CN114316807B - Low-viscosity yellowing-resistant quick-setting stone surface adhesive and preparation method and application thereof - Google Patents
Low-viscosity yellowing-resistant quick-setting stone surface adhesive and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a stone face adhesive with low viscosity, yellowing resistance and quick fixation, a preparation method and application thereof, wherein the face adhesive comprises a first component and a second component which are mutually independent, and the first component 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 first and second two-component components is low at the normal temperature of 25 ℃, the mixing viscosity of the two-component components is about 100 mPas and is far lower than 500 mPas of an epoxy system, the operation is very easy, and the operation is very convenient even at the lower temperature (0-5 ℃) in winter. The gel time is 3 min-8 min at normal temperature of 25 ℃, and a certain use strength is achieved quickly, and the gel can be solidified in a short time at low temperature (0-5 ℃), so that the mechanical operation is convenient.
Description
Technical Field
The invention belongs to the technical field of stone surface adhesives, and particularly relates to a low-viscosity yellowing-resistant quick-setting stone surface adhesive, and a preparation method and application thereof.
Background
Along with the high-speed development of the building industry, a series of standards are formulated for stone materials and stone adhesives for building in China to ensure the safety of the building, wherein the stone adhesives have higher requirements on the mechanical strength, and the adhesive for facing stone of GB 24264-2009 has regulations on various mechanical standards of adhesives for facing stone. In life, people have high requirements on the beauty, flatness and acid and alkali resistance of the stone for decoration, especially in the aspect of facing the stone. Therefore, the surface adhesive for decorating the stone surface is provided to protect the stone and improve the beauty of the stone.
Stone surface adhesives have been widely used with unsaturated resins, acrylic resins and epoxy resins. However, the unsaturated resin and the acrylic resin have the defects of large shrinkage and poor water resistance in the use process, and the surface of the unsaturated resin stone surface adhesive is easy to fall off, so that the surface of the cured product is sticky. Acrylic resins are inferior in strength, oxygen prevents polymerization during radical curing, and the cured surface sticks to hands, because both materials are eventually eliminated. At present, the stone surface adhesive on the market is commonly epoxy resin stone surface adhesive. The epoxy resin has high viscosity and low curing speed, and is more obvious at low temperature (0-5 ℃), so that the epoxy resin is inconvenient for subsequent mechanical operation and has poor yellowing resistance. The current increasing high-grade stone materials are applied to building decoration, and the commercial stone surface adhesives can not meet the requirements of white stone materials, light-colored stone materials and the like on the yellowing resistance of the stone surface adhesives.
Aiming at the defects of the stone surface sizing agent, in daily industrial application, the following method is generally adopted to solve the problems:
1. acrylic acid of the acrylic resin topcoat is made into a self-drying and photo-curing resin to avoid oxygen from blocking it. However, the process difficulty is increased, the production cost of the product is increased, 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 high.
3. A large amount of diluent is added, so that the viscosity of the resin is reduced, the operability is improved, but the strength of the product body is influenced to a certain extent.
4. When the epoxy stone surface adhesive is produced, part of ultraviolet absorbent is added, so that the yellowing resistance of the product is improved. However, the ultraviolet absorber itself has a certain color, and the epoxy resin structure has a benzene ring which is easy to yellow, so that the yellowing resistance is not ideal.
According to the document, patent CN 109266277A, namely transparent, high-hardness and yellowing-resistant epoxy stone face glue and a preparation process thereof, adopts epoxy resin as a main body, benzyl alcohol and low-molecular-weight epoxy as diluents, and adopts a curing principle that amine and epoxy react in a ring-opening manner, and a small amount of accelerator is added to accelerate the reaction speed. The scheme still has the defects of the epoxy stone surface adhesive, is slightly improved, and does not fundamentally solve the problems.
Disclosure of Invention
In order to overcome the above-mentioned shortcomings of the prior art, a first object of the present invention is to provide a stone surface adhesive with low viscosity, yellowing resistance and fast curing. The invention starts from the solidification reactivity of the bi-component stone face glue, adopts the reaction of the high-activity multifunctional acrylic ester monomer and the organic amine curing agent, has large reactivity and high curing speed, and is convenient for subsequent mechanical operation. Meanwhile, the high-activity multifunctional acrylate monomer has low viscosity and strong permeability, and can generate strong adhesive force to stone in a short time.
The second aim of the invention is to provide a preparation method of the low-viscosity yellowing-resistant quick-setting stone surface adhesive.
The third purpose of the invention is to provide the application of the low-viscosity yellowing-resistant quick-setting stone surface adhesive.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention provides a low-viscosity yellowing-resistant quick-setting stone face adhesive, which comprises a first component and a second component which are mutually independent, wherein the first component 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.
