CN110791165A - Single-component anti-sagging exposed modified polyurethane waterproof coating and preparation method thereof - Google Patents
Single-component anti-sagging exposed modified polyurethane waterproof coating and preparation method thereof Download PDFInfo
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- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- 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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- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention discloses a single-component anti-sagging exposed modified polyurethane waterproof coating and a preparation method thereof, wherein the preparation method comprises the following steps: uniformly mixing hydroxyl-terminated polyether polyol, a plasticizer, a filler, a thixotropic agent and an optional pigment, grinding and dehydrating; cooling, adding isocyanate, carrying out contact reaction, then heating, and continuing to carry out contact reaction; cooling, adding a first acrylate monomer, and carrying out contact reaction at 60-80 ℃; keeping the temperature at 60-80 ℃, adding an initiator, a chain transfer agent and a second acrylic ester monomer, and continuing to perform contact reaction; cooling, adding a latent curing agent, a catalyst, a solvent and optionally other auxiliary agents, and uniformly stirring and mixing to obtain the single-component anti-sagging exposed modified polyurethane waterproof coating. The invention improves the physical property, the ultraviolet resistance, the pressure resistance and the weather resistance of the polyurethane coating film by adopting the acrylate monomer modified polyurethane.
Description
Technical Field
The invention belongs to the technical field of polyurethane waterproof coatings, and particularly relates to a single-component anti-sagging exposed modified polyurethane waterproof coating and a preparation method thereof.
Background
The polyurethane waterproof paint belongs to a chemical reaction type waterproof paint, is a rubber-like high-elasticity coating film after being cured, is seamless as a whole, is called a liquid coiled material in the industry because of excellent comprehensive performance, and is widely applied in the world. The polyurethane waterproof coating in China has been developed for more than 20 years, is rich in product types and excellent in performance, and occupies an important position in the building waterproof industry. However, most polyurethane products on the market today are aromatic polyurethanes, i.e. the isocyanate monomer used is an aromatic isocyanate. Aromatic polyurethane cannot be used for exposed construction due to poor ultraviolet resistance. The traditional aromatic single-component polyurethane waterproof paint adopts aromatic isocyanate, and the curing mechanism is that a prepolymer containing-NCO end groups and moisture in a base layer or air are cured to form a film and CO is released2The traditional aromatic single-component polyurethane waterproof coating is easy to be interfered by the humidity of a construction environment in the construction process, the construction cannot be thick-coated, the cured coating film is easy to have the phenomena of incompact, bubbles, pinholes and the like, and the traditional aromatic single-component polyurethane is low in strength, cannot ensure the weather resistance if applied to an exposed type, and is easy to crack due to the influence of external force to influence the construction performance. Meanwhile, the exposed polyurethane waterproof coating can be frequently used on vertical walls with larger gradient, such as high-rise buildings, reservoirs, dams and the like when in use, but the existing polyurethane waterproof coating is usedThe single-component polyurethane waterproof coating has poor anti-sagging performance, can generate serious sagging phenomenon when a vertical wall with higher height is used, has the phenomenon of thinness at the top and thickness at the bottom, can reach the specified thickness after being coated for many times, wastes manpower and material resources, and delays the construction period.
Most of the existing acrylic waterproof coatings suitable for exposed construction are acrylic waterproof coatings which have excellent weather resistance and corrosion resistance and can be used for exposed construction. But the physical property and low-temperature flexibility of the acrylic coating are poor, and the acrylic coating is easy to crack and leak under the action of external force.
