Preparation method of two-component ceramic tile back adhesive emulsion and two-component ceramic tile back adhesive

Abstract

The present application belongs to the field of ceramic tile back adhesive, and particularly relates to a two-component ceramic tile back adhesive emulsion, which comprises the following components in parts by weight: styrene 33-110, n-butyl acrylate 303-410, iso-octyl acrylate 105-215, beta-carboxyethyl acrylate 7-11, hydroxyethyl methacrylate 14-20, acrylamide 2.4-4, acetoacetoxy ethyl methacrylate 3.5-6, defoaming agent 0.4-0.8, bactericide 1.8-2.5, initiator 0.6-2, emulsifier 4.5-13, and curing agent 3-6. The back adhesive emulsion of the present application does not contain APEO, is free of formaldehyde and ammonia, has no other pollution emissions, has good product stability, solves the problems of poor water resistance and low bonding strength of the two-component ceramic tile back adhesive emulsion, has good powder compatibility and good toughness, and finally has excellent product performance and is green and environmentally friendly.

Description

TECHNICAL FIELD

[0001] The application belongs to the field of ceramic tile back adhesive, and particularly relates to a preparation method of a two-component ceramic tile back adhesive emulsion and a two-component ceramic tile back adhesive. BACKGROUND

[0002] Traditional ceramic tile sticking is carried out by using cement mortar, but only applicable to ceramic tiles with high water absorption, and ceramic tiles with low water absorption are easy to cause hollowing or even falling off when stuck by using cement mortar. The two-component product composed of various polymer emulsions and inorganic silicate materials has the characteristics of good waterproof performance, small drying shrinkage, good toughness, strong bonding force with cement-based materials and the like, and avoids the easy hollowing or falling off after ceramic tile paving construction. The two-component back adhesive has excellent bonding force, and can be used for sticking various ceramic tile specifications and interface treatment. SUMMARY

[0003] In order to solve the problems in the prior art, the application provides a ceramic tile back coating interface agent emulsion. The back adhesive emulsion of the application does not contain APEO, is free of formaldehyde and ammonia, has no other pollution emissions, has good product stability, solves the problems of poor water resistance and low bonding strength of the two-component ceramic tile back adhesive emulsion, and has good powder compatibility, good toughness and the like. The final product has excellent performance and is green and environmentally friendly.

[0004] The application adopts the specific technical scheme:

[0005] The two-component ceramic tile back adhesive emulsion comprises the following components in parts by weight: styrene 33-110 parts, n-butyl acrylate 303-410 parts, iso-octyl acrylate 105-215 parts, beta-carboxyethyl acrylate 7-11 parts, hydroxyethyl methacrylate 14-20 parts, acrylamide 2.4-4 parts, acetoacetoxy methyl methacrylate 3.5-6 parts, defoaming agent 0.4-0.8 parts, bactericide 1.8-2.5 parts, initiator 0.6-2 parts, emulsifier 4.5-13 parts, and curing agent 3-6 parts.

[0006] Further, the emulsifier comprises reaction-type anionic emulsifier 4-11 parts and reaction-type nonionic emulsifier 0.5-2 parts.

[0007] A preparation method of a two-component ceramic tile back adhesive emulsion comprises the following steps:

[0008] A. Preparation of core layer pre-emulsion: water 160-200 parts, reaction-type anionic emulsifier 3-8 parts, styrene 30-100 parts, n-butyl acrylate 300-400 parts, iso-octyl acrylate 100-200 parts, beta-carboxyethyl acrylate 5-8 parts, hydroxyethyl methacrylate 12-17 parts, and acetoacetoxy methyl methacrylate 3.5-6 parts are added into a container a, and then uniformly stirred to obtain the core layer pre-emulsion;

[0009] B, preparation of shell pre-emulsion, add water 20-60 parts, reactive non-ionic emulsifier 0.5-2 parts, styrene 3-10 parts, isooctyl acrylate 5-15 parts, n-butyl acrylate 3-10 parts, acrylamide 2.4-4 parts, beta-carboxyethyl acrylate 2-3 parts, and hydroxyethyl methacrylate 2-3 parts to container b, then stir uniformly to obtain shell pre-emulsion;

[0010] C, preparation of initiator: the initiator includes seed initiator, core layer initiator and shell initiator, wherein the seed initiator: 0.2-0.8 parts of initiator is dissolved in 12-18 parts of water; the core layer initiator: 0.3-1 parts of initiator is dissolved in 26-32 parts of water; the shell initiator: 0.1-0.2 parts of initiator is dissolved in 4-7 parts of water;

