CN113025255B - Double-component polyaspartic acid ester seam beautifying agent and preparation method thereof - Google Patents
Double-component polyaspartic acid ester seam beautifying agent and preparation method thereof Download PDFInfo
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- CN113025255B CN113025255B CN202110568505.8A CN202110568505A CN113025255B CN 113025255 B CN113025255 B CN 113025255B CN 202110568505 A CN202110568505 A CN 202110568505A CN 113025255 B CN113025255 B CN 113025255B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/02—Polyureas
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- 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
- C08G18/40—High-molecular-weight compounds
- C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
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- C09J11/06—Non-macromolecular additives organic
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention relates to the technical field of seam beautifying agents, and provides a two-component polyaspartic acid ester seam beautifying agent and a preparation method thereof. The double-component polyaspartic ester seam beautifying agent comprises a component A and a component B, wherein the component A comprises a prepolymer containing polyisocyanate, fumed silica, Portland cement, lime powder, a defoaming agent, a leveling agent and isocyanate silane; the component B comprises polyaspartic acid ester, titanium dioxide, a molecular sieve, fumed silica, a silane coupling agent, a dispersing agent, a defoaming agent, a leveling agent and pigment. The double-component polyaspartic acid ester seam beautifying agent provided by the invention is a solvent-free double-component seam beautifying agent, is environment-friendly and non-toxic, is simple and convenient to use, has small shrinkage rate, and has good maintenance and recoating performances; the matrix resin does not contain an aromatic structure which is easy to yellow, does not yellow when being applied outdoors or applied for a long time, and has excellent weather resistance; firm bonding with the interface, high adhesion strength, excellent mechanical toughness, good abrasion resistance and difficult scratching.
Description
Technical Field
The invention relates to the technical field of seam beautifying agents, in particular to a two-component polyaspartic acid ester seam beautifying agent and a preparation method thereof.
Background
The gap position of modern house ceramic tile, marble material is usually along with the increase of live time, can receive the influence of smoke and dust, greasy dirt and by the white blacken that changes, and not only influence pleasing to the eye for a long time not handling, breed mould easily moreover, produce the peculiar smell, and then influence the house environment, is the common problem of puzzlement decoration industry and family health. The seam beautifying agent is an upgrading product of the traditional white cement and joint mixture, is mainly applied to the joint of ceramic tiles or stone materials, and solves the problems of unattractive appearance, dirty black, ash falling and the like of the joint of the ceramic tiles or the stone materials.
The current seam beautifying agents on the market can be mainly divided into single-component seam beautifying agents and double-component seam beautifying agents. The single-component crack sealer is mainly water-based acrylic acid, can be directly coated and applied without ingredients before use, but is generally low in solid content, large in shrinkage rate, poor in water resistance after curing and poor in adhesion to a base material, so that the crack sealer falls off. Meanwhile, due to the defects of hot sticking and cold brittleness of the acrylate polymer, the unification of high elasticity and high strength is difficult to realize, and the long-term use effect and the attractiveness of the seam beautifying agent are easily influenced. The two-component seam beautifying agent mostly uses epoxy resin as matrix resin, and has the advantages of good adhesion, high brightness, good chemical stability, low cost and the like, but because the epoxy resin has poor yellowing resistance and weather resistance, and the internal crosslinking density of an epoxy resin system is high, the prepared seam beautifying agent is hard, is easy to form microcracks when being stressed by external stress, is easy to embrittle and crack at low temperature, and is not suitable for preparing outdoor seam beautifying agents or light-colored seam beautifying agent products. In addition, most of the existing two-component seam beautifying agents are solvent type seam beautifying agents, and the problem of large shrinkage rate caused by solvent volatilization also exists.
Therefore, it is necessary to develop a crack sealer which has strong adhesion with a substrate, high adhesion strength, excellent mechanical toughness, is not easily yellowed, and has no significant volume shrinkage after curing.
Disclosure of Invention
The invention aims to provide a crack sealer which is firm in bonding, high in adhesive strength, excellent in mechanical toughness, not easy to yellow and free of obvious shrinkage after curing, and aims to solve the technical problems that in the prior art, the crack sealer is large in shrinkage rate, poor in substrate adhesive force, not ideal in toughness, resistant to yellow and poor in weather resistance.
In order to achieve the purpose, the invention adopts the technical scheme that:
in a first aspect, the invention provides a two-component polyaspartic acid ester seam beautifying agent, which comprises a component A and a component B, wherein the component A comprises the following components in parts by mass:
polyisocyanate-containing prepolymer 65-90
Fumed silica 5-10
3-5 parts of Portland cement
1-2 parts of lime powder
0.05-0.2% of defoaming agent
0.1-1 parts of leveling agent
1-3 parts of isocyanate silane;
the component B comprises the following components in parts by mass:
70-90 of polyaspartic acid ester
6-12 parts of titanium dioxide
Molecular sieve 4-8
Fumed silica 5-10
Silane coupling agent 0.1-3
0.5-1.5% of dispersant
0.05-0.2% of defoaming agent
0.1-1 parts of leveling agent
0 to 0.2 portion of pigment.
