Single-component paste-like back adhesive for floor heating and preparation method thereof

Abstract

This invention belongs to the field of adhesive technology. This invention provides a single-component paste-like adhesive for underfloor heating and its preparation method. The single-component paste-like adhesive for underfloor heating comprises the following components by mass percentage: 73.5-76% pure acrylic emulsion, 0.24-0.27% wetting and dispersing agent, 10-12% granulated blast furnace slag powder, 0.26-0.35% preservative, 1.2-1.5% thickener, 9-11% water, and 2.4-2.8% aluminum sulfate-polyacrylamide; wherein the aluminum sulfate-polyacrylamide is prepared by mixing aluminum sulfate and polyacrylamide at a mass ratio of 1:3. This invention further improves the tensile bond strength of the prepared adhesive by further increasing the amount of wetting and dispersing agent.

Description

Technical Field

[0001] This invention belongs to the field of adhesive technology, and in particular relates to a single-component paste-like adhesive for underfloor heating and its preparation method. Background Technology

[0002] Single-component tile adhesive is mainly made of high-molecular polymer emulsion, supplemented with high-performance additives such as defoamers, wetting and dispersing agents, and mildew inhibitors. When using it, apply it to the substrate or the back of the tile. Depending on the product characteristics, after drying or immediately, use the matching adhesive mortar / tile adhesive to stick the tile. It can effectively solve problems such as hollowing and falling off.

[0003] In existing technologies, wetting and dispersing agents can promote the deagglomeration of agglomerated particles. As the dosage / addition amount of wetting and dispersing agent increases, the fluidity of the adhesive improves, thereby increasing defoaming efficiency and reducing microbubbles in the coating film. This is beneficial for improving the uniformity and density of the coating film, and consequently, for improving the bonding strength.

[0004] However, when the amount of wetting and dispersing agent is increased to a certain level, the wetting ability reaches its maximum within the range, and the bond strength reaches its upper limit. Further increasing the amount of wetting and dispersing agent cannot further improve the bond strength. Summary of the Invention

[0005] To address the aforementioned problems, this invention proposes a single-component paste-like adhesive for underfloor heating and its preparation method. By further increasing the amount of wetting and dispersing agent, the tensile bond strength of the prepared adhesive is further improved.

[0006] To achieve the above objectives, in a first aspect, the present invention provides a single-component paste-like adhesive for underfloor heating, comprising, by mass percentage: 73.5-76% pure acrylic emulsion, 0.24-0.27% wetting and dispersing agent, 10-12% granulated blast furnace slag powder, 0.26-0.35% preservative, 1.2-1.5% thickener, 9-11% water, and 2.4-2.8% aluminum sulfate-polyacrylamide; wherein the aluminum sulfate-polyacrylamide is prepared by mixing aluminum sulfate and polyacrylamide in a mass ratio of 1:3.

[0007] Furthermore, the preparation method of the aluminum sulfate-polyacrylamide is as follows: aluminum sulfate and polyacrylamide are weighed according to the mass ratio and then mixed evenly by mechanical stirring to obtain the product.

[0008] Furthermore, the solid content of the pure acrylic emulsion (TX168 from Dongying Jinyoulai Industry and Trade Co., Ltd.) is 50%.

[0009] Furthermore, the granulated blast furnace slag powder (model SS600) has a specific surface area of ​​600 m². 2 / Kg.

[0010] Furthermore, the wetting and dispersing agent is Dow TRIRON@CF-10.

[0011] Furthermore, the preservative is Sol HF bactericide and fungicide.

[0012] Furthermore, the thickener is Dow RM-8W thickener.

[0013] Secondly, the present invention provides a method for preparing the above-mentioned single-component paste-like adhesive for underfloor heating, comprising the following steps:

[0014] S1. Mix and stir pure acrylic emulsion, water and preservative at room temperature to obtain a mixed water emulsion;

[0015] S2. Mix and stir the granulated blast furnace slag powder and the mixed water emulsion obtained in S1 to obtain the first mixture;

[0016] S3. Mix and stir the wetting and dispersing agent, aluminum sulfate-polyacrylamide and the initial mixture obtained in S2 to obtain the second mixture;

[0017] S4. Mix the thickener and the second mixture obtained in S3 to obtain the single-component paste-like adhesive for underfloor heating.

