CN114409342B - Preparation method of ceramic tile glue - Google Patents
Preparation method of ceramic tile glue Download PDFInfo
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- CN114409342B CN114409342B CN202210134153.XA CN202210134153A CN114409342B CN 114409342 B CN114409342 B CN 114409342B CN 202210134153 A CN202210134153 A CN 202210134153A CN 114409342 B CN114409342 B CN 114409342B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/1018—Coating or impregnating with organic materials
- C04B20/1029—Macromolecular compounds
- C04B20/1037—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/12—Chemically modified polycondensates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0666—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0672—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00637—Uses not provided for elsewhere in C04B2111/00 as glue or binder for uniting building or structural materials
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- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Structural Engineering (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
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- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
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- Finishing Walls (AREA)
Abstract
The invention discloses a preparation method of a ceramic tile adhesive, which comprises the steps of preparing a ceramic tile side adhesive additive S1, preparing a cement-based ceramic tile side adhesive S2, preparing a wall side adhesive additive S3 and preparing a wall side adhesive S4; the ceramic tile adhesive with excellent performance parameters such as bonding strength, compression-fracture ratio, 28d shrinkage rate, 25 ℃ linear expansion coefficient and the like is obtained by respectively preparing the adhesive cement additive on the ceramic tile side and the wall side and the cement-based material matched with the corresponding additive and optimizing the proportion of the additive and the corresponding cement-based material.
Description
Technical Field
The invention relates to the field of ceramic tile glue, in particular to a preparation method of ceramic tile glue.
Background
The phenomena of hollowing and shedding of the ceramic tile after pasting construction are caused by the following four main reasons: (1) the reason for the tile itself is: the ceramic tile has the characteristics of high density and low water absorption, so that the ceramic tile has poor adhesion, and is difficult to be effectively adhered with adhesives such as ceramic tile glue and the like; (2) influence of tile glue: the ceramic tile adhesive has poor adhesion and is easy to generate larger deformation stress and shearing force, has higher requirements on the adhesive property of the ceramic tile adhesive, not only needs to ensure the adhesive strength, but also needs to have enough flexibility and deformation stress, and the adhesive properties such as the adhesive strength, the flexibility and the like of the traditional ceramic tile adhesive can not completely meet the requirements of the ceramic tile; (3) external environmental factors: the ceramic tile has different thermal expansion coefficients with the cement substrate and the ceramic tile glue, and when the external temperature changes, the whole bonding system can generate larger deformation stress and shearing force, thereby causing hollowing and falling-off phenomena; (4) influence of the construction process: the phenomena of hollowing, falling and the like can be caused by the factors such as the tile adhesive sticking thickness, the seam leaving treatment or the cleanness degree of the back surface of the tile.
The traditional ceramic tile adhesive improvement method is to improve the bonding performance and appearance of the ceramic tile adhesive to a certain extent by adding a small amount of additives into the ceramic tile adhesive, and in the ceramic tile bonding process, the ceramic tile is directly bonded through the film forming effect of the adhesive powder except the chemical effect of a cement hydration product. Can play a certain complementary role, and relieve the external impact and temperature change mainly by improving the rigidity of the cement. The added other materials such as cellulose ether generally play a role in retaining water and thickening the tile adhesive, the lignocellulose is used for increasing the yield stress of the tile adhesive, the calcium formate is used for improving the early strength of the tile adhesive, and the starch ether can improve the rheological property and the application property of the dry powder mortar.
However, the above additives account for about 1-2% of the mixed material, the main material of the material is cement-based composite material, and the added materials are mostly used for compensating shrinkage and the degree of coupling in the material, so that the adhesion principle of the material bonding and the control of the thermal expansion and cold contraction performance of the material cannot be fundamentally improved.
Therefore, the invention develops a novel tile adhesive based on a double-layer composite material technology, and is used for improving the bonding performance and the expansion and contraction performance of the tile adhesive.
Disclosure of Invention
The invention aims to provide a preparation method of a ceramic tile adhesive, which greatly improves the bonding property and the expansion and contraction properties of the ceramic tile adhesive.