It is further preferred that 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 first component: the high-activity multifunctional acrylate monomer is selected from trimethylolpropane triacrylate (TMPTA) and pentaerythritol tetraacrylate (PET 4A); the polymerization inhibitor is selected from hydroquinone; the first coupling agent is selected from 3- (2, 3-glycidoxy) propyl trimethoxy silane; the first defoamer is selected from a foam breaking polymer solution without silicone; the first leveling agent is selected from polyacrylate solutions.
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), isophoronediamine (IPDA), 4' -diaminodicyclohexylmethane (HMDA); the second coupling agent is selected from 3-aminopropyl triethoxysilane; the second defoamer is selected from methyl alkyl polysiloxanes; the second leveling agent is selected from polymethylalkyl-methylarylalkylsiloxane.
In a second aspect, the invention also provides a preparation method of the low-viscosity yellowing-resistant quick-setting stone surface adhesive, which comprises the following steps:
and (3) preparation of a component A:
weighing a raw material 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 portion ratio, then putting all the materials into a stirrer, stirring uniformly until the polymerization inhibitor is completely dissolved, and discharging after vacuum treatment to obtain a component A;
and (2) preparing a component B:
firstly preparing a modified amine curing agent according to a modification method, then weighing the raw material modified amine curing agent, a second coupling agent, a second defoaming agent and a second leveling agent according to the weight portion ratio, then putting all the materials into a stirrer, uniformly stirring, vacuum-treating and discharging to obtain the component B.
Preferably, the stirring and vacuum treatment methods of the two components A and B comprise the following steps: the rotating speed is controlled to be 50-80r/min, stirring is carried out for more than 30min until the stirring is completely uniform, and defoaming is carried out for 5min under the condition of minus 0.1 MPa.
Preferably, the modification method of the modified amine curing agent comprises the following steps:
adding basic amine raw materials into reaction equipment, heating to 30-40 ℃ under stirring, and adding a modifier in batches every 20-30min under continuous stirring, wherein the reaction ratio of the basic amine and the modifier is the basic amine: and (3) adding modifier=100 (40-100), heating to 70-80 ℃ after the addition of the materials, carrying out heat preservation reaction for 1.5-2h, and discharging at normal temperature 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-epoxytetrahydrophthalic acid diglycidyl ester.
In a third aspect, the invention also provides application of the low-viscosity yellowing-resistant quick-setting stone surface adhesive, wherein the components A and B in the technical scheme are selected, and the weight ratio of the components A to B is (1): 1-2, and can be quickly cured at room temperature and at low temperature.
Compared with the prior art, the low-temperature rapid curing composition prepared by the invention has the following beneficial effects:
1. the viscosity of the bi-component of the stone surface adhesive is low at the normal temperature of 25 ℃, the mixing viscosity of the bi-component is about 100 mPa.s and is far lower than 500 mPa.s of an epoxy system, the operation is very easy, and the bi-component adhesive can better permeate into stone to repair fine gaps of the stone and reinforce the stone due to the low viscosity of the stone surface adhesive. The operation is very convenient even at lower temperature (0-5 ℃) in winter.
2. The stone surface adhesive has excellent yellowing resistance, and does not have any yellowing sign after being irradiated under an ultraviolet lamp for 7 days. Because the high-activity multifunctional acrylate monomer is used for the component A in the selection of raw materials, the resin has no benzene ring structure and better yellowing resistance, and the modified amine curing agent selected by the component B also radically eliminates the existence of the benzene ring structure, so the stone surface adhesive has good yellowing resistance effect.
3. The stone surface adhesive has a high curing speed, the gel time is 3-8 min at the normal temperature of 25 ℃ according to different raw materials and formulas, and the stone surface adhesive can be cured in a short time at a low temperature (0-5 ℃) so as to be convenient for mechanical operation.
4. The stone surface adhesive also has good mechanical properties, 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 will be described in detail with reference to examples, but it should not be construed as being limited thereto, but by way of example only. While at the same time becoming clearer and more readily understood by way of illustration of the advantages of the present invention.
The test methods or test methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials, unless otherwise specified, are obtained from conventional commercial sources or prepared in conventional manner.
Experimental discussion of the reaction ratio of the base amine raw material and the modifier for the modified amine curing agent:
the modification method of the modified amine curing agent comprises the following steps:
adding basic amine raw materials into reaction equipment, heating to 30-40 ℃ under stirring, adding modifier in batches every 20-30min under continuous stirring, heating to 70-80 ℃ after the addition, reacting for 1.5-2h under heat preservation, and discharging at normal temperature to obtain the modified amine curing agent.
