyrrole throat copolymer；
(4) sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer is prepared
In 100mL dry three-necked bottle, sequentially add 1 gram the polyetheramine-hyperbranched poly pyrrole throat copolymer and
The concentrated sulfuric acid of the mass fraction 98% of 10mL after stirring 180min at 40 DEG C, pours into ice water under nitrogen protection, uses ice water
After washing the product repeatedly, filter and collected polymer, in vacuum drying oven, the sulfonated polyether amine-to obtain the final product of 60 DEG C of drying 24 hours
Hyperbranched poly pyrrole throat copolymer.
Test method
Coating obtained by embodiment 1-4 is coated on timber structure, and test performance.
According to GB12441-2005 standard testing, specifically:
1, surface drying time answers≤5h
2, adhesive force/grade :≤3
3, impact resistance/cm: >=20
4, after water resistance/h:24h, coating is wrinkle resistant, does not fall off
5, after humidity resistance/h:48h, coating is not blistering, does not fall off
6, resistance to combustion time/min: >=15
Anti-microbial property: it is measured according to Japanese Industrial Standards JISZ2801.
Antibacterial stability: made sample being immersed in 80 DEG C of water, after a week, tests the loss of its antibacterial activity value
Amount, calculation method are as follows: activity value loss amount=(Escherichia coli antibacterial is living after Escherichia coli antibacterial activity value-test before testing
Property value)/test before Escherichia coli antibacterial activity values.
Test result is shown in Table 1.
Table 1
Above data can be seen that compared with existing coating, and coating of the invention has obvious better performance, therefore
Provide advantageous effects of the invention.
Claims (1)
1. a kind of construction timber transparent fire-resisting paint, which is characterized in that be made of A, B, C, the mass ratio of described A, B, C are 1:
(0.1~0.5): (0.1~0.5)；
The mass fraction of each component in the A are as follows: 50~80 parts of waterglass, 10~30 parts of deionized water, modified calcium carbonate 15~
50 parts, 1~3 part of amidogen ether of polyoxyethylene polyoxy propyl alcohol, sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer
15~30 parts；
The mass fraction of each component in the B are as follows: 60~80 parts of ethyl orthosilicate, 2,2', 2'', 2'''- [1,2- union II methylene
Base four (4,1- phenylene methylene oxygen)] 15~30 parts of tetraoxane, 5~10 parts of bromo- 1, the 2- oxepane of 6-, ethyl alcohol 5-10
Part；
The mass fraction of each component in the C are as follows: 30~50 parts of modified manometer silicon dioxide, 10~20 parts of dimethyl sulfoxide, second
5~10 parts of glycol, 5~10 parts of KH-550, N, 1~5 part of N'- carbonyl dimidazoles；
Wherein, the modified calcium carbonate the preparation method comprises the following steps:
(1) bromine sealing end polyquaternium is prepared
In 1000mL dry three-necked bottle, be added 1,12- dibromo-dodecane 0.1mol, Isosorbide-5-Nitrae-lupetazin 0.092mol with
And solvent dimethyl sulfoxide 80mL adds N- methylimidazole 0.0025mol and N- methyl after reacting 5 hours at 50 DEG C
Quinoline 0.0025mol, after reacting 5 hours at 50 DEG C, vacuum distillation removal solvent obtains bromine sealing end polyquaternium；
(2) amino-terminated polyetheramine is prepared
In 1000mL dry three-necked bottle, the benzylamine and 700 grams of diformazans of 95 grams epoxy resin E51,0.26mol are sequentially added
Base sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and reacts 6h, after reaction, be down to room temperature,
And pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water, filter simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain amino-terminated polyetheramine；
(3) modified calcium carbonate is prepared
In 100mL three-necked bottle, the amino envelope that the bromine that step (1) obtains blocks 0.4 gram of polyquaternium, step (2) obtains is added
1.3 grams of polyetheramine and dimethyl sulfoxide 50mL are held, stirs at room temperature to polymer after being completely dissolved, sequentially adds average grain diameter
3 grams of the calcium carbonate of 2000 mesh, 3 grams of the calcium carbonate of 2500 mesh of average grain diameter, 2 grams of the calcium carbonate of 3000 mesh of average grain diameter, average grain
2 grams of the calcium carbonate of 800 mesh of diameter and 1 gram of cylite are down to room temperature, filter and collect solid after stirring 5 hours at 60 DEG C of heating
Product, in vacuum drying oven, 50 DEG C drying 24 hours, obtain modified calcium carbonate；
The modified manometer silicon dioxide the preparation method comprises the following steps:
(1) epoxy-capped polyetheramine is prepared
In 1000mL dry three-necked bottle, sequentially add 100 grams epoxy resin E51,0.25mol benzylamine and 700 gram two
Methyl sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and react 6h, after reaction, be down to room
Temperature, and pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water, take out
Filter and collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain epoxy-capped polyetheramine；
(2) modified manometer silicon dioxide is prepared
