CN113801566B - Moisture-curing concrete sealing interface agent coating and preparation method thereof - Google Patents
Moisture-curing concrete sealing interface agent coating and preparation method thereof Download PDFInfo
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- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
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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
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Abstract
The invention discloses a moisture-curing concrete sealing interface agent coating, which comprises the following components: the self-catalyzed silane modified polyurethane prepolymer comprises the following components: the epoxy resin modified by blocked amine, the silane coupling agent modified by blocked amine, m-xylylene diisocyanate, castor oil modified polyester polyol, KH-560 and 4, 4-diphenylmethane diisocyanate. The invention is applied to the wet concrete base material, has excellent adhesive force with the concrete base material, high surface drying speed, good permeability and high strength, and further improves the surface strength and the construction efficiency of the concrete.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a moisture-curing concrete sealing interface agent coating and a preparation method thereof.
Background
Along with the rapid development of the high-speed railway industry in China and the requirement on the protection period, the quality of the concrete base material is more and more emphasized, and meanwhile, higher requirements are also put forward on the protection of the concrete base material. The high-speed train constructed high-speed railway bridge base material is mainly of a reinforced concrete structure, the surface of the base material is provided with a certain hole structure, micro cracks can be generated under external stress, and the bearing capacity of the bridge can not be influenced in a short time; but along with rain wash and infiltration, the reinforcing steel bar is corroded, so that the bearing capacity of the bridge is weakened, the service life is shortened, and more importantly, hidden dangers are brought to traffic transportation. Therefore, the waterproof and protective device has important significance for waterproof and protective of the bridge main body, the bridge deck expansion joint and other parts.
At present, the polyurethane elastic waterproof coating is used as a lot of bridge and expansion joint waterproof materials, and has the characteristics of convenience in construction, good low-temperature flexibility, high elongation, high strength and the like. However, when the polyurethane elastic waterproof coating is used alone on a concrete surface with certain holes and loose, the defects of bubbling, easy peeling, low bonding strength of a wet interface and the like can occur, so that an interface agent coating with excellent permeability is needed, has a certain crosslinking density, can seal the holes, and can prevent water from permeating after being cured.
The most commonly used concrete interface agent coating at present is epoxy interface agent coating and polyurethane interface agent coating. The epoxy interface agent coating has the characteristics of adjustable crosslinking density, good permeability, high strength, excellent adhesion with a concrete substrate and the like, but has low curing speed, is difficult to cure at low temperature and has low construction efficiency. The polyurethane interface agent coating has high curing speed, but has the defects of short pot life, surface foaming and the like. At present, an organosilicon modified polyurethane moisture-curing concrete sealing interface agent coating needs to be matched with other auxiliary agents for use, for example, an organosilicon modified polyurethane moisture-curing concrete sealing interface agent coating with an additional catalyst, but the isocyanate group of the organosilicon modified polyurethane moisture-curing concrete sealing interface agent coating directly reacts with water to generate CO2The gas can cause defects such as bubbling, cracking, acne and the like on the surface of the interface agent, and the surface state of the interface agent coating is seriously influenced after the interface agent coating is cured, so that the adhesive force of the interface agent coating on a wet substrate is seriously reduced; and the tack-free time is long.
Disclosure of Invention
The technical problem to be solved by the invention is to provide the autocatalytic organic silicon modified polyurethane moisture-cured concrete sealing interface agent coating and the preparation method thereof, the prepared coating is used on a moisture concrete base material, has excellent adhesive force with the concrete base material, and has the advantages of high surface drying speed, good permeability and high strength, and the surface strength and the construction efficiency of the concrete can be further improved.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows.
A moisture-curing concrete sealing interface agent coating comprises the following components in parts by weight:
self-catalytic silane modified polyurethane prepolymer | 20-50 parts of |
Solvent(s) | 30-60 parts |
Defoaming agent | 0.2 to 1 portion |
Leveling agent | 0.2 to 1 portion |
Anti-settling aid | 2-5 parts of |
Wetting and dispersing agent | 1-4 parts of |
Color paste | 3 to 6 portions of |
Blocked acids | 0.1 to 0.3 portion |
Quartz sand | 5-20Portions are |
The self-catalytic silane modified polyurethane prepolymer is an organosilane coupling agent modified polyurethane prepolymer containing a closed amine.