[0018] Furthermore, in S1, the stirring speed is 350-450 r / min, and the stirring time is 5-8 min;

[0019] In S2, the stirring speed is 450-550 r / min and the stirring time is 20-25 min;

[0020] In S3, the stirring speed is 550-650 r / min and the stirring time is 30-45 min;

[0021] In S4, the stirring speed is 550-650 r / min and the stirring time is 20-25 min.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] In the preparation of the single-component paste-like adhesive for underfloor heating in this invention, aluminum sulfate-polyacrylamide is added (i.e., polyacrylamide and aluminum sulfate are added simultaneously); aluminum sulfate releases low-valence metal ions (Al). 3+ The process involves reducing the zeta potential, disrupting the electrostatic repulsion balance, and triggering rapid flocculation. In this composite system, polyacrylamide can optimize the structure of the primary flocs that have already formed. Polyacrylamide, with its long chain structure, interpenetrates between the formed micro-flocs, dividing them into submicron-level uniform units. This weakens / counters macroscopic defects (the negative impact of introducing aluminum sulfate alone) while retaining appropriate thixotropy to facilitate leveling during construction.

[0024] The long-chain structure of polyacrylamide runs through the entire coating layer, forming a continuous submicron-scale network skeleton. This network not only restricts the free movement of particles, transforming the originally loose flocs into uniformly distributed reinforcing units, but also significantly improves the material's resistance to deformation by limiting the movement of molecular chain segments. Physical thickening and steric hindrance work together to regulate and thus synergistically improve the tensile bond strength of the resulting adhesive. Attached Figure Description

[0025] Figure 1 This is a comparative trend chart of the adhesive strength performance test data of the backing adhesives prepared in Examples 1-3 and Comparative Examples 1-5 of the present invention. Detailed Implementation

[0026] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0027] Unless otherwise specified, the raw materials used in the embodiments and comparative examples of this application are all commercially available.

[0028] Example 1: (a) Preparation of aluminum sulfate-polyacrylamide, the preparation method is as follows: aluminum sulfate and polyacrylamide are weighed at a mass ratio of 1:3 and mixed evenly by mechanical stirring to obtain aluminum sulfate-polyacrylamide. Aluminum sulfate (CAS No.: 10043-01-3) was purchased from Hubei Shiteng Chemical Technology Co., Ltd. Polyacrylamide (cationic type) was purchased from Hebei Huashuo Chemical Additives Co., Ltd.

[0029] (ii) Preparation of a single-component paste-like adhesive for underfloor heating, which, by mass percentage, includes the following components: 75.2% pure acrylic emulsion, 0.25% wetting and dispersing agent, 11% granulated blast furnace slag powder, 0.3% preservative, 1.3% thickener, 9.55% water, and 2.4% aluminum sulfate-polyacrylamide (equivalent to 0.6% aluminum sulfate and 1.8% polyacrylamide).

[0030] The preparation method of this single-component paste-like adhesive for underfloor heating includes the following steps:

[0031] S1. Mix and stir pure acrylic emulsion, water and preservative at room temperature for 7 minutes at a stirring speed of 400 r / min to obtain a mixed water emulsion.

[0032] S2. Mix the granulated blast furnace slag powder and the mixed water emulsion obtained in S1 at a stirring speed of 500 r / min for 23 min to obtain the first mixture.

[0033] S3. Mix and stir the wetting and dispersing agent, aluminum sulfate-polyacrylamide and the initial mixture obtained in S2 at a stirring speed of 600 r / min for 40 min to obtain the second mixture.

[0034] S4. Mix the thickener and the second mixture obtained in S3 at a stirring speed of 600 r / min for 23 min to obtain a single-component paste-like adhesive for underfloor heating.

[0035] The pure acrylic emulsion (TX168 from Dongying Jinyoulai Industry and Trade Co., Ltd.) has a solid content of 50%. The granulated blast furnace slag powder (model SS600) has a specific surface area of ​​600 m². 2 / kg. Wetting and dispersing agent: Dow TRIRON@CF-10. Preservative: Sol HF bactericide and fungicide. Thickener: Dow RM-8W thickener.