In 100mL three-necked bottle, 0.5 gram of epoxy-capped polyetheramine and dimethyl sulfoxide 20mL that step (1) obtains, room is added
After the lower stirring of temperature is completely dissolved to polymer, 5 grams of silica of 300 nanometers of average grain diameter are added, stirring 5 is small at 60 DEG C of heating
Shi Hou is down to room temperature, filters and collect solid product, in vacuum drying oven, 50 DEG C drying 24 hours, obtain modified nano-silica
SiClx；
Sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat the terpolymer the preparation method comprises the following steps:
(1) amino-terminated polyetheramine is prepared
In 1000mL dry three-necked bottle, the benzylamine and 700 grams of diformazans of 95 grams epoxy resin E51,0.26mol are sequentially added
Base sulfoxide leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heats up 95 DEG C and reacts 6h, after reaction, be down to room temperature,
And pour into rapidly in 2000mL deionized water, obtain a large amount of solid precipitatings；After washing the product repeatedly with deionized water, filter simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C drying 24 hours, obtain amino-terminated polyetheramine；
(2) amino-terminated polybenzimidazoles is prepared
By the 3 of 0.1mol, 3 ', 4,4 '-tetramino benzophenone, the 5- sulfonic acid M-phthalic acid and 0.065mol of 0.03mol
Adipic acid be dissolved in 300g polyphosphoric acids, lead to nitrogen protection after 0.5 hour, after being warming up to 180 DEG C of reactions for 24 hours, will react
Liquid pours into ice water, and then neutralizing the aqueous solution to pH with sodium hydroxide is 5, then filters and is washed repeatedly with deionized water
This is finally deposited in vacuum drying oven 80 DEG C of dry l0h to get amino-terminated polybenzimidazoles by the precipitating arrived；
(3) hyperbranched poly pyrrole throat is prepared
In 100mL dry three-necked bottle, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) benzene, three acid anhydride are sequentially added
It with 25mL metacresol, stirs under nitrogen protection, after three acid anhydrides are completely dissolved, 0.006 mole of 3,3 '-benzidines is added
Amine after 60min is stirred at room temperature, is heated to 80 DEG C, reacts 4h, then at 185 DEG C, reacts 10h；After reaction, it is down to
Room temperature, and pour into rapidly in 2000mL methanol, obtain a large amount of solid precipitatings；After washing the product repeatedly with methanol, filters and receive
Collect polymer, in vacuum drying oven, 50 DEG C drying 24 hours to get the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
(4) polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer is prepared
In 100mL dry three-necked bottle, 1 gram of the amino-terminated polyetheramine, 0.4 gram of naphthalene anhydride sealing end are sequentially added
Hyperbranched poly pyrrole throat, 0.2 gram of the amino-terminated polybenzimidazoles, the dimethyl sulfoxide of 10mL and the metacresol of 10mL,
After stirring 60min under nitrogen protection, 80 DEG C are heated to, reacts 4h, then at 185 DEG C, reacts 10h；After reaction, it is down to
Room temperature, and pour into rapidly in 2000mL methanol, obtain a large amount of solid precipitatings；After washing the product repeatedly with methanol, filters and receive
Collect polymer, in vacuum drying oven, 50 DEG C are total to for drying 24 hours to get polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat ternary
Polymers；
(5) sulfonated polyether amine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer is prepared
In 100mL dry three-necked bottle, 1 gram of the polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat ternary is sequentially added
The concentrated sulfuric acid of the mass fraction 98% of copolymer and 10mL after stirring 180min at 40 DEG C, pours into ice water under nitrogen protection
In, after washing the product repeatedly with ice water, filter and collected polymer, in vacuum drying oven, the sulphur to obtain the final product of 60 DEG C of drying 24 hours
Change polyetheramine-polybenzimidazoles-hyperbranched poly pyrrole throat terpolymer.
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| CN106243792A (en) * | 2016-08-22 | 2016-12-21 | 北京佑琳生科技有限公司 | A kind of timber structure transparent fire-resisting paint |
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| CN106318128A (en) * | 2016-09-18 | 2017-01-11 | 北京佑琳生科技有限公司 | Outdoor ultrathin fireproof coating |
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| CN104829870A (en) * | 2015-05-13 | 2015-08-12 | 苏州巨峰电气绝缘系统股份有限公司 | Modified nano-silicon dioxide and preparation method and application thereof |
| CN106319198A (en) * | 2015-06-19 | 2017-01-11 | 中国科学院过程工程研究所 | Method for separating boron and iron from ludwigite |
| CN106243792A (en) * | 2016-08-22 | 2016-12-21 | 北京佑琳生科技有限公司 | A kind of timber structure transparent fire-resisting paint |
| CN106318128A (en) * | 2016-09-18 | 2017-01-11 | 北京佑琳生科技有限公司 | Outdoor ultrathin fireproof coating |
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|---|---|
| CN106752941A (en) | 2017-05-31 |
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