A preparation method of a tile glue comprises the following steps:
: preparing the ceramic tile side adhesive glue additive,
adding 400g of deionized water 300-400g into a 1000ml beaker at room temperature, adding 5-12g of AEO-9 emulsifier, uniformly stirring, adding 6-8g of urea, 0.1-0.2g of ammonium nitrate, 0.1-0.2g of phenol and 0.5-2g of formic acid, slowly dropwise adding 1wt.% hydrochloric acid according to mass fraction to adjust the pH value of the solution to about 4, adding 0.5-1.2g of epoxy resin E-44 and 2-5g of ethyl acetate, and emulsifying for 25min at the rotation speed of rpm 1900; and transferring the emulsion formed in the step into a three-neck flask, slowly adding 5-9g of 37% formaldehyde, starting a water bath kettle, starting to heat to 60 ℃, maintaining the temperature for reaction for 1h, performing vacuum filtration on turbid liquid after the reaction is finished, washing with deionized water and absolute ethyl alcohol respectively to obtain a filter cake, putting the filter cake into a vacuum drying oven, and drying at 50 ℃ to constant weight to obtain solid particles, namely the microsphere particles.
: preparing cement-based tile side bonding glue,
preparing cement-based tile side bonding glue according to the following mixture ratio:
the weight portion ratio is as follows:
100-150g of ordinary portland cement, 5-32g of slag, 10-30g of quartz sand, 10-55g of water, 0.15-0.2g of PVA fiber, 3-5g of microsphere particles with the particle size of 150 mu m and 2-10g of tetraethylenepentamine;
firstly, pouring cement, slag, quartz sand, PVA fiber and water into a stirrer to be mixed for 1min, then adding tetraethylenepentamine and microsphere particles at a constant speed, and mixing the materials in the running state of the stirrer for later use;
: preparing the additive of the wall side adhesive glue,
weighing 100-150g of levulinic acid, preparing the levulinic acid aqueous solution by using 10g of KOH aqueous solution with the mass fraction of 10%, and then dissolving 3-5g of dopamine and 1-2g of potassium persulfate initiator by using 50g of distilled water to prepare an initiator aqueous solution; adding 4-6g of polyglycerol monostearate and 5-8g of cyclohexane into a four-mouth bottle provided with a thermometer, a condenser pipe, a stirring device and a nitrogen inlet pipe, introducing nitrogen to remove oxygen, heating and stirring the mixed solution, reacting at 95 ℃ for a period of time, supplementing 2-5g of ethylene glycol ethyl ether propionate after 5min to form core-shell structures with different cross-linking densities, cooling and discharging after the expected conversion rate is reached, and washing and drying to obtain spherical particles.
: preparing wall side adhesive, coating the wall side adhesive on the cement-based tile side adhesive, and uniformly mixing the wall side adhesive and the cement-based tile side adhesive;
weighing 40-100g of ordinary portland cement, 150-200g of I-grade fly ash, 20-50g of silica fume, 300-600g of quartz fine sand, 150-250g of water, 15-20g of spherical particles obtained in the step S3 and 15-20g of PVA fiber, and stirring for 5min on a stirrer with the rotating speed of 1500rpm to obtain a finished product; the obtained finished product is coated on the cement-based tile side adhesive, and the coating effect is better before the cement-based tile side adhesive is initially set.
Preferably, the weight part ratio of the urea to the epoxy resin E-44 is 10: 1.
preferably, the weight part ratio of the dopamine to the polyglycerol monostearate to the cyclohexane is 4: 4: 7.
for the ceramic tile side adhesive glue additive, the invention firstly uses the composite microsphere method technology, composite microspheres containing a repairing agent are put into a base material, the material generates cracks under the action of external force, the cracks are expanded to crack partial composite microspheres, the bonding component containing the repairing agent is dispersed in the base material, and the repairing agent generates chemical reaction under the action of a catalyst in the base body to realize automatic healing reaction. After the repairing agent is successfully coated and the composite microspheres with self-repairing capability are prepared, the composite microspheres are continuously embedded into the cement base material. The composite microspheres are directly added into the common cement base material and then constructed, so that the automatic healing reaction of the repairing agent in a matrix can be greatly limited. According to the invention, according to the micromechanics design principle, the addition amount of the composite microsphere additive is determined by optimizing the formula, comparing and analyzing the influence of the composite microsphere content, the water-cement ratio, the sand-cement ratio, the fly ash seepage amount and the PVA fiber amount on the product bonding performance and the thermal expansion and cold contraction performance and combining the test results of a compression test and a bending test.