Table one: reaction ratio of basic amine raw material and modifier
Wherein 1,3-BAC is 1, 3-cyclohexanedimethylamine, IPDA is isophorone diamine, and HMDA is 4,4' -diaminodicyclohexylmethane.
TMPTA (trimethylolpropane triacrylate) and the modified amine curing agent are uniformly mixed according to the proportion of 1:1, cured for 7 days and tested for mechanical properties, and the specific results are as follows:
and (II) table: modified amine curing agent example Performance test
| Sequence 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 data shows that the preferred curing agents are 2, 8, 14, with the best performance of curing agent 14.
And (3) preparation of a component A:
weighing a raw material 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 portion ratio, then, putting all the materials into a stirrer, controlling the rotating speed to be 50-80r/min, stirring for more than 30min till the polymerization inhibitor is completely dissolved, stopping stirring, defoaming for 5min under the condition of minus 0.1MPa, and discharging to obtain a component A;
and (2) preparing a component B:
firstly preparing a modified amine curing agent according to a modification method, weighing a raw material modified amine curing agent, a second coupling agent, a second defoaming agent and a second leveling agent according to the weight portion ratio, then putting all the materials into a stirrer, controlling the rotating speed to be 50-80r/min, stirring for more than 30min to be completely uniform, stopping stirring, defoaming for 5min under the condition of minus 0.1MPa, and discharging to obtain the component B.
The modified amine curing agent is brought into the preparation scheme of the component A and the component B, and the stone surface adhesive prepared by the invention is obtained.
Table three: the specific implementation scheme of the component A and the component B is as follows:
note that: the stabilizer, the defoamer, the leveling agent and the coupling agent are all added in conventional amounts.
TMPTA is trimethylolpropane triacrylate, PET4A is pentaerythritol tetraacrylate, KH-560 is the trade name of 3- (2, 3-glycidoxy) propyl trimethoxysilane, BYK-051 is the trade name of a bubble breaking polymer solution without silicone, BYK-354 is the trade name of a polyacrylate solution, BYK-085 is the trade name of a methylalkylpolysiloxane, KH-550 is the trade name of 3-aminopropyl triethoxysilane, BYK-323 is the trade name of a polymethylalkyl-methylarylalkylsiloxane.
Mixing the components according to the mixing ratio of the component A and the component B, curing for 7 days, and testing the mechanical properties, wherein the specific results are as follows:
table four: example Performance test
Note that: the detection criteria referred to in tables two and four are as follows, appearance: the sample was poured into a cuvette of 3ml and the color chart was visually checked.
Viscosity, pot life: GB/T12954-1991 building adhesive general test method.
Hardness: GB/T531.1-2008 was tested.
Tensile shear strength: GB/T2567-2008 was tested.
Yellowing resistance: GB/T23983-2009 test was carried out using UVB340 lamp with an irradiation intensity of 0.68W/m 2 The irradiation time was accumulated for 7d.
Gloss level: GB/T9754-2007.
The coating effect of the white stone surface adhesive: the two components are uniformly mixed and smeared on the surface of the white stone, the surface is maintained for 2 days at 25 ℃, and whether air bubbles exist on the surface is visually inspected.
As can be seen from Table four, the data shows that the performance of examples one, two and three is better than the commercial product (example 13), 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 coating effect (whether air bubbles exist) and the like, and has obvious overall performance improving effect.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended 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 such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (8)
1. The low-viscosity yellowing-resistant quick-setting 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;
the basic amine raw material of the modified amine curing agent is selected from 1, 3-diaminomethylcyclohexane, isophoronediamine, 4' -diaminodicyclohexylmethane;
the modification method of the modified amine curing agent comprises the following steps:
adding basic amine raw materials into reaction equipment, heating to 30-40 ℃ under stirring, and adding a modifier in batches every 20-30min under continuous stirring, wherein the reaction ratio of the basic amine and the modifier is the basic amine: modifier=100 (40-100), after the addition of the materials, heating to 70-80 ℃, preserving heat for reaction for 1.5-2h, and discharging at normal temperature to obtain the modified amine curing agent;
the modifier is selected from 1, 2-cyclohexanediol diglycidyl ether and 4, 5-epoxy tetrahydrophthalic acid diglycidyl ester.
2. The low-viscosity yellowing-resistant quick-setting stone face adhesive according to 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 quick-setting stone face adhesive according to 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 setting stone face adhesive of 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 trimethoxysilane; the first defoamer is selected from a foam breaking polymer solution without silicone; the first leveling agent is selected from polyacrylate solutions.
