CN114316807A - Low-viscosity yellowing-resistant fast-curing stone surface adhesive and preparation method and application thereof - Google Patents
Low-viscosity yellowing-resistant fast-curing stone surface adhesive and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a low-viscosity yellowing-resistant fast-curing stone surface adhesive as well as a preparation method and application thereof, and the low-viscosity yellowing-resistant fast-curing stone surface adhesive comprises two mutually independent components A and B, wherein the component A comprises the following raw materials in parts by weight: 100 parts of high-activity multifunctional acrylate monomer, 0.1-1 part of polymerization inhibitor, 0.1-1 part of first coupling agent, 0.1-1 part of first defoaming agent and 0.1-1 part of first leveling agent; the component B comprises the following raw materials in parts by weight: 60-100 parts of modified amine curing agent, 0.1-1 part of second coupling agent, 0.1-1 part of second defoaming agent and 0.1-1 part of second leveling agent. The viscosity of the components of the methyl-ethyl double-component is low at the normal temperature of 25 ℃, the mixed viscosity of the two components is about 100mPa & s which is far lower than 500mPa & s of an epoxy system, the operation is very easy, and the operation is very convenient even at a lower temperature (0-5 ℃) in winter. The gel time is 3-8 min at the normal temperature of 25 ℃, a certain use strength is quickly reached, and the gel can be solidified in a short time at a low temperature (0-5 ℃) so as to be convenient for mechanical operation.
Description
Technical Field
The invention belongs to the technical field of stone surface glues, and particularly relates to a low-viscosity yellowing-resistant quick-setting stone surface glue and a preparation method and application thereof.
Background
With the rapid development of the building industry, in order to ensure the specifications of the building industry, a series of standards are established for building stones and stone adhesives in China to ensure the safety of buildings, wherein higher requirements are made on the mechanical strength of the stone adhesives, and various mechanical standards of the adhesives for facing stones are specified in GB 24264 plus-material glue for facing stones 2009. People in life have higher requirements on the appearance, flatness and acid and alkali resistance of the decorative stone, especially on the aspect of facing stone. Therefore, the surface glue for decorating the surface of the stone is provided, the stone is protected, and the attractiveness of the stone is improved.
Since the use of stone surface cement, unsaturated resins, acrylic resins and epoxy resins are widely used for the stone surface cement. However, the defects of unsaturated resin and acrylic resin are large in the using process, the cured product of the unsaturated resin stone surface adhesive is large in shrinkage and poor in water resistance and is easy to fall off, and the surface of the cured product can be sticky to hands. Acrylic resins are inferior in strength, oxygen prevents them from polymerizing during radical curing, and the surface of the cured product sticks to hands, both of which are finally rejected because of these disadvantages. At present, the common stone surface adhesive on the market is epoxy resin stone surface adhesive. The epoxy resin has high viscosity and low curing speed, is more obvious at low temperature (0-5 ℃), is inconvenient for subsequent mechanical operation, and has poor yellowing resistance. At present, more and more high-grade stones are applied to building decoration, and the commercially available stone surface adhesive cannot meet the requirements of white stones, light-colored stones and the like on the yellowing resistance of the stone surface adhesive.
Aiming at the above deficiency of stone surface glue, in daily industrial application, in order to solve the above problems, the following methods are generally adopted:
1. the acrylic acid of the acrylic resin surface glue is made into self-drying type and light-curing type resin to avoid oxygen from blocking the resin. But the process difficulty is increased, the production cost of the product is improved, and the production is not facilitated.
2. When in use, the epoxy stone surface adhesive is heated to reduce the viscosity of the product and improve the reactivity. But the operation is troublesome and the energy consumption is large.
3. A large amount of diluent is added, so that the viscosity of the resin is reduced, the operability is improved, and the strength of the product body is influenced to a certain extent.
4. Part of ultraviolet absorbent can be added in the epoxy stone surface adhesive during production, so that the yellowing resistance of the product is improved. However, the ultraviolet absorber has a certain color, and the epoxy resin has a structure in which benzene rings are easy to yellow, so that the anti-yellowing effect is not ideal.