There are also partially exposed polyurethane waterproof coatings on the market, but the coatings are generally two-component exposed polyurethane waterproof coatings. For example, the component A is an isocyanate-terminated prepolymer formed by blending two or three of polyether polyol and Toluene Diisocyanate (TDI), 4-diphenylmethane diisocyanate (MDI) and 1, 6-Hexamethylene Diisocyanate (HDI), the component B is a mixed polyether or castor oil added as a main body, various pigments are added, and the component A, B is mixed to form the colored polyurethane waterproof coating. The polyurethane coating film prepared by adding 1, 6-Hexamethylene Diisocyanate (HDI) has excellent light stability and weather resistance, and the polyurethane main chain formed by the reaction of the added castor oil and the component A has no double-bond structure, so that the polyurethane prepared by the scheme has excellent alkali resistance, heat resistance and ageing resistance. The other is that the component A adopts isophorone diisocyanate (IPDI) to react with polyether polyol to form isocyanate-terminated prepolymer, and the component B adopts polyether, plasticizer, curing agent 3,3 '-dichloro-4, 4' -diaminodiphenylmethane (MOCA) and powder blending. A, B components are blended and reacted to form a film in the construction, wherein isophorone diisocyanate (IPDI) is aliphatic isocyanate, and the film has the characteristics of strong ultraviolet resistance, good weather resistance, no yellowing and the like, so that the film is suitable for exposed application construction. However, when the double-component polyurethane waterproof coating is constructed on site, the materials are required to be mixed according to a certain proportion, mechanical stirring is carried out, bubbles and materials introduced in the stirring process are inaccurate, and the construction quality and the coating performance are affected by uneven stirring, so that waterproof quality accidents are caused occasionally; the single-component polyurethane waterproof coating is a single component, can be used immediately after being opened, does not need stirring, is reliable in construction, and is widely applied. However, the exposed single-component polyurethane waterproof coating on the market has no sagging resistance, so that the sagging phenomenon is inevitably generated during the facade construction, the construction is complicated, and the construction period is prolonged.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, develop a single-component polyurethane waterproof coating which has high strength, compact film, no sagging in vertical construction and excellent physical properties and weather resistance, is used for exposed construction, and expands the application range of the polyurethane waterproof coating in the field of building waterproofing.
In order to achieve the above object, an aspect of the present invention provides a preparation method of a one-component sag-resistant exposed modified polyurethane waterproof coating, the preparation method comprising:
(1) uniformly mixing hydroxyl-terminated polyether polyol, a plasticizer, a filler, a thixotropic agent and an optional pigment, grinding and dehydrating;
(2) cooling, adding isocyanate, carrying out contact reaction, then heating, and continuing to carry out contact reaction;
(3) cooling, adding a first acrylate monomer, and carrying out contact reaction at 60-80 ℃; keeping the temperature at 60-80 ℃, adding an initiator, a chain transfer agent and a second acrylic ester monomer, and continuing to perform contact reaction;
(4) cooling, adding a latent curing agent, a catalyst, a solvent and optionally other auxiliary agents, and uniformly stirring and mixing to obtain the single-component anti-sagging exposed modified polyurethane waterproof coating.
The invention also provides the single-component anti-sagging exposed modified polyurethane waterproof coating prepared by the preparation method.
The technical scheme of the invention has the following advantages:
(1) the invention improves the physical property, the ultraviolet resistance, the pressure resistance and the weather resistance of the polyurethane coating film by adopting the acrylate monomer modified polyurethane.
(2) The invention adopts a latent curing technology to improve the compactness of a coating film and further improve the water resistance and impermeability.
(3) According to the invention, the aliphatic isocyanate is adopted, so that the polyurethane coating has stronger ultraviolet resistance and chemical corrosion resistance, and the single-component polyurethane waterproof coating has good waterproof performance and excellent weather resistance effect under the synergistic effect of the modification of the acrylate monomer, and is suitable for the construction of an exposed base layer.
(4) According to the invention, through the interaction of adding a plurality of thixotropic agents, the polyurethane waterproof coating has thixotropy, does not flow when being coated on a vertical surface, has small viscosity increase, and can be sprayed for construction.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
One aspect of the invention provides a preparation method of a single-component anti-sagging exposed modified polyurethane waterproof coating, which comprises the following steps:
(1) uniformly mixing hydroxyl-terminated polyether polyol, a plasticizer, a filler, a thixotropic agent and an optional pigment, grinding and dehydrating;
(2) cooling, adding isocyanate, carrying out contact reaction, then heating, and continuing to carry out contact reaction;
(3) cooling, adding a first acrylate monomer, and carrying out contact reaction at 60-80 ℃; keeping the temperature at 60-80 ℃, adding an initiator, a chain transfer agent and a second acrylic ester monomer, and continuing to perform contact reaction;
(4) cooling, adding a latent curing agent, a catalyst, a solvent and optionally other auxiliary agents, and uniformly stirring and mixing to obtain the single-component anti-sagging exposed modified polyurethane waterproof coating.