The double-component polyaspartic acid ester seam beautifying agent provided by the invention is a solvent-free double-component seam beautifying agent, is environment-friendly, non-toxic and simple and convenient to use, overcomes the problem of large shrinkage rate caused by solvent volatilization of a solvent type seam beautifying agent, and has good maintenance and recoating performances; firm bonding with the interface, high adhesion strength, excellent mechanical toughness, good abrasion resistance and difficult scratching.
The component A of the double-component polyaspartic ester seam beautifying agent provided by the invention is introduced with isocyanate silane, isocyanate group at one end of the silane can react with polyaspartic ester or other structures containing active hydrogen, and silane at the other end can be chemically bonded with filler and a gap interface to be filled, so that the bonding force between the seam beautifying agent and the gap can be increased, the bonding force between matrix resin and the filler can be improved, and the mechanical property of the seam beautifying agent can be improved.
The polyaspartic ester in the component B of the double-component polyaspartic ester seam beautifying agent provided by the invention is an isocyanate curing agent containing a secondary amine structure, the hardness of the seam beautifying agent can be increased by ester group and aliphatic characteristics contained in the structure, and the good toughness and elasticity of matrix resin of the seam beautifying agent can be endowed by combining the polyaspartic ester seam beautifying agent with a prepolymer containing polyisocyanate in the component A, so that the seam beautifying agent has excellent impact resistance and wear resistance. Meanwhile, the whole matrix resin system of the double-component polyaspartic acid ester seam beautifying agent provided by the invention does not contain an aromatic structure which is easy to yellow, and the double-component polyaspartic acid ester seam beautifying agent does not yellow when being applied outdoors or applied for a long time, and has excellent weather resistance and strong decoration.
In the invention, the Portland cement, the defoaming agent, the leveling agent, the molecular sieve, the silane coupling agent and the dispersing agent can be selected from the types or models commonly used in the preparation of the crack sealing agent. For example, the Portland cement can be 42.5# ordinary Portland cement. The antifoaming agent can be tributyl phosphate, antifoaming agent dele 3100, antifoaming agent BYK088, etc. The leveling agent can be selected from BYK-300, BYK-306, BYK-310 and the like. The molecular sieve can be selected from 3A molecular sieve, 4A molecular sieve, etc. The silane coupling agent can be selected from KH550, KH560 and the like. The dispersant may be selected from sodium hexametaphosphate, sodium polycarboxylate, etc.
As a preferred scheme of the two-component polyaspartic ester seam beautifying agent provided by the invention, the preparation method of the prepolymer containing polyisocyanate comprises the following steps:
adding polyether diol, polyether triol and/or polyolefin into a reaction device, adding isophorone diisocyanate under stirring at 50-70 ℃, uniformly mixing, heating to 80-85 ℃, reacting until the-NCO content is 9-11%, quickly cooling, adding hexamethylene diisocyanate trimer, and uniformly mixing to prepare the prepolymer with the-NCO content of 15-17%.
In the two-component polyaspartic ester seam beautifying agent provided by the invention, a prepolymer containing polyisocyanate of the component A and polyaspartic ester of the component B form a matrix resin system of the two-component polyaspartic ester seam beautifying agent. The polyether diol, the polyether triol and/or the polyolefin which are/is introduced into the prepolymer containing the polyisocyanate to react can increase the adhesive force of a matrix resin system, so that the service life of the crack sealer is prolonged.
Further preferably, the polyether diol is polyoxypropylene diol with molecular weight of 1000-2000-, the polyether triol is polyoxypropylene triol with molecular weight of 500-2000-, and the polyolefin is hydroxyl-terminated polybutadiene with molecular weight of 2000-2500.
Further preferably, the mass ratio of the polyether diol to the polyether triol and/or the polyolefin is 1.5-4: 1.
further preferably, the mass ratio of the polyether diol to the polyether triol to the polyolefin is 3-4: 1: 1. the prepared seam beautifying agent has better adhesion.
As another preferable scheme of the two-component polyaspartic ester crack sealer provided by the invention, the isocyanatosilane is at least one of 1,3, 5-tri (trimethoxysilylpropyl) isocyanurate, 3-isocyanatopropyltriethoxysilane and 3-isocyanatopropyltrimethoxysilane.
As another preferable scheme of the two-component polyaspartic ester seam beautifying agent provided by the invention, the use mass ratio of the component A to the component B is 1: 1-1.5.