[0011] D, preparation of emulsion: add water 200-220 parts, reactive anionic emulsifier 1-3 parts to container c, stir and heat to 80-85 DEG C, first add 2.5%-5% of core layer pre-emulsion, then add seed initiator and keep warm for 20-30 min, then add the remaining core layer pre-emulsion and core layer initiator dropwise, after dropwise addition, keep warm for 30-40 min, then add shell pre-emulsion and shell initiator dropwise, after dropwise addition, keep warm for 45-75 min, after the end of keeping warm, adjust pH to 7-8, add curing agent 3-6 parts, add defoaming agent 0.4-0.8 parts and bactericide 1.8-2.5 parts, filter to obtain two-component ceramic tile back adhesive emulsion.

[0012] Further, when the pH is adjusted to 7-8 after the end of keeping warm, the temperature needs to be reduced to below 40 DEG C first.

[0013] A two-component ceramic tile back adhesive based on the above two-component ceramic tile back adhesive emulsion, comprising the following components by weight: water 500-700 parts, two-component ceramic tile back adhesive emulsion 350-450 parts, cement 450-600 parts, defoaming agent 0.5-3 parts, bactericide 2-5 parts, sand 400-560 parts, cellulose 1-3 parts.

[0014] Further, the sand includes 80-120 mesh sand 120-180 parts and 40-80 mesh sand 280-380 parts.

[0015] The beneficial effects of the present application are:

[0016] 1, the back adhesive emulsion of the present application does not contain APEO, and is free of formaldehyde, ammonia and other pollution emissions, and has good product stability, solves the problems of poor water resistance and low bonding strength of two-component ceramic tile back adhesive emulsion, and has good powder compatibility, good toughness and other advantages, and the final product has excellent performance and is green and environmentally friendly.

[0017] 2、The polymeric core layer of the present application introduces acetoacetoxy ethyl methacrylate into the core layer, and the particle deformation is completed before crosslinking begins, the polymer chains in the particle diffuse and penetrate, and the crosslinking reaction can only begin when the diffusion reaches a certain depth in the adjacent particle, the compactness of the polymer colloidal film is improved, and good initial adhesion is provided for the coating film.

[0018] 3、The low glass transition temperature acrylic monomer beta-carboxyethyl acrylate introduced in the present application replaces acrylic acid, improves the flexibility and initial adhesion of the emulsion film, and improves the adhesion.

[0019] 4、The introduction of hydroxyethyl methacrylate polar monomer into the core and shell layers of the polymerization process of the present application improves the stability of the emulsion particles and the crosslinking degree of the emulsion particles, improves the hydrophobicity, and also improves the bonding strength due to its polarity.

[0020] 5、The emulsion of the present application adopts a core-shell structure, and the shell layer introduces a reactive nonionic emulsifier and a hydrophilic monomer, which improves the thickness of the particle hydration layer, increases the stability of the emulsion particles, and improves the compatibility with the powder. DETAILED DESCRIPTION

[0021] The technical solutions in the embodiments of the present application will be clearly and completely described below in combination with the embodiments of the present application.

[0022] The defoaming agent in the present application is NXZ defoaming agent produced by BASF, Germany, the fungicide is BIT20 fungicide produced by Shandong Xiwu Chemical Technology Co., Ltd., and the water is deionized water; other raw materials used can be purchased from the market if not specifically mentioned. I. Specific embodiments Specific embodiment 1

[0025] A. Preparation of the core layer pre-emulsion, 180 parts of water, 5 parts of a reactive anionic emulsifier, 50 parts of styrene, 350 parts of n-butyl acrylate, 150 parts of isooctyl acrylate, 6 parts of beta-carboxyethyl acrylate, 15 parts of hydroxyethyl methacrylate, and 5 parts of acetoacetoxy ethyl methacrylate were added to a reaction kettle a, and then stirred uniformly to obtain a core layer pre-emulsion;

[0026] B. Preparation of the shell layer pre-emulsion, 40 parts of water, 1 part of a reactive nonionic emulsifier, 5 parts of styrene, 10 parts of isooctyl acrylate, 8 parts of n-butyl acrylate, 3 parts of acrylamide, 2.4 parts of beta-carboxyethyl acrylate, and 2.4 parts of hydroxyethyl methacrylate were added to a reaction kettle b, and then stirred uniformly to obtain a shell layer pre-emulsion;

