A ceramic tile back coating interface agent emulsion and preparation method thereof

Abstract

A tile back-coating interface agent emulsion, belonging to the field of tile interface agents, comprises the following components by weight: 40-60 parts styrene, 260-300 parts butyl acrylate, 100-140 parts 2-ethylhexyl acrylate, 2-3 parts acrylic acid, 12-18 parts hydroxyethyl methacrylate, 2-4 parts coupling agent, 1-3 parts cross-linking agent, 3-5 parts film-forming aid, 2-3 parts initiator, 7.3-12.8 parts emulsifier, 0.5-1 part defoamer, and 2-4 parts bactericide. The emulsifier includes 7-12 parts sodium dodecylbenzenesulfonate and 0.3-0.8 parts sodium vinylbenzenesulfonate. The tile back-coating interface agent emulsion prepared in the present invention and a preparation method thereof are proposed. This solves the problems of poor water and alkali resistance of current tile back-coating interface agent emulsions, while also having the advantages of excellent bonding strength and low water absorption.

Description

Technical Field

[0001] The invention belongs to the field of tile interface agents, and particularly relates to a tile back-coating interface agent emulsion and a preparation method thereof. Background Art

[0002] Ceramic tiles are an indispensable material in modern home renovations, primarily used for walls and floors. As people pursue higher living standards, the use of high-end tiles, such as microcrystalline stone, vitrified tiles, and marble, is also increasing. While these high-end tiles are elegant and aesthetically pleasing, enhancing the quality of a space, they are prone to tile peeling. Against this backdrop, tile back-coating interface agents have emerged. They are used to treat the backside of wet-laid tiles, effectively improving the bond between the tile and the adhesive, and addressing the common hollowing and peeling issues associated with wet-laid tiles. They are also suitable for treating the backsides of stone and other brick materials with low water absorption, a dense texture, and a smooth surface. Therefore, tile back-coating interface agents have become essential for tile wall installation.

[0003] Although there are some products for tile back coating interface agents on the market, their water and alkali resistance are poor. Moreover, when the tiles are pasted, the slurry contains a large amount of water and substances such as strong alkaline cement, which can easily destroy the adhesion between the coating and the tiles, resulting in low bonding strength, tile falling off and other problems. Summary of the Invention

[0004] In order to solve the problems existing in the above-mentioned prior art, the present invention provides a tile back coating interface agent emulsion and a preparation method thereof. By combining the various components in the emulsion, the problems of poor water resistance and alkali resistance of the tile back coating interface agent emulsion are solved, and at the same time, the emulsion has the advantages of good bonding strength and low water absorption.

[0005] The specific technical solution adopted in the present invention is:

[0006] A tile back coating interface agent emulsion comprises the following components in parts by weight: 40-60 parts of styrene, 260-300 parts of butyl acrylate, 100-140 parts of 2-ethylhexyl acrylate, 2-3 parts of acrylic acid, 12-18 parts of hydroxyethyl methacrylate, 2-4 parts of a coupling agent, 1-3 parts of a crosslinking agent, 3-5 parts of a film-forming aid, 2-3 parts of an initiator, 7.3-12.8 parts of an emulsifier, 0.5-1 part of a defoamer, and 2-4 parts of a bactericide. The emulsifier comprises 7-12 parts of sodium dodecylbenzene sulfonate and 0.3-0.8 parts of sodium vinylbenzene sulfonate.

[0007] Furthermore, the tile back coating interface agent emulsion includes the following components in parts by weight: 50 parts of styrene, 280 parts of butyl acrylate, 120 parts of 2-ethylhexyl acrylate, 3 parts of acrylic acid, 15 parts of hydroxyethyl methacrylate, 3 parts of coupling agent, 2 parts of cross-linking agent, 4 parts of film-forming aid, 2.4 parts of initiator, 9 parts of sodium dodecylbenzenesulfonate, 0.5 part of sodium vinylbenzenesulfonate, 0.5 part of defoaming agent, and 3 parts of bactericide.

[0008] Furthermore, the coupling agent is a silane coupling agent.

[0009] Furthermore, the coupling agent is silane coupling agent A-174.

[0010] Furthermore, the cross-linking agent is divinylbenzene.