In a second aspect, the invention provides a preparation method of the two-component polyaspartic acid ester seam beautifying agent, which comprises the following steps:
the preparation method of the component A comprises the following steps: adding a defoaming agent, a leveling agent and isocyanate silane into a prepolymer containing polyisocyanate, stirring at the rotating speed of 300-500r/min for 10-20min to be uniform, then slowly adding fumed silica, Portland cement and lime powder, continuously stirring and dispersing for 10-20min to be uniform, and vacuumizing to obtain a component A;
the preparation method of the component B comprises the following steps: adding a silane coupling agent, a dispersing agent, a defoaming agent, a leveling agent and a pigment into polyaspartic acid ester, stirring at the rotating speed of 300-500r/min for 10-20min until the mixture is uniform, then slowly adding titanium dioxide, increasing the rotating speed to 800-1100r/min, dispersing for 30-40min until the fineness is not higher than 60 mu m, then adding a molecular sieve and fumed silica, dispersing until no colloidal particles can be seen by naked eyes, and vacuumizing to obtain the component B.
In a third aspect, the invention provides another preparation method of the two-component polyaspartic acid ester seam beautifying agent, which comprises the following steps:
the preparation method of the component A comprises the following steps: adding fumed silica into isocyanate silane and a part of prepolymer containing polyisocyanate, shearing and stirring at a high speed for 30-60min to obtain premix, adding the premix into a co-rotating double-screw extruder, and extruding at normal temperature to obtain an extrusion mixture, wherein the screw rotating speed is 400-500rpm, and the feeding speed is 0.8-1.0 kg/h; mixing the extrusion mixture with the rest of the component A, shearing and stirring at a high speed for 30-60min, adding a co-rotating double-screw extruder, and extruding at normal temperature, wherein the screw rotating speed is 200 plus 300rpm, and the feeding speed is 0.8-1.5 kg/h; vacuumizing to obtain a component A;
the preparation method of the component B comprises the following steps: mixing the components, shearing and stirring at a high speed for 30-60min, adding into a co-rotating double-screw extruder, extruding at normal temperature, wherein the screw rotating speed is 200 plus 300rpm, and the feeding speed is 0.8-1.5 kg/h; vacuumizing to obtain the component B.
According to the invention, the isocyanate silane and the fumed silica are firstly stirred and mixed at a high speed and extruded and mixed by a co-rotating double-screw extruder, and then the isocyanate silane and the fumed silica are mixed with other components at a high speed and extruded and mixed by a co-rotating double-screw extruder to prepare the agent A, so that the isocyanate silane and the fumed silica are favorably and uniformly dispersed in the crack sealer, and the effects of improving the adhesive property of the crack sealer and the binding force of matrix resin and filler in the crack sealer are achieved.
Furthermore, the mass ratio of the isocyanate silane and a part of prepolymer containing polyisocyanate to the fumed silica is 1-1.5: 1.
In the invention, the mass ratio of the isocyanate silane and a part of prepolymer containing polyisocyanate to the fumed silica is limited to 1-1.5:1, so that the extrusion mixing is smoothly carried out, and the isocyanate silane is uniformly coated on the surface of the fumed silica as much as possible, so that the isocyanate silane and the fumed silica are uniformly dispersed in the crack sealer.
The invention has the beneficial effects that:
the two-component polyaspartic acid ester seam beautifying agent provided by the invention is a solvent-free two-component seam beautifying agent, is environment-friendly, non-toxic and simple and convenient to use, overcomes the problem of large shrinkage rate caused by solvent volatilization of a solvent type seam beautifying agent, and has good maintenance and recoating performances. The whole matrix resin system of the double-component polyaspartic acid ester seam beautifying agent does not contain an aromatic structure which is easy to yellow, and the double-component polyaspartic acid ester seam beautifying agent does not yellow when being applied outdoors or applied for a long time and has excellent weather resistance. The double-component polyaspartic acid ester seam beautifying agent has the advantages of firm bonding with an interface, high adhesion strength, excellent mechanical toughness, good abrasion resistance and difficult scratching.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more apparent, the present invention is further described in detail below with reference to specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present patent and do not limit the scope of the invention in any way.
The invention provides a two-component polyaspartic ester seam beautifying agent which comprises a component A and a component B, wherein the component A comprises the following components in parts by mass:
polyisocyanate-containing prepolymer 65-90
Fumed silica 5-10
3-5 parts of Portland cement
1-2 parts of lime powder
0.05-0.2% of defoaming agent
0.1-1 parts of leveling agent
1-3 parts of isocyanate silane;
the component B comprises the following components in parts by mass:
70-90 of polyaspartic acid ester
6-12 parts of titanium dioxide
Molecular sieve 4-8
Fumed silica 5-10
Silane coupling agent 0.1-3
0.5-1.5% of dispersant
0.05-0.2% of defoaming agent
0.1-1 parts of leveling agent
0 to 0.2 portion of pigment.
The preparation method of the prepolymer containing the polyisocyanate comprises the following steps: adding polyether diol, polyether triol and/or polyolefin into a reaction device, adding isophorone diisocyanate under stirring at 50-70 ℃, uniformly mixing, heating to 80-85 ℃, reacting until the-NCO content is 9-11%, quickly cooling, adding hexamethylene diisocyanate trimer, and uniformly mixing to prepare the prepolymer with the-NCO content of 15-17%.