For the wall side adhesive glue, the invention also takes dopamine and ethylene glycol ethyl ether propionate as cross-linking agents, and synthesizes the double-layer composite microsphere with a core-shell structure by adjusting the concentrations of the cross-linking agents of the inner core and the outer shell, the cross-linking density of the inner core of the microsphere is small, the cross-linking density of the outer shell is large, and the cross-linking density of the inner core is small, so that the double-layer composite microsphere has high liquid absorption capacity; and the shell has higher crosslinking density, so the gel has good gel strength, dry and comfortable surface and other properties. And then dispersing the adhesive in the cement-based material on the wall side, and successfully applying the adhesive to the wall side.
Drawings
FIG. 1 is a morphological diagram of the ceramic tile side adhesive additive composite microspheres of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The specifications and sources of the chemical reagents used in the present invention are detailed below:
main raw materials and specifications
The fiber parameters are as follows:
the test ceramic tile is a standard tile for detecting ceramic tile glue produced by Advance corporation, the water absorption rate of the test ceramic tile is less than or equal to 0.2 percent, the test ceramic tile is not glazed, the test ceramic tile has the size of 48mm multiplied by 48mm, and the back of the test ceramic tile has no dovetail groove and no release agent.
Testing the performance of the ceramic tile adhesive:
an electronic balance: KD-1000 type electronic balance, max =1000g, d =0.01g, fuzhou ketdy electronics technologies, inc;
a bonding strength detector: ZQS6-2000A model high precision bonding strength detector, Beijing Shengshiwei science and technology Limited;
cement bending (compression) resistance tester: tin-free construction equipment, ltd;
a full-automatic linear expansion coefficient measuring instrument RPZ-03P, Loyang atlas Instrument Co., Ltd;
the test method comprises the following steps:
bond strength testing method
1) Shaping of test block
Uniformly coating a layer of mixed bonding mortar on a tile with the thickness of (45 +/-1) mmx (45 +/-1) mm by using a straight-edge trowel, placing the tile on a concrete slab or a ceramic plate, and knocking and compacting to keep the thickness of the bonding mortar to be about 2 mm.
2) Determination of the bond Strength
And (3) carrying out natural curing under the conditions that the indoor relative humidity RH =50 +/-5% and the temperature T =20 ℃, wherein the circulating air speed of the test area is lower than 0.2 m/s. And after 28 days of maintenance, adhering the drawing joint to the ceramic tile by using ceramic tile glue, and after 24 hours, carrying out a drawing test by using a bonding strength detector, and recording the original tensile bonding strength of each group of test blocks.
3) Determination of compressive and flexural strengths
The test was carried out with reference to GB/T1767 l-1999 method for testing the strength of Cement mortar (ISO method). And (3) maintenance: curing for 1d under standard laboratory conditions after molding, demolding, and curing for 28d under standard laboratory conditions. And (4) after the compression strength and the bending strength are tested, calculating the compression ratio of the bonding mortar.
4) Determination of drying shrinkage
In combination with the actual thickness of the tile adhesive mortar, three small test pieces each having a size of 6mm × 6mm × 40mm were prepared in this study (the test pieces were naturally cured at room relative humidity RH =50 ± 5% and temperature T =20 ℃ for a predetermined age, and the lengths of the test pieces 1d, 3d, 7d, 14d, 21d, and 28d were measured, and the shrinkage values of 1d, 3d, 7d, 14d, 21d, and 28d were calculated according to the following equation.
5) Determination of thermal expansion Rate and expansion coefficient
Forming a small test piece with the size of 6mm multiplied by 40mm, polishing the four sides of the test piece by using a grinding wheel, and placing the test piece into a full-automatic high-temperature thermal expansion instrument for measurement. The initial temperature of the test was room temperature (20 ℃ C.) and the temperature rise interval was 25 ℃ C.
The first embodiment is as follows:
s1: preparing an additive of the tile side bonding glue,
adding 400g of deionized water 300-400g into a 1000ml beaker at room temperature, adding 5-12g of AEO-9 emulsifier, uniformly stirring, adding 6-8g of urea, 0.1-0.2g of ammonium nitrate, 0.1-0.2g of phenol and 0.5-2g of formic acid, slowly dropwise adding 1wt.% hydrochloric acid according to mass fraction to adjust the pH value of the solution to about 4, adding 0.5-1.2g of epoxy resin E-44 and 2-5g of ethyl acetate, and emulsifying for 25min at the rotation speed of rpm 1900; and transferring the emulsion formed in the step into a three-neck flask, slowly adding 5-9g of 37% formaldehyde, starting a water bath kettle, starting to heat to 60 ℃, maintaining the temperature for reaction for 1h, performing vacuum filtration on turbid liquid after the reaction is finished, washing with deionized water and absolute ethyl alcohol respectively to obtain a filter cake, putting the filter cake into a vacuum drying oven, and drying at 50 ℃ to constant weight to obtain solid particles, namely the microsphere particles.