According to the literature, patent CN 109266277 a "a transparent, high hardness, yellowing resistant epoxy stone surface adhesive and its preparation process" still uses epoxy resin as the main body, benzyl alcohol and low molecular weight epoxy as the diluent, and the curing principle is still the ring-opening reaction of amine and epoxy, and adds a small amount of accelerator to accelerate the reaction speed. The technical scheme of the patent still has the defects of the epoxy stone surface adhesive, only slightly improves the epoxy stone surface adhesive, and does not fundamentally solve the problem.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a stone surface adhesive which has low viscosity, yellowing resistance and quick curing. The invention starts from the curing reaction activity of the bi-component stone surface adhesive, adopts the reaction of the high-activity multifunctional acrylate monomer and the organic amine curing agent, has high reaction activity and high curing speed, and is convenient for subsequent mechanical operation. Meanwhile, the high-activity multifunctional acrylate monomer is low in viscosity and strong in permeability, can generate strong adhesive force to the stone in a short time, and is not easy to yellow because the two components of the high-activity multifunctional acrylate monomer do not contain benzene ring structures.
The second purpose of the invention is to provide a preparation method of the low-viscosity yellowing-resistant fast-curing stone surface adhesive.
The third purpose of the invention is to provide the application of the low-viscosity yellowing-resistant quick-curing stone surface adhesive.
In order to solve the technical problems, the invention is realized by the following technical scheme:
in a first aspect, the invention provides a low-viscosity yellowing-resistant fast-curing stone surface adhesive, which comprises two mutually independent components A and B, wherein the component A comprises the following raw materials in parts by weight: 100 parts of high-activity multifunctional acrylate monomer, 0.1-1 part of polymerization inhibitor, 0.1-1 part of first coupling agent, 0.1-1 part of first defoaming agent and 0.1-1 part of first leveling agent; the component B comprises the following raw materials in parts by weight: 60-100 parts of modified amine curing agent, 0.1-1 part of second coupling agent, 0.1-1 part of second defoaming agent and 0.1-1 part of second leveling agent.
Preferably, the component A comprises the following raw materials in parts by weight: 100 parts of high-activity multifunctional acrylate monomer, 0.4-0.8 part of polymerization inhibitor, 0.5-0.8 part of first coupling agent, 0.5-0.8 part of first defoaming agent and 0.5-0.8 part of first leveling agent; the component B comprises the following raw materials in parts by weight: 60-100 parts of modified amine curing agent, 0.5-0.8 part of second coupling agent, 0.5-0.8 part of second defoaming agent and 0.5-0.8 part of second leveling agent.
Further preferably, the component A comprises the following raw materials in parts by weight: 100 parts of high-activity multifunctional acrylate monomer, 0.5 part of polymerization inhibitor, 0.5 part of first coupling agent, 0.5 part of first defoaming agent and 0.5 part of first leveling agent; the component B comprises the following raw materials in parts by weight: 60-100 parts of modified amine curing agent, 0.5 part of second coupling agent, 0.5 part of second defoaming agent and 0.5 part of second leveling agent.
Preferably, in the component A: the high-activity multifunctional acrylate monomer is selected from trimethylolpropane triacrylate (TMPTA), pentaerythritol tetraacrylate (PET 4A); the polymerization inhibitor is selected from hydroquinone; the first coupling agent is selected from 3- (2, 3-epoxypropoxy) propyl trimethoxy silane; the first defoaming agent is selected from a silicone-free foam breaking polymer solution; the first leveling agent is selected from a polyacrylate solution.
Preferably, in the component B: the basic amine raw material of the modified amine curing agent is selected from 1, 3-diaminomethylcyclohexane (1,3-BAC), isophorone diamine (IPDA), 4' -diaminodicyclohexylmethane (HMDA); the second coupling agent is selected from 3-aminopropyltriethoxysilane; the second antifoaming agent is selected from methyl alkyl polysiloxane; the second leveling agent is selected from the group consisting of polymethylalkyl-methyl aralkyl siloxanes.
In a second aspect, the invention also provides a preparation method of the low-viscosity yellowing-resistant fast-curing stone surface adhesive, which comprises the following steps:
preparation of a component A:
weighing raw materials of a high-activity multifunctional acrylate monomer, a polymerization inhibitor, a first coupling agent, a first defoaming agent and a first leveling agent according to the weight part ratio, then putting all the raw materials into a stirrer, uniformly stirring until the polymerization inhibitor is completely dissolved, and discharging after vacuum treatment to obtain a component A;
b, preparation of a component B:
preparing a modified amine curing agent according to a modification method, weighing the raw materials of the modified amine curing agent, a second coupling agent, a second defoaming agent and a second leveling agent according to the weight part ratio, putting all the raw materials into a stirrer, uniformly stirring, performing vacuum treatment, and discharging to obtain a component B.