Further preferably, the polyether diol is a polyoxypropylene diol having a molecular weight of 1000-2000-.
Further preferably, the mass ratio of the polyether diol to the polyether triol and/or the polyolefin is 1.5-4: 1.
further preferably, the mass ratio of the polyether diol to the polyether triol to the polyolefin is 3-4: 1: 1.
the isocyanato silane is at least one of 1,3, 5-tri (trimethoxysilylpropyl) isocyanurate, 3-isocyanatopropyl triethoxysilane and 3-isocyanatopropyl trimethoxysilane.
The preparation method of the double-component polyaspartic acid ester seam beautifying agent comprises the following steps:
the first method comprises the following steps:
the preparation method of the component A comprises the following steps: adding a defoaming agent, a leveling agent and isocyanate silane into a prepolymer containing polyisocyanate, stirring at the rotating speed of 300-500r/min for 10-20min to be uniform, then slowly adding fumed silica, Portland cement and lime powder, continuously stirring and dispersing for 10-20min to be uniform, and vacuumizing to obtain a component A;
the preparation method of the component B comprises the following steps: adding a silane coupling agent, a dispersing agent, a defoaming agent, a leveling agent and a pigment into polyaspartic acid ester, stirring at the rotating speed of 300-500r/min for 10-20min until the mixture is uniform, then slowly adding titanium dioxide, increasing the rotating speed to 800-1100r/min, dispersing for 30-40min until the fineness is not higher than 60 mu m, then adding a molecular sieve and fumed silica, dispersing until no colloidal particles can be seen by naked eyes, and vacuumizing to obtain the component B.
The second method comprises the following steps:
the preparation method of the component A comprises the following steps: adding fumed silica into isocyanate silane and a part of prepolymer containing polyisocyanate, shearing and stirring at a high speed for 30-60min to obtain premix, adding the premix into a co-rotating double-screw extruder, and extruding at normal temperature to obtain an extrusion mixture, wherein the screw rotating speed is 400-500rpm, and the feeding speed is 0.8-1.0 kg/h; mixing the extrusion mixture with the rest of the component A, shearing and stirring at a high speed for 30-60min, adding a co-rotating double-screw extruder, and extruding at normal temperature, wherein the screw rotating speed is 200 plus 300rpm, and the feeding speed is 0.8-1.5 kg/h; vacuumizing to obtain a component A;
the preparation method of the component B comprises the following steps: mixing the components, shearing and stirring at a high speed for 30-60min, adding into a co-rotating double-screw extruder, extruding at normal temperature, wherein the screw rotating speed is 200 plus 300rpm, and the feeding speed is 0.8-1.5 kg/h; vacuumizing to obtain the component B.
In the second production method, it is preferable that the mass ratio of the isocyanatosilane and a part of the polyisocyanate-containing prepolymer to the fumed silica is 1 to 1.5: 1.
For example:
adding 0.15g of defoaming agent, 0.8g of flatting agent and 2.5g of 3-isocyanatopropyl trimethoxy silane into 68g of prepolymer containing polyisocyanate, stirring at the rotating speed of 500r/min for 10-20min until the mixture is uniform, then slowly adding 7g of fumed silica, 4g of silicate cement and 1g of lime powder, continuously stirring and dispersing for 10-20min until the mixture is uniform, and vacuumizing to obtain a component A;
the preparation method of the prepolymer containing the polyisocyanate comprises the following steps: adding 3g of polyoxypropylene diol 1000 and 1g of polyoxypropylene triol 2000 into a reaction device, adding 2.6g of isophorone diisocyanate at the temperature of 50 ℃ under stirring, uniformly mixing, heating to 85 ℃, reacting until the-NCO content is 9%, quickly cooling, adding 6.7g of hexamethylene diisocyanate trimer, and uniformly mixing to prepare a prepolymer with the-NCO content of 16.5%;
adding 1g of silane coupling agent, 1g of dispersing agent, 0.1g of defoaming agent, 0.8g of flatting agent and 0.2g of pigment into 77g of polyaspartic acid ester, stirring at the rotation speed of 500r/min for 10-20min until the mixture is uniform, then slowly adding 7g of titanium dioxide, increasing the rotation speed to 1100r/min, dispersing for 30-40min until the fineness is not higher than 60 mu m, then adding 5g of molecular sieve and 8g of fumed silica, dispersing until no visible colloidal particles exist, and vacuumizing to obtain the component B.