S2: preparing cement-based tile side bonding glue,
preparing cement-based tile side bonding glue according to the following mixture ratio:
the weight portion ratio is as follows:
100-150g of ordinary portland cement, 5-32g of slag, 10-30g of quartz sand, 10-55g of water, 0.15-0.2g of PVA fiber, 3-5g of microsphere particles with the particle size of 150 mu m and 2-10g of tetraethylenepentamine;
firstly, pouring cement, slag, quartz sand, PVA fiber and water into a stirrer to be mixed for 1min, then adding tetraethylenepentamine and microsphere particles at a constant speed, and mixing the materials in the running state of the stirrer for use;
s3: preparing the additive of the wall side adhesive glue,
weighing 100-150g of levulinic acid, preparing the levulinic acid aqueous solution by using 10g of KOH aqueous solution with the mass fraction of 10%, and dissolving 3-5g of dopamine and 1-2g of potassium persulfate initiator by using 50g of distilled water to prepare an initiator aqueous solution; adding 4-6g of polyglycerol monostearate and 5-8g of cyclohexane into a four-mouth bottle provided with a thermometer, a condenser pipe, a stirring device and a nitrogen inlet pipe, introducing nitrogen to remove oxygen, heating and stirring the mixed solution, reacting at 95 ℃ for a period of time, supplementing 2-5g of ethylene glycol ethyl ether propionate after 5min to form core-shell structures with different cross-linking densities, cooling and discharging after the expected conversion rate is reached, and washing and drying to obtain spherical particles.
S4: preparing wall side adhesive, coating the wall side adhesive on the cement-based tile side adhesive, and uniformly mixing the wall side adhesive and the cement-based tile side adhesive;
weighing 40-100g of ordinary portland cement, 150-200g of I-grade fly ash, 20-50g of silica fume, 300-600g of quartz fine sand, 150-250g of water, 15-20g of spherical particles obtained in the step S3 and 15-20g of PVA fiber, and stirring for 5min on a stirrer with the rotating speed of 1500rpm to obtain a finished product;
example two:
under the condition that the process operation steps are not adjusted, only the addition amount of each substance in each process section is changed:
s1: preparing a ceramic tile side adhesive glue additive:
400g of deionized water
12g of AEO-9 emulsifier
8g of urea
0.2g ammonium nitrate
0.2g phenol
2g of formic acid
1.2g of epoxy resin E-44
5g of ethyl acetate
9g of 37% formaldehyde
S2: preparing cement-based tile side bonding glue:
150g ordinary portland cement
32g slag
30g of quartz sand
55g of water
0.2g of PVA fiber
5g of 150 μm microspheroidal particles
10g of tetraethylenepentamine
S3: preparing a wall body side adhesive glue additive:
150g levulinic acid
5g dopamine
2g of Potassium persulfate initiator
6g of polyglycerol monostearate
8g of cyclohexane
5g of ethylene glycol ethyl ether propionate
S4: preparing wall side adhesive glue:
100g ordinary portland cement
200g of grade I fly ash
50g of silica fume
600g of fine quartz sand
250g of water
20g of spherical particles
20g of PVA fiber
Example three:
under the condition that the process operation steps are not adjusted, only the addition amount of each substance in each process section is changed:
s1: preparing the ceramic tile side adhesive glue additive,
350g of deionized water
9g of AEO-9 emulsifier
7g of urea
0.15g ammonium nitrate
0.15g phenol
1.5g of formic acid
0.9g of epoxy resin E-44
3g of ethyl acetate
7g of 37% formaldehyde
S2: preparing cement-based tile side bonding glue:
125g ordinary portland cement
20g of slag
20g of quartz sand
35g of water
0.18g of PVA fiber
4g of 150 μm microspheroidal particles
7g of tetraethylenepentamine
S3: preparing a wall body side adhesive glue additive:
125g levulinic acid
4g dopamine
1.5g of Potassium persulfate initiator
5g of polyglycerol monostearate
7g cyclohexane
4g of ethylene glycol monoethyl ether propionate
S4: preparing wall side adhesive glue:
70g ordinary portland cement
175g of class I fly ash
35g of silica fume
450g of quartz fine sand
200g of water
17g of spherical particles
17g of PVA fiber content
Example four:
under the condition that the process operation steps are not adjusted, only the addition amount of each substance in each process section is changed:
s1: preparing a ceramic tile side adhesive glue additive:
300g of deionized water