Preferably, the stirring and vacuum treatment method of the two components comprises the following steps: controlling the rotating speed to be 50-80r/min, stirring for more than 30min until the mixture is completely uniform, stopping stirring, and defoaming for 5min under the condition of-0.1 MPa.
Preferably, the method for modifying the modified amine curing agent comprises:
adding a basic amine raw material into a reaction device, heating to 30-40 ℃ under stirring, adding a modifier in batches every 20-30min under continuous stirring, wherein the reaction ratio of the basic amine to the modifier is that of the basic amine: and (3) adding 100 parts of modifier (40-100), heating to 70-80 ℃, reacting for 1.5-2 hours under the condition of heat preservation, cooling to normal temperature, and discharging to obtain the modified amine curing agent.
It is further preferred that the modifier is selected from the group consisting of 1, 2-cyclohexanediol diglycidyl ether and 4, 5-epoxy tetrahydrophthalic acid diglycidyl ester.
In a third aspect, the invention also provides an application of the low-viscosity yellowing-resistant fast-curing stone surface adhesive, wherein the A component and the B component in the technical scheme are selected, and when the A component and the B component are used, the weight ratio of the A component to the B component is 1: 1-2, the coating can be constructed after being mixed, can finish rapid curing at room temperature, and can be cured at low temperature.
Compared with the prior art, the low-temperature fast curing composition prepared by the invention has the following beneficial effects:
1. the viscosity of the two components of the stone surface adhesive is low at the normal temperature of 25 ℃, the mixed viscosity of the two components is about 100mPa & s which is far lower than 500mPa & s of an epoxy system, the operation is very easy, and the stone surface adhesive can well permeate into stone to play the roles of repairing small gaps of the stone and reinforcing the stone. The operation is very convenient even at lower temperatures (0-5 ℃) in winter.
2. The stone surface adhesive has excellent yellowing resistance, and has no yellowing sign after being irradiated under an ultraviolet lamp for 7 days. Because the component A selects the high-activity multifunctional acrylate monomer, the resin has no benzene ring structure and has better yellowing resistance, and the modified amine curing agent selected from the component B also fundamentally avoids the existence of the benzene ring structure, the stone surface adhesive has good yellowing resistance.
3. The stone surface adhesive has high curing speed, has the gelation time of 3-8 min at the normal temperature of 25 ℃ according to different raw materials and formulas, can be gelled and cured in a short time at a low temperature (0-5 ℃) and is convenient for mechanical operation.
4. The stone surface adhesive also has good mechanical property, and the high-activity multifunctional acrylate monomer in the component A and the modified amine curing agent can form a compact three-dimensional network structure, so that the stone surface adhesive has excellent properties in the aspects of tensile shear strength, hardness and the like.
Detailed Description
The present invention is described in detail below with reference to examples, but the present invention is not limited to these examples. While the advantages of the invention will be apparent and readily appreciated by the description.
The test methods or test methods described in the following examples are conventional methods unless otherwise specified; the reagents and materials, unless otherwise indicated, are conventionally obtained commercially or prepared by conventional methods.
Experimental discussion on the reaction ratios of the base amine starting material and the modifier for the modified amine curing agent:
the modification method of the modified amine curing agent comprises the following steps:
adding a basic amine raw material into a reaction device, heating to 30-40 ℃ under stirring, adding a modifier in batches every 20-30min under continuous stirring, heating to 70-80 ℃ after adding the modifier, reacting for 1.5-2h under heat preservation, cooling to normal temperature, and discharging to obtain the modified amine curing agent.
Table one: reaction ratio of basic amine raw material and modifier
Wherein the 1,3-BAC is 1, 3-cyclohexyldimethylamine, the IPDA is isophoronediamine, and the HMDA is 4, 4' -diaminodicyclohexylmethane.
TMPTA (trimethylolpropane triacrylate) and the modified amine curing agent are uniformly mixed according to the ratio of 1:1, cured for 7 days after curing, and tested for mechanical properties, and the specific results are as follows:
table two: modified amine curing agent examples Performance testing
| Serial number | Hardness (Shore D) | Tensile shear Strength (MPa) |
| 1 | 75 | 13.2 |
| 2 | 93 | 15.0 |
| 3 | 80 | 14.1 |
| 4 | 77 | 13.6 |
| 5 | 90 | 14.7 |
| 6 | 82 | 14.3 |
| 7 | 72 | 13.0 |
| 8 | 92 | 15.2 |
| 9 | 81 | 13.9 |
| 10 | 76 | 13.4 |
| 11 | 90 | 14.8 |
| 12 | 82 | 14.2 |
| 13 | 77 | 13.7 |
| 14 | 95 | 15.5 |
| 15 | 83 | 14.4 |
| 16 | 74 | 13.6 |
| 17 | 90 | 14.7 |
| 18 | 85 | 14.3 |
The table two data indicate that the preferred curing agents are 2, 8, 14, with curing agent 14 performing best.