Another example is:
adding 0.9kg of fumed silica into 0.3kg of 3-isocyanatopropyl trimethoxy silane and 0.9kg of polyisocyanate-containing prepolymer, shearing and stirring at a high speed for 30min to obtain a premix, adding the premix into a co-rotating double-screw extruder, and extruding at normal temperature to obtain an extrusion mixture, wherein the rotating speed of a screw is 400rpm, and the feeding speed is 1.0 kg/h; mixing the extrusion mixture with 6kg of polyisocyanate-containing prepolymer, 0.4kg of Portland cement, 0.1kg of lime powder, 0.015kg of defoaming agent and 0.08kg of flatting agent, shearing and stirring at a high speed for 30min, adding into a co-rotating double-screw extruder, and extruding at normal temperature, wherein the rotating speed of a screw is 300rpm, and the feeding speed is 1.0 kg/h; vacuumizing to obtain a component A;
the preparation method of the prepolymer containing the polyisocyanate comprises the following steps: adding 3kg of polyoxypropylene glycol 1000 and 1kg of polyoxypropylene triol 2000 into a reaction device, adding 2.6kg of isophorone diisocyanate at the temperature of 50 ℃ under stirring, uniformly mixing, heating to 85 ℃, reacting until the-NCO content is 9%, quickly cooling, adding 6.7kg of hexamethylene diisocyanate trimer, and uniformly mixing to prepare a prepolymer with the-NCO content of 16.5%;
the preparation method of the component B comprises the following steps: mixing 7.5kg of polyaspartic acid ester, 1kg of titanium dioxide, 0.7kg of molecular sieve, 0.7kg of fumed silica, 0.1kg of silane coupling agent, 0.1kg of dispersing agent, 0.01kg of defoaming agent, 0.05kg of flatting agent and 0.01kg of pigment, shearing and stirring at a high speed for 30min, adding the mixture into a co-rotating double-screw extruder, extruding at normal temperature, wherein the rotating speed of a screw is 300rpm, and the feeding speed is 1.0 kg/h; vacuumizing to obtain the component B.
The invention is described in more detail by referring to a part of the tests, which are carried out in sequence, and the following detailed description is given by combining specific examples:
unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the raw materials, instruments, equipment and the like used in the following examples are either commercially available or available by existing methods; the dosage of the reagent is the dosage of the reagent in the conventional experiment operation if no special description exists; the experimental methods are conventional methods unless otherwise specified.
Example 1
A two-component polyaspartic ester seam beautifying agent comprises a component A and a component B, wherein the component A comprises: 8kg of polyisocyanate-containing prepolymer, 0.9kg of fumed silica, 0.4kg of No. 42.5 ordinary portland cement, 0.12kg of lime powder, 10g of defoaming agent (BYK 088), 50g of leveling agent (BYK-306) and 0.15kg of 3-isocyanatopropyl triethoxysilane;
the preparation method of the prepolymer containing the polyisocyanate comprises the following steps: dehydrating 4kg of polyoxypropylene diol 2000 and 1kg of polyoxypropylene triol 1000, adding the dehydrated materials into a four-neck flask provided with a stirrer, a thermometer and a nitrogen protection device, adding 5.5kg of isophorone diisocyanate under stirring at 60 ℃, heating to 80 ℃ after uniform mixing, reacting until the-NCO content is 10.9%, quickly cooling, adding 6.15kg of hexamethylene diisocyanate trimer, and preparing a prepolymer with the-NCO content of 17% after uniform mixing;
the component B comprises: 8.6kg of polyaspartic acid ester, 1kg of titanium dioxide, 0.6kg of molecular sieve, 0.7kg of fumed silica, 50g of silane coupling agent (KH 560), 50g of sodium hexametaphosphate (dispersing agent), 10g of defoaming agent (BYK 088), 50g of flatting agent (BYK-306) and 10g of pigment;
the preparation method of the two-component polyaspartic ester seam beautifying agent of the embodiment comprises the following steps:
the preparation method of the component A comprises the following steps: adding a defoaming agent (BYK 088), a flatting agent (BYK-306) and isocyanate silane into the prepolymer containing polyisocyanate, stirring at the rotating speed of 400r/min for 10-20min until the mixture is uniform, then slowly adding fumed silica, 42.5# ordinary portland cement and lime powder, continuously stirring and dispersing for 10-20min until the mixture is uniform, and vacuumizing to obtain a component A;
the preparation method of the component B comprises the following steps: adding a silane coupling agent (KH 560), sodium hexametaphosphate, a defoaming agent (BYK 088), a leveling agent (BYK-306) and a pigment into polyaspartic acid ester, stirring at a rotation speed of 400r/min for 10-20min until the mixture is uniform, then slowly adding titanium dioxide, increasing the rotation speed to 1000r/min, dispersing for 30-40min until the fineness is not higher than 60 mu m, then adding a molecular sieve and fumed silica, dispersing until no colloidal particles visible to naked eyes exist, and vacuumizing to obtain a component B.