5g of AEO-9 emulsifier
6g of urea
0.1g ammonium nitrate
0.1g of phenol
0.5g of formic acid
0.5g of epoxy resin E-44
2g of ethyl acetate
5g of 37% formaldehyde
S2: preparing cement-based tile side bonding glue:
150g ordinary portland cement
32g slag
30g of quartz sand
55g of water
0.2g of PVA fiber
5g of 150 μm microspheroidal particles
10g of tetraethylenepentamine
S3: preparing a wall body side adhesive glue additive:
100g levulinic acid
3g dopamine
1g of Potassium persulfate initiator
4g of polyglycerol monostearate
5g cyclohexane
2g of ethylene glycol monoethyl ether propionate
S4: preparing wall side adhesive glue:
100g ordinary portland cement
200g of class I fly ash
50g of silica fume
600g of fine quartz sand
250g of water
20g of spherical particles
20g of PVA fiber
Example five:
under the condition that the process operation steps are not adjusted, only the addition amount of each substance in each process section is changed:
s1: preparing a ceramic tile side adhesive glue additive:
400g of deionized water
12g of AEO-9 emulsifier
8g of urea
0.2g ammonium nitrate
0.2g phenol
2g of formic acid
1.2g of epoxy resin E-44
5g of ethyl acetate
9g of 37% formaldehyde
S2: preparing cement-based tile side bonding glue:
100g ordinary portland cement
5g slag
10g of quartz sand
10g of water
0.15g of PVA fiber
3g of 150 μm microspheroidal particles
2g of tetraethylenepentamine
S3: preparing a wall body side adhesive glue additive:
150g levulinic acid
5g dopamine
2g of Potassium persulfate initiator
6g of polyglycerol monostearate
8g cyclohexane
5g of ethylene glycol monoethyl ether propionate
S4: preparing wall side adhesive glue:
40g ordinary portland cement
150g of class I fly ash
20g of silica fume
300g of fine quartz sand
150g of water
15g of spherical particles
15g of PVA fiber content
Example six:
under the condition that the process operation steps are not adjusted, only the addition amount of each substance in each process section is changed:
s1: preparing a ceramic tile side adhesive glue additive:
350g of deionized water
9g of AEO-9 emulsifier
7g of urea
0.15g ammonium nitrate
0.15g of phenol
1.5g of formic acid
0.9g of epoxy resin E-44
3g of ethyl acetate
7g of 37% formaldehyde
S2: preparing cement-based tile side bonding glue:
150g ordinary portland cement
32g slag
30g of quartz sand
55g of water
0.2g of PVA fiber
5g of 150 μm microspheroidal particles
10g of tetraethylenepentamine
S3: preparing a wall body side adhesive glue additive:
125g levulinic acid
4g dopamine
1.5g of Potassium persulfate initiator
5g of polyglycerol monostearate
7g cyclohexane
4g of ethylene glycol monoethyl ether propionate
S4: preparing wall side adhesive glue:
100g ordinary portland cement
200g of class I fly ash
50g of silica fume
600g of fine quartz sand
250g of water
20g of spherical particles
20g of PVA fiber
Example seven:
under the condition that the process operation steps are not adjusted, only the addition amount of each substance in each process section is changed:
s1: preparing the ceramic tile side adhesive glue additive,
350g of deionized water
9g of AEO-9 emulsifier
7g of urea
0.15g ammonium nitrate
0.15g phenol
1.5g of formic acid
0.7g of epoxy resin E-44
3g of ethyl acetate
7g of 37% formaldehyde
S2: preparing cement-based tile side bonding glue,
150g ordinary portland cement
32g slag
30g of quartz sand
55g of water
0.2g of PVA fiber
5g of 150 μm microspheroidal particles
10g of tetraethylenepentamine
S3: preparing the additive of the wall side adhesive glue,
120g of levulinic acid
4g dopamine
1.5g of Potassium persulfate initiator
4g of polyglycerol monostearate
7g cyclohexane
4g of ethylene glycol monoethyl ether propionate
S4: preparing wall side adhesive glue;
100g ordinary portland cement
200g of class I fly ash
50g of silica fume
600g of fine quartz sand
250g of water
20g of spherical particles
20g of PVA fiber
Comparative example one:
s1: preparing cement-based tile side bonding glue:
preparing cement-based tile side bonding glue according to the following mixture ratio in parts by weight:
100g of ordinary portland cement, 5g of slag, 10g of quartz sand, 10g of water, 0.15g of PVA fiber and 2g of tetraethylenepentamine;
firstly, pouring cement, slag, quartz sand, PVA fiber and water into a stirrer to be mixed for 1min, then adding tetraethylenepentamine at a constant speed, and mixing the materials in the running state of the stirrer for use;