The moisture-curing concrete sealing interface agent coating is prepared from the following components in parts by weight:
blocked amine modified epoxy resins | 15-30 parts of |
Blocked amine modified silane coupling agents | 2-5 parts of |
M-xylylene diisocyanate | 20-40 parts of |
Castor oil modified polyester polyol | 10-15 parts of |
KH-560 | 1-5 parts of |
4, 4' -diphenylmethane diisocyanate | 15-35 parts of |
The sealing amine modified epoxy resin is prepared from the following components in parts by weight:
epoxy resin E-44 | 63 parts of |
Ethanolamine | 17 portions of |
Isobutyraldehyde | 20 portions of |
The sealing amine modified epoxy resin is prepared by the following method:
s1, adding ethanolamine into a four-mouth bottle with a water separator, mechanical stirring and a thermometer, adding epoxy resin E-44 in 4 equal parts in batches, keeping the temperature within 30 ℃ for reaction for 2 hours, heating to 45 ℃, continuing to react for 3 hours, and stopping heating after the epoxy value is determined to be 0;
s2, adding isobutyraldehyde in 2 equal parts according to batches, stirring while adding, keeping the temperature at 45 ℃ for reacting for 2 hours, adding toluene with a water-carrying agent, reacting for 3-4 hours at a set temperature of 90-110 ℃, and removing the toluene with the water-carrying agent in the four-mouth bottle under reduced pressure after the water yield reaches a theoretical value to obtain the closed amine modified epoxy resin.
The chemical reaction formula of the blocked amine modified epoxy resin is as follows.
The moisture-curing concrete sealing interface agent coating is characterized in that the sealing amine modified silane coupling agent is prepared from the following components in parts by weight:
KH-550 | 66 portions of |
Benzaldehyde | 34 portions of |
The sealing amine modified silane coupling agent is prepared by the following method: adding KH-550 into a four-mouth bottle with a mechanical stirring device, a distilling device and a constant pressure dropping funnel, dropwise adding benzaldehyde while stirring, setting the temperature at 95 ℃, decompressing and removing water, and keeping the vacuum degree at 0.095 MPa; and after the dropwise addition is finished, continuously vacuumizing, setting the temperature to be 105 ℃, continuously reacting for 2h, and stopping heating to obtain the blocked amine modified silane coupling agent.
The chemical reaction formula of the blocked amine modified silane coupling agent is as follows.
The moisture-curing concrete sealing interface agent coating is prepared from the following components in parts by weight:
polyethylene terephthalate | 34 portions of |
Ethylene glycol | 2 portions of |
Castor oil | 64 portions |
According to the moisture-curing concrete sealing interface agent coating, the castor oil modified polyester polyol is prepared by the following method: adding polyethylene terephthalate, ethylene glycol and castor oil into a four-mouth bottle with mechanical stirring and nitrogen protection, setting the temperature to be 120 ℃, after the polyethylene terephthalate is dissolved, setting the temperature to be 180 ℃ for reaction for 2 hours, gradually raising the temperature to be 220 ℃ within 30min, carrying out transesterification reaction for 3 hours, and stopping heating to obtain the castor oil modified polyester polyol.
The self-catalytic silane modified polyurethane prepolymer is prepared by the following method: adding KH-560, 4-diphenylmethane diisocyanate and m-xylylene diisocyanate into a four-mouth bottle with mechanical stirring and nitrogen protection, setting the temperature to be 120 ℃ for reaction for 3h, adding the blocked amine modified epoxy resin and the castor oil modified polyester polyol after measuring the content of the isocyanate group to be 32w% -42w%, setting the temperature to be 80-85 ℃ for reaction for 3h, cooling to room temperature after measuring the content of the isocyanate group to be 16w% -18.5w%, adding the blocked amine modified silane coupling agent, and uniformly mixing to obtain the autocatalytic silane modified polyurethane prepolymer.
The moisture-curing concrete sealing interface agent coating is prepared from the following components in parts by weight:
polyether 330N | 10 to 20 portions of |
Polyether 220 | 15-35 |
Titanium white powder | 20-40 parts of |
Carbon black | 5 to 10 portions of |
Wetting and dispersing agent | 5-8 parts of |
Defoaming agent | 2-6 parts of |
The moisture-curing concrete sealing interface agent coating is prepared from the following color paste by the following method: adding polyether 330N, polyether 220, carbon black and wetting dispersant into a sand mill according to the formula amount, and stirring for 10-15 minutes at 1000-1200 rpm; adding titanium dioxide and a defoaming agent, stirring for 15-20 minutes at 1000-1200 rpm, grinding to below 30um, and discharging.
A preparation method of a moisture-curing concrete sealing interface agent coating comprises the following steps: adding the autocatalysis silane modified polyurethane prepolymer and the solvent into a closed high-speed stirring kettle according to the formula amount, stirring for 10-15 minutes at 800 revolutions per minute, adding color paste, a defoaming agent, a leveling agent, an anti-precipitation auxiliary agent, a wetting dispersant, quartz sand and enclosed acid, stirring for 20-35 minutes at 600 revolutions per minute and discharging.
Due to the adoption of the technical scheme, the technical progress of the invention is as follows.
The invention is particularly suitable for plugging concrete base materials with holes or loose surfaces in a humid environment, is also suitable for protecting bridge deck expansion joints and other positions, and has the characteristics of excellent adhesive force with the concrete base materials, high surface drying speed, good permeability and high strength.
