CN115678413B - Bi-component polyurethane waterproof paint and preparation method thereof - Google Patents

Bi-component polyurethane waterproof paint and preparation method thereof Download PDF

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Publication number
CN115678413B
CN115678413B CN202211117117.9A CN202211117117A CN115678413B CN 115678413 B CN115678413 B CN 115678413B CN 202211117117 A CN202211117117 A CN 202211117117A CN 115678413 B CN115678413 B CN 115678413B
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polyurethane waterproof
waterproof paint
component polyurethane
temperature
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CN115678413A (en
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赵梦然
于杰
韩海军
刘雪峰
刘巩全
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Xuzhou Woniushan New Waterproof Materials Co ltd
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Xuzhou Woniushan New Waterproof Materials Co ltd
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Abstract

The invention belongs to the field of waterproof coatings, and particularly relates to a bi-component polyurethane waterproof coating and a preparation method thereof. The component A comprises the following components: polyether polyol, first plasticizer, isocyanate; the component B comprises: the adhesive comprises a second plasticizer, a first curing agent, a second curing agent, heavy calcium carbonate, talcum powder, a solvent, a thixotropic agent and a catalyst. After the bi-component polyurethane waterproof coating is coated or sprayed, the bonding strength of the waterproof layer and the base layer can reach more than 2.0MPa, and the bonding strength is far more than or equal to 1.0MPa specified by national standards.

Description

Bi-component polyurethane waterproof paint and preparation method thereof
Technical Field
The invention belongs to the field of waterproof coatings, and in particular relates to a double-component polyurethane waterproof coating and a preparation method thereof.
Background
Polyurethane waterproof paint belongs to chemical reaction waterproof paint, and after curing and forming, a flexible and seamless rubber waterproof film is formed, and is called as a 'liquid coiled material' in industry due to the excellent comprehensive performance. Polyurethane waterproof paint is divided into two main types of single-component polyurethane waterproof paint and double-component polyurethane waterproof paint according to the composition and curing mechanism. The two-component polyurethane waterproof paint is widely applied because of high cost performance.
Because the two components of the double-component polyurethane waterproof coating are cured into a film through chemical reaction, the whole reaction time plays a decisive influence on project construction period, and the curing reaction time is required to be shortened on the premise of ensuring the performance of each index of the material; because the adhesive property of the two-component polyurethane waterproof paint on the market is not ideal and basically wanders around 1.0MPa specified by national standards, the adhesive property of the two-component polyurethane waterproof paint needs to be improved to prolong or improve the service life of the material, and the advantages of the polyurethane waterproof paint are truly reflected.
Disclosure of Invention
The invention aims to solve the problems and provide a two-component polyurethane waterproof coating and a preparation method thereof.
The first aspect of the present invention provides a two-component polyurethane waterproof paint comprising an a component and a B component,
the component A comprises the following components: 60-80 parts by weight of polyether polyol, 12-19 parts by weight of first plasticizer and 10-14 parts by weight of isocyanate;
the component B comprises: 30-38 parts of a second plasticizer, 3-4 parts of a first curing agent, 0.1-0.3 part of a second curing agent, 40-50 parts of heavy calcium carbonate, 4-10 parts of talcum powder, 5-7 parts of a solvent, 0.2-0.35 part of a thixotropic agent, 0.1-0.4 part of a catalyst and 0-1 part of other auxiliary agents;
the first curing agent is at least one selected from methylene bis-o-chloroaniline, diethyl toluenediamine and dimethyl thiotoluenediamine;
the second curing agent is methyl hexahydrophthalic anhydride and/or methyl tetrahydrophthalic anhydride.
In the invention, the component A is a prepolymer, the component B is a curing agent, the component A and the component B are uniformly mixed according to a certain mass ratio (generally 1:2-3) and then coated on a base layer, and an integral waterproof layer with certain flexibility and no seam is formed through chemical reaction of active ingredients in the component A and the component B, so that the waterproof effect of the base layer is achieved.
