CN106833374A - A kind of impermeable mildewproof waterproof coating of environmental protection and preparation method thereof - Google Patents
A kind of impermeable mildewproof waterproof coating of environmental protection and preparation method thereof Download PDFInfo
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- CN106833374A CN106833374A CN201710018431.4A CN201710018431A CN106833374A CN 106833374 A CN106833374 A CN 106833374A CN 201710018431 A CN201710018431 A CN 201710018431A CN 106833374 A CN106833374 A CN 106833374A
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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
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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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- 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
- C09D171/00—Coating compositions based on polyethers obtained by reactions forming an ether link in the main chain; Coating compositions based on derivatives of such polymers
- C09D171/02—Polyalkylene oxides
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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
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- 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
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- 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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- 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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a kind of impermeable mildewproof waterproof coating of environmental protection, it is included：Calcium carbonate, china clay, portland cement, APES, epoxy resin E51, polyquaternium modification sulphonation polyetheramine hyperbranched poly pyrrole throat copolymer, 7,7 ' imido double (naphthalene sulfonic acids of 4 hydroxyl 2), deionized water and propylene glycol monomethyl ether.The invention also discloses the preparation method of the impermeable mildewproof waterproof coating of the environmental protection.
Description
Technical field
The invention belongs to technical field of coatings, more particularly it relates to a kind of impermeable mould proof waterproof of environmental protection
Coating and preparation method thereof.
Background technology
With the development of construction industry, the market prospects of water-repellent paint are become better and better.However, existing building water-proof paint with
Acrylic emulsion, using poisonous organic solvent as decentralized medium, both to harm, and is produced as film forming matter to environment
Pollution, further, since the weatherability of acrylic polymer, anti-flammability, water resistance and fungicidal properties are bad, leverages
The service life of building water-proof paint.
Accordingly, it would be desirable to prepare the novel green ring with excellent weather resistance, anti-flammability, water resistance and antimildew and antibacterial performance
Protect impermeable mildewproof waterproof coating.
The content of the invention
In order to solve the above problems, one aspect of the present invention provides a kind of impermeable mildewproof waterproof coating of environmental protection,
In parts by weight, its preparing raw material includes following components：
Calcium carbonate 3-15 parts
China clay 4-15 parts
Portland cement 1-5 parts
APES 5-10 parts
1-5 parts of epoxy resin E51
Polyquaternium modification sulphonation polyetheramine -5-10 parts of hyperbranched poly pyrrole throat copolymer
1-5 parts of 7,7 '-imido double (4- hydroxyl -2- naphthalene sulfonic acids)
Deionized water 10-30 parts
Propylene glycol monomethyl ether 0.1-8 parts.
Preferably, the impermeable mildewproof waterproof coating of described environmental protection, in parts by weight, its preparing raw material is comprising following
Component：
Calcium carbonate 4-10 parts
China clay 5-7 parts
Portland cement 1-3 parts
APES 6-9 parts
1-3 parts of epoxy resin E51
Polyquaternium modification sulphonation polyetheramine -6-9 parts of hyperbranched poly pyrrole throat copolymer
1-3 parts of 7,7 '-imido double (4- hydroxyl -2- naphthalene sulfonic acids)
Deionized water 15-25 parts
Propylene glycol monomethyl ether 0.3-1 parts.
It is highly preferred that the impermeable mildewproof waterproof coating of described environmental protection, in parts by weight, its preparing raw material include with
Lower component：
8 parts of calcium carbonate
6 parts of china clay
2 parts of portland cement
7 parts of APES
2 parts of epoxy resin E51
Polyquaternium modification sulphonation polyetheramine -7 parts of hyperbranched poly pyrrole throat copolymer
2 parts of 7,7 '-imido double (4- hydroxyl -2- naphthalene sulfonic acids)
20 parts of deionized water
0.3 part of propylene glycol monomethyl ether.