[0011] Furthermore, the film-forming aid is lauryl alcohol ester.

[0012] Furthermore, the initiator is ammonium persulfate.

[0013] A method for preparing the above-mentioned tile back coating interface agent emulsion comprises the following steps:

[0014] A: According to the ratio of tile back coating interface agent emulsion, weigh each component and set aside;

[0015] B: Add 180-220 parts of water to a stirring container, add sodium dodecylbenzenesulfonate and sodium vinylbenzenesulfonate, stir evenly, then add styrene, butyl acrylate, 2-ethylhexyl acrylate, acrylic acid, hydroxyethyl methacrylate, divinylbenzene, and dodecyl alcohol, and continue stirring and emulsifying for 15-30 minutes to prepare a pre-emulsion;

[0016] C. Add 180-220 parts of water to the reaction vessel, add the remaining sodium dodecylbenzene sulfonate, raise the temperature to 80-85° C., add 3-8% of the pre-emulsion and 1-1.2 parts of the initiator, continue to heat, and add the remaining pre-emulsion and initiator dropwise after the temperature no longer rises. The addition temperature is controlled at 84-86° C. and the addition time is controlled to be 180-200 min. When the addition reaches 120-150 min, the silane coupling agent is added and stirred evenly. After the pre-emulsion and initiator are all added dropwise, the mixture is kept warm for 25-40 min, then cooled to 65-68° C., 0.2-0.6 parts of the oxidant and 0.2-0.6 parts of the reducing agent are added dropwise at the same time, and the addition time is 25-40 min. After the addition is complete, the mixture is kept warm for 20-30 min, and the pH is adjusted to 7.5-8 with a pH regulator. A defoamer and a bactericide are added, and the mixture is stirred evenly and filtered to obtain an interface agent emulsion.

[0017] The beneficial effects of the present invention are:

[0018] 1. In the present invention, a conventional emulsifier sodium dodecylbenzenesulfonate without double bonds is combined with a reactive anionic emulsifier sodium vinylbenzenesulfonate to reduce the water absorption rate of the interface agent emulsion. The conventional and reactive anions are combined. The conventional emulsifier has low cost and good emulsification effect. The reactive anionic emulsifier participates in the polymerization reaction, reduces free emulsifier, reduces the hydrophilicity of the oligomer, and reduces the water-absorbing groups formed by the aggregation of free emulsifier and hydrophilic oligomer, thereby reducing the water absorption rate.

[0019] 2. In order to reduce the water absorption rate, the present invention also introduces silane coupling agent A-174 and cross-linking agent divinylbenzene by polymerization. By increasing the cross-linking degree and increasing the molecular weight, the hydrophobicity of the coating is improved and the water absorption rate is reduced. At the same time, the hydroxyl groups formed by the partial hydrolysis of the silane coupling agent react with the substrate to improve the bonding strength and reduce the problem of tile falling off.

[0020] 3. The present invention introduces dodecyl alcohol ester. Dodecyl alcohol ester is added during the polymerization process, which has the effects of softening polymer chains, reducing polymer chain crystallinity, and increasing polymerization molecular weight. In the film-forming process, dodecyl alcohol ester has a plasticizing effect on polymer particles, thereby increasing the flexibility of the emulsion film and the initial adhesion. It still has good flexibility and adhesion in a relatively low temperature environment, reducing the shedding of tiles caused by the high rigidity of the emulsion film due to low temperature. At the same time, due to the hydrophobic effect of dodecyl alcohol ester, the water resistance of the coating is further enhanced.

[0021] 4. Hydroxyethyl methacrylate polar monomer is introduced into the polymerization process of the present invention. Hydroxyethyl methacrylate polar monomer can improve the stability of emulsion particles. The hydroxyl group contained in it reacts with groups such as carboxyl to increase the crosslinking degree of the emulsion particles. Due to its polar effect, it can also improve the bonding strength.

[0022] 5. The silane coupling agent, divinylbenzene and hydroxyethyl methacrylate in the present invention form an interpenetrating network crosslinking structure through self-crosslinking and mutual crosslinking, forming a dense protective layer on the surface of the coating, thereby improving the water resistance and alkali resistance of the interface agent emulsion.