In the invention, because the closed amine modified epoxy resin in the autocatalytic silane modified polyurethane prepolymer has oxazolidine, the tertiary amine has higher catalytic effect on the moisture curing of polyurethane and silane; meanwhile, oxazolidine and imine structures are easy to hydrolyze, the reactivity is far higher than that of isocyanate and water, amino containing hydroxyl and having active hydrogen is generated by hydrolysis, and the amino can react with isocyanate to generate groups with larger cohesive force such as carbamido and carbamate bonds and the like and can generate hydrogen bonds with a concrete substrate, so that the surface strength of concrete is improved, the mechanical property of the concrete can be better improved by the interface agent coating which permeates into the concrete, and the surface drying time and the actual drying time are greatly shortened.
Detailed Description
A moisture-curing concrete sealing interface agent coating comprises the following components in parts by weight:
self-catalytic silane modified polyurethane prepolymer | 20-50 parts of |
Solvent(s) | 30-60 parts |
Defoaming agent | 0.2 to 1 portion |
Leveling agent | 0.2 to 1 portion |
Anti-settling aid | 2-5 parts of |
Wetting and dispersing agent | 1 to 4 portions of |
Color paste | 3-6 parts of |
Blocked acids | 0.1 to 0.3 portion |
Quartz sand | 5-20 parts of |
Wherein the self-catalytic silane modified polyurethane prepolymer is an organosilane coupling agent modified polyurethane prepolymer containing blocked amine; the autocatalytic silane modified polyurethane prepolymer is prepared from the following components in parts by weight:
blocked amine modified epoxy resins | 15-30 parts of |
Blocked amine modified silane coupling agents | 2-5 parts of |
M-xylylene diisocyanate | 20-40 parts of |
Castor oil modified polyester polyol | 10 to 15 portions of |
KH-560 | 1-5 parts of |
4, 4' -diphenylmethane diisocyanate | 15-35 parts of |
The blocked amine modified epoxy resin in the autocatalytic silane modified polyurethane prepolymer is prepared from the following components in parts by weight:
epoxy resin E-44 | 63 parts of |
Ethanolamine | 17 portions of |
Isobutyraldehyde | 20 portions of |
The blocked amine modified epoxy resin is prepared by the following method: s1, adding ethanolamine into a four-mouth bottle with a water separator, mechanical stirring and a thermometer, adding epoxy resin E-44 in 4 equal parts in batches, keeping the temperature within 30 ℃ for reaction for 2 hours, heating to 45 ℃, continuing to react for 3 hours, and stopping heating after the epoxy value is determined to be 0; s2, adding isobutyraldehyde in 2 equal parts in batches, stirring while adding, reacting for 2 hours at the temperature of 45 ℃, adding 10 parts of water-carrying agent toluene, reacting for 3-4 hours at the set temperature of 90-110 ℃, measuring the water yield to reach 5 parts, and removing the water-carrying agent toluene in the four-mouth bottle under reduced pressure to obtain the closed amine modified epoxy resin.
The blocked amine modified silane coupling agent in the autocatalytic silane modified polyurethane prepolymer is prepared from the following components in parts by weight:
KH-550 | 66 portions of |
Benzaldehyde | 34 portions of |
The blocked amine modified silane coupling agent is prepared by the following method: adding KH-550 into a four-mouth bottle with a mechanical stirring device, a distilling device and a constant pressure dropping funnel, dropwise adding benzaldehyde while stirring, setting the temperature at 95 ℃, decompressing and removing water, and keeping the vacuum degree at 0.095 MPa; and after the dropwise addition is finished, continuously vacuumizing, setting the temperature to be 105 ℃, continuously reacting for 2h, and stopping heating to obtain the blocked amine modified silane coupling agent.
The castor oil modified polyester polyol in the autocatalytic silane modified polyurethane prepolymer is prepared from the following components in parts by weight:
polyethylene terephthalate | 34 portions of |
Ethylene glycol | 2 portions of |
Castor oil | 64 portions |
The castor oil modified polyester polyol is prepared by the following method: adding polyethylene terephthalate, ethylene glycol and castor oil into a four-mouth bottle with mechanical stirring and nitrogen protection, setting the temperature to be 120 ℃, after the polyethylene terephthalate is dissolved, setting the temperature to be 180 ℃ for reaction for 2 hours, gradually raising the temperature to be 220 ℃ within 30min, carrying out transesterification reaction for 3 hours, and stopping heating to obtain the castor oil modified polyester polyol.
The autocatalytic silane modified polyurethane prepolymer is prepared by the following method: adding KH-560, 4' -diphenylmethane diisocyanate and m-xylylene diisocyanate into a four-mouth bottle with mechanical stirring and nitrogen protection, setting the temperature to be 120 ℃ for reaction for 3h, adding the blocked amine modified epoxy resin and the castor oil modified polyester polyol after measuring the content of the isocyanate group to be 32w% -42w%, setting the temperature to be 80-85 ℃ for reaction for 3h, cooling to room temperature after measuring the content of the isocyanate group to be 16w% -18.5w%, adding the blocked amine modified silane coupling agent, and uniformly mixing to obtain the autocatalytic silane modified polyurethane prepolymer.