The inventor researches and discovers that: the acrylate waterproof coating has excellent weather resistance, but has poor physical properties and low-temperature flexibility, and the polyurethane coating has good physical properties and low-temperature flexibility and poor weather resistance. If the two are fused, the acrylate resin is added into the polyurethane prepolymer, the acrylate resin can be separated out, and the effect of complementing the advantages of the two cannot be achieved. Therefore, the inventor of the application thinks that the polyurethane prepolymer is modified by acrylate substances, and the acrylate monomer containing hydroxyl is reacted with the NCO of the polyurethane prepolymer, so that the prepolymer becomes a polyurethane prepolymer with NCO at one end and acrylate groups at the other end; then introducing a hydroxyl-free acrylate monomer, adding an initiator and a chain transfer agent to enable the polyurethane prepolymer containing the acrylate group and the hydroxyl-free acrylate monomer to be subjected to free radical combination, connecting the hydroxyl-free acrylate monomer to the polyurethane prepolymer containing the acrylate group, and adding the chain transfer agent to prevent the molecular weight of the polymerization reaction from being too large and simultaneously reduce the viscosity of a polyurethane system. Meanwhile, a plurality of thixotropic agents are added into the system for interaction, so that the polyurethane waterproof coating has thixotropy, does not flow when being coated on a vertical surface, has low viscosity and can be sprayed for construction.
The single-component polyurethane coating disclosed by the invention adopts multiple technologies, so that the coating is compact and seamless, has high strength and good construction performance, can be integrated with a structural base layer, and has excellent physical and chemical resistance and better weather resistance.
According to the present invention, preferably, in step (1), the grinding is performed using a colloid mill; the dehydration treatment is to dehydrate for 2-3h under the vacuum condition with the temperature of 100-120 ℃ and the pressure of-0.09 to-0.1 MPa;
in the step (2), cooling to 50-70 ℃, adding isocyanate, carrying out contact reaction for 1-2h, then heating to 71-100 ℃, and continuing to carry out contact reaction for 2-3 h;
in the step (3), the temperature is reduced to below 60 ℃, a first acrylate monomer is added, and the contact reaction is carried out for 2-3h at the temperature of 60-80 ℃; keeping the temperature at 60-80 ℃, adding an initiator, a chain transfer agent and a second acrylic ester monomer, and continuing to perform contact reaction for 2-4 h;
in the step (4), the temperature is reduced to below 50 ℃.
According to the present invention, it is preferable that the isocyanate is used in an amount of 5 to 20 parts by weight, the hydroxyl-terminated polyether polyol is used in an amount of 20 to 40 parts by weight, the first acrylate monomer is used in an amount of 1 to 10 parts by weight, the second acrylate monomer is used in an amount of 1 to 10 parts by weight, the latent curing agent is used in an amount of 0.2 to 5 parts by weight, the plasticizer is used in an amount of 5 to 15 parts by weight, the solvent is used in an amount of 5 to 20 parts by weight, the filler is used in an amount of 10 to 30 parts by weight, the catalyst is used in an amount of 0.2 to 1 part by weight, the chain transfer agent is used in an amount of 0.1 to 1 part by weight, the initiator is used in an amount of 0.2 to 1 part by weight, the thixotropic agent is used in an amount of 1 to 20 parts by weight, the pigment is used in an amount of 0 to 1.
In the present invention, it is preferable that the isocyanate is used in an amount of 5 to 10 parts by weight, the first acrylate monomer is used in an amount of 1 to 5 parts by weight, the initiator is used in an amount of 0.2 to 0.5 part by weight, the chain transfer agent is used in an amount of 0.1 to 0.5 part by weight, the latent curing agent is used in an amount of 0.2 to 2 parts by weight, the thixotropic agent is used in an amount of 1 to 15 parts by weight, and the catalyst is used in an amount of 0.2 to 0.5 part by weight.
The other auxiliary agents used in the present invention are generally auxiliary agents commonly used in the art, and for example, may be at least one of an antifoaming agent, a leveling agent, an anti-settling agent, a coupling agent, an antioxidant and a retarder. Preferably, the other auxiliary agents comprise 0-0.2 part by weight of antioxidant, 0-0.5 part by weight of defoaming agent and 0-0.5 part by weight of dustproof agent.
