CN106752801A - A kind of multifunctional nano waterproof interlayer coating and preparation method thereof - Google Patents
A kind of multifunctional nano waterproof interlayer coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of multifunctional nano waterproof interlayer coating, it is included：Montmorillonite, nano silicon, portland cement, APES phosphate, KH 560, polyquaternium modification sulphonation polyetheramine hyperbranched poly pyrrole throat copolymer, polyisocyanates, deionized water and dimethyl sulfoxide (DMSO).The invention also discloses the preparation method of the multifunctional nano waterproof interlayer coating.
Description
Technical field
The invention belongs to technical field of coatings, more particularly it relates to a kind of multifunctional nano waterproof interlayer coating
And preparation method thereof.
Background technology
With continuing to develop for building trade, the usage amount of building water-proof paint constantly increases.In the prior art, build anti-
Water paint is general using acrylic emulsion as film forming matter, using water as decentralized medium, and it has reduction volatile organic matter
Discharge capacity, reduces energy consumption, reduce coating production, construction, using etc. the harm to human body and the pollution to environment etc. in link
Advantage.But, because the weatherability of acrylic polymer, anti-flammability and water resistance are bad, leverage buildings waterproof
The service life of coating, additionally, this kind of coating does not possess the performance of antimildew and antibacterial yet.
Accordingly, it would be desirable to pass through formula improve, preparing has excellent weather resistance, anti-flammability, water resistance and antimildew and antibacterial
The novel multifunctional nano waterproof interlayer coating of energy.
The content of the invention
In order to solve the above problems, one aspect of the present invention provides a kind of multifunctional nano waterproof interlayer coating, with weight
Amount part meter, its preparing raw material includes following components：
Montmorillonite 5-15 parts
Nano silicon 5-10 parts
Portland cement 1-3 parts
5-10 parts of APES phosphate
KH-560 5-9 parts
Polyquaternium modification sulphonation polyetheramine -5-10 parts of hyperbranched poly pyrrole throat copolymer
Polyisocyanates 1-3 parts
Deionized water 15-25 parts
Dimethyl sulfoxide (DMSO) 1-5 parts.
Preferably, described multifunctional nano waterproof interlayer coating, in parts by weight, its preparing raw material is included with the following group
Point：
Montmorillonite 6-8 parts
Nano silicon 6-8 parts
Portland cement 1-2 parts
7-9 parts of APES phosphate
KH-560 6-8 parts
Polyquaternium modification sulphonation polyetheramine -6-9 parts of hyperbranched poly pyrrole throat copolymer
Polyisocyanates 1-2 parts
Deionized water 17-20 parts
Dimethyl sulfoxide (DMSO) 2-3 parts.
It is highly preferred that described multifunctional nano waterproof interlayer coating, in parts by weight, its preparing raw material is included with the following group
Point：
7 parts of montmorillonite
7 parts of nano silicon
2 parts of portland cement
8 parts of APES phosphate
7 parts of KH-560
Polyquaternium modification sulphonation polyetheramine -8 parts of hyperbranched poly pyrrole throat copolymer
2 parts of polyisocyanates
19 parts of deionized water
2 parts of dimethyl sulfoxide (DMSO).
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 kind is preferably carried out mode, described multifunctional nano waterproof interlayer coating, in parts by weight, its preparation
Raw material also includes following components：
1-3 parts of 4- azabenzimidazoles
Aniline 1-3 parts of 4- (imidazoles -1- bases)；
Preferably, described multifunctional nano waterproof interlayer coating, in parts by weight, its preparing raw material also includes following components：
2 parts of 4- azabenzimidazoles
4- (imidazoles -1- bases) 2 parts of aniline.
In one kind is preferably carried out mode, described high performance water proof mildew resistant paint, in parts by weight, its preparing raw material
Also include following components：
0.5 part of 2,4,6- trisbromomethyls trimethylbenzene.
Another aspect of the present invention provides a kind of preparation method of multifunctional nano waterproof interlayer coating, including：Will be described
Material component add mixer in be sufficiently mixed 1-100 minutes after, discharging is obtained.