Preparation of a component A:
weighing high-activity multifunctional acrylate monomers, a polymerization inhibitor, a first coupling agent, a first defoaming agent and a first leveling agent according to the weight parts, then putting all the monomers into a stirrer, controlling the rotating speed to be 50-80r/min, stirring for more than 30min till the monomers are completely uniform until the polymerization inhibitor is completely dissolved, stopping stirring, defoaming under the condition of-0.1 MPa for 5min, and discharging to obtain a component A;
b, preparation of a component B:
firstly preparing a modified amine curing agent according to a modification method, then weighing the raw materials of the modified amine curing agent, a second coupling agent, a second defoaming agent and a second leveling agent according to the weight part ratio, then putting all the raw materials into a stirrer, controlling the rotating speed to be 50-80r/min, stirring for more than 30min till the raw materials are completely uniform, stopping stirring, defoaming for 5min under the condition of-0.1 MPa, and then discharging to obtain the component B.
The stone surface adhesive prepared by the invention can be prepared by substituting the modified amine curing agent into the preparation schemes of the component A and the component B.
Table three: the specific embodiment of the component A and the component B is as follows:
note: the stabilizer, the defoamer, the flatting agent and the coupling agent are all added in conventional dosage.
TMPTA is trimethylolpropane triacrylate, PET4A is pentaerythritol tetraacrylate, KH-560 is the trade name of 3- (2, 3-glycidoxy) propyltrimethoxysilane, BYK-051 is the trade name of a silicone-free foam breaking polymer solution, BYK-354 is the trade name of a polyacrylate solution, BYK-085 is the trade name of methylalkylpolysiloxane, KH-550 is the trade name of 3-aminopropyltriethoxysilane, and BYK-323 is the trade name of polymethylalkyl-methylalkylsiloxane.
Mixing the components A and B according to the mixing ratio, curing for 7 days and testing the mechanical property, wherein the specific result is as follows:
table four: examples Performance testing
Note: the test standards referred to in tables two and four are as follows, appearance: the sample was poured into a cuvette of 3ml and the colorimetric card was visually checked.
Viscosity, pot life: GB/T12954-1991 general test method for building adhesives.
Hardness: GB/T531.1-2008.
Tensile shear strength: GB/T2567-2008 performs the test.
Yellowing resistance: GB/T23983-2009 carries out the test, and UVB340 lamp tubes are adopted, the irradiation intensity is 0.68W/m2The irradiation time 7d is accumulated.
Gloss: GB/T9754-2007.
The white stone surface glue has the following smearing effect: the two components are uniformly mixed and smeared on the surface of the white stone, the white stone is maintained at 25 ℃ for 2 days, and whether bubbles exist on the surface is visually observed.
As can be seen from Table four, the data shows that the performance of examples one, two, and three are superior to the commercial product (example 13), with the most preferred example being example three. The stone surface adhesive has obvious advantages in performance indexes such as viscosity (permeability), 25 ℃ pot life (initial setting time), 0 ℃ pot life (initial setting time), adhesive layer hardness, tensile shear strength, yellowing resistance, glossiness, white stone smearing effect (whether bubbles exist) and the like, and the overall performance improvement effect of the stone surface adhesive is obvious.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (10)
1. The low-viscosity yellowing-resistant fast-curing stone surface adhesive is characterized by comprising two mutually independent components A and B, wherein the component A comprises the following raw materials in parts by weight: 100 parts of high-activity multifunctional acrylate monomer, 0.1-1 part of polymerization inhibitor, 0.1-1 part of first coupling agent, 0.1-1 part of first defoaming agent and 0.1-1 part of first leveling agent; the component B comprises the following raw materials in parts by weight: 60-100 parts of modified amine curing agent, 0.1-1 part of second coupling agent, 0.1-1 part of second defoaming agent and 0.1-1 part of second leveling agent.