The color paste in the moisture-cured concrete sealing interface agent coating is prepared from the following components in parts by weight:
polyether 330N | 10-20 parts of |
Polyether 220 | 15-35 |
Titanium white powder | 20 to 40 portions of |
Carbon black | 5-10 parts of |
Wetting and dispersing agent | 5-8 parts of |
Defoaming agent | 2-6 parts of |
The color paste is prepared by the following method: adding polyether 330N, polyether 220, carbon black and wetting dispersant into a sand mill according to the formula amount, and stirring for 10-15 minutes at 1000-1200 rpm; adding titanium dioxide and a defoaming agent, stirring for 15-20 minutes at 1000-1200 rpm, grinding to below 30um, and discharging.
The solvent in the moisture-cured concrete sealing interface agent coating is one or more mixed solvents of propyl acetate, butyl acetate, propylene glycol monomethyl ether acetate and No. 150 solvent oil; the antifoaming agent is KMT-2024; the leveling agent is KMT-1023; the wetting dispersant is KMT-310; the anti-precipitation auxiliary agent is KMT-4007; the blocked acid is HJ-001.
The invention provides a preparation method of a moisture-curing concrete sealing interface agent coating, which comprises the following steps: adding the autocatalysis silane modified polyurethane prepolymer and the solvent into a closed high-speed stirring kettle according to the formula amount, stirring for 10-15 minutes at 800 revolutions per minute, adding color paste, a defoaming agent, a leveling agent, an anti-precipitation auxiliary agent, a wetting dispersant, quartz sand and a closed acid, stirring for 20-35 minutes at 600 revolutions per minute and discharging. The addition of the blocked acid can react with the blocked amine to form a quaternary ammonium salt, thereby promoting the hydrolysis of the blocked amine.
The present invention will be described in further detail with reference to specific embodiments, but the examples of the present invention are merely illustrative and the present invention is not limited to the embodiments in any way.
Example 1
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 1
Adding 5 parts of KH-560, 20 parts of m-xylylene diisocyanate and 35 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 32.8-33.1 w%, adding 20 parts of blocked amine modified epoxy resin and 15 parts of castor oil modified polyester polyol, heating to 80 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 16.0-16.2 w%, adding 5 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer # 1.
Step 2), preparing the moisture-curing concrete sealing interface agent coating
Adding 19 parts by weight of autocatalytic silane modified polyurethane prepolymer No. 1, 11 parts by weight of propyl acetate, 18 parts by weight of butyl acetate and 24.9 parts by weight of No. 150 solvent oil into a closed high-speed stirring kettle, stirring for 10 minutes at 800 r/min, adding 3 parts by weight of color paste, 0.2 part by weight of defoaming agent KMT-2024, 0.8 part by weight of leveling agent KMT-1023, 5 parts by weight of anti-precipitation auxiliary agent KMT-4007, 4 parts by weight of wetting dispersant KMT-310, 20 parts by weight of 200-mesh quartz sand and 0.1 part by weight of enclosed acid, stirring for 30 minutes at 500 r/min, and discharging.
Example 2
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 1
Adding 5 parts of KH-560, 20 parts of m-xylylene diisocyanate and 35 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 32.8-33.1 w%, adding 20 parts of blocked amine modified epoxy resin and 15 parts of castor oil modified polyester polyol, heating to 85 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 16.0-16.2 w%, adding 5 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer # 1.
Step 2), preparing the moisture-curing concrete sealing interface agent coating
Adding 20 parts by weight of autocatalytic silane modified polyurethane prepolymer No. 1, 4.9 parts by weight of propyl acetate, 18 parts by weight of butyl acetate and 25 parts by weight of No. 150 solvent oil into a closed high-speed stirring kettle, stirring for 15 minutes at 500 revolutions per minute, adding 3 parts by weight of color paste, 0.2 part by weight of defoaming agent KMT-2024, 0.8 part by weight of leveling agent KMT-1023, 5 parts by weight of anti-precipitation auxiliary agent KMT-4007, 4 parts by weight of wetting dispersant KMT-310, 20 parts by weight of 200-mesh quartz sand and 0.1 part by weight of enclosed acid, stirring for 20 minutes at 600 revolutions per minute, and discharging.
Example 3
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 1
Adding 5 parts of KH-560, 20 parts of m-xylylene diisocyanate and 35 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 32.8-33.1 w%, adding 20 parts of blocked amine modified epoxy resin and 15 parts of castor oil modified polyester polyol, heating to 82 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 16.0-16.2 w%, adding 5 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer # 1.