In one embodiment, the preparation of the polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer
Method is：
（1）Prepare polyquaternium
In the dry three-necked bottles of 1000ml, add 1,12- dibromo-dodecanes 0.1mol, Isosorbide-5-Nitrae-lupetazin 0.092mol with
And solvent dimethyl sulfoxide (DMSO) 80ml, after being reacted 5 hours at 50 DEG C, add N- methylimidazole 0.0025mol and N- methyl
Quinoline 0.0025mol, after being reacted 5 hours at 50 DEG C, vacuum distillation removal solvent obtains polyquaternium；
（2）Prepare amino-terminated polyetheramine
In the dry three-necked bottles of 1000mL, 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, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
（3）Prepare hyperbranched poly pyrrole throat
In the dry three-necked bottles of 100mL, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) acid anhydrides of benzene three are sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, add the 3 of 0.006 mole, 3 '-benzidine
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 terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methyl alcohol, obtain a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration is simultaneously received
Collection polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain final product the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
（4）Prepare polyetheramine-hyperbranched poly pyrrole throat copolymer
In the dry three-necked bottles of 100mL, 1 gram of described amino-terminated polyetheramine, 0.6 gram of naphthalene anhydride end-blocking is sequentially added
The metacresol of hyperbranched poly pyrrole throat, the dimethyl sulfoxide (DMSO) of 10mL and 10mL, after stirring 60min under nitrogen protection, is heated to
80 DEG C, 4h is reacted, then at 185 DEG C, react 10h；After reaction terminates, room temperature is down to, and poured into rapidly in 2000mL methyl alcohol, obtained
To a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 50 DEG C of dryings
24 hours, obtain final product polyetheramine-hyperbranched poly pyrrole throat copolymer；
（5）Prepare sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer
In the dry three-necked bottles of 100mL, 1 gram of the polyetheramine-hyperbranched poly pyrrole throat copolymer and 10mL is sequentially added
Mass fraction 98% the concentrated sulfuric acid, under nitrogen protection, at 40 DEG C stir 180min after, pour into frozen water, washed repeatedly with frozen water
After washing the product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings obtain final product sulfonated polyether amine-hyperbranched for 24 hours
Poly- pyrrole throat copolymer；
（6）Prepare polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer
In 100ml three-necked bottles, step is added（1）0.2 gram of the polyquaternium for obtaining, step（5）The sulfonated polyether amine for obtaining-
0.5 gram of hyperbranched poly pyrrole throat copolymer, 0.2 gram of hexamethylene diamine, 0.05 gram of NaOH, deionized water 2mL and dimethyl sulfoxide (DMSO)
50ml, after stirring at room temperature；After being reacted 10 hours at 60 DEG C, room temperature is down to, and poured into rapidly in 2000mL methyl alcohol, obtained
To a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings
24 hours, obtain polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer.
In one embodiment, the impermeable mildewproof waterproof coating of described environmental protection, in parts by weight, it prepares former
Material also includes following components：
1-5 parts of 2- aminobenzimidazoles
1-5 parts of 2- (2- methoxyphenyls) -4,5- -1,2 '-dimers of diphenyl-imidazole；
Preferably, the impermeable mildewproof waterproof coating of described environmental protection, in parts by weight, its preparing raw material is also included with the following group
Point：
3 parts of 2- aminobenzimidazoles
3 parts of -1,2 '-dimer of 2- (2- methoxyphenyls) -4,5- diphenyl-imidazoles.
Another aspect of the present invention provides a kind of preparation method of the impermeable mildewproof waterproof coating of environmental protection, including：Will be described
Material component add mixer in be sufficiently mixed 10-200 minutes after, discharging is obtained.
In one embodiment, the well-mixed time is 45 minutes.
In one embodiment, the stir speed (S.S.) of the mixer is 10 ~ 1000 revs/min；Preferably, the mixer
Stir speed (S.S.) be 600 revs/min.
Beneficial effects of the present invention are：
1st, the addition of polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer, can both provide excellent weatherability,
Intensity higher, good fire resistance and excellent anti-microbial property, and plasticization can be played prevent system mistake
It is crisp, processing step can also be greatly reduced, so as to provide Advantageous Effects of the invention.
2nd, the addition of 2- aminobenzimidazoles and 2- (2- methoxyphenyls) -4,5- -1,2 '-dimers of diphenyl-imidazole
The rigidity and the crosslink density by improving system with sulfonic ionomer of system can be improved, further, strengthens coating
Intensity and water resistance so that provide Advantageous Effects of the invention.