In the invention, the first curing agent and the second curing agent are selected for compounding, and the first curing agent exerts the self curing performance; the second curing agent not only exerts the self curing performance, but also enables the obtained double-component polyurethane waterproof coating to have the bonding strength of more than or equal to 2MPa with the base layer, and the bonding strength is far more than or equal to 1.0MPa specified by national standards, because the property of the cured polymer depends on the performance of the curing agent, and the cured polyurethane coating has better stability because the molecular structure of the second curing agent does not contain double bonds; the polyurethane generated by the reaction of the second curing agent and the prepolymer has higher crosslinking degree, so that the molecular chain has more three-dimensional network structure, and the bonding strength of the polyurethane coating is improved. Meanwhile, the polyurethane produced by curing the second curing agent has the characteristic of higher thermal deformation temperature, so that the curing time required by the whole drying process is shorter.
According to the present invention, other auxiliary agents may be added as needed, and preferably, the other auxiliary agents include at least one of a dispersant, a defoamer and a leveling agent. When other auxiliary agents are required, the addition amount is preferably 0.4 to 1 part by weight. As a further preferable scheme, the weight ratio of the dispersing agent, the defoaming agent and the leveling agent is 1: (0.6-1): (0.3-0.8).
Preferably, the polyether polyol is at least one selected from polyether diol and polyether triol.
As a further preferred embodiment, the polyether glycol has an average molecular weight of 1000 to 3000 and a hydroxyl number of 50 to 60mg KOH/g.
As a further preferred embodiment, the polyether triol has an average molecular weight of 4000-5000 and a hydroxyl number of 30-39mg KOH/g.
Preferably, the first plasticizer and the second plasticizer are each at least one selected from tributyl citrate, trioctyl citrate, 52# chlorinated paraffin and dimethyl nylon acid.
Preferably, the isocyanate is at least one selected from toluene diisocyanate, diphenylmethane diisocyanate and polyphenyl polymethylene polyisocyanate.
Preferably, the mesh number of the heavy calcium carbonate is 600-1000; the heavy calcium plays a role in filling.
Preferably, the mesh number of the talcum powder is 1000-1500; talcum powder has effects of tackifying and preventing sinking.
As a preferable scheme, the solvent is at least one selected from isooctyl acetate, ethylene glycol diacetate, dearomatized environment-friendly chemical solvent oil D70 and dearomatized environment-friendly chemical solvent oil D90.
Preferably, the thixotropic agent is at least one selected from bentonite, fumed silica, polyamide wax and hydrogenated castor oil.
Preferably, the catalyst is at least one selected from dibutyl tin dilaurate, stannous octoate, triethylamine, tetramethyl ethylenediamine and N-methylimidazole.
The second aspect of the present invention provides a method for preparing the above two-component polyurethane waterproof paint, which comprises:
the preparation method of the component A comprises the following steps:
step A1: mixing and stirring polyether polyol and a first plasticizer, and then carrying out reduced pressure dehydration;
step A2: the water content of the system under normal pressure is controlled to be less than or equal to 500ppm;
step A3: adding isocyanate for reaction;
step A4: after the reaction of the step A3 is finished, heating to continue the reaction;
step A5: after the reaction of the step A4 is finished, cooling and degassing are carried out to obtain a component A;
the preparation method of the component B comprises the following steps:
step B1: stirring a second plasticizer, optionally other adjuvants;
step B2: adding a first curing agent, heavy calcium, talcum powder and thixotropic agent, mixing and stirring, and decompressing and dehydrating;
step B3: the water content of the system under normal pressure is controlled to be less than or equal to 500ppm;
step B4: adding a catalyst, a second curing agent and a solvent, and stirring under a micro-positive pressure state;
step B5: degassing under reduced pressure to obtain component B.
In the preferred scheme, in the step A1, the temperature of the system is controlled to be 110-115 ℃, the vacuum condition of decompression dehydration is minus 0.085 to minus 0.1MPa, and the time of decompression dehydration is 1-2h.
In the preferred scheme, in the step A2, the temperature is reduced to 55-65 ℃ after the moisture content of the system is controlled to be less than or equal to 500ppm under normal pressure.
In a preferred embodiment, in step A3, the reaction temperature is 70-76℃and the reaction time is 1-2 hours.
In the preferred scheme, in the step A4, the temperature after temperature rising is 83-88 ℃, and the continuous reaction time is 1-2h.
In the preferred scheme, in the step A5, the temperature is reduced to 45-55 ℃ for degassing, the vacuum condition of degassing is minus 0.075 to minus 0.085MPa, and the degassing time is 0.5-1h.
In the preferred scheme, in the step B1, the temperature of the system after stirring is controlled to be 100-105 ℃.