According to the invention, preferably, the isocyanate is selected from 1, 6-Hexamethylene Diisocyanate (HDI) and/or isophorone diisocyanate (IPDI);
the hydroxyl-terminated polyether polyol is at least one of polyether diol, polyether triol and polyether tetraol; the weight-average molecular weight of the hydroxyl-terminated polyether polyol is 500-5000, and the hydroxyl value is 40-400mg KOH/g;
the hydroxyl-terminated polyether polyol is at least one selected from the group consisting of PPG polyether polyol, POP polymer polyether polyol, and polytetrahydrofuran ether polyol (PTMEG polyether polyol).
According to the present invention, preferably, the first acrylate monomer is a hydroxyl-containing acrylate monomer, preferably at least one of hydroxyethyl acrylate, hydroxyethyl methacrylate and hydroxypropyl acrylate;
the second acrylic ester monomer is an acrylic ester monomer without hydroxyl, and preferably at least one of methyl acrylate, ethyl acrylate, 2-methyl methacrylate and 2-ethyl methacrylate.
According to the present invention, preferably, the latent curing agent is an imine-type latent curing agent and/or a weakly basic oxazolidine-type latent curing agent;
the weakly basic oxazolidine type latent curing agent is preferably at least one of 2-isopropyloxazolidine, 2-dihydrooxazolidine, 2-isopropyl-N-hydroxyethyl-oxazolidine and 2, 2-dihydro-N-hydroxyethyl-oxazolidine;
the chain transfer agent is at least one of aliphatic mercaptan, dithioester and iodoform; the aliphatic mercaptan is preferably dodecyl mercaptan;
the initiator is Azobisisobutyronitrile (AIBN) and/or dibenzoyl peroxide (BPO);
the catalyst is an organic metal catalyst and/or a tertiary amine catalyst;
the organometallic catalyst is preferably at least one of dibutyltin dilaurate, stannous octoate and lead isooctanoate.
In the invention, the chain transfer agents are all oil-soluble chain transfer agents. The tertiary amine catalyst may be any tertiary amine catalyst in the art, and is preferably at least one of an aliphatic tertiary amine catalyst, an alicyclic tertiary amine catalyst, an aromatic tertiary amine catalyst, an alcohol amine catalyst, an ammonium salt of an aliphatic tertiary amine catalyst, an ammonium salt of an alicyclic tertiary amine catalyst, an ammonium salt of an aromatic tertiary amine catalyst, and an ammonium salt of an alcohol amine catalyst.
According to the present invention, preferably, the plasticizer is at least one of dioctyl phthalate, dibutyl phthalate, diisononyl phthalate, chlorinated paraffin and citrate-based plasticizer;
the filler is at least one of kaolin, cement, heavy calcium, barium sulfate, magnesium oxide, calcium oxide, wollastonite, silicon micropowder and talcum powder;
the pigment is at least one of carbon black, titanium dioxide, phthalocyanine blue, indigo, iron yellow, iron red, iron brown and bright yellow;
the solvent is at least one of toluene, xylene, 100# solvent oil, 120# solvent oil, 150# solvent oil, ethyl acetate and butyl acetate.
The plasticizer used in the invention has good compatibility with polyurethane, basically no migration or little migration, and remarkable stability and cooperativity.
According to the present invention, preferably, the thixotropic agent comprises, based on the total weight of the thixotropic agent: 90-100 wt% of nano calcium carbonate and 0-10 wt% of other thixotropic agents;
the other thixotropic agent is at least one of organic bentonite, polyamide wax powder, hydrogenated castor oil and gas-phase silicon dioxide.
In the present invention, the particle size of the nano calcium carbonate is preferably 20 to 100 nm.
The invention also provides the single-component anti-sagging exposed modified polyurethane waterproof coating prepared by the preparation method.