2. The low-viscosity yellowing-resistant fast-curing stone facing adhesive as claimed in claim 1, wherein the component A comprises the following raw materials in parts by weight: 100 parts of high-activity multifunctional acrylate monomer, 0.4-0.8 part of polymerization inhibitor, 0.5-0.8 part of first coupling agent, 0.5-0.8 part of first defoaming agent and 0.5-0.8 part of first leveling agent; the component B comprises the following raw materials in parts by weight: 60-100 parts of modified amine curing agent, 0.5-0.8 part of second coupling agent, 0.5-0.8 part of second defoaming agent and 0.5-0.8 part of second leveling agent.
3. The low-viscosity yellowing-resistant fast-curing stone facing adhesive as claimed in claim 2, wherein the component A comprises the following raw materials in parts by weight: 100 parts of high-activity multifunctional acrylate monomer, 0.5 part of polymerization inhibitor, 0.5 part of first coupling agent, 0.5 part of first defoaming agent and 0.5 part of first leveling agent; the component B comprises the following raw materials in parts by weight: 60-100 parts of modified amine curing agent, 0.5 part of second coupling agent, 0.5 part of second defoaming agent and 0.5 part of second leveling agent.
4. The low viscosity yellowing resistant fast curing stone topping as claimed in claim 1, wherein in the component A: the high-activity multifunctional acrylate monomer is selected from trimethylolpropane triacrylate and pentaerythritol tetraacrylate; the polymerization inhibitor is selected from hydroquinone; the first coupling agent is selected from 3- (methacryloyloxy) propyl trimethoxy silane; the first defoaming agent is selected from a silicone-free foam breaking polymer solution; the first leveling agent is selected from a polyacrylate solution.
5. The low-viscosity yellowing-resistant fast-curing stone facing adhesive as claimed in claim 1, wherein in the component B: the basic amine raw material of the modified amine curing agent is selected from 1, 3-diaminomethylcyclohexane, isophorone diamine and 4, 4' -diaminodicyclohexylmethane; the second coupling agent is selected from 3-aminopropyltriethoxysilane; the second antifoaming agent is selected from methyl alkyl polysiloxane; the second leveling agent is selected from the group consisting of polymethylalkyl-methyl aralkyl siloxanes.
6. A method for preparing the low viscosity yellowing resistant fast setting stone facing adhesive according to any one of claims 1 to 5, comprising:
preparation of a component A:
weighing raw materials of a high-activity multifunctional acrylate monomer, a polymerization inhibitor, a first coupling agent, a first defoaming agent and a first leveling agent according to the weight part ratio, then putting all the raw materials into a stirrer, uniformly stirring the raw materials until the polymerization inhibitor is completely dissolved, and discharging the mixture after vacuum treatment to obtain a component A;
b, preparation of a component B:
preparing a modified amine curing agent according to a modification method, weighing the raw materials of the modified amine curing agent, a second coupling agent, a second defoaming agent and a second leveling agent according to the weight part ratio, putting all the raw materials into a stirrer, uniformly stirring, performing vacuum treatment, and discharging to obtain a component B.
7. The process for preparing a low viscosity yellowing resistant fast setting stone facing glue according to claim 6, wherein the stirring and vacuum treatment method of the two components A and B comprises: controlling the rotating speed to be 50-80r/min, stirring for more than 30min until the mixture is completely uniform, stopping stirring, and defoaming for 5min under the condition of-0.1 MPa.
8. The method for preparing the low-viscosity yellowing-resistant fast-curing stone facing adhesive as claimed in claim 6, wherein the method for modifying the modified amine curing agent comprises the following steps:
adding a basic amine raw material into a reaction device, heating to 30-40 ℃ under stirring, adding a modifier in batches every 20-30min under continuous stirring, wherein the reaction ratio of the basic amine to the modifier is that of the basic amine: and (3) adding a modifier (100) (40-100), heating to 70-80 ℃, reacting for 1.5-2h under heat preservation, cooling to normal temperature, and discharging to obtain the modified amine curing agent.
9. The method as claimed in claim 8, wherein the modifier is selected from 1, 2-cyclohexanediol diglycidyl ether and 4, 5-epoxy tetrahydrophthalic acid diglycidyl ester.
10. The application of the low-viscosity yellowing-resistant fast-curing stone facing adhesive is characterized in that the A component and the B component are selected according to any one of claims 1 to 5, and when the A component and the B component are used, the weight ratio of the A component to the B component is 1: 1-2, and mixing to construct.
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| 韩亚芳;涂园园;林树东;杨公华;胡继文;王永超;李登峰;: "高性能环氧锚固胶的制备与性能研究" * |
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