s2: preparing wall side adhesive, coating the wall side adhesive on the cement-based tile side adhesive, and uniformly mixing the wall side adhesive and the cement-based tile side adhesive;
weighing 40g of ordinary portland cement, 150g of I-grade fly ash, 20g of silica fume, 300g of quartz fine sand, 150g of water and 15g of PVA fiber, and stirring for 5min on a stirrer with the rotation speed of 1500rpm to obtain a finished product;
the experimental results are as follows:
| test No | Adhesive Strength (MPa) | Folding ratio | 28d shrinkage (%) | Linear expansion coefficient at 25 (%) | Linear expansion coefficient (%) at 30 DEG C | Linear expansion coefficient (%) at 35 DEG C |
| Example one | 0.658 | 2.471 | 0.075 | 0.042 | 0.044 | 0.047 |
| Example two | 0.703 | 2.264 | 0.069 | 0.038 | 0.041 | 0.042 |
| EXAMPLE III | 0.725 | 2.014 | 0.064 | 0.034 | 0.036 | 0.039 |
| Example four | 0.794 | 1.856 | 0.052 | 0.028 | 0.027 | 0.025 |
| EXAMPLE five | 0.716 | 2.042 | 0.059 | 0.030 | 0.032 | 0.035 |
| EXAMPLE six | 0.817 | 1.103 | 0.029 | 0.019 | 0.021 | 0.025 |
| EXAMPLE seven | 0.845 | 0.954 | 0.022 | 0.014 | 0.016 | 0.017 |
| Comparative example 1 | 0.207 | 8.757 | 0.231 | 0.281 | 0.333 | 0.394 |
And (4) analyzing results:
the ceramic tile side adhesive glue additive is synthesized based on an in-situ polymerization method, and a monomer and an initiator are completely dissolved in the capsule core or outside the capsule core. Since the monomer is soluble in one phase and the resulting polymer is insoluble in the whole system, the polymer will be deposited on the surface of the core material droplet.
The process adopts a one-step method, namely, a reaction monomer is directly added in the polymerization process, and the monomer is subjected to condensation reaction under the acidic condition to generate a polymer to be deposited on the surface of the core material; in the process of preparing the composite microspheres by in-situ polymerization, the following parameters need to be controlled:
(1) the thickness of the composite microsphere wall is moderate, so that the composite microsphere wall can bear the pressure caused by the molding processing of the polymer matrix composite material and can also feel the force caused by the extension of cracks; (2) the composite microspheres must not be too hard to allow cracks to pass through, rather than around; (3) the quantity and volume of the embedded composite microspheres are proper, so that the original performance of the material is not influenced.
As shown in fig. 1, the synthesized composite microspheres have a morphology as shown in the figure, and the particle size distribution of the synthesized composite microspheres is mainly 100 μm.
In the process of preparing the composite microspheres by an in-situ polymerization method, the emulsification of the core material is a crucial step. The performance of the core material emulsion is a key factor of whether the urea-formaldehyde resin is formed by the condensation polymerization reaction on the surface of emulsion liquid drops so as to achieve a good coating effect. The emulsification rate of rotation has a great influence on the droplet size of the emulsion and its stability. The emulsification rotating speed is too low, the mixing of the core material tung oil and the emulsifier is not uniform, the emulsification is not sufficient, and even the emulsion can be layered; when the stirring speed is increased, the core material can be dispersed into smaller liquid drops, and the pH value of the reaction medium is different, so that the reaction process, the structure and the performance of the generated polymer are greatly different. Therefore, the pH value of the reaction medium needs to be well controlled in the process of preparing the composite microspheres.
Specifically, the urea resin composite microspheres which are prepared by a one-step in-situ polymerization method and take an organic solvent as an internal phase are prepared. The phase interface characteristic in the reaction system has an important influence on the composite microsphere formation process, and in order to prepare the composite microsphere with good appearance and strength, the reaction speed needs to be controlled under the condition of a proper system modifier, so that the system is subjected to smooth and sufficient liquid-liquid phase separation.