5. The low-viscosity yellowing-resistant fast-setting stone face adhesive according to claim 1, wherein in the component b: the second coupling agent is selected from 3-aminopropyl triethoxysilane; the second defoamer is selected from methyl alkyl polysiloxanes; the second leveling agent is selected from polymethylalkyl-methylarylalkylsiloxane.
6. A method for preparing the low-viscosity yellowing-resistant fast-setting stone face adhesive according to any one of claims 1 to 5, comprising the steps of:
and (3) preparation of a component A:
weighing a raw material 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 portion ratio, then putting all the raw material high-activity multifunctional acrylate monomer, the polymerization inhibitor, the first coupling agent, the first defoaming agent and the first leveling agent into a stirrer, stirring uniformly until the polymerization inhibitor is completely dissolved, and discharging after vacuum treatment to obtain a component A;
and (2) preparing a component B:
firstly preparing a modified amine curing agent according to a modification method, then weighing the raw material modified amine curing agent, a second coupling agent, a second defoaming agent and a second leveling agent according to the weight portion ratio, then putting all the materials into a stirrer, uniformly stirring, vacuum-treating and discharging to obtain the component B.
7. The method for preparing the low-viscosity yellowing-resistant quick-setting stone surface adhesive according to claim 6, wherein the stirring and vacuum treatment methods of the two components of A and B comprise the following steps: the rotating speed is controlled to be 50-80r/min, stirring is carried out for more than 30min until the stirring is completely uniform, and defoaming is carried out for 5min under the condition of minus 0.1 MPa.
8. The application of the low-viscosity yellowing-resistant quick-setting stone surface adhesive is characterized in that the component A and the component B are selected and used according to the weight ratio of 1: and 1-2, and then the construction can be carried out after the mixture is mixed.
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| JP4753196B2 (en) * | 2002-08-29 | 2011-08-24 | 綜研化学株式会社 | Optical member pressure-sensitive adhesive composition and optical member-use pressure-sensitive adhesive sheet using the pressure-sensitive adhesive composition |
| JP5076459B2 (en) * | 2006-11-28 | 2012-11-21 | 住友金属鉱山株式会社 | UV curable adhesive for optical isolators |
| EP2028207A1 (en) * | 2007-08-14 | 2009-02-25 | Swancor Industrial Co., Ltd. | Resin composition for composite material parts |
| JP5320712B2 (en) * | 2007-09-25 | 2013-10-23 | 住友金属鉱山株式会社 | UV curable adhesive for optical isolators |
| CN101974304A (en) * | 2010-11-08 | 2011-02-16 | 武汉理工大学 | Vinylester resin stone adhesive and preparation method thereof |
| EP2468792A1 (en) * | 2010-12-23 | 2012-06-27 | 3M Innovative Properties Company | Curable adhesive composition |
| CN102167962B (en) * | 2011-03-22 | 2013-04-10 | 深圳市飞世尔实业有限公司 | Photocuring adhesive used for adhering optic glass lenses and preparation method thereof |
| CN103087639B (en) * | 2011-10-31 | 2014-07-16 | 北京天山新材料技术股份有限公司 | Waterproof dual-component acrylate adhesive and its preparation method |
| CN103571413B (en) * | 2013-11-13 | 2015-06-03 | 苏州市姑苏新型建材有限公司 | Dry-hanging stone curtain wall epoxy adhesive and preparation method thereof |
| CN109266277A (en) * | 2018-09-28 | 2019-01-25 | 湖北绿色家园材料技术股份有限公司 | A kind of transparent, high rigidity, color inhibition epoxy stone material surface glue and its preparation process |
| CN110982469A (en) * | 2019-11-29 | 2020-04-10 | 湖南柯盛新材料有限公司 | Stone repairing adhesive and application thereof |
| CN111560233B (en) * | 2020-05-18 | 2022-03-22 | 杭州华圩新材料科技有限公司 | High-performance low-toxicity medical UV adhesive and preparation method thereof |
| CN113150700B (en) * | 2021-03-25 | 2022-03-04 | 湖南神力铃胶粘剂制造有限公司 | Epoxy stone repair face adhesive with yellowing resistance, low viscosity and hydrophilic curing and preparation method thereof |
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Effective date of registration: 20230925 Address after: No. 6 Danjin Road, Industrial Concentration Zone, Baita Town, Jintan District, Changzhou City, Jiangsu Province, 213299 Patentee after: Jiangsu Hercules Marble Care Materials Co.,Ltd. Address before: 430040 No.26, Jinhai Industrial Park Road, Jinyinhu office, Dongxihu District, Wuhan City, Hubei Province Patentee before: WUHAN KEDA MARBLE PROTECTIVE MATERIALS Co.,Ltd. |
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