The single-component anti-sagging exposed modified polyurethane waterproof coating disclosed by the invention is a polyurethane waterproof coating which is high in strength, compact in coating, free from sagging in vertical surface construction and excellent in weather resistance, and realizes that the single-component polyurethane waterproof coating has good waterproof performance and excellent weather resistance, does not flow in vertical surface construction, is compact in coating and seamless, can be integrated with a structural base layer, and is suitable for construction of an exposed base surface.
The invention is further illustrated by the following examples:
the polyether diols used in the following examples were obtained from the Van der Chemie group, Inc. under the type C2020, and had a weight average molecular weight of 2000; the polyether triol is purchased from Wanhua chemical group GmbH, with the model number of F3135 and the weight average molecular weight of 5000; the latent curative 2959 was purchased from bayer corporation, model 2959; latent curative Incozol 4, available from Incorez corporation, model number Incozol 4; the latent curing agent ALT-101 is purchased from Ailite chemical Co., Ltd, and the model is ALT-101; the nano calcium carbonate is purchased from England porcelain (West lake) Limited, brand M400, and has a particle size of 80 nm; the organic bentonite is purchased from Zhejiang Fenghong new material Co., Ltd, and has the model of AF-300A; the organotin catalyst is purchased from air chemistry, and is T-12; the polyamide wax powder is purchased from Huanyu chemical company, and the model is SLX; defoamers are available from Bick chemical company as BYK-064, BYK-066N.
Example 1
The raw material ratio is as follows:
wherein the latent curing agent 2959 is a weakly basic oxazolidine latent curing agent; the solvent is No. 150 solvent oil; the polyether diol C2020 and the polyether triol F3135 are both PPG polyether polyol; the antioxidant is T-501, and the defoaming agent is BYK-064;
the preparation method comprises the following steps:
a. adding polyether diol C2020, polyether triol F3135, chlorinated paraffin, coarse whiting, titanium pigment, nano calcium carbonate and organic bentonite into a reaction container, stirring, grinding twice by a colloid mill, pouring into the reactor, heating to 100 ℃, and dehydrating for 3 hours under the condition of vacuum of-0.1 MPa;
b. cooling to 60 ℃, adding isocyanate IPDI, stirring and reacting for 1h, and continuing to react for 2h under the stirring state at 80 ℃;
c. cooling to 60 ℃, adding hydroxyethyl acrylate, heating to 70 ℃ and reacting for 2 h;
d. maintaining the temperature at 70 ℃, adding an initiator Azobisisobutyronitrile (AIBN) and a chain transfer agent dodecyl mercaptan, dropwise adding 2-ethyl methacrylate, and continuously reacting for 2 hours;
e. cooling to below 50 ℃, adding the latent curing agent, the organic tin catalyst T-12, the antioxidant, the defoaming agent and the solvent, stirring for 2 hours, dispersing uniformly, cooling to 30-40 ℃, charging nitrogen for protection, and discharging.
The polyurethane waterproof coating prepared in example 1 is coated to a thickness of about 1.5mm, and the coating is tested according to GB/T19250-2013 polyurethane waterproof coating, and the specific test result is as follows: the tensile strength is 3.8MPa, the elongation at break is 650 percent, and the tear strength is 22N/mm; after 1000h of artificial accelerated aging, the polyurethane coating film is not yellowed and cracked, and the strength retention rate is 114%. The water-proof paint of example 1 was subjected to sagging performance test using a sagging instrument according to the GB/T9264-88 standard, and the test result was that the paint did not sag after being painted once on the facade with a thickness of 1.0 mm. The viscosity is 12000mPa.s, and the paint can be sprayed and constructed.
Example 2
The raw material ratio is as follows:
wherein the latent curing agent Incozol 4 is 2-isopropyloxazolidine; the solvent is 100# solvent oil; the polyether diol C2020 and the polyether triol F3135 are both PPG polyether polyol; the antioxidant is 1010, and the defoaming agent is BYK-066;
the preparation method comprises the following steps:
a. adding polyether diol C2020, polyether triol F3135, chlorinated paraffin, barium sulfate, nano calcium carbonate, polyamide wax powder, titanium dioxide and indigo into a reaction container, stirring, grinding twice by using a colloid mill, pouring into the reactor, heating to 110 ℃, and dehydrating for 2.5 hours under the condition of vacuum of-0.1 MPa;
b. cooling to 60 ℃, adding isocyanate HDI, stirring to react for 1.5h, and continuing to react for 2.5h under the stirring state at 80 ℃;
c. cooling to 60 ℃, adding butyl acrylate, heating to 70 ℃ and reacting for 2.5 h;
d. maintaining the temperature at 70 ℃, adding an initiator Azobisisobutyronitrile (AIBN) and a chain transfer agent aliphatic mercaptan, dropwise adding 2-methyl methacrylate, and continuously reacting for 3 hours;
e. cooling to below 50 ℃, adding the latent curing agent, the organic tin catalyst T-12, the antioxidant, the defoaming agent and the solvent, stirring for 2 hours, dispersing uniformly, cooling to 30-40 ℃, charging nitrogen for protection, and discharging.