In one embodiment, the well-mixed time is 18 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 300 revs/min.
Compared with prior art, beneficial effects of the present invention are：
1st, by the addition of single substance（That is the addition of polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer）Both
Excellent weatherability can be provided, intensity higher, good fire resistance and excellent anti-microbial property, and can rise again
Prevent system excessively crisp to plasticization, processing step can also be greatly reduced, so as to provide Advantageous Effects of the invention.
2nd, the addition of 4- azabenzimidazoles and 4- (imidazoles -1- bases) aniline can improve system rigidity and by with
Sulfonic ionomer improves the crosslink density of system, further, strengthens the intensity and water resistance of coating, so as to provide
Advantageous Effects of the invention.
The addition of the 3rd, 2,4,6- trisbromomethyl trimethylbenzenes can further effectively improve the crosslink density of system, shorten surface drying
Time, strengthen the intensity and water resistance of coating, so as to provide Advantageous Effects of the invention.
Specific embodiment
Raw material:
Montmorillonite（800 mesh）Purchased from Lingshou County Wo Ao mineral products processings factory.Nano silicon is purchased from the auspicious crystalline substance in Xuancheng, average grain diameter
It is 20nm, model VK-SP20.Portland cement is common conch board cement, purchased from the pure and fresh Cement Co., Ltd in Guangdong.Alkyl
Phenol polyethenoxy ether phosphate APE-10P brands are Ecocare.Polyisocyanates is that Hensel steps MDI, model 5005/
44V20.3,3 '-diaminobenzidine is purchased from CTI, and directly uses, without being further purified.Styrene-acrylic emulsion is purchased from Henkel,
The trade mark is 1863.Epoxy silane coupling agent KH-560 is purchased from Chemical Reagent Co., Ltd., Sinopharm Group.1,3,5- tri- (4- naphthalene oxygen
Base -1,8- diacid) acid anhydride of benzene three prepared according to method disclosed in patent CN101270111B.Other raw materials are purchased from Aladdin reagent
Co., Ltd.
Embodiment 1
By 7 grams of montmorillonite, 7 grams of nano silicon, 2 grams of portland cement, 8 grams of APES phosphate,
7 grams of KH-560, polyquaternium modification sulphonation polyetheramine -8 grams of hyperbranched poly pyrrole throat copolymer, 2 grams of polyisocyanates, go from
After being sufficiently mixed 18 minutes in 2 grams of addition mixers of 19 grams of sub- water and dimethyl sulfoxide (DMSO), discharging is obtained, and stir speed (S.S.) is
300 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 7 grams of montmorillonite, 7 grams of nano silicon, 2 grams of portland cement, 8 grams of APES phosphate,
7 grams of KH-560, polyquaternium modified polyether amine -8 grams of hyperbranched poly pyrrole throat copolymer, 2 grams of polyisocyanates, deionized water
After being sufficiently mixed 18 minutes in 19 grams and 2 grams of addition mixers of dimethyl sulfoxide (DMSO), discharging is obtained, and stir speed (S.S.) is 300 turns/
Point；
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 7 grams of montmorillonite, 7 grams of nano silicon, 2 grams of portland cement, 8 grams of APES phosphate,
7 grams of KH-560, sulfonated polyether amine -8 grams of hyperbranched poly pyrrole throat copolymer, 2 grams of polyisocyanates, 19 grams of deionized water and
After being sufficiently mixed 18 minutes in 2 grams of addition mixers of dimethyl sulfoxide (DMSO), discharging is obtained, and stir speed (S.S.) is 300 revs/min；
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 7 grams of montmorillonite, 7 grams of nano silicon, 2 grams of portland cement, 8 grams of APES phosphate,
7 grams of KH-560,4 grams of polyetheramine, 4 grams of hyperbranched poly pyrrole throat copolymer, 2 grams of polyisocyanates, 19 grams of deionized water and two
After being sufficiently mixed 18 minutes in 2 grams of addition mixers of methyl sulfoxide, discharging is obtained, and stir speed (S.S.) is 300 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 7 grams of montmorillonite, 7 grams of nano silicon, 2 grams of portland cement, 8 grams of APES phosphate,
7 grams of KH-560,15 grams of styrene-acrylic emulsion, 2 grams of polyisocyanates, the 2 grams of additions of 19 grams of deionized water and dimethyl sulfoxide (DMSO) are stirred
Mixing after be sufficiently mixed in machine 18 minutes, discharging is obtained, stir speed (S.S.) is 300 revs/min.
