High-performance ceramic tile adhesive and preparation method thereof

Abstract

The invention provides a high-performance ceramic tile adhesive and a preparation method thereof, belongs to the technical field of building materials, and aims to solve the problem that the traditional ceramic tile adhesive cannot systematically meet the comprehensive requirements of the high-performance ceramic tile adhesive on airing time, sagging resistance, strength and workability in construction all day, and the high-performance ceramic tile adhesive comprises HPMC, multi-element starch ether, an anti-sagging agent and a dispersing agent, the multi-element starch ether, the anti-sagging agent and the high and low temperature stable dispersing agent are synergistically compounded, so that the synergistic enhancement of various properties is realized.

Description

Technical Field

[0001] This invention belongs to the field of building materials technology, and more specifically, relates to a high-performance tile adhesive and its preparation method. Background Technology

[0002] Tile adhesive, as an important building decoration material binder, directly affects construction efficiency, project quality, and long-term durability. Hydroxypropyl methylcellulose (HPMC) is an indispensable key additive in tile adhesive, mainly playing a role in water retention, thickening, and improving workability. With the continuous improvement of material performance requirements in the construction industry, especially in complex climatic conditions and harsh construction environments, the market demand for high-performance tile adhesives is growing.

[0003] Conventional HPMC has a low gel temperature. In cement-based tile adhesive systems, especially under high summer temperatures or low winter temperatures, its viscosity loss is significant, and its water retention decreases sharply, leading to incomplete cement hydration. This severely affects the bond strength and freeze-thaw resistance of the tile adhesive, failing to meet the stability requirements of high-grade tile adhesives such as C2TE in all-weather construction. To improve certain properties of HPMC, it is often modified by physically blending with other additives (such as single starch ether). However, this method often results in an imbalance of various properties in the modified HPMC product, generally exhibiting problems such as insufficient strength development, substandard water retention, poor anti-slip effect, rough application feel, and poor batch-to-batch stability. It cannot systematically meet the comprehensive requirements of high-performance tile adhesives for setting time, anti-sagging properties, strength, and workability.

[0004] Therefore, in view of this, we will study and improve the existing structure and its shortcomings, and provide a high-performance tile adhesive and its preparation method, in order to achieve a more practical value. Summary of the Invention

[0005] To address the aforementioned technical problems, this invention provides a high-performance tile adhesive and its preparation method.

[0006] The purpose and effects of this invention, which describes a high-performance tile adhesive and its preparation method, are achieved through the following specific technical means:

[0007] The specific preparation process of a high-performance tile adhesive is as follows: S1. Raw material preparation and feeding: The reactants are cellulose, liquid alkali, chloromethane, and propylene oxide, with a molar ratio of 1:2.32:2.09:0.46.

[0008] S2. Special etherification process: In a closed reactor, the temperature is gradually increased to the etherification reaction temperature of 60-100℃. The etherification reaction is carried out at this temperature for 120-250 min. The pressure is maintained at 1.0-2.5 MPa during the reaction to prepare low hydroxypropoxy cellulose ether slurry.

[0009] S3. Special washing and granulation treatment: The crude product after etherification is added to a centrifugal washing device, and salt is removed by using hot water at 80-95℃ and high-speed centrifugal washing. Subsequently, the density is improved by using -10℃~0℃ chilled water to make the product reach a suitable bulk density.

[0010] S4. Drying and pulverizing: The intermediate product after granulation is dried in an airflow drying tower at 100-120℃. The dried product is then sieved through an 80-120 mesh sieve to obtain high gel temperature and low ash hydroxypropyl methylcellulose.

[0011] S5: Physical Mixing: The high-performance HPMC pure product prepared above is physically dry-mixed with poly-starch ether, anti-sagging agent, and high and low temperature stabilizing dispersant in a specific ratio of 1:(0.1~0.2):(0.02~0.04):(0.01:0.04). Using an airflow mixing device, at room temperature and pressure, the HPMC pure product and each additive are added to the mixer. The mixing speed and time are controlled, and the mixture is mixed three times. The pressure of the first mixing is 1.0~1.3 MPa, with an interval of 3 minutes. The pressure of the last two mixings is greater than 1.0 MPa to ensure thorough and uniform physical mixing.