The polyurethane waterproof coating prepared in example 2 is coated to a thickness of about 1.5mm, and the coating is tested according to GB/T19250-2013 polyurethane waterproof coating, and the specific test result is as follows: the tensile strength is 3.2MPa, the elongation at break is 710%, and the tear strength is 16.5N/mm; after 1000h of artificial accelerated aging, the polyurethane coating film is not yellowed and cracked, and the strength retention rate is 115%. The water-proof paint of example 2 was subjected to sagging performance test using a sagging instrument according to the GB/T9264-88 standard, and the test result was that the paint was not sagging after being painted once on the vertical surface with a thickness of 1.5 mm. The viscosity is 15000mPa.s, and the paint can be sprayed and constructed.
Example 3
The raw material ratio is as follows:
wherein the latent curing agent ALT-101 is 2-isopropyl-N-hydroxyethyl-oxazolidine; the solvent is No. 150 solvent oil; the polyether diol C2020 and the polyether triol C3135 are both PPG polyether polyol; the antioxidant is 1076, and the defoaming agent is BYK-066N;
the preparation method comprises the following steps:
a. adding polyether diol C2020, polyether triol F3135, chlorinated paraffin, calcium carbonate, talcum powder, nano calcium carbonate, hydrogenated castor oil, titanium dioxide and bright yellow into a reaction container, stirring, grinding twice by using a colloid mill, pouring into the reactor, heating to 120 ℃, and dehydrating for 2 hours under the condition of vacuum of-0.1 MPa;
b. cooling to 60 ℃, adding isocyanate IPDI, stirring to react for 2 hours, and continuing to react for 3 hours at the temperature of 90 ℃ under the stirring state;
c. cooling to 60 ℃, adding hydroxyethyl acrylate, heating to 70 ℃ and reacting for 3 hours;
d. maintaining the temperature at 70 ℃, adding an initiator Azobisisobutyronitrile (AIBN) and a chain transfer agent dithioester, dropwise adding methyl acrylate, and continuing to react for 4 hours;
e. cooling to below 50 ℃, adding the latent curing agent, the organic tin catalyst T-12, the antioxidant, the defoaming agent and the solvent, stirring for 2 hours, dispersing uniformly, cooling to 30-40 ℃, charging nitrogen for protection, and discharging.
The polyurethane waterproof coating prepared in example 3 is coated to a thickness of about 1.5mm, and the coating is tested according to GB/T19250-2013 polyurethane waterproof coating, and the specific test result is as follows: the tensile strength is 3.8MPa, the elongation at break is 670 percent, and the tearing strength is 20.2N/mm; after 1000h of artificial accelerated aging, the polyurethane coating does not crack, and the strength retention rate is 102%. The water-proof paint of example 3 was subjected to sagging performance test using a sagging instrument according to the GB/T9264-88 standard, and the test result was that the paint was not sagging even if the paint was coated once on the vertical surface and the thickness was 0.5 mm. The viscosity is 8500mPa.s, and the paint can be sprayed for construction.