In the step B2, the temperature of the stirred system is controlled to be 105-110 ℃, the vacuum condition of decompression dehydration is minus 0.085 to minus 0.1MPa, and the time of decompression dehydration is 1-2h.
In the preferred scheme, in the step B3, after the moisture content of the system is controlled to be less than or equal to 500ppm under normal pressure, the temperature of the system is controlled to be 65-75 ℃.
In the preferred scheme, in the step B4, the temperature is 68-72 ℃ under the micro-positive pressure state, and the stirring time is 0.4-0.6h.
In the preferred scheme, in the step B5, the system temperature is controlled to be lower than 55 ℃ to carry out reduced pressure degassing, the vacuum condition of the reduced pressure degassing is-0.075 to-0.085 MPa, and the time of the reduced pressure degassing is 0.5 to 1h.
The invention has the beneficial effects that:
1. after the bi-component polyurethane waterproof coating is coated or sprayed, the bonding strength of the waterproof layer and the base layer can reach more than 2.0MPa, and the bonding strength is far more than or equal to 1.0MPa specified by national standards.
2. After the bi-component polyurethane waterproof paint is painted or sprayed, the drying speed is very high, the bi-component polyurethane waterproof paint can be dried for the second time under the normal temperature condition for 2 hours, and the construction progress is greatly improved.
3. The two-component polyurethane waterproof paint has higher bonding strength, so that the two-component polyurethane waterproof paint has the capability of reducing cracks or fissures of a building caused by foundation settlement.
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 preferred embodiments of the present invention are described below, it should be understood that the present invention may be embodied in various forms and should not be limited to 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.
In the examples of the present invention, the sources of the respective raw materials are shown in Table 1.
TABLE 1
Raw materials Manufacturer' s Number plate
Polyether glycol Wanhua chemistry C2020
Polyether triols Wanhua chemistry F3135
Isocyanate(s) Basoff' s T80
Defoaming agent Ephaven sodium 2024
Leveling agent Ephaven sodium 3663
MOCA Coastal Ming Sheng II
Heavy calcium carbonate Omega of omega 800 mesh
Methyl hexahydrophthalic anhydride Is of the order of yang Hui Cheng Auxiliary agent
Dibutyl tin dilaurate Tianjin Ake li Auxiliary agent
Table 2 shows the specific amounts of the A and B components used in each example.
TABLE 2
The preparation method of the component A comprises the following steps:
step A1: mixing and stirring polyether polyol and a first plasticizer, and then carrying out reduced pressure dehydration; the temperature of the system is controlled to be 110 ℃, the vacuum condition of decompression dehydration is minus 0.1MPa, and the time of decompression dehydration is 1.5h;
step A2: controlling the water content of the system to be less than or equal to 500ppm under normal pressure, and cooling to 60 ℃;
step A3: adding isocyanate for reaction; the reaction temperature is 73 ℃ and the reaction time is 1.5h;
step A4: after the reaction of the step A3 is finished, heating to continue the reaction; the temperature after heating is 85 ℃, and the continuous reaction time is 1.5h;
step A5: after the reaction of the step A4 is finished, the temperature is reduced by 50 ℃ to carry out degassing, the vacuum condition of the degassing is minus 0.08MPa, and the degassing time is 1h, so that the component A is obtained;
the preparation method of the component B comprises the following steps:
step B1: stirring the second plasticizer and optional other auxiliary agents, and controlling the temperature of the stirred system to be 102 ℃;
step B2: adding a first curing agent, heavy calcium, talcum powder and thixotropic agent, mixing and stirring, controlling the temperature of the system after stirring to be 108 ℃, and decompressing and dehydrating for 1.5h under-0.1 MPa;
step B3: controlling the system temperature to be 70 ℃ after controlling the water content of the system at normal pressure to be less than or equal to 500ppm;
step B4: adding a catalyst, a second curing agent and a solvent, and stirring for 0.5h at 70 ℃ under a micro-positive pressure state;
step B5: the system temperature is controlled to be lower than 55 ℃ for decompression and degassing, the vacuum condition of decompression and degassing is minus 0.08MPa, and the time of decompression and degassing is 0.6h, thus obtaining the component B.
The two-component polyurethane waterproof paint finished products (the mass ratio of the component A to the component B is 1:2.5) prepared in each example and the comparative example are tested according to the national standard GB/T19250-2013I, and specific test results are shown in Table 3.