Embodiment 6
By 7 grams of montmorillonite, 7 grams of nano silicon, 2 grams of portland cement, 8 grams of APES phosphate,
7 grams of KH-560, polyquaternium modification sulphonation polyetheramine -8 grams of hyperbranched poly pyrrole throat copolymer, 2 grams of polyisocyanates, go from
19 grams of sub- water, 2 grams of dimethyl sulfoxide (DMSO), 2 grams of 2 grams and 4- of 4- azabenzimidazoles (imidazoles -1- bases) aniline add stirring
After 18 minutes are sufficiently mixed in machine, discharging is obtained, and stir speed (S.S.) is 300 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 7
By 7 grams of montmorillonite, 7 grams of nano silicon, 2 grams of portland cement, 8 grams of APES phosphate,
7 grams of KH-560, polyquaternium modification sulphonation polyetheramine -8 grams of hyperbranched poly pyrrole throat copolymer, 2 grams of polyisocyanates, go from
19 grams of sub- water, 2 grams of dimethyl sulfoxide (DMSO), 2 grams of 4- azabenzimidazoles, 2 grams and 2,4,6- tri- of 4- (imidazoles -1- bases) aniline
After being sufficiently mixed 18 minutes in 0.5 gram of addition mixer of bromomethyl trimethylbenzene, discharging is obtained, and stir speed (S.S.) is 300 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.
Method of testing
By embodiment 1-7 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 | Embodiment 7 |
| Drying time, surface drying/h | 2.6 | 4.8 | 2.6 | 18.1 | 8.9 | 2.1 | 1.6 |
| Initially dry crack resistance | Flawless | Flawless | Flawless | There are 2 Cracks | Flawless | Flawless | Flawless |
| Adhesion strength/Mpa | 0.50 | 0.38 | 0.59 | 0.08 | 0.23 | 0.65 | 0.73 |
| Water resistance/h | 233 | 127 | 261 | 6 | 27 | 311 | 389 |
| Cold-hot cyclicity/number of times | 144 | 93 | 149 | 10 | 49 | 221 | 255 |
| Fire endurance/h | 3.8 | 3.3 | 3.9 | 0.7 | 1.8 | 4.8 | 4.9 |
| Rub resistance number of times | 1817 | 1234 | 1912 | 30 | 356 | 2209 | 2509 |
| Staphylococcus glucose bacterium antibacterial activity value | 3.0 | 3.0 | 0 | 0 | 0 | 3.0 | 3.0 |
| Escherichia coli antibacterial activity value | 3.0 | 3.0 | 0 | 0 | 0 | 3.0 | 3.0 |
| Antibacterial activity value loss amount（%） | 2.8 | 8.1 | - | - | - | 1.0 | 0.5 |
Data above can be seen that and not use polyquaternium modification sulphonation polyetheramine-hyperbranched poly pyrrole throat copolymer, 4- azepines
Benzimidazole, 4- (imidazoles -1- bases) aniline and 2, the coating of 4,6- trisbromomethyl trimethylbenzenes are compared, coating tool of the invention
There is obvious better performance, be thus provided that Advantageous Effects of the invention.
Claims (10)
1. a kind of multifunctional nano waterproof interlayer coating, it is characterised in that in parts by weight, its preparing raw material is included with the following group
Point：
Montmorillonite 5-15 parts
Nano silicon 5-10 parts
Portland cement 1-3 parts
5-10 parts of APES phosphate
KH-560 5-9 parts
Polyquaternium modification sulphonation polyetheramine -5-10 parts of hyperbranched poly pyrrole throat copolymer
Polyisocyanates 1-3 parts
Deionized water 15-25 parts
Dimethyl sulfoxide (DMSO) 1-5 parts.