Specific embodiment
Raw material:
3,3 '-diaminobenzidine is purchased from CTI, and directly uses, without being further purified.Styrene-acrylic emulsion is purchased from Henkel, board
Number be 1863.Epoxy silane coupling agent KH-560 is purchased from Chemical Reagent Co., Ltd., Sinopharm Group.1,3,5- tri- (4- naphthoxys-
1,8- diacid) acid anhydride of benzene three prepared according to method disclosed in patent CN101270111B.Calcium carbonate is purchased from Suzhou name craftsman, particle diameter 1250
Mesh, the trade mark is MJF-1250.China clay is purchased from BASF, and the trade mark is ASP-200.Portland cement is limited purchased from platform mud Shenyang cement
Company.Other raw materials are purchased from Aladdin reagent Co., Ltd.
Embodiment 1
By 8 grams of calcium carbonate, 6 grams of china clay, 2 grams of portland cement, 7 grams of APES, 2 grams of epoxy resin E51,
Double (the 4- hydroxyl -2- naphthalene sulfonic acids) 2 of polyquaternium modification sulphonation polyetheramine -7 grams of hyperbranched poly pyrrole throat copolymer, 7,7 '-imido
Gram, be sufficiently mixed 45 minutes in 0.3 gram of addition mixer of 20 grams of deionized water and propylene glycol monomethyl ether after, discharging is obtained, and is stirred
Speed is mixed for 600 revs/min；
The preparation method of the polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer is：
（1）Prepare polyquaternium
In the dry three-necked bottles of 1000ml, add 1,12- dibromo-dodecanes 0.1mol, Isosorbide-5-Nitrae-lupetazin 0.092mol with
And solvent dimethyl sulfoxide (DMSO) 80ml, after being reacted 5 hours at 50 DEG C, add N- methylimidazole 0.0025mol and N- methyl
Quinoline 0.0025mol, after being reacted 5 hours at 50 DEG C, vacuum distillation removal solvent obtains polyquaternium；
（2）Prepare amino-terminated polyetheramine
In the dry three-necked bottles of 1000mL, 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, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
（3）Prepare hyperbranched poly pyrrole throat
In the dry three-necked bottles of 100mL, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) acid anhydrides of benzene three are sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, add the 3 of 0.006 mole, 3 '-benzidine
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 terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methyl alcohol, obtain a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration is simultaneously received
Collection polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain final product the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
（4）Prepare polyetheramine-hyperbranched poly pyrrole throat copolymer
In the dry three-necked bottles of 100mL, 1 gram of described amino-terminated polyetheramine, 0.6 gram of naphthalene anhydride end-blocking is sequentially added
The metacresol of hyperbranched poly pyrrole throat, the dimethyl sulfoxide (DMSO) of 10mL and 10mL, after stirring 60min under nitrogen protection, is heated to
80 DEG C, 4h is reacted, then at 185 DEG C, react 10h；After reaction terminates, room temperature is down to, and poured into rapidly in 2000mL methyl alcohol, obtained
To a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 50 DEG C of dryings
24 hours, obtain final product polyetheramine-hyperbranched poly pyrrole throat copolymer；
（5）Prepare sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer
In the dry three-necked bottles of 100mL, 1 gram of the polyetheramine-hyperbranched poly pyrrole throat copolymer and 10mL is sequentially added
Mass fraction 98% the concentrated sulfuric acid, under nitrogen protection, at 40 DEG C stir 180min after, pour into frozen water, washed repeatedly with frozen water
After washing the product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings obtain final product sulfonated polyether amine-hyperbranched for 24 hours
Poly- pyrrole throat copolymer；
（6）Prepare polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer
In 100ml three-necked bottles, step is added（1）0.2 gram of the polyquaternium for obtaining, step（5）The sulfonated polyether amine for obtaining-
0.5 gram of hyperbranched poly pyrrole throat copolymer, 0.2 gram of hexamethylene diamine, 0.05 gram of NaOH, deionized water 2mL and dimethyl sulfoxide (DMSO)
50ml, after stirring at room temperature；After being reacted 10 hours at 60 DEG C, room temperature is down to, and poured into rapidly in 2000mL methyl alcohol, obtained
To a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings
24 hours, obtain polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer.