Step 2), preparing the moisture-curing concrete sealing interface agent coating
Adding 25 parts by weight of autocatalytic silane modified polyurethane prepolymer No. 1, 20 parts by weight of butyl acetate, 23 parts by weight of No. 150 solvent oil and 17 parts by weight of propylene glycol methyl ether acetate into a closed high-speed stirring kettle, stirring for 12 minutes at 600 revolutions per minute, adding 2.8 parts by weight of color paste, 0.2 part by weight of defoamer KMT-2024, 0.8 part by weight of flatting agent KMT-1023, 2 parts by weight of anti-precipitation aid KMT-4007, 2 parts by weight of wetting dispersant KMT-310, 7 parts by weight of 200-mesh quartz sand and 0.3 part by weight of enclosed acid, stirring for 35 minutes at 300 revolutions per minute, and discharging.
Example 4
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 1
Adding 5 parts of KH-560, 20 parts of m-xylylene diisocyanate and 35 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 32.8-33.1 w%, adding 20 parts of blocked amine modified epoxy resin and 15 parts of castor oil modified polyester polyol, heating to 83 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 16.0-16.2 w%, adding 5 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer # 1.
Step 2), preparing the moisture-cured concrete sealing interface agent coating
Adding 40 parts by weight of autocatalytic silane modified polyurethane prepolymer No. 1, 10 parts by weight of butyl acetate, 10 parts by weight of No. 150 solvent oil and 15 parts by weight of propylene glycol methyl ether acetate into a closed high-speed stirring kettle, stirring for 15 minutes at 500 revolutions per minute, adding 6 parts by weight of color paste, 0.5 part by weight of defoaming agent KMT-2024, 0.5 part by weight of leveling agent KMT-1023, 2 parts by weight of anti-precipitation auxiliary agent KMT-4007, 1 part by weight of wetting dispersant KMT-310, 14.8 parts by weight of 200-mesh quartz sand and 0.2 part by weight of enclosed acid, stirring for 30 minutes at 400 revolutions per minute, and discharging.
Example 5
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 1
Adding 5 parts of KH-560, 20 parts of m-xylylene diisocyanate and 35 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 32.8-33.1 w%, adding 20 parts of blocked amine modified epoxy resin and 15 parts of castor oil modified polyester polyol, heating to 80 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 16.0-16.2 w%, adding 5 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer # 1.
Step 2), preparing the moisture-cured concrete sealing interface agent coating
Adding 50 parts of polyurethane prepolymer No. 1, 15 parts of butyl acetate, 10 parts of No. 150 solvent oil and 10 parts of propylene glycol methyl ether acetate into a closed high-speed stirring kettle in parts by weight, stirring for 10 minutes at 800 revolutions per minute, adding 4 parts of color paste, 1 part of defoaming agent KMT-2024, 1 part of flatting agent KMT-1023, 1 part of anti-settling auxiliary agent KMT-4007, 2.8 parts of wetting dispersant KMT-310, 5 parts of 200-mesh quartz sand and 0.2 part of enclosed acid, stirring for 20 minutes at 600 revolutions per minute, and discharging.
Example 6
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 2
Adding 1 part of KH-560, 40 parts of m-xylylene diisocyanate and 15 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 40.5-40.7 w%, adding 30 parts of blocked amine modified epoxy resin and 10 parts of castor oil modified polyester polyol, heating to 85 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 17.9-18.1 w%, adding 4 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer No. 2.
Step 2), preparing the moisture-curing concrete sealing interface agent coating
Adding 20 parts by weight of autocatalytic silane modified polyurethane prepolymer No. 2, 4.9 parts by weight of propyl acetate, 18 parts by weight of butyl acetate and 25 parts by weight of No. 150 solvent oil into a closed high-speed stirring kettle, stirring for 13 minutes at 700 r/min, adding 3 parts by weight of color paste, 0.2 part by weight of defoaming agent KMT-2024, 0.8 part by weight of leveling agent KMT-1023, 5 parts by weight of anti-precipitation auxiliary agent KMT-4007, 4 parts by weight of wetting dispersant KMT-310, 20 parts by weight of 200-mesh quartz sand and 0.1 part by weight of enclosed acid, stirring for 25 minutes at 500 r/min, and discharging.
Example 7
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 2
Adding 1 part of KH-560, 40 parts of m-xylylene diisocyanate and 15 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 40.5-40.7 w%, adding 30 parts of blocked amine modified epoxy resin and 10 parts of castor oil modified polyester polyol, heating to 84 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 17.9-18.1 w%, adding 4 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer No. 2.
Step 2), preparing the moisture-curing concrete sealing interface agent coating
Adding 25 parts by weight of autocatalytic silane modified polyurethane prepolymer No. 2, 20 parts by weight of butyl acetate, 23 parts by weight of No. 150 solvent oil and 17 parts by weight of propylene glycol methyl ether acetate into a closed high-speed stirring kettle, stirring for 12 minutes at 650 revolutions per minute, adding 2.8 parts by weight of color paste, 0.2 part by weight of defoamer KMT-2024, 0.8 part by weight of flatting agent KMT-1023, 2 parts by weight of anti-precipitation aid KMT-4007, 2 parts by weight of wetting dispersant KMT-310, 7 parts by weight of 200-mesh quartz sand and 0.3 part by weight of enclosed acid, stirring for 25 minutes at 500 revolutions per minute, and discharging.