2. multifunctional nano waterproof interlayer coating according to claim 1, it is characterised in that in parts by weight, its preparation
Raw material includes following components：
Montmorillonite 6-8 parts
Nano silicon 6-8 parts
Portland cement 1-2 parts
7-9 parts of APES phosphate
KH-560 6-8 parts
Polyquaternium modification sulphonation polyetheramine -6-9 parts of hyperbranched poly pyrrole throat copolymer
Polyisocyanates 1-2 parts
Deionized water 17-20 parts
Dimethyl sulfoxide (DMSO) 2-3 parts.
3. multifunctional nano waterproof interlayer coating according to claim 1, it is characterised in that in parts by weight, its preparation
Raw material includes following components：
7 parts of montmorillonite
7 parts of nano silicon
2 parts of portland cement
8 parts of APES phosphate
7 parts of KH-560
Polyquaternium modification sulphonation polyetheramine -8 parts of hyperbranched poly pyrrole throat copolymer
2 parts of polyisocyanates
19 parts of deionized water
2 parts of dimethyl sulfoxide (DMSO).
4. multifunctional nano waterproof interlayer coating according to claim 1, it is characterised in that the polyquaternium is modified sulphur
Change polyetheramine-hyperbranched poly pyrrole throat copolymer preparation method be：
（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 multifunctional nano waterproof interlayer coating according to claim any one of 1-4, it is characterised in that with weight portion
Meter, its preparing raw material also includes following components：
1-3 parts of 4- azabenzimidazoles
Aniline 1-3 parts of 4- (imidazoles -1- bases).
6. multifunctional nano waterproof interlayer coating according to claim 5, it is characterised in that in parts by weight, its preparation
Raw material also includes following components：
2 parts of 4- azabenzimidazoles
4- (imidazoles -1- bases) 2 parts of aniline.
7. a kind of preparation method of multifunctional nano waterproof interlayer coating, including：By the material described in claim any one of 1-6
Composition is added after being sufficiently mixed 1-100 minutes in mixer, and discharging is obtained.
8. the preparation method of multifunctional nano waterproof interlayer coating according to claim 7, it is characterised in that it is described fully
The time of mixing is 18 minutes.
9. the preparation method of multifunctional nano waterproof interlayer coating according to claim 7, it is characterised in that the stirring
The stir speed (S.S.) of machine is 10 ~ 1000 revs/min.
10. the preparation method of multifunctional nano waterproof interlayer coating according to claim 9, it is characterised in that described to stir
The stir speed (S.S.) for mixing machine is 300 revs/min.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402517A (en) * | 2008-10-23 | 2009-04-08 | 马鞍山市天锦云漆业有限公司 | Waterproof coating material for water-proof buildings |
| CN105623325A (en) * | 2016-03-28 | 2016-06-01 | 云南佑琳生科技有限公司 | Thick steel-structure fireproof radiation protective paint |
| 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 |
| CN106116095A (en) * | 2016-08-01 | 2016-11-16 | 郑经耀 | A kind of sludge dryer and the method using this drying machine drying mud |
| CN106318128A (en) * | 2016-09-18 | 2017-01-11 | 北京佑琳生科技有限公司 | Outdoor ultrathin fireproof coating |
-
2017
- 2017-01-16 CN CN201710027425.5A patent/CN106752801A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101402517A (en) * | 2008-10-23 | 2009-04-08 | 马鞍山市天锦云漆业有限公司 | Waterproof coating material for water-proof buildings |
| CN105623325A (en) * | 2016-03-28 | 2016-06-01 | 云南佑琳生科技有限公司 | Thick steel-structure fireproof radiation protective paint |
| 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 |
| CN106116095A (en) * | 2016-08-01 | 2016-11-16 | 郑经耀 | A kind of sludge dryer and the method using this drying machine drying mud |
| 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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