[0012] The aforementioned multi-component starch ether includes one or more of mono-component starch ether, di-component starch ether, and ternary starch ether; the aforementioned anti-sagging agent includes one or more of polyacrylamide, sodium polyacrylate, polyethylene oxide, and polyethylene glycol; and the high and low temperature stabilizing dispersant includes one or more of sodium gluconate, sodium tripolyphosphate, and sodium pyrophosphate.

[0013] Compared with the prior art, the present invention has the following beneficial effects:

[0014] 1. By adjusting the content of methoxy and hydroxypropoxy groups in HPMC through a "special etherification reaction process," the gel temperature of HPMC is essentially increased. This allows the modified HPMC to maintain stable water retention and consistency over a wide temperature range of 0℃ to 50℃, effectively solving the problem of performance fluctuations of traditional HPMC under extreme weather conditions and ensuring the construction quality of tile adhesive in both winter and summer.

[0015] 2. By "synergistically compounding" multi-element starch ethers, anti-sagging agents, and high and low temperature stabilizing dispersants, the synergistic enhancement of various properties is achieved.

[0016] 3. The adopted "dry blending process" is mature, reliable, and easy to industrialize. Combined with the "special granulation and washing process" for pure HPMC, the ash content of the product is effectively reduced, and the uniformity of fineness and bulk density is improved, ensuring the high consistency and reliability of the final modified HPMC product performance from the raw material end. Detailed Implementation

[0017] The embodiments of the present invention will be described in further detail below with reference to examples. These examples are for illustrative purposes only and should not be construed as limiting the scope of the invention.

[0018] In the description of this invention, unless otherwise stated, "a plurality of" means two or more; the terms "upper," "lower," "left," "right," "inner," "outer," "front end," "rear end," "head," "tail," etc., indicate orientations or positional relationships based on the shown orientations or positional relationships, and are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this invention. Furthermore, the terms "first," "second," "third," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0019] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "connected" and "linked" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0020] Example 1:

[0021] This invention provides a high-performance tile adhesive, the core of which lies in optimizing the structure of HPMC raw materials and synergistically compounding various functional additives to obtain a modified HPMC product with excellent comprehensive performance through dry mixing. Specific steps include: adding high-concentration liquid alkali, propylene oxide, and chloromethane to cellulose; reacting under vacuum for a period of time; adding an etherifying agent for special etherification treatment; and completing the etherification reaction. Finally, after washing, granulation, drying, and pulverizing, multi-functional starch ether, anti-sagging agent, and high- and low-temperature stabilizing dispersant are added and mixed to obtain the modified HPMC for high-performance tile adhesive.

[0022] The tile adhesive comprises hydroxypropyl methylcellulose (HPMC), polysaccharide starch ether, anti-sagging agent, and dispersant, in a mass ratio of 1:(0.1~0.2):(0.02~0.04):(0.01:0.04).

[0023] Hydroxypropyl methylcellulose comprises cellulose, caustic soda, chloromethane, and propylene oxide in a molar ratio of 1:2.32:2.09:0.46.

[0024] The aforementioned multi-component starch ether includes one or more of mono-component starch ether, di-component starch ether, and ternary starch ether; the aforementioned anti-sagging agent includes one or more of polyacrylamide, sodium polyacrylate, polyethylene oxide, and polyethylene glycol; and the high and low temperature stabilizing dispersant includes one or more of sodium gluconate, sodium tripolyphosphate, and sodium pyrophosphate.

[0025] The specific preparation process of this high-performance tile adhesive using modified HPMC is as follows:

[0026] S1. Raw material preparation and feeding: The reactants are cellulose, liquid alkali, chloromethane, and propylene oxide, with a molar ratio of 1:2.32:2.09:0.46.