[0027] C. Preparation of initiator: the initiator includes seed initiator, core layer initiator and shell layer initiator, wherein seed initiator: 0.5 parts of initiator is dissolved in 15 parts of water; core layer initiator: 0.5 parts of initiator is dissolved in 30 parts of water; shell layer initiator: 0.15 parts of initiator is dissolved in 6 parts of water;

[0028] D. Preparation of emulsion: 210 parts of water, 2 parts of reactive anionic emulsifier are added into the reaction kettle c, stirred and heated to 83°C, 3.5% of core layer pre-emulsion is added first, then seed initiator is added and kept for 25 min, then the remaining core layer pre-emulsion and core layer initiator are added dropwise, after the dropwise addition is completed, it is kept for 35 min, then shell layer pre-emulsion and shell layer initiator are added dropwise, after the dropwise addition is completed, it is kept for 60 min, after the keeping is completed, it is cooled to 38°C and the pH is adjusted to 7.5 by using ammonia water, 5 parts of curing agent, 0.6 parts of defoaming agent and 2 parts of bactericide are added, and then a two-component ceramic tile back adhesive emulsion is obtained after filtration.

[0029] E. A two-component ceramic tile back adhesive is obtained by adding water 600 parts, two-component ceramic tile back adhesive emulsion 400 parts, cement 500 parts, defoaming agent 0.6 parts, bactericide 3 parts, 100 mesh sand 150 parts, 60 mesh sand 350 parts, cellulose 2 parts into the container, and then stirring uniformly. Specific embodiment 2

[0031] A. Preparation of core layer pre-emulsion: 160 parts of water, 3 parts of reactive anionic emulsifier, 30 parts of styrene, 300 parts of n-butyl acrylate, 100 parts of isooctyl acrylate, 5 parts of β-carboxyethyl acrylate, 12 parts of hydroxyethyl methacrylate, and 3.5 parts of acetoacetoxy methacrylate are added into the reaction kettle a, and then stirred uniformly to obtain the core layer pre-emulsion;

[0032] B. Preparation of shell layer pre-emulsion: 20 parts of water, 0.5 parts of reactive nonionic emulsifier, 3 parts of styrene, 5 parts of isooctyl acrylate, 3 parts of n-butyl acrylate, 2 parts of acrylamide, 2 parts of β-carboxyethyl acrylate, and 2 parts of hydroxyethyl methacrylate are added into the reaction kettle b, and then stirred uniformly to obtain the shell layer pre-emulsion;

[0033] C. Preparation of initiator: the initiator includes seed initiator, core layer initiator and shell layer initiator, wherein seed initiator: 0.2 parts of initiator is dissolved in 12 parts of water; core layer initiator: 0.3 parts of initiator is dissolved in 26 parts of water; shell layer initiator: 0.1 parts of initiator is dissolved in 4 parts of water;

[0034] D. Preparation of the emulsion: add 200 parts of water, 1 part of reactive anionic emulsifier to the reaction kettle c, stir and heat to 80°C, first add 2.5% of the core layer pre-emulsion, then add the seed initiator and keep for 20 min, then add the remaining core layer pre-emulsion and core layer initiator, after the dropwise addition is completed, keep for 30 min, then add the shell layer pre-emulsion and shell layer initiator, after the dropwise addition is completed, keep for 45 min, after the end of the incubation, cool to 35°C and adjust the pH to 7 with ammonia, add 3 parts of curing agent, 0.4 parts of defoaming agent and 1.8 parts of bactericide, filter to obtain a two-component ceramic tile back adhesive emulsion.

[0035] E. Add 500 parts of water, 350 parts of two-component ceramic tile back adhesive emulsion, 450 parts of cement, 0.5 parts of defoaming agent, 2 parts of bactericide, 120 parts of 80 mesh sand, 280 parts of 40 mesh sand, and 2 parts of cellulose to the container, then stir uniformly to obtain a two-component ceramic tile back adhesive. Specific embodiment 3

[0037] A. Preparation of the core layer pre-emulsion, add 200 parts of water, 8 parts of reactive anionic emulsifier, 100 parts of styrene, 400 parts of n-butyl acrylate, 200 parts of isooctyl acrylate, 8 parts of β-carboxyethyl acrylate, 17 parts of hydroxyethyl methacrylate, and 6 parts of acetoacetoxy methacrylate to the reaction kettle a, then stir uniformly to obtain the core layer pre-emulsion;