The reaction process can also be divided into three steps of liquid-liquid phase separation, wetting wrapping and film layer curing: the molecular weight of the urea formaldehyde condensation product is gradually increased along with the reaction of ammonium nitrate and formaldehyde, when the condensation polymerization reaction is carried out to a certain degree, the polymer solution with higher concentration and larger molecular weight is separated from the water phase to form a coacervate phase, one part of the coacervate phase is dispersed in the water phase to form an emulsion, one part of the coacervate phase is wrapped on the surface of oil drops to form a liquid film, and the coacervate phase wrapped on the surface of the oil drops is further subjected to condensation polymerization, crosslinking and curing to finally form the composite microsphere capsule wall.
The synthesized composite microspheres are basically spherical, the particle size distribution is uniform, the average particle size is 100 micrometers, referring to fig. 1, the surfaces of the composite microspheres are rough and compact, the rough surfaces are favorable for increasing the contact area between the composite microspheres and a base material, and the interface bonding force between the composite microspheres and a matrix is improved, so that the repair efficiency of the self-repair material is improved, and the performance of the self-repair coating can be better exerted.
The wall materials applied to the self-repairing system are the most common high polymer materials at present, and mainly comprise amino resin, including urea-formaldehyde resin, melamine-formaldehyde resin and melamine-formaldehyde resin. The invention adopts urea-formaldehyde resin (UF) as a wall material, and the material can be used for preparing compact and firm composite microspheres, so that the formed composite microspheres have good toughness, permeability resistance and wear resistance.
The particle size distribution and the average particle size of the composite microspheres can be greatly influenced by different using amounts of the emulsifier, insufficient emulsification is caused by insufficient using amount of the emulsifier, and the composite microspheres are caused by non-uniform sizes. If excessive emulsifier is added, the surface tension of the oil-water two-phase interface is obviously reduced, the deposition and coating of the polyurea-formaldehyde particles to the surface of oil drops can be promoted, the agglomeration phenomenon of the polyurea-formaldehyde in the water phase is obviously reduced, the surface of the composite microsphere is compact and smooth, and the particle size of the composite microsphere is reduced.
Use of the microcapsule base layer:
the repairing effect of the composite microspheres in the cement-based material mainly depends on the following factors: 1) curing reaction of the repairing agent; 2) permeability of the repair agent in the crack; 3) the fractured form of the composite microspheres in the cement matrix; 4) The bonding strength of the repairing agent on the surface of the cement matrix.
In order to be matched with the composite microspheres for use, the composite microsphere is compounded with a cement-based material, so that the use amount of the composite microspheres in the fiber reinforced cement-based composite material is optimized.
The water-absorbent resin is added into the fiber reinforced cement-based composite material, and the result shows that the expansion and contraction effect of the fiber reinforced cement-based composite material is obviously reduced, and the resin and the fiber jointly form a buffer area of the cement-based composite material.
The larger the crosslinking density of the water-absorbent resin is, the larger the rubber elasticity is, the smaller the liquid absorption capacity and the stickiness and moisture after water absorption are, and the gel strength, the water absorption speed and the permeability are all improved; the prepared polymer surface has higher crosslinking density than the interior, and has higher shear modulus after absorbing water, thereby preventing gel blocking.
The wall side adhesive additive takes cyclohexane as a continuous phase, potassium persulfate as an initiator and dopamine and ethylene glycol ethyl ether propionate as a cross-linking agent, and double-layer composite particles with a core-shell structure are synthesized by controlling the concentrations of the cross-linking agents of the inner core and the outer shell. The crosslinking density of the inner core is small, the crosslinking density of the outer shell is large, and the crosslinking density of the inner core is small, so that the liquid-absorbing capacity is high; and the shell has higher crosslinking density, so the gel has good gel strength, dry surface and other properties. The cement-based composite material is matched for use, and the wall side bonding glue forms a structure similar to a sponge body. Under the humid environment, the moisture absorption capacity of the wall side bonding glue is obviously enhanced, and in the dry environment, the wall side bonding glue can rapidly lose moisture, but the effects of dry shrinkage resistance and thermal expansion and cold shrinkage resistance are very obvious: the composite particles and the fibers together form a buffer zone of the cement-based composite material.
The reason why the bonding strength is obviously improved after the ceramic tile side bonding adhesive additive and the wall side bonding adhesive are compounded is that the composite microspheres in the ceramic tile side bonding adhesive additive and the double-layer composite particles in the wall side bonding adhesive are respectively embedded and locked in the ceramic tile side bonding adhesive additive and the wall side bonding adhesive and are compounded with the PVA material to form a flexible net-shaped structure, and the composite microspheres in the ceramic tile side bonding adhesive additive can be partially broken to release the epoxy resin with extremely high bonding property. By adopting a double-layer composite structure, expansion and shrinkage complementation can be realized between two layers of bonding glue.