Embodiment 2
By 8 grams of calcium carbonate, 6 grams of china clay, 2 grams of portland cement, 7 grams of APES, 2 grams of epoxy resin E51,
2 grams of polyquaternium modified polyether amine -7 grams of hyperbranched poly pyrrole throat copolymer, 7,7 '-imido double (4- hydroxyl -2- naphthalene sulfonic acids), go
After being sufficiently mixed 45 minutes in 0.3 gram of addition mixer of 20 grams of ionized water and propylene glycol monomethyl ether, discharging is obtained, stir speed (S.S.)
It is 600 revs/min；
The preparation method of the polyquaternium modified polyether amine-hyperbranched poly pyrrole throat copolymer is：
（1）Prepare polyquaternium
In the dry three-necked bottles of 1000ml, add 1,12- dibromo-dodecanes 0.1mol, Isosorbide-5-Nitrae-lupetazin 0.092mol with
And solvent dimethyl sulfoxide (DMSO) 80ml, after being reacted 5 hours at 50 DEG C, add N- methylimidazole 0.0025mol and N- methyl
Quinoline 0.0025mol, after being reacted 5 hours at 50 DEG C, vacuum distillation removal solvent obtains polyquaternium；
（2）Prepare amino-terminated polyetheramine
In the dry three-necked bottles of 1000mL, 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, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
（3）Prepare hyperbranched poly pyrrole throat
In the dry three-necked bottles of 100mL, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) acid anhydrides of benzene three are sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, add the 3 of 0.006 mole, 3 '-benzidine
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 terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methyl alcohol, obtain a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration is simultaneously received
Collection polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain final product the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
（4）Prepare polyetheramine-hyperbranched poly pyrrole throat copolymer
In the dry three-necked bottles of 100mL, 1 gram of described amino-terminated polyetheramine, 0.6 gram of naphthalene anhydride end-blocking is sequentially added
The metacresol of hyperbranched poly pyrrole throat, the dimethyl sulfoxide (DMSO) of 10mL and 10mL, after stirring 60min under nitrogen protection, is heated to
80 DEG C, 4h is reacted, then at 185 DEG C, react 10h；After reaction terminates, room temperature is down to, and poured into rapidly in 2000mL methyl alcohol, obtained
To a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 50 DEG C of dryings
24 hours, obtain final product polyetheramine-hyperbranched poly pyrrole throat copolymer；
（5）Prepare polyquaternium modified polyether amine-hyperbranched poly pyrrole throat copolymer
In 100ml three-necked bottles, step is added（1）0.2 gram of the polyquaternium for obtaining, step（4）Polyetheramine-the over-expense for obtaining
Change poly- 0.5 gram of pyrrole throat copolymer, 0.2 gram of hexamethylene diamine, 0.05 gram of NaOH, deionized water 2mL and dimethyl sulfoxide (DMSO) 50ml,
After stirring at room temperature；After being reacted 10 hours at 60 DEG C, room temperature is down to, and poured into rapidly in 2000mL methyl alcohol, obtain big
Amount solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings 24 are small
When, obtain polyquaternium modified polyether amine-hyperbranched poly pyrrole throat copolymer.