[0038] B. Preparation of the shell layer pre-emulsion, add 60 parts of water, 2 parts of reactive nonionic emulsifier, 10 parts of styrene, 15 parts of isooctyl acrylate, 10 parts of n-butyl acrylate, 4 parts of acrylamide, 3 parts of β-carboxyethyl acrylate, and 3 parts of hydroxyethyl methacrylate to the reaction kettle b, then stir uniformly to obtain the shell layer pre-emulsion;

[0039] C. Preparation of the initiator: the initiator includes seed initiator, core layer initiator and shell layer initiator, wherein the seed initiator: 0.8 parts of initiator is dissolved in 18 parts of water; the core layer initiator: 1 part of initiator is dissolved in 32 parts of water; the shell layer initiator: 0.2 parts of initiator is dissolved in 7 parts of water;

[0040] D. Preparation of the emulsion: add 220 parts of water, 3 parts of reactive anionic emulsifier to the reaction kettle c, stir and heat to 85°C, first add 5% of the core layer pre-emulsion, then add the seed initiator and keep for 30 min, then add the remaining core layer pre-emulsion and core layer initiator, after the dropwise addition is completed, keep for 40 min, then add the shell layer pre-emulsion and shell layer initiator, after the dropwise addition is completed, keep for 75 min, after the end of the incubation, cool to 38°C and adjust the pH to 8 with ammonia, add 6 parts of curing agent, 0.8 parts of defoaming agent and 2.5 parts of bactericide, filter to obtain a two-component ceramic tile back adhesive emulsion.

[0041] E. Add water 700 parts, two-component ceramic tile back adhesive emulsion 450 parts, cement 600 parts, defoaming agent 3 parts, bactericide 5 parts, 120 mesh sand 180 parts, 80 mesh sand 380 parts, cellulose 3 parts into the container, then stir uniformly to obtain two-component ceramic tile back adhesive.

[0042] Comparative Example 1,

[0043] The difference between Comparative Example 1 and Example 1 is only that the core-shell structure is not used in Comparative Example 1;

[0044] A. Preparation of pre-emulsion: add water 220 parts, reactive anionic emulsifier 6 parts, styrene 55 parts, n-butyl acrylate 360 parts, n-butyl acrylate 8 parts, isooctyl acrylate 150 parts, β-carboxyethyl acrylate 8.4 parts, acrylamide 3 parts, hydroxyethyl methacrylate 17.4 parts, acetoacetoxy methacrylate 5 parts into the reaction kettle, then stir uniformly to obtain the pre-emulsion;

[0045] B. Preparation of initiator: the initiator includes seed initiator, and the seed initiator is prepared by dissolving 0.5 parts of initiator in 15 parts of water;

[0046] C. Preparation of emulsion: add water 210 parts, reactive anionic emulsifier 2 parts into the reaction kettle c, stir and heat to 83℃, first add 3.5% of the pre-emulsion, then add the seed initiator and keep for 25 min, then add the remaining pre-emulsion dropwise, keep for 35 min after the dropwise addition is completed, then cool to 38℃ and adjust the pH to 7.5 by using ammonia water, add curing agent 5 parts, defoaming agent 0.6 parts and bactericide 2 parts, filter to obtain two-component ceramic tile back adhesive emulsion.

[0047] D. Add water 600 parts, two-component ceramic tile back adhesive emulsion 400 parts, cement 500 parts, defoaming agent 0.6 parts, bactericide 3 parts, 100 mesh sand 150 parts, 60 mesh sand 350 parts, cellulose 2 parts into the container, then stir uniformly to obtain two-component ceramic tile back adhesive.

[0048] II. Performance test

[0049] The two-component ceramic tile back adhesive prepared in the above examples and comparative examples is tested according to the standard JC / T547-2017 ceramic tile adhesive, and the test results are shown in Table 1.

[0050] Table 1

[0051]

[0052] From Table 1, the two-component ceramic tile back adhesive prepared in the embodiment has a bonding strength ≥1.30 MPa, a bonding strength after immersion ≥1.24 MPa, a bonding strength after heat aging ≥1.48 MPa, and a bonding strength after freeze-thaw cycles ≥1.18 MPa.