TABLE 3 Table 3
Referring to the table 3 of the drawing,
for the tack-free time: since the second curing agent added in the examples has a characteristic of higher heat distortion temperature, the examples take shorter time for the tack-drying than the comparative examples.
For the dry time: the second curing agent added in the examples can also react with the prepolymer, and the second curing agent has the characteristic of higher heat distortion temperature, and the time for the actual drying of the examples is shorter than that of the comparative examples because of the fact that the second curing agent is matched with the catalyst to catalyze the whole reaction process.
For tensile strength: the second curing agent added in the embodiment can react and crosslink with the prepolymer to form a molecular structure with a three-dimensional network, so that the strength of the polyurethane coating is enhanced, and the tensile strength of the embodiment is superior to that of the comparative example; the examples all added with the second curing agent, so the tensile strength difference between the examples is not obvious.
Elongation at break: since the tensile strength of the examples is not very different from that of the comparative examples, the materials in nature are either rigid only or ductile only, and it is impossible to combine hardness and softness. Therefore, in the case where the tensile strength of the examples and the comparative examples is not greatly changed, it is not obvious that the elongation of the toughness is also.
For bond strength: the second curing agent is added in the embodiment, so that the drying speed of the surface is higher, the coating can be quickly cured to improve the strength after wetting the base layer and penetrating into the pores of the base layer, and the coating cannot be separated from the pores of the base layer due to shrinkage of the coating caused by untimely improvement of the strength after the material is cured, so that the coating can be fully meshed with the pores of the base layer, the coating can firmly grasp the base layer, and meanwhile, the tensile strength of the embodiment with the second curing agent is better than that of the comparative example, so that the bonding strength of the embodiment is obviously higher than that of the comparative example.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or 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 various embodiments described.

Claims (12)

1. A two-component polyurethane waterproof paint is characterized in that the two-component polyurethane waterproof paint comprises a component A and a component B,
the component A comprises the following components: 60-80 parts by weight of polyether polyol, 12-19 parts by weight of first plasticizer and 10-14 parts by weight of isocyanate;
the component B comprises: 30-38 parts of a second plasticizer, 3-4 parts of a first curing agent, 0.1-0.3 part of a second curing agent, 40-50 parts of heavy calcium carbonate, 4-10 parts of talcum powder, 5-7 parts of a solvent, 0.2-0.35 part of a thixotropic agent, 0.1-0.4 part of a catalyst and 0-1 part of other auxiliary agents;
the first curing agent is at least one selected from methylene bis-o-chloroaniline, diethyl toluenediamine and dimethyl thiotoluenediamine;
the second curing agent is methyl hexahydrophthalic anhydride and/or methyl tetrahydrophthalic anhydride.
2. The two-component polyurethane waterproof paint according to claim 1, wherein,
the other auxiliary agent comprises at least one of a dispersing agent, a defoaming agent and a leveling agent.
3. The two-component polyurethane waterproof paint according to claim 2, wherein,
the weight ratio of the dispersing agent, the defoaming agent and the leveling agent is 1: (0.6-1): (0.3-0.8).
4. The two-component polyurethane waterproof paint according to claim 1, wherein,
the polyether polyol is at least one selected from polyether glycol and polyether triol.
5. The two-component polyurethane waterproof paint according to claim 4, wherein,
the average molecular weight of the polyether glycol is 1000-3000, and the hydroxyl value is 50-60mg KOH/g;
the average molecular weight of the polyether triol is 4000-5000, and the hydroxyl value is 30-39mg KOH/g.
6. The two-component polyurethane waterproof paint according to claim 1, wherein,
the first plasticizer and the second plasticizer are respectively selected from at least one of tributyl citrate, trioctyl citrate, 52# chlorinated paraffin and dimethyl nylon acid.
7. The two-component polyurethane waterproof paint according to claim 1, wherein,
the isocyanate is at least one selected from toluene diisocyanate, diphenylmethane diisocyanate and polyphenyl polymethylene polyisocyanate.
8. The two-component polyurethane waterproof paint according to claim 1, wherein,
the mesh number of the heavy calcium carbonate is 600-1000;
the mesh number of the talcum powder is 1000-1500.