Embodiment 3
By 8 grams of calcium carbonate, 6 grams of china clay, 2 grams of portland cement, 7 grams of APES, 2 grams of epoxy resin E51,
2 grams of sulfonated polyether amine -7 grams of hyperbranched poly pyrrole throat copolymer, 7,7 '-imido double (4- hydroxyl -2- naphthalene sulfonic acids), deionized water 20
Gram and 0.3 gram of addition mixer of propylene glycol monomethyl ether in be sufficiently mixed 45 minutes after, discharging is obtained, stir speed (S.S.) be 600 turns/
Point；
The preparation method of the sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer is：
（1）Prepare amino-terminated polyetheramine
In the dry three-necked bottles of 1000mL, 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, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
（2）Prepare hyperbranched poly pyrrole throat
In the dry three-necked bottles of 100mL, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) acid anhydrides of benzene three are sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, add the 3 of 0.006 mole, 3 '-benzidine
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 terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methyl alcohol, obtain a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration is simultaneously received
Collection polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain final product the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
（3）Prepare polyetheramine-hyperbranched poly pyrrole throat copolymer
In the dry three-necked bottles of 100mL, 1 gram of described amino-terminated polyetheramine, 0.6 gram of naphthalene anhydride end-blocking is sequentially added
The metacresol of hyperbranched poly pyrrole throat, the dimethyl sulfoxide (DMSO) of 10mL and 10mL, after stirring 60min under nitrogen protection, is heated to
80 DEG C, 4h is reacted, then at 185 DEG C, react 10h；After reaction terminates, room temperature is down to, and poured into rapidly in 2000mL methyl alcohol, obtained
To a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 50 DEG C of dryings
24 hours, obtain final product polyetheramine-hyperbranched poly pyrrole throat copolymer；
（4）Prepare sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer
In the dry three-necked bottles of 100mL, 1 gram of the polyetheramine-hyperbranched poly pyrrole throat copolymer and 10mL is sequentially added
Mass fraction 98% the concentrated sulfuric acid, under nitrogen protection, at 40 DEG C stir 180min after, pour into frozen water, washed repeatedly with frozen water
After washing the product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings obtain final product sulfonated polyether amine-hyperbranched for 24 hours
Poly- pyrrole throat copolymer.
Embodiment 4
By 8 grams of calcium carbonate, 6 grams of china clay, 2 grams of portland cement, 7 grams of APES, 2 grams of epoxy resin E51,
2 grams of 4 grams of polyetheramine, 3 grams of hyperbranched poly pyrrole throat copolymer, 7,7 '-imido double (4- hydroxyl -2- naphthalene sulfonic acids), 20 grams of deionized water
And after in 0.3 gram of addition mixer of propylene glycol monomethyl ether being sufficiently mixed 45 minutes, discharging is obtained, stir speed (S.S.) is 600 revs/min；
The preparation method of the polyetheramine is：
In the dry three-necked bottles of 1000mL, 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, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
The preparation method of the hyperbranched poly pyrrole throat is：
In the dry three-necked bottles of 100mL, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) acid anhydrides of benzene three are sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, add the 3 of 0.006 mole, 3 '-benzidine
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 terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methyl alcohol, obtain a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration is simultaneously received
Collection polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain final product the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride.
Embodiment 5
By 8 grams of calcium carbonate, 6 grams of china clay, 2 grams of portland cement, 7 grams of APES, 2 grams of epoxy resin E51,
2 grams of 12 grams of styrene-acrylic emulsion, 7,7 '-imido double (4- hydroxyl -2- naphthalene sulfonic acids), 20 grams of deionized water and propylene glycol monomethyl ether 0.3
After being sufficiently mixed 45 minutes in gram addition mixer, discharging is obtained, and stir speed (S.S.) is 600 revs/min；
Embodiment 6
By 8 grams of calcium carbonate, 6 grams of china clay, 2 grams of portland cement, 7 grams of APES, 2 grams of epoxy resin E51,
Double (the 4- hydroxyl -2- naphthalene sulfonic acids) 2 of polyquaternium modification sulphonation polyetheramine -7 grams of hyperbranched poly pyrrole throat copolymer, 7,7 '-imido
Gram, 20 grams of deionized water, 0.3 gram of propylene glycol monomethyl ether, 3 grams and 2- (2- methoxyphenyls) -4,5- of 2- aminobenzimidazoles
Diphenyl-imidazole -1, after being sufficiently mixed 45 minutes in 2 '-dimer, 3 grams of addition mixers, discharging is obtained, and stir speed (S.S.) is 600
Rev/min；
The preparation method of the polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer is：
（1）Prepare polyquaternium
In the dry three-necked bottles of 1000ml, add 1,12- dibromo-dodecanes 0.1mol, Isosorbide-5-Nitrae-lupetazin 0.092mol with
And solvent dimethyl sulfoxide (DMSO) 80ml, after being reacted 5 hours at 50 DEG C, add N- methylimidazole 0.0025mol and N- methyl