[0023] 6. The preparation method of the present invention ensures the stability and full progress of the reaction by strictly controlling parameters such as temperature and dropwise addition rate, so as to ensure that each component fully exerts its own function. DETAILED DESCRIPTION

[0024] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention.

[0025] The defoaming agent in the present invention is NXZ defoaming agent produced by BASF, Germany, the bactericide is BIT20 bactericide produced by Shandong Xinwei Chemical Technology Co., Ltd., the oxidant is tert-butyl hydroperoxide, the reducing agent is sodium bisulfite, and the water is deionized water; unless otherwise specified, other raw materials used can be purchased from the market. 1. Specific embodiments Specific embodiment 1

[0028] A: According to the ratio of the interface agent emulsion, weigh 50 parts of styrene propene, 280 parts of butyl acrylate, 120 parts of 2-ethylhexyl acrylate, 3 parts of acrylic acid, 15 parts of hydroxyethyl methacrylate, 3 parts of coupling agent, 2 parts of cross-linking agent, 4 parts of film-forming aid, 2.4 parts of initiator, 9 parts of sodium dodecylbenzenesulfonate, 0.5 parts of sodium vinylbenzenesulfonate, 0.5 parts of defoamer, and 3 parts of fungicide;

[0029] B: Add 200 parts of deionized water to a pre-emulsification kettle, start stirring, add 8 parts of sodium dodecylbenzenesulfonate and 0.5 parts of sodium vinylbenzenesulfonate, and after 15 minutes, add 50 parts of styrene, 280 parts of n-butyl acrylate, 120 parts of 2-ethylhexyl acrylate, 3 parts of acrylic acid, 15 parts of hydroxyethyl methacrylate, 2 parts of divinylbenzene, and 4 parts of lauryl alcohol, and continue emulsifying at high speed for 20 minutes to prepare a pre-emulsion;

[0030] C. In reactor, add 210 parts of deionized water, open stirring, add 1 part of dodecylbenzene sodium sulfonate, when being warming up to 85 ℃, add 5% of the pre-emulsion total amount and 1.2 parts of initiators, continue to heat up, wait 2 minutes after treating that temperature no longer rises, drip remaining pre-emulsion and initiator, the dropping temperature is controlled at 85 ℃, and the control dropping time is 200 minutes, and 3 parts of coupling agents will be added and stir when being added dropwise to 150 minutes, after pre-emulsion and initiator are all added dropwise, be incubated 30 minutes, then cool to 66 ℃, simultaneously drip 0.5 part of oxidant, 0.5 part of reducing agent, the dropping time is 30 minutes, after being added dropwise, be incubated 25 minutes, adopt 15% sodium hydroxide solution to adjust pH to 7.8 again, add 0.5 part of defoamer and 3 parts of bactericide, stir and filter to obtain interface agent emulsion. Specific embodiment 2

[0032] A: According to the ratio of the interface agent emulsion, weigh 40 parts of styrene propene, 260 parts of butyl acrylate, 100 parts of 2-ethylhexyl acrylate, 2.4 parts of acrylic acid, 12 parts of hydroxyethyl methacrylate, 2 parts of coupling agent, 1 part of crosslinking agent, 3 parts of film-forming aid, 2 parts of initiator, 7 parts of sodium dodecylbenzenesulfonate, 0.3 parts of sodium vinylbenzenesulfonate, 0.8 parts of defoamer, and 2 parts of fungicide;

[0033] B: Add 180 parts of deionized water to a pre-emulsification kettle, start stirring, add 6 parts of sodium dodecylbenzenesulfonate and 0.3 parts of sodium vinylbenzenesulfonate, stir for 15 minutes, then add 40 parts of styrene, 260 parts of n-butyl acrylate, 100 parts of 2-ethylhexyl acrylate, 2.4 parts of acrylic acid, 12 parts of hydroxyethyl methacrylate, 1 part of divinylbenzene, and 3 parts of lauryl alcohol, and continue to stir at high speed for 30 minutes to prepare a pre-emulsion;