[0027] S2. Special etherification process: In a closed reactor, the temperature is gradually increased to the etherification reaction temperature of 60-100℃. The etherification reaction is carried out at this temperature for 120-250 min. The pressure is maintained at 1.0-2.5 MPa during the reaction to prepare low hydroxypropoxy cellulose ether slurry.

[0028] S3. Special washing and granulation treatment: The crude product after etherification is added to a centrifugal washing device, and salt is removed by using hot water at 80-95℃ and high-speed centrifugal washing. Subsequently, the density is improved by using -10℃~0℃ chilled water to make the product reach a suitable bulk density.

[0029] S4. Drying and Pulverizing: The intermediate product after granulation is dried in an airflow drying tower at 100-120℃. The dried product is then sieved through an 80-120 mesh sieve to obtain high gel temperature and low ash hydroxypropyl methylcellulose. After preparation, gel temperature, fineness, and bulk density are tested according to JCT 2190-2024 standard. See Table 1.

[0030] Table 1

[0031] Test Project Standard requirements Test value Loss on drying ≤6.0% 3.5% gel temperature 70~90℃ 75.1℃ Fineness ≤3.0% 0.5% Bulk density / <![CDATA[325kg / cm 3 ]]>

[0032] Next, 1 kg of pure hydroxypropyl methylcellulose, 0.1 kg of ternary starch ether, 0.02 kg of anti-sagging agent (polyacrylamide and sodium polyacrylate mixed in a 3:1 ratio), and 0.01 kg of sodium tripolyphosphate were simultaneously placed in an air-jet mixer and mixed thoroughly. The mixture was then discharged. Water retention rate and final setting time difference were measured according to JCT 2190-2024 standard, and anti-slip and strength tests were performed according to JC / T 547-2017 standard. See Tables 2 and 3.

[0033] The formula for water retention rate and final setting time difference is: 250g cement and 750g standard sand.

[0034] The formula for anti-slip and strength testing is: 380g cement, 640.5g graded sand, 40g adhesive powder, 3.5g HPMC, and 3.0g calcium formate.

[0035] Table 2

[0036] Test Project Standard requirements Test value Water retention rate ≥80% 93.2% Final setting time difference ≤360min 200min

[0037] Table 3

[0038] Test Project Standard requirements Test value Anti-slip ≤0.5mm 0.53mm Tensile bond strength ≥1.0MPa 1.64 Tensile bond strength after immersion in water ≥1.0MPa 1.11 Heat aging tensile bond strength ≥1.0MPa 1.22 Tensile bond strength after 30 minutes of drying ≥0.5MPa 0.45

[0039] Example 2:

[0040] The difference between this embodiment and Example 1 is that 1 kg of pure hydroxypropyl methylcellulose, 0.15 kg of ternary starch ether, 0.03 kg of anti-sagging agent (polyacrylamide and sodium polyacrylate mixed in a 3:1 ratio), and 0.02 kg of sodium tripolyphosphate were simultaneously placed in an air-jet mixer and mixed thoroughly before being discharged. The water retention rate and final setting time difference were measured according to JCT 2190-2024 standard, and the anti-slip and strength tests were performed according to JC / T 547-2017 standard. See Tables 4 and 5.

[0041] The formula for water retention rate and final setting time difference is: 250g cement and 750g standard sand.

[0042] The formula for anti-slip and strength testing is: 380g cement, 640.5g graded sand, 40g adhesive powder, 3.5g HPMC, and 3.0g calcium formate.

[0043] Table 4

[0044] Test Project Standard requirements Test value Water retention rate ≥80% 93.8% Final setting time difference ≤360min 224min

[0045] Table 5

[0046] Test Project Standard requirements Test value Anti-slip ≤0.5mm 0.41mm Tensile bond strength ≥1.0MPa 1.57 Tensile bond strength after immersion in water ≥1.0MPa 1.10 Heat aging tensile bond strength ≥1.0MPa 1.18 Tensile bond strength after 30 minutes of drying ≥0.5MPa 0.67

[0047] Example 3:

[0048] The difference between this embodiment and Example 1 is that 1 kg of pure hydroxypropyl methylcellulose, 0.20 kg of ternary starch ether, 0.04 kg of anti-sagging agent (polyacrylamide and sodium polyacrylate mixed in a 3:1 ratio), and 0.03 kg of sodium tripolyphosphate were simultaneously placed in an air-jet mixer and mixed thoroughly before being discharged. The water retention rate and final setting time difference were measured according to JCT 2190-2024 standard, and the anti-slip and strength tests were performed according to JC / T 547-2017 standard. See Tables 6 and 7.