Quinoline 0.0025mol, after being reacted 5 hours at 50 DEG C, vacuum distillation removal solvent obtains polyquaternium；
（2）Prepare amino-terminated polyetheramine
In the dry three-necked bottles of 1000mL, 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, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
（3）Prepare hyperbranched poly pyrrole throat
In the dry three-necked bottles of 100mL, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) acid anhydrides of benzene three are sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, add the 3 of 0.006 mole, 3 '-benzidine
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 terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methyl alcohol, obtain a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration is simultaneously received
Collection polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain final product the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
（4）Prepare polyetheramine-hyperbranched poly pyrrole throat copolymer
In the dry three-necked bottles of 100mL, 1 gram of described amino-terminated polyetheramine, 0.6 gram of naphthalene anhydride end-blocking is sequentially added
The metacresol of hyperbranched poly pyrrole throat, the dimethyl sulfoxide (DMSO) of 10mL and 10mL, after stirring 60min under nitrogen protection, is heated to
80 DEG C, 4h is reacted, then at 185 DEG C, react 10h；After reaction terminates, room temperature is down to, and poured into rapidly in 2000mL methyl alcohol, obtained
To a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 50 DEG C of dryings
24 hours, obtain final product polyetheramine-hyperbranched poly pyrrole throat copolymer；
（5）Prepare sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer
In the dry three-necked bottles of 100mL, 1 gram of the polyetheramine-hyperbranched poly pyrrole throat copolymer and 10mL is sequentially added
Mass fraction 98% the concentrated sulfuric acid, under nitrogen protection, at 40 DEG C stir 180min after, pour into frozen water, washed repeatedly with frozen water
After washing the product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings obtain final product sulfonated polyether amine-hyperbranched for 24 hours
Poly- pyrrole throat copolymer；
（6）Prepare polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer
In 100ml three-necked bottles, step is added（1）0.2 gram of the polyquaternium for obtaining, step（5）The sulfonated polyether amine for obtaining-
0.5 gram of hyperbranched poly pyrrole throat copolymer, 0.2 gram of hexamethylene diamine, 0.05 gram of NaOH, deionized water 2mL and dimethyl sulfoxide (DMSO)
50ml, after stirring at room temperature；After being reacted 10 hours at 60 DEG C, room temperature is down to, and poured into rapidly in 2000mL methyl alcohol, obtained
To a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings
24 hours, obtain polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer.
Method of testing
By embodiment 1-6 gained coating, it is coated on structural steel, according to GB/14907-2002 standard testings, specially：
1st, surface drying time answers≤12h
2nd, crack resistance：The Crack of appearance 1 ~ 3, its width is allowed to answer≤0.5mm
3rd, adhesion strength >=0.15Mpa
4th, water resistance：After 24h, coating does not ftracture, aliquation, obscission
5th, cold-hot cyclicity/number of times：After 15 times, coating does not ftracture, aliquation, obscission
6th, fire endurance：Coating layer thickness is 5mm, and fire endurance is not less than 1h.
Antifriction performance：By standard GB/T1768-79 (89, method of testing is to use alcohol wear-resistant tester, plus 500g weight
Counterweight, the alcohol of 99.7% concentration is infiltrated with white cotton, is rubbed back and forth, and recording ink starts number of times during destruction.
Anti-microbial property：It is measured according to Japanese Industrial Standards JISZ2801.
Antibacterial stability：Made sample is immersed in 80 DEG C of water, after one week, the loss of its antibacterial activity value is tested
Measure, its computational methods is：Activity value loss amount=（Escherichia coli antibacterial activity after Escherichia coli antibacterial activity value-test before test
Value）Escherichia coli antibacterial activity value before/test.
Test result is shown in Table 1.
Table 1
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Drying time, surface drying/h | 2.7 | 4.5 | 2.6 | 19.5 | 9.7 | 1.3 |
| Initially dry crack resistance | Flawless | Flawless | Flawless | There are 3 Cracks | Flawless | Flawless |
| Adhesion strength/Mpa | 0.51 | 0.39 | 0.57 | 0.07 | 0.23 | 0.68 |
| Water resistance/h | 255 | 132 | 279 | 8 | 20 | 403 |
| Cold-hot cyclicity/number of times | 144 | 91 | 150 | 7 | 49 | 312 |
| Fire endurance/h | 3.7 | 3.3 | 4.5 | 0.8 | 1.7 | 5.5 |
| Rub resistance number of times | 1811 | 1139 | 1905 | 40 | 359 | 2888 |
| Staphylococcus glucose bacterium antibacterial activity value | 3.0 | 2.8 | 0 | 0 | 0 | 3.0 |
| Escherichia coli antibacterial activity value | 3.0 | 2.9 | 0 | 0 | 0 | 3.0 |
| Antibacterial activity value loss amount（%） | 2.3 | 8.8 | - | - | - | 1.2 |
Data above can be seen that and not use polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer, 2- amino
Benzimidazole and 2- (2- methoxyphenyls) -4,5- diphenyl-imidazole -1, the coating of 2 '-dimer are compared, painting of the invention
Material has obvious better performance, is thus provided that Advantageous Effects of the invention.