Comparative example 1
The raw material ratio is as follows:
wherein the latent curing agent ALT-101 is 2-isopropyl-N-hydroxyethyl-oxazolidine; the solvent is No. 150 solvent oil; the polyether diol C2020 and the polyether triol F3135 are both PPG polyether polyol; the antioxidant is 1076, and the defoaming agent is BYK-066N;
the preparation method comprises the following steps:
a. adding polyether dibasic C2020, polyether trihydric alcohol F3135, chlorinated paraffin, calcium carbonate, talcum powder, nano calcium carbonate, hydrogenated castor oil, titanium dioxide and bright yellow into a reaction container, stirring, grinding twice by using a colloid mill, pouring into the reactor, heating to 120 ℃, and dehydrating for 3 hours under the condition of vacuum of-0.1 MPa;
b. cooling to 60 ℃, adding isocyanate IPDI, stirring to react for 2 hours, and continuing to react for 3 hours at the temperature of 90 ℃ under the stirring state;
c. cooling to below 50 ℃, adding the latent curing agent, the organic tin catalyst T-12, the antioxidant, the defoaming agent and the solvent, stirring for 2 hours, dispersing uniformly, cooling to 30-40 ℃, charging nitrogen for protection, and discharging.
The polyurethane waterproof paint prepared in the comparative example 1 is coated to a thickness of about 1.5mm, and the test is carried out according to GB/T19250-2013 polyurethane waterproof paint, and the specific test result is as follows: the tensile strength is 3.1MPa, the elongation at break is 720 percent, and the tear strength is 16N/mm; after 1000h of artificial accelerated aging, the polyurethane coating cracks, and the strength retention rate is 58%; and (3) carrying out a sagging performance test on the waterproof coating of the comparative example 1 by using a sagging instrument according to the GB/T9264-88 standard, wherein the test result shows that the waterproof coating does not sag after being coated once on the vertical surface and the thickness of the waterproof coating is 0.5 mm. The viscosity is 7500mPa.s, and the paint can be sprayed and constructed.
Comparative example 2
The difference between the comparative example and the example 3 is that the formula does not contain 5 weight parts of nano calcium carbonate, and other components, the using amount and the preparation method are the same as those of the example 3.
And (3) carrying out a sagging performance test on the waterproof coating of the comparative example 2 by using a sagging instrument according to the GB/T9264-88 standard, wherein the test result shows that the sagging is serious when the waterproof coating is coated once on the vertical surface, and the thickness of the waterproof coating is 0.5 mm. The viscosity is 4000 mPa.s.
Comparative example 3
The comparative example is different from example 3 in that 2 parts by weight of organobentonite is used instead of 5 parts by weight of nano calcium carbonate, and the other components and the amounts and the preparation method are the same as those of example 3.
Carrying out a sagging performance test on the waterproof coating of the comparative example 3 by using a sagging instrument according to the GB/T9264-88 standard, wherein the test result is that the waterproof coating does not sag after being coated once on the vertical surface and has the thickness of 0.5 m; however, the viscosity was 35000mPa.s, and the spray coating could not be carried out.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (10)
1. A preparation method of a single-component anti-sagging exposed modified polyurethane waterproof coating is characterized by comprising the following steps:
(1) uniformly mixing hydroxyl-terminated polyether polyol, a plasticizer, a filler, a thixotropic agent and an optional pigment, grinding and dehydrating;
(2) cooling, adding isocyanate, carrying out contact reaction, then heating, and continuing to carry out contact reaction;
(3) cooling, adding a first acrylate monomer, and carrying out contact reaction at 60-80 ℃; keeping the temperature at 60-80 ℃, adding an initiator, a chain transfer agent and a second acrylic ester monomer, and continuing to perform contact reaction;
(4) cooling, adding a latent curing agent, a catalyst, a solvent and optionally other auxiliary agents, and uniformly stirring and mixing to obtain the single-component anti-sagging exposed modified polyurethane waterproof coating.
2. The production method according to claim 1,
in the step (1), the grinding is carried out by using a colloid mill; the dehydration treatment is to dehydrate for 2-3h under the vacuum condition with the temperature of 100-120 ℃ and the pressure of-0.09 to-0.1 MPa;
in the step (2), cooling to 50-70 ℃, adding isocyanate, carrying out contact reaction for 1-2h, then heating to 71-100 ℃, and continuing to carry out contact reaction for 2-3 h;
in the step (3), the temperature is reduced to below 60 ℃, a first acrylate monomer is added, and the contact reaction is carried out for 2-3h at the temperature of 60-80 ℃; keeping the temperature at 60-80 ℃, adding an initiator, a chain transfer agent and a second acrylic ester monomer, and continuing to perform contact reaction for 2-4 h;
in the step (4), the temperature is reduced to below 50 ℃.