[0049] The formula for water retention rate and final setting time difference is: 250g cement and 750g standard sand.

[0050] The formula for anti-slip and strength testing is: 380g cement, 640.5g graded sand, 40g adhesive powder, 3.5g HPMC, and 3.0g calcium formate.

[0051] Table 6

[0052] Test Project Standard requirements Test value Water retention rate ≥80% 94.3% Final setting time difference ≤360min 253min

[0053] Table 7

[0054] Test Project Standard requirements Test value Anti-slip ≤0.5mm 0.33mm Tensile bond strength ≥1.0MPa 1.55 Tensile bond strength after immersion in water ≥1.0MPa 1.12 Heat aging tensile bond strength ≥1.0MPa 1.15 Tensile bond strength after 30 minutes of drying ≥0.5MPa 0.68

[0055] Example 4:

[0056] The difference between this embodiment and Example 1 is that 1 kg of pure hydroxypropyl methylcellulose, 0.20 kg of ternary starch ether, 0.04 kg of anti-sagging agent (polyacrylamide and sodium polyacrylate mixed in a 3:1 ratio), and 0.03 kg of high and low temperature dispersant (sodium tripolyphosphate and pyrophosphate mixed in a 2:1 ratio) are simultaneously placed into an air-jet mixer and mixed thoroughly. After thorough mixing, the mixture is discharged. The water retention rate and final setting time difference are measured according to JCT 2190-2024 standard, and the anti-slip and strength tests are measured according to JC / T 547-2017 standard. See Tables 8 and 9.

[0057] The formula for water retention rate and final setting time difference is: 250g cement and 750g standard sand.

[0058] The formula for anti-slip and strength testing is: 380g cement, 640.5g graded sand, 40g adhesive powder, 3.5g HPMC, and 3.0g calcium formate.

[0059] Table 8

[0060] Test Project Standard requirements Test value Water retention rate ≥80% 93.5% Final setting time difference ≤360min 268min

[0061] Table 9

[0062] Test Project Standard requirements Test value Anti-slip ≤0.5mm 0.33mm Tensile bond strength ≥1.0MPa 1.43 Tensile bond strength after immersion in water ≥1.0MPa 1.03 Heat aging tensile bond strength ≥1.0MPa 1.10 Tensile bond strength after 30 minutes of drying ≥0.5MPa 0.75

[0063] Example 5:

[0064] The difference between this embodiment and Example 1 is that 1 kg of pure hydroxypropyl methylcellulose, 0.20 kg of ternary starch ether, 0.04 kg of anti-sagging agent (polyacrylamide and sodium polyacrylate mixed in a 3:1 ratio), and 0.04 kg of high and low temperature dispersant (sodium tripolyphosphate and pyrophosphate mixed in a 3:1 ratio) were simultaneously placed into an air-jet mixer and mixed thoroughly. After thorough mixing, the mixture was discharged. The water retention rate and final setting time difference were measured according to JCT 2190-2024 standard, and the anti-slip and strength tests were performed according to JC / T 547-2017 standard. See Tables 10 and 11.

[0065] The formula for water retention rate and final setting time difference is: 250g cement and 750g standard sand.

[0066] The formula for anti-slip and strength testing is: 380g cement, 640.5g graded sand, 40g adhesive powder, 3.5g HPMC, and 3.0g calcium formate.