Claims (10)
1. the impermeable mildewproof waterproof coating of a kind of environmental protection, it is characterised in that in parts by weight, its preparing raw material is comprising following
Component：
Calcium carbonate 3-15 parts
China clay 4-15 parts
Portland cement 1-5 parts
APES 5-10 parts
1-5 parts of epoxy resin E51
Polyquaternium modification sulphonation polyetheramine -5-10 parts of hyperbranched poly pyrrole throat copolymer
1-5 parts of 7,7 '-imido double (4- hydroxyl -2- naphthalene sulfonic acids)
Deionized water 10-30 parts
Propylene glycol monomethyl ether 0.1-8 parts.
2. the impermeable mildewproof waterproof coating of environmental protection according to claim 1, it is characterised in that in parts by weight, its
Preparing raw material includes following components：
Calcium carbonate 4-10 parts
China clay 5-7 parts
Portland cement 1-3 parts
APES 6-9 parts
1-3 parts of epoxy resin E51
Polyquaternium modification sulphonation polyetheramine -6-9 parts of hyperbranched poly pyrrole throat copolymer
1-3 parts of 7,7 '-imido double (4- hydroxyl -2- naphthalene sulfonic acids)
Deionized water 15-25 parts
Propylene glycol monomethyl ether 0.3-1 parts.
3. the impermeable mildewproof waterproof coating of environmental protection according to claim 1, it is characterised in that in parts by weight, its
Preparing raw material includes following components：
8 parts of calcium carbonate
6 parts of china clay
2 parts of portland cement
7 parts of APES
2 parts of epoxy resin E51
Polyquaternium modification sulphonation polyetheramine -7 parts of hyperbranched poly pyrrole throat copolymer
2 parts of 7,7 '-imido double (4- hydroxyl -2- naphthalene sulfonic acids)
20 parts of deionized water
0.3 part of propylene glycol monomethyl ether.
4. the impermeable mildewproof waterproof coating of environmental protection according to claim 1, it is characterised in that the polyquaternium changes
The preparation method of property sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer is：
（1）Prepare polyquaternium
In the dry three-necked bottles of 1000ml, add 1,12- dibromo-dodecanes 0.1mol, Isosorbide-5-Nitrae-lupetazin 0.092mol with
And solvent dimethyl sulfoxide (DMSO) 80ml, after being reacted 5 hours at 50 DEG C, add N- methylimidazole 0.0025mol and N- methyl
Quinoline 0.0025mol, after being reacted 5 hours at 50 DEG C, vacuum distillation removal solvent obtains polyquaternium；
（2）Prepare amino-terminated polyetheramine
In the dry three-necked bottles of 1000mL, 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, heat up 95 DEG C of reaction 6h, after reaction terminates, is down to room temperature,
And pour into rapidly in 2000mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, suction filtration is simultaneously
Collected polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain amino-terminated polyetheramine；
（3）Prepare hyperbranched poly pyrrole throat
In the dry three-necked bottles of 100mL, the 1 of 0.01 mole, 3,5- tri- (4- naphthoxy -1,8- diacid) acid anhydrides of benzene three are sequentially added
With 25ml metacresols, stir under nitrogen protection, after three acid anhydrides are completely dissolved, add the 3 of 0.006 mole, 3 '-benzidine
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 terminates, it is down to
Room temperature, and pour into rapidly in 2000mL methyl alcohol, obtain a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration is simultaneously received
Collection polymer, in vacuum drying oven, 50 DEG C of dryings 24 hours obtain final product the terminated hyperbranched poly- pyrrole throat of naphthalene anhydride；
（4）Prepare polyetheramine-hyperbranched poly pyrrole throat copolymer
In the dry three-necked bottles of 100mL, 1 gram of described amino-terminated polyetheramine, 0.6 gram of naphthalene anhydride end-blocking is sequentially added
The metacresol of hyperbranched poly pyrrole throat, the dimethyl sulfoxide (DMSO) of 10mL and 10mL, after stirring 60min under nitrogen protection, is heated to