3. The production method according to claim 1, the usage amount of the isocyanate is 5-20 parts by weight, the usage amount of the hydroxyl-terminated polyether polyol is 20-40 parts by weight, the usage amount of the first acrylate monomer is 1-10 parts by weight, the usage amount of the second acrylate monomer is 1-10 parts by weight, the usage amount of the latent curing agent is 0.2-5 parts by weight, the usage amount of the plasticizer is 5-15 parts by weight, the usage amount of the solvent is 5-20 parts by weight, the usage amount of the filler is 10-30 parts by weight, the usage amount of the catalyst is 0.2-1 part by weight, the usage amount of the chain transfer agent is 0.1-1 part by weight, the usage amount of the initiator is 0.2-1 part by weight, the usage amount of the thixotropic agent is 1-20 parts by weight, the usage amount of the pigment is 0-1 part by weight, and the usage amount of other auxiliary agents is 0-1.
4. The preparation method according to claim 3, wherein the other auxiliary agents are 0 to 0.2 part by weight of an antioxidant, 0 to 0.5 part by weight of a defoaming agent, and 0 to 0.5 part by weight of a dust preventive.
5. The production method according to claim 1, wherein the isocyanate is selected from 1, 6-hexamethylene diisocyanate and/or isophorone diisocyanate;
the hydroxyl-terminated polyether polyol is at least one of polyether diol, polyether triol and polyether tetraol; the weight-average molecular weight of the hydroxyl-terminated polyether polyol is 500-5000, and the hydroxyl value is 40-400mg KOH/g;
the hydroxyl-terminated polyether polyol is at least one selected from PPG polyether polyol, POP polymer polyether polyol and polytetrahydrofuran polyether polyol.
6. The preparation method according to claim 1, wherein the first acrylate monomer is a hydroxyl group-containing acrylate monomer, preferably at least one of hydroxyethyl acrylate, hydroxyethyl methacrylate and hydroxypropyl acrylate;
the second acrylic ester monomer is an acrylic ester monomer without hydroxyl, and preferably at least one of methyl acrylate, ethyl acrylate, 2-methyl methacrylate and 2-ethyl methacrylate.
7. The production method according to claim 1, wherein the latent curing agent is an imine-type latent curing agent and/or a weakly basic oxazolidine-type latent curing agent;
the weakly basic oxazolidine type latent curing agent is preferably at least one of 2-isopropyloxazolidine, 2-dihydrooxazolidine, 2-isopropyl-N-hydroxyethyl-oxazolidine and 2, 2-dihydro-N-hydroxyethyl-oxazolidine;
the chain transfer agent is at least one of aliphatic mercaptan, dithioester and iodoform;
the initiator is azobisisobutyronitrile and/or dibenzoyl peroxide;
the catalyst is an organic metal catalyst and/or a tertiary amine catalyst;
the organometallic catalyst is preferably at least one of dibutyltin dilaurate, stannous octoate and lead isooctanoate.
8. The production method according to claim 1, wherein the plasticizer is at least one of dioctyl phthalate, dibutyl phthalate, diisononyl phthalate, chlorinated paraffin, and a citrate-based plasticizer;
the filler is at least one of kaolin, cement, heavy calcium, barium sulfate, magnesium oxide, calcium oxide, wollastonite, silicon micropowder and talcum powder;
the pigment is at least one of carbon black, titanium dioxide, phthalocyanine blue, indigo, iron yellow, iron red, iron brown and bright yellow;
the solvent is at least one of toluene, xylene, 100# solvent oil, 120# solvent oil, 150# solvent oil, ethyl acetate and butyl acetate.
9. The production method according to claim 1, wherein the thixotropic agent comprises, based on the total weight of the thixotropic agent: 90-100 wt% of nano calcium carbonate and 0-10 wt% of other thixotropic agents;
the other thixotropic agent is at least one of organic bentonite, polyamide wax powder, hydrogenated castor oil and gas-phase silicon dioxide.
10. The one-component anti-sagging exposure type modified polyurethane waterproof coating prepared by the preparation method of any one of claims 1 to 9.
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