[0034] C. In reactor, 180 parts of deionized water are added, stirring is opened, 1 part of sodium dodecylbenzene sulfonate is added, when being warming up to 80 ℃, 3% of the total amount of pre-emulsion and 1 part of initiator are added, continue heating, wait 2min after treating that temperature no longer rises, drip remaining pre-emulsion and initiator, the dropping temperature is controlled at 84 ℃, and the control dropping time is 180min. When being added dropwise to 120min, 3 parts of coupling agents will be added and stir, after pre-emulsion and initiator are all dropped, insulation is 25min, then cool to 65 ℃, simultaneously drip 0.2 part of oxidant, 0.2 part of reducing agent, the dropping time is 25min, after dropping, insulation is 20min, adopt 15% sodium hydroxide solution to adjust pH to 7.5 again, add 0.8 part of defoamer and 2 parts of bactericide, filter and obtain interfacial agent emulsion after stirring. Specific embodiment 3

[0036] A: According to the ratio of the interface agent emulsion, weigh 60 parts of styrene propene, 300 parts of butyl acrylate, 140 parts of 2-ethylhexyl acrylate, 2 parts of acrylic acid, 18 parts of hydroxyethyl methacrylate, 4 parts of coupling agent, 3 parts of cross-linking agent, 5 parts of film-forming aid, 3 parts of initiator, 12 parts of sodium dodecylbenzenesulfonate, 0.8 parts of sodium vinylbenzenesulfonate, 1 part of defoamer, and 4 parts of fungicide;

[0037] B: Add 220 parts of deionized water to a pre-emulsification kettle, start stirring, add 10 parts of sodium dodecylbenzenesulfonate and 0.8 parts of sodium vinylbenzenesulfonate, and after 15 minutes, add 60 parts of styrene, 300 parts of n-butyl acrylate, 140 parts of 2-ethylhexyl acrylate, 2 parts of acrylic acid, 18 parts of hydroxyethyl methacrylate, 3 parts of divinylbenzene, and 5 parts of lauryl alcohol, and continue emulsifying at high speed for 15 minutes to prepare a pre-emulsion;

[0038] C. In reactor, add 220 parts of deionized water, open stirring, add 2 parts of sodium dodecylbenzene sulfonate, when being warming up to 82 ℃, add 8% of the pre-emulsion total amount and 1.1 parts of initiator, continue heating, wait 2 minutes after treating that temperature no longer rises, drip remaining pre-emulsion and initiator, the dropping temperature is controlled at 85 ℃, and the control dropping time is 185 minutes, and 4 parts of coupling agents will be added and stir when being added dropwise to 135 minutes, after pre-emulsion and initiator are all dropped, insulation 40 minutes, then cool to 68 ℃, drip 0.6 part of oxidant, 0.6 part of reducing agent simultaneously, the dropping time is 40 minutes, after dropping, insulation 30 minutes, adopt 15% sodium hydroxide solution to adjust pH to 8 again, add 1 part of defoamer and 4 parts of bactericide, stir and filter to obtain interface agent emulsion.

[0039] Comparative Example 1

[0040] The only difference between Comparative Example 1 and Example 1 is that the emulsifier in Comparative Example 1 includes only sodium dodecylbenzenesulfonate and does not contain sodium vinylbenzenesulfonate.

[0041] The only difference between Comparative Example 2 and Example 1 is that the emulsifier in Comparative Example 2 includes only sodium vinylbenzenesulfonate and does not contain sodium dodecylbenzenesulfonate.

[0042] 2. Performance Testing

[0043] The tile back coating interface agent emulsions prepared in the above examples and comparative examples were tested, wherein the bonding strength was tested according to the standard JC / T 547-2017 Ceramic Tile Adhesive; the water absorption rate was measured by immersing an emulsion film of size 2.0 cm*1.5 cm*0.06 cm in deionized water at 23°C according to GB / T1034-1998. The test results are shown in Table 1.

[0044] Table 1

[0045]

[0046] As can be seen from Table 1, the tile back coating interface agent emulsion prepared in the embodiment of the present invention has a bonding strength of ≥1.48, a bonding strength after immersion in water of ≥1.26 MPa, a bonding strength after heat aging of ≥1.51 MPa, a freeze-thaw cycle bonding strength of ≥1.23 MPa, and an emulsion film water absorption rate of ≤4.2%.