Example 2
A two-component polyaspartic ester seam beautifying agent comprises a component A and a component B, wherein the component A comprises: 8kg of polyisocyanate-containing prepolymer, 0.5kg of fumed silica, 0.4kg of No. 42.5 ordinary portland cement, 0.2kg of lime powder, 10g of defoaming agent (BYK 088), 50g of flatting agent (BYK-306) and 0.1kg of 3-isocyanatopropyl triethoxysilane;
the preparation method of the prepolymer containing the polyisocyanate comprises the following steps: dehydrating 4kg of polyoxypropylene diol 2000 and 1kg of polyoxypropylene triol 1000, adding the dehydrated materials into a four-neck flask provided with a stirrer, a thermometer and a nitrogen protection device, adding 2.85kg of isophorone diisocyanate under stirring at 60 ℃, heating to 80 ℃ after uniform mixing, reacting until the-NCO content is 10%, quickly cooling, adding 3.95kg of hexamethylene diisocyanate trimer, and preparing a prepolymer with the-NCO content of 15% after uniform mixing;
the component B comprises: 7.6kg of polyaspartic acid ester, 0.8kg of titanium dioxide, 0.4kg of molecular sieve, 0.6kg of fumed silica, 50g of silane coupling agent (KH 560), 50g of sodium hexametaphosphate, 10g of defoaming agent (BYK 088), 10g of flatting agent (BYK-306) and 5g of pigment;
the preparation method of the two-component polyaspartic acid ester seam beautifying agent is the same as that of the embodiment 1.
Example 3
A two-component polyaspartic ester seam beautifying agent comprises a component A and a component B, wherein the component A comprises: 6.5kg of prepolymer containing polyisocyanate, 0.5kg of fumed silica, 0.3kg of No. 42.5 ordinary portland cement, 0.1kg of lime powder, 10g of defoaming agent (BYK 088), 50g of flatting agent (BYK-306) and 0.1kg of 1,3, 5-tri (trimethoxysilylpropyl) isocyanurate;
the preparation method of the prepolymer containing the polyisocyanate comprises the following steps: dehydrating 4kg of polyoxypropylene diol 2000 and 1kg of polyoxypropylene triol 1000, adding the dehydrated materials into a four-neck flask provided with a stirrer, a thermometer and a nitrogen protection device, adding 2.6kg of isophorone diisocyanate under stirring at 60 ℃, uniformly mixing, heating to 80 ℃, reacting until the-NCO content is 9%, quickly cooling, adding 6.7kg of hexamethylene diisocyanate trimer, and uniformly mixing to prepare a prepolymer with the-NCO content of 16.5%;
the component B comprises: 7kg of polyaspartic acid ester, 0.6kg of titanium dioxide, 0.4kg of molecular sieve, 0.5k0g fumed silica, 50g of silane coupling agent (KH 560), 50g of sodium hexametaphosphate, 10g of defoaming agent (BYK 088), 50g of flatting agent (BYK-306) and 10g of pigment;
the preparation method of the two-component polyaspartic acid ester seam beautifying agent is the same as that of the embodiment 1.
Example 4
A two-component polyaspartic ester seam beautifying agent comprises a component A and a component B, wherein the component A comprises: 9kg of polyisocyanate-containing prepolymer, 1kg of fumed silica, 0.5kg of No. 42.5 ordinary portland cement, 0.2kg of lime powder, 10g of defoaming agent (BYK 088), 50g of flatting agent (BYK-306) and 0.3kg of 1,3, 5-tris (trimethoxysilylpropyl) isocyanurate;
the preparation method of the prepolymer containing the polyisocyanate comprises the following steps: dehydrating 4kg of polyoxypropylene diol 2000 and 1kg of polyoxypropylene triol 1000, adding the dehydrated materials into a four-neck flask provided with a stirrer, a thermometer and a nitrogen protection device, adding 2.9kg of isophorone diisocyanate under stirring at 60 ℃, uniformly mixing, heating to 80 ℃, reacting until the-NCO content is 10.2%, rapidly cooling, adding 5.1kg of hexamethylene diisocyanate trimer, and uniformly mixing to prepare a prepolymer with the-NCO content of 16%;
the component B comprises: 9kg of polyaspartic acid ester, 1.2kg of titanium dioxide, 0.8kg of molecular sieve, 1kg of fumed silica, 50g of silane coupling agent (KH 560), 50g of sodium hexametaphosphate, 10g of defoaming agent (BYK 088), 50g of leveling agent (BYK-306) and 10g of pigment;
the preparation method of the two-component polyaspartic acid ester seam beautifying agent is the same as that of the embodiment 1.
Example 5
A two-component polyaspartic acid ester crack sealer, which is different from the embodiment 1 in that the preparation method of the prepolymer containing polyisocyanate comprises the following steps: 3kg of polyoxypropylene diol 2000, 1kg of polyoxypropylene triol 1000 and 1kg of hydroxyl-terminated polybutadiene 2000 are dehydrated and then added into a four-neck flask provided with a stirrer, a thermometer and a nitrogen protection device, 5.5kg of isophorone diisocyanate is added under stirring at 60 ℃, after uniform mixing, the temperature is raised to 80 ℃, after reaction is carried out until the-NCO content is 10.9%, the temperature is rapidly reduced, 6.15kg of hexamethylene diisocyanate trimer is added, and after uniform mixing, a prepolymer with 17% of-NCO content is prepared.