Example 8
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 2
Adding 1 part of KH-560, 40 parts of m-xylylene diisocyanate and 15 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 40.5-40.7 w%, adding 30 parts of blocked amine modified epoxy resin and 10 parts of castor oil modified polyester polyol, heating to 85 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 17.9-18.1 w%, adding 4 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer No. 2.
Step 2), preparing the moisture-curing concrete sealing interface agent coating
Adding 40 parts by weight of autocatalytic silane modified polyurethane prepolymer No. 2, 10 parts by weight of butyl acetate, 10 parts by weight of 150# solvent oil and 15 parts by weight of propylene glycol methyl ether acetate into a closed high-speed stirring kettle, stirring for 10 minutes at 800 r/min, adding 6 parts by weight of color paste, 0.5 part by weight of defoamer KMT-2024, 0.5 part by weight of flatting agent KMT-1023, 2 parts by weight of anti-precipitation auxiliary agent KMT-4007, 1 part by weight of wetting dispersant KMT-310, 14.8 parts by weight of 200-mesh quartz sand and 0.2 part by weight of enclosed acid, stirring for 20 minutes at 600 r/min, and discharging.
Example 9
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 2
Adding 1 part of KH-560, 40 parts of m-xylylene diisocyanate and 15 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 40.5-40.7 w%, adding 30 parts of blocked amine modified epoxy resin and 10 parts of castor oil modified polyester polyol, heating to 80 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 17.9-18.1 w%, adding 4 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer No. 2.
Step 2), preparing the moisture-cured concrete sealing interface agent coating
Adding 50 parts of polyurethane prepolymer 2#, 15 parts of butyl acetate, 10 parts of 150# solvent oil and 10 parts of propylene glycol methyl ether acetate into a closed high-speed stirring kettle in parts by weight, stirring for 15 minutes at 500 revolutions per minute, adding 4 parts of color paste, 1 part of defoaming agent KMT-2024, 1 part of flatting agent KMT-1023, 1 part of anti-settling auxiliary agent KMT-4007, 2.8 parts of wetting dispersant KMT-310, 5 parts of 200-mesh quartz sand and 0.2 part of enclosed acid, stirring for 20 minutes at 600 revolutions per minute, and discharging.
Example 10
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 3
Adding 4 parts of KH-560, 36 parts of m-xylylene diisocyanate and 20 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 38.6 w% -36.8 w%, adding 25 parts of blocked amine modified epoxy resin and 13 parts of castor oil modified polyester polyol, heating to 80 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 17.2 w% -17.4 w%, adding 2 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer No. 3.
Step 2), preparing the moisture-cured concrete sealing interface agent coating
Adding 20 parts by weight of autocatalytic silane modified polyurethane prepolymer No. 3, 4.9 parts by weight of propyl acetate, 18 parts by weight of butyl acetate and 25 parts by weight of 150# solvent oil into a closed high-speed stirring kettle, stirring for 15 minutes at 500 revolutions per minute, adding 3 parts by weight of color paste, 0.2 part by weight of defoaming agent KMT-2024, 0.8 part by weight of leveling agent KMT-1023, 5 parts by weight of anti-precipitation auxiliary agent KMT-4007, 4 parts by weight of wetting dispersant KMT-310, 20 parts by weight of 200-mesh quartz sand and 0.1 part by weight of enclosed acid, stirring for 35 minutes at 300 revolutions per minute, and discharging.
Example 11
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 3
Adding 4 parts of KH-560, 36 parts of m-xylylene diisocyanate and 20 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 38.6-36.8 w%, adding 25 parts of blocked amine modified epoxy resin and 13 parts of castor oil modified polyester polyol, heating to 85 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 17.2-17.4 w%, adding 2 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer No. 3.
Step 2), preparing the moisture-curing concrete sealing interface agent coating
Adding 25 parts by weight of autocatalytic silane modified polyurethane prepolymer No. 3, 20 parts by weight of butyl acetate, 23 parts by weight of No. 150 solvent oil and 17 parts by weight of propylene glycol methyl ether acetate into a closed high-speed stirring kettle, stirring for 12 minutes at 600 revolutions per minute, adding 2.8 parts by weight of color paste, 0.2 part by weight of defoamer KMT-2024, 0.8 part by weight of flatting agent KMT-1023, 2 parts by weight of anti-precipitation aid KMT-4007, 2 parts by weight of wetting dispersant KMT-310, 7 parts by weight of 200-mesh quartz sand and 0.3 part by weight of enclosed acid, stirring for 30 minutes at 500 revolutions per minute, and discharging.
Example 12
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 3
Adding 4 parts of KH-560, 36 parts of m-xylylene diisocyanate and 20 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 38.6-36.8 w%, adding 25 parts of blocked amine modified epoxy resin and 13 parts of castor oil modified polyester polyol, heating to 85 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 17.2-17.4 w%, adding 2 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer No. 3.