[0036] Example 2: The difference between this example and Example 1 is that: a single-component paste-like adhesive for underfloor heating is prepared, which, by mass percentage, includes the following components: 73.5% pure acrylic emulsion, 0.27% wetting and dispersing agent, 12% granulated blast furnace slag powder, 0.35% preservative, 1.5% thickener, 9.58% water, and 2.8% aluminum sulfate-polyacrylamide.

[0037] The preparation method of this single-component paste-like adhesive for underfloor heating includes the following steps:

[0038] S1. Mix and stir pure acrylic emulsion, water and preservative at room temperature at a stirring speed of 350 r / min for 8 min to obtain a mixed water emulsion.

[0039] S2. Mix the granulated blast furnace slag powder and the mixed water emulsion obtained in S1 at a stirring speed of 450 r / min for 25 min to obtain the first mixture.

[0040] S3. Mix and stir the wetting and dispersing agent, aluminum sulfate-polyacrylamide and the initial mixture obtained in S2 at a stirring speed of 550 r / min for 45 min to obtain the second mixture.

[0041] S4. Mix the thickener and the second mixture obtained in S3 at a stirring speed of 550 r / min for 25 min to obtain a single-component paste-like adhesive for underfloor heating.

[0042] Example 3: The difference between this example and Example 1 is that: a single-component paste-like adhesive for underfloor heating is prepared, which, by mass percentage, includes the following components: 76% pure acrylic emulsion, 0.24% wetting and dispersing agent, 10% granulated blast furnace slag powder, 0.26% preservative, 1.2% thickener, 9.8% water, and 2.5% aluminum sulfate-polyacrylamide.

[0043] The preparation method of this single-component paste-like adhesive for underfloor heating includes the following steps:

[0044] S1. Mix and stir pure acrylic emulsion, water and preservative at room temperature for 5 minutes at a stirring speed of 450 r / min to obtain a mixed water emulsion.

[0045] S2. Mix the granulated blast furnace slag powder and the mixed water emulsion obtained in S1 at a stirring speed of 550 r / min for 20 min to obtain the first mixture.

[0046] S3. Mix and stir the wetting and dispersing agent, aluminum sulfate-polyacrylamide and the initial mixture obtained in S2 at a stirring speed of 650 r / min for 30 min to obtain the second mixture.

[0047] S4. Mix the thickener and the second mixture obtained in S3 at a stirring speed of 650 r / min for 20 min to obtain a single-component paste-like adhesive for underfloor heating.

[0048] Comparative Example 1: The difference between this comparative example and Example 1 is that in the preparation of the single-component paste-like adhesive for underfloor heating, aluminum sulfate-polyacrylamide is not added (i.e., aluminum sulfate-polyacrylamide is replaced with granulated blast furnace slag powder), and the amount (mass percentage) of wetting and dispersing agent is 0.2%.

[0049] Specifically, a single-component paste-like adhesive for underfloor heating is prepared, comprising the following components by mass percentage: 75.2% pure acrylic emulsion, 0.2% wetting and dispersing agent, 13.45% granulated blast furnace slag powder, 0.3% preservative, 1.3% thickener, and 9.55% water.

[0050] Comparative Example 2: The difference between this comparative example and Example 1 is that aluminum sulfate-polyacrylamide is not added in the preparation of the single-component paste-like adhesive for underfloor heating (i.e., aluminum sulfate-polyacrylamide is replaced with granulated blast furnace slag powder).

[0051] Specifically, a single-component paste-like adhesive for underfloor heating is prepared, comprising the following components by mass percentage: 75.2% pure acrylic emulsion, 0.25% wetting and dispersing agent, 13.4% granulated blast furnace slag powder, 0.3% preservative, 1.3% thickener, and 9.55% water.

[0052] Comparative Example 3: The difference between this comparative example and Example 1 is that the amount (mass percentage) of wetting and dispersing agent used in the preparation of the single-component paste-like adhesive for underfloor heating is 0.2%.

[0053] Specifically, a single-component paste-like adhesive for underfloor heating is prepared, comprising the following components by mass percentage: 75.2% pure acrylic emulsion, 0.2% wetting and dispersing agent, 11.05% granulated blast furnace slag powder, 0.3% preservative, 1.3% thickener, 9.55% water, and 2.4% aluminum sulfate-polyacrylamide.

[0054] Comparative Example 4: The difference between this comparative example and Example 1 is that in the preparation of the single-component paste-like adhesive for underfloor heating, only aluminum sulfate is added, and no polyacrylamide is added (i.e., polyacrylamide is replaced with granulated blast furnace slag powder).