[0047] It can be seen from Example 1 and Comparative Examples 1-2 that the emulsifier in Comparative Example 1 is solely the conventional emulsifier sodium dodecylbenzenesulfonate without double bonds, and the emulsifier in Comparative Example 2 is solely the reactive anionic emulsifier sodium vinylbenzenesulfonate. Through the performance of the prepared tile back coating interface agent emulsion, it can be found that, under the premise that the total amount of emulsifier remains unchanged, the emulsion obtained by using the conventional emulsifier in combination with the reactive anionic emulsifier has better performance than that of using a single emulsifier. This is because the conventional emulsifier has low cost and good emulsification effect, and the reactive anionic emulsifier participates in the polymerization reaction, reduces the free emulsifier, reduces the hydrophilicity of the oligomer, and reduces the water-absorbing groups formed by the aggregation of the free emulsifier and the hydrophilic oligomer, thereby reducing the water absorption rate.

Claims

1. A tile back coating interface agent emulsion, characterized in that: The invention comprises the following components in parts by weight: 40-60 parts of styrene, 260-300 parts of butyl acrylate, 100-140 parts of 2-ethylhexyl acrylate, 2-3 parts of acrylic acid, 12-18 parts of hydroxyethyl methacrylate, 2-4 parts of coupling agent, 1-3 parts of crosslinking agent, 3-5 parts of film-forming aid, 2-3 parts of initiator, 7.3-12.8 parts of emulsifier, 0.5-1 part of defoamer, and 2-4 parts of fungicide, wherein the emulsifier comprises 7-12 parts of sodium dodecylbenzene sulfonate and 0.3-0.8 parts of sodium vinylbenzene sulfonate. The coupling agent is a silane coupling agent; The cross-linking agent is divinylbenzene; The film-forming aid is lauryl alcohol ester.

2. A tile back coating interface agent emulsion according to claim 1, characterized in that: The invention comprises the following components in parts by weight: 50 parts of styrene, 280 parts of butyl acrylate, 120 parts of 2-ethylhexyl acrylate, 3 parts of acrylic acid, 15 parts of hydroxyethyl methacrylate, 3 parts of coupling agent, 2 parts of crosslinking agent, 4 parts of film-forming aid, 2.4 parts of initiator, 9 parts of sodium dodecylbenzenesulfonate, 0.5 parts of sodium vinylbenzenesulfonate, 0.5 parts of defoaming agent and 3 parts of bactericide.

3. The tile back coating interface agent emulsion according to claim 1, characterized in that: The coupling agent is silane coupling agent A-174.

4. A tile back coating interface agent emulsion according to any one of claims 1-2, characterized in that: The initiator is ammonium persulfate.

5. A method for preparing the tile back coating interface agent emulsion according to any one of claims 1 to 2, characterized in that: The following steps are involved: A: According to the ratio of tile back coating interface agent emulsion, weigh each component and set aside; B: Add 180-220 parts of water to a stirring container, add sodium dodecylbenzenesulfonate and sodium vinylbenzenesulfonate, stir evenly, then add styrene, butyl acrylate, 2-ethylhexyl acrylate, acrylic acid, hydroxyethyl methacrylate, divinylbenzene, and dodecyl alcohol, and continue stirring and emulsifying for 15-30 minutes to prepare a pre-emulsion; C. Add 180-220 parts of water to the reaction vessel, add the remaining sodium dodecylbenzene sulfonate, raise the temperature to 80-85°C, add 3-8% of the pre-emulsion and 1-1.2 parts of the initiator, continue to heat, and add the remaining pre-emulsion and initiator dropwise after the temperature no longer rises. The addition temperature is controlled at 84-86°C and the addition time is controlled to be 180-200min. When the addition reaches 120-150min, the silane coupling agent is added and stirred evenly. After the pre-emulsion and initiator are all added dropwise, keep warm for 25-40min, then cool to 65-68°C, and simultaneously add 0.2-0.6 parts of the oxidant and 0.2-0.6 parts of the reducing agent dropwise for 25-40min. After the addition is complete, keep warm for 20-30min, then adjust the pH to 7.5-8 with a pH regulator, add a defoamer and a bactericide, stir evenly, and filter to obtain an interface agent emulsion.

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