Step 2), preparing the moisture-curing concrete sealing interface agent coating
Adding 40 parts by weight of autocatalytic silane modified polyurethane prepolymer No. 3, 10 parts by weight of butyl acetate, 10 parts by weight of 150# solvent oil and 15 parts by weight of propylene glycol methyl ether acetate into a closed high-speed stirring kettle, stirring for 10 minutes at 800 r/min, adding 6 parts by weight of color paste, 0.5 part by weight of defoamer KMT-2024, 0.5 part by weight of flatting agent KMT-1023, 2 parts by weight of anti-precipitation auxiliary agent KMT-4007, 1 part by weight of wetting dispersant KMT-310, 14.8 parts by weight of 200-mesh quartz sand and 0.2 part by weight of enclosed acid, stirring for 20 minutes at 600 r/min, and discharging.
Example 13
Step 1), preparing autocatalytic silane modified polyurethane prepolymer No. 3
Adding 4 parts of KH-560, 36 parts of m-xylylene diisocyanate and 20 parts of 4, 4-diphenylmethane diisocyanate into a four-mouth bottle, gradually heating to 120 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 38.6-36.8 w%, adding 25 parts of blocked amine modified epoxy resin and 13 parts of castor oil modified polyester polyol, heating to 80 ℃ for reaction for 3 hours, measuring the content of isocyanate to be 17.2-17.4 w%, adding 2 parts of blocked amine modified silane coupling agent, and stopping heating to obtain the autocatalytic silane modified polyurethane prepolymer No. 3.
Step 2), preparing the moisture-curing concrete sealing interface agent coating
Adding 50 parts of polyurethane prepolymer No. 3, 15 parts of butyl acetate, 10 parts of No. 150 solvent oil and 10 parts of propylene glycol methyl ether acetate into a closed high-speed stirring kettle in parts by weight, stirring for 12 minutes at 600 revolutions per minute, adding 4 parts of color paste, 1 part of defoaming agent KMT-2024, 1 part of flatting agent KMT-1023, 1 part of anti-settling auxiliary agent KMT-4007, 2.8 parts of wetting dispersant KMT-310, 5 parts of 200-mesh quartz sand and 0.2 part of enclosed acid, stirring for 30 minutes at 500 revolutions per minute, and discharging.
Comparative example 1
The prepolymer was a silane-modified polyurethane prepolymer, as in example 2.
Comparative example 2
The prepolymer was a silane-modified polyurethane prepolymer, as in example 3.
Comparative example 3
The prepolymer was a silane-modified polyurethane prepolymer, as in example 4.
Comparative example 4
The prepolymer was a silane-modified polyurethane prepolymer, as in example 5.
Comparative example 5
The prepolymer is prepared from 1:1 autocatalytic silane modified polyurethane prepolymer No. 1 and silane modified polyurethane prepolymer, and the rest is the same as example 2.
Comparative example 6
The prepolymer was made from 1:1 autocatalytic silane-modified polyurethane prepolymer # 2 and silane-modified polyurethane prepolymer, as in example 3.
Comparative example 7
The prepolymer is prepared from a 1:1 autocatalytic silane modified polyurethane prepolymer No. 3 and a silane modified polyurethane prepolymer, and the rest is the same as in example 4.
The adhesion of the examples and comparative examples was tested in accordance with GB/T16777-2008, Chapter A7, the tack free time of the examples and comparative examples was tested in accordance with GB/T16777-. The test results are given in table 1 below.
TABLE 1
As can be seen from Table 1, the surface drying time of the autocatalysis organic silicon modified polyurethane moisture curing concrete sealing interface agent coating prepared by the polyurethane prepolymer containing the sealing amine modified epoxy resin and the sealing amine modified silane coupling agent in the examples 1-13 is within 3min, and the actual drying time is within 6 min. Comparative examples 1 to 4 are prepared organosilicon modified polyurethane moisture-curing concrete sealing interface agent coatings without a sealing amine modified epoxy and a sealing amine modified silane coupling agent, the surface drying time is 11 to 25min, and the actual drying time is 20 to 40min, and comparative examples 5 to 7 are double-spliced organosilicon modified polyurethane moisture-curing concrete sealing interface agent coatings, the surface drying time is 5 to 6min, and the actual drying time is 10 to 15 min.
The data analysis shows that when the content of the autocatalytic organosilicon modified polyurethane is too low, the matching adhesion force is poor, and interlayer cracking is caused due to small winding and interaction force between the elastomer and the interface agent coating molecules and poor interlayer adhesion force; with the increase of the content of the autocatalysis organic silicon modified polyurethane, the permeability of the sealing interface agent on the surface of the concrete is increased, the surface strength of the concrete is improved, the surface drying time and the actual drying time are both greatly shortened, and the construction efficiency is further improved.