Example 6
A two-component polyaspartic acid ester seam beautifying agent, which is different from the embodiment 1 in that the preparation method of the two-component polyaspartic acid ester seam beautifying agent comprises the following steps:
the preparation method of the component A comprises the following steps: adding fumed silica into isocyanate silane and 0.75kg of prepolymer containing polyisocyanate, shearing and stirring at a high speed for 40min to obtain premix, adding the premix into a co-rotating double-screw extruder, and extruding at normal temperature to obtain an extrusion mixture, wherein the screw rotating speed is 400rpm, and the feeding speed is 0.8 kg/h; mixing the extrusion mixture with the rest 7.25kg of prepolymer containing polyisocyanate, 42.5# ordinary portland cement, lime powder, defoamer (BYK 088) and leveling agent (BYK-306), shearing and stirring at high speed for 40min, adding a co-rotating double-screw extruder, and extruding at normal temperature, wherein the rotating speed of the screw is 200rpm, and the feeding speed is 1.0 kg/h; vacuumizing to obtain a component A;
the preparation method of the component B comprises the following steps: mixing the components, shearing and stirring at a high speed for 40min, adding into a co-rotating double-screw extruder, and extruding at normal temperature, wherein the screw rotating speed is 200rpm, and the feeding speed is 1.0 kg/h; vacuumizing to obtain the component B.
Comparative example 1
A crack sealer, which is different from example 1, does not include 0.15kg of 3-isocyanatopropyltriethoxysilane in component A.
Comparative example 2
A crack sealer, different from example 1, comprises 0.05kg of 3-isocyanatopropyltriethoxysilane in component A.
Comparative example 3
Different from the embodiment 1, the preparation method of the two-component polyaspartic acid ester seam beautifying agent comprises the following steps:
the preparation method of the component A comprises the following steps: mixing the components, shearing and stirring at a high speed for 40min, adding into a co-rotating double-screw extruder, and extruding at normal temperature, wherein the screw rotating speed is 200rpm, and the feeding speed is 1.0 kg/h; vacuumizing to obtain a component A;
the preparation method of the component B comprises the following steps: mixing the components, shearing and stirring at a high speed for 40min, adding into a co-rotating double-screw extruder, and extruding at normal temperature, wherein the screw rotating speed is 200rpm, and the feeding speed is 1.0 kg/h; vacuumizing to obtain the component B.
Evaluation of crack-beautifying agent Performance
The two-component polyaspartate joint sealers of examples 1-6 and the joint sealers of comparative examples 1-3 were tested for performance data and the test results are shown in table 1.
Wherein, the use ratio of the component A and the component B of each group of the crack sealer is 1: 1.
TABLE 1 seam allowance performance test results
And (3) analyzing test results:
comparing the two-component polyaspartate seam sealers of examples 1 and 5, the two-component polyaspartate seam sealers of example 5 have better adhesion strength. From these results, it is known that in the preparation of a polyisocyanate-containing prepolymer, a polyoxypropylene diol 2000, a polyoxypropylene triol 1000 and a hydroxyl-terminated polybutadiene 2000 were prepared in the following manner: 1: 1, compared with the prepolymer containing polyisocyanate prepared by only adopting the polyoxypropylene diol 2000 and the polyoxypropylene triol 1000, the seam beautifying agent prepared by the method has better adhesion.
Comparing the two-component polyaspartate seam sealers of examples 1 and 6 with the seam sealer of comparative example 3, the two-component polyaspartate seam sealers of example 6 have the best tensile strength and adhesion strength. Therefore, the preparation method is characterized in that the isocyanatosilane and the fumed silica are firstly stirred and mixed at a high speed and extruded and mixed by a co-rotating double-screw extruder, and then the isocyanatosilane and the fumed silica are mixed at a high speed and extruded and mixed by a co-rotating double-screw extruder to prepare the agent A, so that the isocyanatosilane and the fumed silica are favorably and uniformly dispersed in the crack sealer, and the bonding property of the crack sealer and the bonding force of matrix resin and a filler in the crack sealer are improved.
Comparing the two-component polyaspartate seam sealers of example 1 with the seam sealers of comparative examples 1 and 2, the tensile strength and adhesion strength of the seam sealers of comparative examples 1 and 2 are significantly inferior to the two-component polyaspartate seam sealers of example 1. From this fact, it is found that the addition of the isocyanatosilane to the caulking agent is advantageous in improving the adhesion of the caulking agent and the binding force between the matrix resin and the filler in the caulking agent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. The double-component polyaspartic acid ester seam beautifying agent is characterized by comprising a component A and a component B, wherein the component A comprises the following components in parts by mass:
polyisocyanate-containing prepolymer 65-90
Fumed silica 5-10
3-5 parts of Portland cement
1-2 parts of lime powder
0.05-0.2% of defoaming agent
0.1-1 parts of leveling agent
1-3 parts of isocyanate silane;
the component B comprises the following components in parts by mass:
70-90 of polyaspartic acid ester
6-12 parts of titanium dioxide
Molecular sieve 4-8
Fumed silica 5-10
Silane coupling agent 0.1-3
0.5-1.5% of dispersant
0.05-0.2% of defoaming agent
0.1-1 parts of leveling agent
0 to 0.2 portion of pigment.