[0055] Specifically, a single-component paste-like adhesive for underfloor heating is prepared, comprising the following components by mass percentage: 75.2% pure acrylic emulsion, 0.25% wetting and dispersing agent, 12.8% granulated blast furnace slag powder, 0.3% preservative, 1.3% thickener, 9.55% water, and 0.6% aluminum sulfate.

[0056] Comparative Example 5: The difference between this comparative example and Example 1 is that in the preparation of the single-component paste-like adhesive for underfloor heating, only polyacrylamide is added, and aluminum sulfate is not added (i.e., aluminum sulfate is replaced by granulated blast furnace slag powder).

[0057] Specifically, a single-component paste-like adhesive for underfloor heating is prepared, comprising the following components by mass percentage: 75.2% pure acrylic emulsion, 0.25% wetting and dispersing agent, 11.6% granulated blast furnace slag powder, 0.3% preservative, 1.3% thickener, 9.55% water, and 1.8% polyacrylamide.

[0058] Comparative Example 6: The difference between this comparative example and Example 1 is that in the preparation of the single-component paste-like backing adhesive for underfloor heating, granulated blast furnace slag powder is replaced with quartz sand (70-120 mesh).

[0059] Specifically, a single-component paste-like adhesive for underfloor heating is prepared, comprising the following components by mass percentage: 75.2% pure acrylic emulsion, 0.25% wetting and dispersing agent, 11% quartz sand, 0.3% preservative, 1.3% thickener, 9.55% water, and 2.4% aluminum sulfate-polyacrylamide.

[0060] Experimental Example 1: The adhesive strength performance of the adhesives prepared in Examples 1-3 and Comparative Examples 1-5 was tested according to the standards T / CBMF93-2020 "Paste Adhesives for Ceramic Tiles" and JC / T547-2017 "Adhesives for Ceramic Tiles". The test results are shown in Table 1.

[0061] Table 1. Experimental data for Example 1

[0062]

[0063] Results Analysis: Combining the data in Table 1 and... Figure 1Analysis of Examples 1-3 shows that the adhesive strength performance test data of the backing adhesive prepared by the present invention (Examples 1-3) reaches above 1.72 MPa; among them, Example 1 is the best, reaching 1.75 MPa.

[0064] Combining the data in Table 1 and Figure 1 Analysis of Example 1 and Comparative Examples 1-5, specifically comparing Comparative Examples 1 and 2, revealed that increasing the amount / mass fraction of the lubricating dispersant from 0.2% (Comparative Example 1) to 0.25% (Comparative Example 2) did not significantly change the adhesive strength performance test data of the resulting adhesive. This is mainly because when the amount / mass fraction of the wetting and dispersing agent is 0.2%, the wetting ability has reached its maximum, and the wetting surface area of ​​the emulsion no longer increases with the increase of the amount of wetting and dispersing agent. Therefore, further increasing the amount of wetting and dispersing agent at this point cannot further improve the adhesive strength; that is, the adhesive strength of the resulting adhesive reaches its maximum when the amount / mass fraction of the wetting and dispersing agent is 0.2%.

[0065] Specifically, by comparing Comparative Example 1 and Comparative Example 3, it can be seen that, compared with Comparative Example 1, the addition of aluminum sulfate-polyacrylamide in Comparative Example 3 resulted in an increase in the adhesive strength performance test data of the prepared backing adhesive from 1.58 MPa (Comparative Example 1) to 1.67 MPa (Comparative Example 3).

[0066] Specifically, comparing Comparative Examples 2 and 4, it can be seen that, compared to Comparative Example 2, the addition of aluminum sulfate alone in Comparative Example 4 resulted in a decrease in the adhesive strength performance test data of the prepared adhesive from 1.58 MPa (Comparative Example 2) to 1.55 MPa (Comparative Example 4). This indicates that adding aluminum sulfate alone actually leads to a decrease in the adhesive strength performance test data of the prepared adhesive. This is mainly because, when aluminum sulfate is added alone, low-valence metal ions (Al... 3+ This causes a decrease in zeta potential, disrupts the electrostatic repulsion balance, and triggers rapid flocculation. The resulting macroscopic flocs contain a large number of air bubbles and have an uneven particle size distribution, which weakens the density of the coating and the effective contact area, thus leading to a decrease in adhesion strength.