[0067] Table 10

[0068] Test Project Standard requirements Test value Water retention rate ≥80% 92.7% Final setting time difference ≤360min 282min

[0069] Table 11

[0070] Test Project Standard requirements Test value Anti-slip ≤0.5mm 0.30mm Tensile bond strength ≥1.0MPa 1.48 Tensile bond strength after immersion in water ≥1.0MPa 1.10 Heat aging tensile bond strength ≥1.0MPa 1.21 Tensile bond strength after 30 minutes of drying ≥0.5MPa 0.70

[0071] Comparative Examples: The modified product of the present invention was compared with commercially available domestic and imported products. Tests were conducted using the anti-slip and strength test formulations described above, and the data are as follows:

[0072] Test Project Standard requirements Japan 6001PF Shandong HK002 Modified HPMC Anti-slip / mm ≤0.5mm 0.54 0.48 0.30 Tensile bond strength / MPa ≥1.0MPa 1.45 1.35 1.61 Tensile bond strength after immersion in water / MPa ≥1.0MPa 0.95 0.87 1.10 Heat-aged tensile bond strength / MPa ≥1.0MPa 1.11 1.03 1.21 Tensile bond strength after 30 minutes of drying / MPa ≥0.5MPa 0.5 0.45 0.70

[0073] By comparing Examples 1-5 with the comparative examples, the performance of the adhesive used for ceramic tiles is superior to that of traditional ceramic tile adhesive.

[0074] The embodiments of the present invention are given for illustrative and descriptive purposes only, and are not intended to be exhaustive or to limit the invention to the forms disclosed. Many modifications and variations will be apparent to those skilled in the art. The embodiments were chosen and described in order to better illustrate the principles and practical application of the invention, and to enable those skilled in the art to understand the invention and to design various embodiments with various modifications suitable for a particular purpose.

Claims

1. A high-performance tile adhesive, characterized in that: It includes HPMC, poly-starch ether, anti-sagging agent and dispersant, with a mass ratio of 1:(0.1~0.2):(0.02~0.04):(0.01:0.04). The HPMC comprises cellulose, liquid alkali, chloromethane, and propylene oxide in a molar ratio of 1:2.32:2.09:0.

46.

2. The high-performance tile adhesive as described in claim 1, characterized in that: The multi-component starch ether includes one or more of mono-component starch ether, di-component starch ether, and ternary starch ether.

3. The high-performance tile adhesive as described in claim 1, characterized in that: The anti-sagging agent includes one or more of polyacrylamide, sodium polyacrylate, polyethylene oxide, and polyethylene glycol.

4. The high-performance tile adhesive as described in claim 1, characterized in that: The dispersant includes one or more of sodium gluconate, sodium tripolyphosphate, and sodium pyrophosphate.

5. The method for preparing tile adhesive as described in claim 1, characterized in that: Includes the following steps: S1; Cellulose, liquid alkali, chloromethane, and propylene oxide are gradually heated in a reactor according to the above molar ratio to etherification reaction. The temperature is 60~100℃, the reaction time is 120-250min, and the pressure is maintained at 1.0-2.5MPa during the reaction to obtain medium and low viscosity hydroxypropoxy cellulose ether slurry. S2; The crude etherified product is added to a centrifugal washing device and hot water at 80-95℃ is used to remove salt under high-speed centrifugal washing. Subsequently, the density is improved by using -10~0℃ chilled water to make the product reach a suitable bulk density. S3; The intermediate product in step S2 is dried in an airflow drying tower at 100-120℃, and the dried product is sieved through an 80-120 mesh sieve to obtain high gel temperature, low ash hydroxypropyl methylcellulose; S4; Using an airflow mixing device, at room temperature and pressure, the hydroxypropyl methylcellulose obtained in step S3, along with poly-starch ether, anti-sagging agent, and high and low temperature stabilizing dispersant, are added to the mixer in a specific ratio. The mixing speed and time are controlled, and the mixture is mixed three times. The pressure for the first mixing is 1.0~1.3 MPa, with an interval of 3 minutes. The pressure for the next two mixing times is greater than 1.0 MPa, to achieve thorough and uniform physical mixing.