2. The crack sealer according to claim 1, wherein the polyisocyanate-containing prepolymer is prepared by a method comprising:
adding polyether diol, polyether triol and/or polyolefin into a reaction device, adding isophorone diisocyanate under stirring at 50-70 ℃, uniformly mixing, heating to 80-85 ℃, reacting until the-NCO content is 9-11%, quickly cooling, adding hexamethylene diisocyanate trimer, and uniformly mixing to prepare a prepolymer with the-NCO content of 15-17%; the polyether diol is polyoxypropylene diol with molecular weight of 1000-2000, the polyether triol is polyoxypropylene triol with molecular weight of 500-2000, and the polyolefin is hydroxyl-terminated polybutadiene with molecular weight of 2000-2500.
3. The crack sealer according to claim 2, wherein the mass ratio of the polyether diol to the polyether triol and/or the polyolefin is 1.5-4: 1.
4. the crack sealer as claimed in claim 3, wherein the mass ratio of the polyether diol, the polyether triol and the polyolefin is 3-4: 1: 1.
5. the crack sealer of claim 1, wherein the isocyanatosilane is at least one of 1,3, 5-tris (trimethoxysilylpropyl) isocyanurate, 3-isocyanatopropyltriethoxysilane, and 3-isocyanatopropyltrimethoxysilane.
6. The crack sealer according to claim 1, wherein the use mass ratio of the component A to the component B is 1: 1-1.5.
7. The method of preparing a two-component polyaspartate crack sealer according to any one of claims 1-6, comprising:
the preparation method of the component A comprises the following steps: adding a defoaming agent, a leveling agent and isocyanate silane into a prepolymer containing polyisocyanate, stirring at the rotating speed of 300-500r/min for 10-20min to be uniform, then slowly adding fumed silica, Portland cement and lime powder, continuously stirring and dispersing for 10-20min to be uniform, and vacuumizing to obtain a component A;
the preparation method of the component B comprises the following steps: adding a silane coupling agent, a dispersing agent, a defoaming agent, a leveling agent and a pigment into polyaspartic acid ester, stirring at the rotating speed of 300-500r/min for 10-20min until the mixture is uniform, then slowly adding titanium dioxide, increasing the rotating speed to 800-1100r/min, dispersing for 30-40min until the fineness is not higher than 60 mu m, then adding a molecular sieve and fumed silica, dispersing until no colloidal particles can be seen by naked eyes, and vacuumizing to obtain the component B.
8. The method of preparing a two-component polyaspartate crack sealer according to any one of claims 1-6, comprising:
the preparation method of the component A comprises the following steps: adding fumed silica into isocyanate silane and a part of prepolymer containing polyisocyanate, shearing and stirring at a high speed for 30-60min to obtain premix, adding the premix into a co-rotating double-screw extruder, and extruding at normal temperature to obtain an extrusion mixture, wherein the screw rotating speed is 400-500rpm, and the feeding speed is 0.8-1.0 kg/h; mixing the extrusion mixture with the rest of the component A, shearing and stirring at a high speed for 30-60min, adding a co-rotating double-screw extruder, and extruding at normal temperature, wherein the screw rotating speed is 200 plus 300rpm, and the feeding speed is 0.8-1.5 kg/h; vacuumizing to obtain a component A;
the preparation method of the component B comprises the following steps: mixing the components, shearing and stirring at a high speed for 30-60min, adding into a co-rotating double-screw extruder, extruding at normal temperature, wherein the screw rotating speed is 200 plus 300rpm, and the feeding speed is 0.8-1.5 kg/h; vacuumizing to obtain the component B.
9. The method according to claim 8, wherein the mass ratio of the isocyanatosilane and a portion of the polyisocyanate-containing prepolymer to the fumed silica is 1-1.5: 1.
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| CN114045141A (en) * | 2021-12-06 | 2022-02-15 | 北京吉时吉兴贸易有限公司 | Two-component polyurea seam beautifying agent |
| CN114410271B (en) * | 2021-12-21 | 2023-11-03 | 日丰企业集团有限公司 | Double-component polyurethane joint beautifying agent and preparation method and application thereof |
| CN114507501B (en) * | 2022-01-29 | 2024-03-12 | 中山市卡施力顿建材有限公司 | Two-component joint beautifying agent and preparation method and application thereof |
| CN115322723A (en) * | 2022-08-10 | 2022-11-11 | 潮州市猛犸象建材科技有限公司 | Preparation method of polyurea sandy seam beautifying agent |
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