[0053] As can be seen from the comparison between Example 1 and Comparative Example 1, the emulsion used in the application adopts a core-shell structure, the acetylacetic acid group of the ethyl methacrylate in the polymer core layer is located in the core layer, and the particle deformation is completed before crosslinking, the polymer chains in the particle diffuse and penetrate, and the crosslinking reaction can be started when the diffusion reaches a certain depth in the adjacent particles, the compactness of the polymer colloid film is improved, good initial adhesion is provided for the coating film, the polar monomer of hydroxyethyl methacrylate is introduced into the core and shell layers respectively in the polymerization process, the stability of the emulsion particles is improved, the crosslinking degree of the emulsion particles is improved, the hydrophobicity is improved, the adhesion strength can also be improved due to the polarity, the reactive non-ionic emulsifier and the hydrophilic monomer are also introduced into the shell layer, the thickness of the particle hydration layer is improved, the stability of the emulsion particles is improved, and the compatibility with the powder is improved.

Claims

1. A two-component tile back latex emulsion characterized in that, Components including the following weight parts: styrene 33-110 parts, n-butyl acrylate 303-410 parts, iso-octyl acrylate 105-215 parts, beta-carboxyethyl acrylate 7-11 parts, hydroxyethyl methacrylate 14-20 parts, acrylamide 2.4-4 parts, acetoacetoxy ethyl methacrylate 3.5-6 parts, defoaming agent 0.4-0.8 parts, bactericide 1.8-2.5 parts, initiator 0.6-2 parts, emulsifier 4.5-13 parts, including reactive anionic emulsifier 4-11 parts and reactive nonionic emulsifier 0.5-2 parts, curing agent 3-6 parts; A preparation method of a two-component ceramic tile back adhesive emulsion, comprising the following steps: A, preparation of core layer pre-emulsion, adding water 160-200 parts, reactive anionic emulsifier 3-8 parts, styrene 30-100 parts, n-butyl acrylate 300-400 parts, iso-octyl acrylate 100-200 parts, beta-carboxyethyl acrylate 5-8 parts, hydroxyethyl methacrylate 12-17 parts, acetoacetoxy ethyl methacrylate 3.5-6 parts into container a, then stirring uniformly to obtain core layer pre-emulsion; B, preparation of shell layer pre-emulsion, adding water 20-60 parts, reactive nonionic emulsifier 0.5-2 parts, styrene 3-10 parts, iso-octyl acrylate 5-15 parts, n-butyl acrylate 3-10 parts, acrylamide 2.4-4 parts, beta-carboxyethyl acrylate 2-3 parts, hydroxyethyl methacrylate 2-3 parts into container b, then stirring uniformly to obtain shell layer pre-emulsion; C, preparation of initiator: the initiator includes seed initiator, core layer initiator and shell layer initiator, wherein the seed initiator: 0.2-0.8 parts of initiator is dissolved in 12-18 parts of water; the core layer initiator: 0.3-1 parts of initiator is dissolved in 26-32 parts of water; the shell layer initiator: 0.1-0.2 parts of initiator is dissolved in 4-7 parts of water; D, preparation of emulsion: adding water 200-220 parts, reactive anionic emulsifier 1-3 parts into container c, stirring and heating to 80-85℃, first adding 2.5%-5% of core layer pre-emulsion, then adding seed initiator and keeping warm for 20-30min, then adding the remaining core layer pre-emulsion and core layer initiator dropwise, keeping warm for 30-40min after dropwise addition is completed, then adding shell layer pre-emulsion and shell layer initiator dropwise, keeping warm for 45-75min after dropwise addition is completed, adjusting pH to 7-8 after keeping warm is completed, adding curing agent 3-6 parts, adding defoaming agent 0.4-0.8 parts and bactericide 1.8-2.5 parts, filtering to obtain two-component ceramic tile back adhesive emulsion.

2. A two-component tile back latex emulsion according to claim 1, characterized in that, The pH is adjusted to 7-8 after keeping warm is completed, which needs to reduce the temperature to below 40℃ first.

3. A two-component tile back adhesive prepared from the two-component tile back adhesive emulsion according to claim 1, characterized in that, Components including the following weight parts: water 500-700 parts, two-component ceramic tile back adhesive emulsion 350-450 parts, cement 450-600 parts, defoaming agent 0.5-3 parts, bactericide 2-5 parts, sand 400-560 parts, cellulose 1-3 parts.

4. A two-component tile back adhesive according to claim 3, characterised in that, The sand includes 80-120 mesh sand 120-180 parts and 40-80 mesh sand 280-380 parts.

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