80 DEG C, 4h is reacted, then at 185 DEG C, react 10h；After reaction terminates, room temperature is down to, and poured into rapidly in 2000mL methyl alcohol, obtained
To a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 50 DEG C of dryings
24 hours, obtain final product polyetheramine-hyperbranched poly pyrrole throat copolymer；
（5）Prepare sulfonated polyether amine-hyperbranched poly pyrrole throat copolymer
In the dry three-necked bottles of 100mL, 1 gram of the polyetheramine-hyperbranched poly pyrrole throat copolymer and 10mL is sequentially added
Mass fraction 98% the concentrated sulfuric acid, under nitrogen protection, at 40 DEG C stir 180min after, pour into frozen water, washed repeatedly with frozen water
After washing the product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings obtain final product sulfonated polyether amine-hyperbranched for 24 hours
Poly- pyrrole throat copolymer；
（6）Prepare polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer
In 100ml three-necked bottles, step is added（1）0.2 gram of the polyquaternium for obtaining, step（5）The sulfonated polyether amine for obtaining-
0.5 gram of hyperbranched poly pyrrole throat copolymer, 0.2 gram of hexamethylene diamine, 0.05 gram of NaOH, deionized water 2mL and dimethyl sulfoxide (DMSO)
50ml, after stirring at room temperature；After being reacted 10 hours at 60 DEG C, room temperature is down to, and poured into rapidly in 2000mL methyl alcohol, obtained
To a large amount of solids of sedimentation；With after the methyl alcohol cyclic washing product, suction filtration and collected polymer, in vacuum drying oven, 60 DEG C of dryings
24 hours, obtain polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer.
5. the impermeable mildewproof waterproof coating of environmental protection according to claim any one of 1-4, it is characterised in that with weight
Part meter, its preparing raw material also includes following components：
1-5 parts of 2- aminobenzimidazoles
1-5 parts of 2- (2- methoxyphenyls) -4,5- -1,2 '-dimers of diphenyl-imidazole.
6. the impermeable mildewproof waterproof coating of environmental protection according to claim 5, it is characterised in that in parts by weight, its
Preparing raw material also includes following components：
3 parts of 2- aminobenzimidazoles
3 parts of -1,2 '-dimer of 2- (2- methoxyphenyls) -4,5- diphenyl-imidazoles.
7. the preparation method of the impermeable mildewproof waterproof coating of a kind of environmental protection, including：By described in claim any one of 1-6
Material component is added after being sufficiently mixed 10-200 minutes in mixer, and discharging is obtained.
8. the preparation method of the impermeable mildewproof waterproof coating of environmental protection according to claim 7, it is characterised in that described
The well-mixed time is 45 minutes.
9. the preparation method of the impermeable mildewproof waterproof coating of environmental protection according to claim 7, it is characterised in that described
The stir speed (S.S.) of mixer is 10 ~ 1000 revs/min.
10. the preparation method of the impermeable mildewproof waterproof coating of environmental protection according to claim 9, it is characterised in that institute
The stir speed (S.S.) for stating mixer is 600 revs/min.
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| CN110628301A (en) * | 2019-09-06 | 2019-12-31 | 广州市五羊油漆(翁源)有限公司 | Special water-based paint for ceramic tiles and application method thereof |
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| CN103601456A (en) * | 2013-11-19 | 2014-02-26 | 青岛广联达精密机械有限公司 | Improved mould-proof and waterproof coating |
| CN105754431A (en) * | 2016-04-01 | 2016-07-13 | 云南佑琳生科技有限公司 | Exterior wall coating material capable of finishing working through one-time painting |
| CN106189404A (en) * | 2016-07-09 | 2016-12-07 | 云南佑琳生科技有限公司 | A kind of dry powder reflecting heat insulation paint |
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