Claims (8)
1. The moisture-curing concrete sealing interface agent coating is characterized by being prepared from the following components in parts by weight:
20-50 parts of self-catalytic silane modified polyurethane prepolymer,
30-60 parts of a solvent, namely,
0.2 to 1 portion of defoaming agent,
0.2 to 1 portion of flatting agent,
2-5 parts of an anti-precipitation auxiliary agent,
1-4 parts of a wetting dispersant,
3-6 parts of color paste,
0.1 to 0.3 portion of closed acid,
5-20 parts of quartz sand;
the autocatalytic silane modified polyurethane prepolymer is prepared from the following components in parts by weight:
15-30 parts of blocked amine modified epoxy resin,
2-5 parts of blocked amine modified silane coupling agent,
20-50 parts of m-xylylene diisocyanate,
10-15 parts of castor oil modified polyester polyol,
KH-5601-5 parts,
5-35 parts of 4, 4-diphenylmethane diisocyanate;
the self-catalytic silane modified polyurethane prepolymer is prepared by the following method: mixing KH-560, 4,Adding diphenylmethane diisocyanate and m-xylylene diisocyanate into a four-mouth bottle with mechanical stirring and nitrogen protection, setting the temperature to be 120 ℃ for reaction for 3 hours, measuring the content of the isocyanic acid radical to be 32w% -42w%, adding blocked amine modified epoxy resin and castor oil modified polyester polyol, setting the temperature to be 80-85 ℃, reacting for 3 hours, measuring the content of the isocyanic acid radical to be 16w% -18.5w%, cooling to room temperature, adding a blocked amine modified silane coupling agent, and uniformly mixing to obtain the autocatalytic silane modified polyurethane prepolymer.
2. The moisture-curable concrete sealing interface agent coating as claimed in claim 1, wherein the sealing amine modified epoxy resin is prepared from the following components in parts by weight: epoxy resin E-4463, ethanolamine 17 and isobutyraldehyde 20.
3. The moisture-curable concrete close-interface agent coating as claimed in claim 2, wherein the close-amine modified epoxy resin is prepared by the following method:
s1, adding ethanolamine into a four-mouth bottle with a water separator, mechanical stirring and a thermometer, adding epoxy resin E-44 in 4 equal parts in batches, keeping the temperature within 30 ℃ for reaction for 2 hours, heating to 45 ℃, continuing to react for 3 hours, and stopping heating after the epoxy value is determined to be 0;
s2, adding isobutyraldehyde in 2 equal parts according to batches, stirring while adding, keeping the temperature at 45 ℃ for reacting for 2 hours, adding toluene with a water-carrying agent, reacting for 3-4 hours at the set temperature of 90-110 ℃, measuring the water yield to reach 5 parts, and removing the toluene with the water-carrying agent in the four-mouth bottle under reduced pressure to obtain the closed amine modified epoxy resin.
4. The moisture-curable concrete sealing interface agent coating as claimed in claim 1, wherein the sealing amine modified silane coupling agent is prepared from the following components in parts by weight: KH-55066 parts and benzaldehyde 34 parts.
5. The moisture-curable concrete blocking interface agent coating as claimed in claim 4, wherein the blocked amine modified silane coupling agent is prepared by the following method: adding KH-550 into a four-mouth bottle with a mechanical stirring device, a distilling device and a constant pressure dropping funnel, dropwise adding benzaldehyde while stirring, setting the temperature at 95 ℃, decompressing and removing water, and keeping the vacuum degree at 0.095 MPa; and after the dropwise addition is finished, continuously vacuumizing, setting the temperature to be 105 ℃, continuously reacting for 2h, and stopping heating to obtain the blocked amine modified silane coupling agent.
6. The moisture-curable concrete sealing interface agent coating as claimed in claim 1, wherein the castor oil-modified polyester polyol is prepared from the following components in parts by weight: 34 parts of polyethylene terephthalate, 2 parts of ethylene glycol and 64 parts of castor oil.
7. The moisture-curable concrete enclosing interface agent coating as claimed in claim 6, wherein the castor oil modified polyester polyol is prepared by the following method: adding polyethylene terephthalate, ethylene glycol and castor oil into a four-mouth bottle with mechanical stirring and nitrogen protection, setting the temperature to be 120 ℃, after the polyethylene terephthalate is dissolved, setting the temperature to be 180 ℃ for reaction for 2 hours, gradually raising the temperature to be 220 ℃ within 30min, carrying out ester exchange reaction for 3 hours, and stopping heating to obtain the castor oil modified polyester polyol.
8. A method of preparing the moisture-curable concrete enclosing interface agent coating according to any one of claims 1-7, comprising the steps of: adding the autocatalysis silane modified polyurethane prepolymer and the solvent into a closed high-speed stirring kettle according to the formula amount, stirring for 10-15 minutes at 800 revolutions per minute, adding color paste, a defoaming agent, a leveling agent, an anti-precipitation auxiliary agent, a wetting dispersant, quartz sand and enclosed acid, stirring for 20-35 minutes at 600 revolutions per minute and discharging.
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