Comparing and analyzing the first to seventh embodiments and the first comparative example, the tile side adhesive additive and the corresponding tile side adhesive additive substrate can be obtained, and the ratio of the wall side adhesive to the corresponding wall side adhesive substrate can greatly affect the adhesive strength of the product, but compared with the first comparative example, the comprehensive performance of the product is obviously improved.
It should be noted that, in the sixth and seventh comparative examples, the mixture ratio of the epoxy resin E-44 and the urea resin greatly affects the overall performance of the product, because the mixture ratio greatly affects the synthesis process of the composite microsphere.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the present invention is not limited to the above-mentioned shapes, and any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. A preparation method of tile glue is characterized by comprising the following steps,
s1: preparing the ceramic tile side adhesive glue additive,
adding 400g of deionized water 300-400g into a 1000ml beaker at room temperature, adding 5-12g of AEO-9 emulsifier, uniformly stirring, adding 6-8g of urea, 0.1-0.2g of ammonium nitrate, 0.1-0.2g of phenol and 0.5-2g of formic acid, slowly dropwise adding 1wt.% hydrochloric acid according to mass fraction to adjust the pH value of the solution to 4, adding 0.5-1.2g of epoxy resin E-44 and 2-5g of ethyl acetate, and emulsifying for 25min at the rotation speed of 1900 rpm; transferring the emulsion formed in the step into a three-neck flask, slowly adding 5-9g of 37% formaldehyde, starting a water bath kettle, starting to heat to 60 ℃, maintaining the temperature for reaction for 1 hour, after the reaction is finished, carrying out vacuum filtration on suspension, respectively washing with deionized water and absolute ethyl alcohol to obtain a filter cake, putting the filter cake into a vacuum drying oven, and drying at 50 ℃ to constant weight to obtain solid particles, namely microsphere particles;
s2: preparing cement-based tile side bonding glue,
preparing cement-based tile side adhesive according to the following proportion,
the weight portion ratio is that 100-150g of ordinary portland cement, 5-32g of slag, 10-30g of quartz sand, 10-55g of water, 0.15-0.2g of PVA fiber, 3-5g of microsphere particles with the diameter of 150 mu m obtained by the step S1, 2-10g of tetraethylenepentamine,
firstly, pouring cement, slag, quartz sand, PVA fiber and water into a stirrer to be mixed for 1min, then adding tetraethylenepentamine and microsphere particles at a constant speed, and mixing the materials in the running state of the stirrer for use;
s3: preparing the additive of the wall side adhesive glue,
weighing 100-150g of levulinic acid, preparing the levulinic acid aqueous solution by using 10g of KOH aqueous solution with the mass fraction of 10%, and dissolving 3-5g of dopamine and 1-2g of potassium persulfate initiator by using 50g of distilled water to prepare an initiator aqueous solution; adding 4-6g of polyglycerol monostearate and 5-8g of cyclohexane into a four-mouth bottle provided with a thermometer, a condenser pipe, a stirring device and a nitrogen inlet pipe, introducing nitrogen to remove oxygen, heating and stirring the mixed solution, reacting at 95 ℃ for a period of time, supplementing 2-5g of ethylene glycol ethyl ether propionate after 5min to form core-shell structures with different cross-linking densities, cooling and discharging after the expected conversion rate is reached, and washing and drying to obtain spherical particles;
s4: preparing wall side adhesive, coating the wall side adhesive on the cement-based tile side adhesive, and uniformly mixing the wall side adhesive and the cement-based tile side adhesive;
weighing 40-100g of ordinary portland cement, 150-200g of I-grade fly ash, 20-50g of silica fume, 300-600g of quartz fine sand, 150-250g of water, 15-20g of spherical particles obtained in the step S3 and 15-20g of PVA fiber, and stirring for 5min on a stirrer with the rotating speed of 1500rpm to obtain a finished product; the finished product obtained is applied on the cement-based tile side adhesive.
2. The tile glue preparation method according to claim 1, characterized in that: the weight portion ratio of the urea to the epoxy resin E-44 is 10: 1.
3. the tile glue preparation method according to claim 1, characterized in that: the weight part ratio of the dopamine to the polyglycerol monostearate to the cyclohexane is 4: 4: 7.
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