9. The two-component polyurethane waterproof paint according to claim 1, wherein,
the solvent is at least one selected from isooctyl acetate, ethylene glycol diacetate, dearomatized environment-friendly chemical solvent oil D70 and dearomatized environment-friendly chemical solvent oil D90;
the thixotropic agent is at least one selected from bentonite, fumed silica, polyamide wax and hydrogenated castor oil;
the catalyst is at least one selected from dibutyl tin dilaurate, stannous octoate, triethylamine, tetramethyl ethylenediamine and N-methylimidazole.
10. The method for preparing the two-component polyurethane waterproof paint as claimed in any one of claims 1 to 9, which is characterized in that the method comprises the following steps:
the preparation method of the component A comprises the following steps:
step A1: mixing and stirring polyether polyol and a first plasticizer, and then carrying out reduced pressure dehydration;
step A2: the water content of the system under normal pressure is controlled to be less than or equal to 500ppm;
step A3: adding isocyanate for reaction;
step A4: after the reaction of the step A3 is finished, heating to continue the reaction;
step A5: after the reaction of the step A4 is finished, cooling and degassing are carried out to obtain a component A;
the preparation method of the component B comprises the following steps:
step B1: stirring a second plasticizer, optionally other adjuvants;
step B2: adding a first curing agent, heavy calcium, talcum powder and thixotropic agent, mixing and stirring, and decompressing and dehydrating;
step B3: the water content of the system under normal pressure is controlled to be less than or equal to 500ppm;
step B4: adding a catalyst, a second curing agent and a solvent, and stirring under a micro-positive pressure state;
step B5: degassing under reduced pressure to obtain component B.
11. The method for producing a two-component polyurethane waterproof paint according to claim 10, wherein,
in the step A1, the temperature of the system is controlled to be 110-115 ℃, the vacuum condition of decompression dehydration is minus 0.085 to minus 0.1MPa, and the time of decompression dehydration is 1-2h;
in the step A2, the temperature is reduced to 55-65 ℃ after the moisture content of the system under normal pressure is controlled to be less than or equal to 500ppm;
in the step A3, the reaction temperature is 70-76 ℃ and the reaction time is 1-2h;
in the step A4, the temperature after temperature rising is 83-88 ℃, and the continuous reaction time is 1-2h;
in the step A5, the temperature is reduced to 45-55 ℃ for degassing, the vacuum condition of degassing is minus 0.075 to minus 0.085MPa, and the degassing time is 0.5-1h.
12. The method for producing a two-component polyurethane waterproof paint according to claim 10, wherein,
in the step B1, the temperature of the system after stirring is controlled to be 100-105 ℃;
in the step B2, the temperature of the stirred system is controlled to be 105-110 ℃, the vacuum condition of decompression and dehydration is minus 0.085 to minus 0.1MPa, and the time of decompression and dehydration is 1-2h;
in the step B3, after the moisture content of the system is controlled to be less than or equal to 500ppm under normal pressure, the temperature of the system is controlled to be 65-75 ℃;
in the step B4, the temperature is 68-72 ℃ and the stirring time is 0.4-0.6h under the micro-positive pressure state;
in the step B5, the system temperature is controlled to be lower than 55 ℃ for decompression and degassing, the vacuum conditions of decompression and degassing are-0.075 to-0.085 MPa, and the time of decompression and degassing is 0.5-1h.
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CN104403547A (en) * 2014-11-27 2015-03-11 山东一诺威新材料有限公司 Environment-friendly high-performance polyurethane waterproof paint and preparing method thereof
CN107641452A (en) * 2017-10-20 2018-01-30 唐山东方雨虹防水技术有限责任公司 One kind spraying thixotropic single-component polyurethane water-proof paint and preparation method thereof
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CN114292376A (en) * 2021-12-30 2022-04-08 清远高新华园科技协同创新研究院有限公司 Polyurethane reaction promoter and preparation method and application thereof

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US6333391B1 (en) * 1997-07-30 2001-12-25 Commonwealth Scientific And Industrial Research Organisation Aqueous polyimide process
CN102757722A (en) * 2012-07-13 2012-10-31 江苏博特新材料有限公司 Bi-component polyurethane coating and preparation method thereof
CN104403547A (en) * 2014-11-27 2015-03-11 山东一诺威新材料有限公司 Environment-friendly high-performance polyurethane waterproof paint and preparing method thereof
CN107641452A (en) * 2017-10-20 2018-01-30 唐山东方雨虹防水技术有限责任公司 One kind spraying thixotropic single-component polyurethane water-proof paint and preparation method thereof
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