[0067] Specifically, by comparing Comparative Example 2 and Comparative Example 5, it can be seen that, compared with Comparative Example 2, the addition of polyacrylamide in Comparative Example 5 resulted in an increase in the adhesive strength performance test data of the backing adhesive from 1.58 MPa (Comparative Example 2) to 1.7 MPa (Comparative Example 5).

[0068] Comparing with Example 1, it can be seen that the addition of aluminum sulfate-polyacrylamide (i.e., the simultaneous addition of aluminum sulfate and polyacrylamide) produces a synergistic effect, jointly improving the tensile bond strength of the resulting adhesive. Furthermore, it can be seen that under the condition of adding aluminum sulfate-polyacrylamide (i.e., the simultaneous addition of aluminum sulfate and polyacrylamide), the adhesive strength of the resulting adhesive reaches its maximum when the dosage / mass fraction of the wetting and dispersing agent is 0.25%.

[0069] Experimental Example 2: The adhesives prepared in Example 1 and Comparative Example 6 were subjected to weather resistance (heat aging) environmental tests. The specific heat aging conditions were 70℃ × 72h, and the relative strength growth rate (%) was calculated. The results are as follows:

[0070] Relative strength growth rate = (bond strength of Example 1 - bond strength of Comparative Example 6) / bond strength of Comparative Example 6 × 100% = 30.4%.

[0071] It can be seen that, compared with the quartz sand in Comparative Example 6, replacing it with granulated blast furnace slag powder in Example 1 resulted in a 30.4% increase in the tensile bond strength of the adhesive under heat aging (70℃×72h) conditions.

[0072] Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A one-component paste type back adhesive for a floor heating, characterized by comprising: By mass percentage, it comprises the following components: pure acrylic emulsion 73.5-76%, wetting dispersant 0.24-0.27%, granulated blast furnace slag powder 10-12%, preservative 0.26-0.35%, thickening agent 1.2-1.5%, water 9-11% and aluminum sulfate-polyacrylamide 2.4-2.8%; wherein, the aluminum sulfate-polyacrylamide is prepared by mixing aluminum sulfate and polyacrylamide in a mass ratio of 1:3; the wetting dispersant is DOW TRIRON CF-10 of Dow.

2. The one-component paste type back adhesive for a floor heating mat according to claim 1, characterized in that, The preparation method of the aluminum sulfate-polyacrylamide is as follows: aluminum sulfate and polyacrylamide are weighed in a mass ratio, then mixed uniformly by mechanical stirring, and the aluminum sulfate-polyacrylamide is obtained.

3. The one-component paste type back adhesive for a floor heating mat according to claim 1, characterized in that, The solid content of the pure acrylic emulsion is 50%.

4. The one-component paste type back adhesive for a floor heating mat according to claim 1, wherein The granulated blast furnace slag powder has a specific surface area of 600 m 2 / Kg.

5. The one-component paste type back adhesive for a floor heating mat according to claim 1, wherein The preservative is Sol HF fungicide.

6. The one-component paste type back adhesive for a floor heating mat according to claim 1, wherein The thickening agent is RM-8W thickening agent of Dow.

7. A method of preparing a one-component paste type back adhesive for a floor heating mat according to any one of claims 1 to 6, characterized in that, It comprises the following steps: S1, mix pure acrylic emulsion, water and preservative at room temperature to obtain a mixed water emulsion; S2, mix granulated blast furnace slag powder and the mixed water emulsion obtained in S1 to obtain a first mixture; S3, mix wetting dispersant, aluminum sulfate-polyacrylamide and the first mixture obtained in S2 to obtain a second mixture; S4, mix thickening agent and the second mixture obtained in S3 to obtain the single-component paste back adhesive for floor heating.

8. The preparation method of the one-component paste type back adhesive for a floor heating according to claim 7, characterized in that, In S1, the stirring speed is 350-450 r / min, and the stirring time is 5-8 min; In S2, the stirring speed is 450-550 r / min, and the stirring time is 20-25 min; In S3, the stirring speed is 550-650 r / min, and the stirring time is 30-45 min; In S4, the stirring speed is 550-650 r / min, and the stirring time is 20-25 min.

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