CN111117521A - Preparation method of quick-drying high-bonding-strength ceramic tile adhesive - Google Patents
Preparation method of quick-drying high-bonding-strength ceramic tile adhesive Download PDFInfo
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- CN111117521A CN111117521A CN201911344294.9A CN201911344294A CN111117521A CN 111117521 A CN111117521 A CN 111117521A CN 201911344294 A CN201911344294 A CN 201911344294A CN 111117521 A CN111117521 A CN 111117521A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J105/00—Adhesives based on polysaccharides or on their derivatives, not provided for in groups C09J101/00 or C09J103/00
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/162—Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a preparation method of quick-drying high-bonding-strength tile glue, and belongs to the field of building materials. The invention adopts carboxymethyl chitosan, guar gum and the like to blend and prepare mixed glue solution, a pretreatment glue solution containing microsphere components is formed under the crosslinking action of auxiliary materials, and a subsequently prepared concentrated material containing titanium dioxide is combined to provide a catalytic drying effect, improve the dispersion stability of the tile glue and provide good bonding strength, the added calcium saccharate is convenient for the internal polymerization, and calcium ions can be combined with sodium alginate to mask partial hydrophilic groups, so that a more stable egg box structure is formed to provide the effect of removing water, the time required by solidification is convenient to shorten, and the bonding strength is maintained for a long time. According to the invention, the metakaolin is modified by adopting trimethylchlorosilane, and a hydrophobic membrane is constructed, so that partial methyl can replace hydroxyl, the number of hydrophilic silicon hydroxyl is reduced, and the compatibility with a sizing material is improved. The invention solves the problems of long cementing time and low bonding strength of the conventional ceramic tile.
Description
Technical Field
The invention belongs to the field of building materials, and particularly relates to a preparation method of quick-drying high-bonding-strength tile glue.
Background
The ceramic tile is used as a decorative material and is widely applied to indoor decoration and outdoor decoration. In the decoration of an outer wall, a large ceramic tile is adopted to improve the aesthetic feeling of decoration, and the method is particularly applied to middle and high-grade public buildings. However, with the rapid development of cities and the increase of high-rise buildings, the cases of breaking cars and hurting passers-by after the tiles on the outer wall slide and fall off in a large area are also rare.
On one hand, the outer wall tiles slide off because the area and the weight of the single tiles for the outer wall are larger and larger, for example, the application of the heavy tiles with the size of 800 multiplied by 800mm in the market is very common; on the other hand, the ceramic tile is more and more compact, and the water absorption rate is lower and lower. In the traditional bonding method, sand and cement are mixed on site to make simple cement mortar, the mortar is then applied to the back of the wetted tile, the mortar-coated tile is then pressed onto the pre-wetted wall surface, and finally the tile is tapped to ensure that the tile has consistent flatness. When the method is used for pasting the low water absorption ceramic tiles of the exterior wall, the ceramic tiles are easy to bulge and fall off, and the construction quality is difficult to ensure.
The ceramic tile adhesive is also called as ceramic tile adhesive, is mainly used for adhering decorative materials such as ceramic tiles, face bricks, floor tiles and the like, and is widely suitable for decorative surface decoration places of buildings such as inner and outer wall surfaces, floors, bathrooms, kitchens and the like. The adhesive is mainly characterized by good water resistance, freeze-thaw resistance and aging resistance, and is an ideal adhesive material. The main components of the traditional tile adhesive are cement, yellow sand and the like, the mortar stirred on the spot by the cement and the yellow sand is used for bonding tiles by a thick pasting method, the cement and the yellow sand are consumed in a large amount, and the defects of complex construction, infirm bonding and easy falling of hollows exist. In addition, cement and mortar are rigid materials, and have the phenomena of low bonding strength, high water absorption, cracking after expansion with heat and contraction with cold and the like, so that the tile is not beautiful, and the fallen tiles can cause personal injury.
With the improvement of aesthetic and waterproof requirements of buildings in recent years, modern ceramic tiles are gradually developed in the direction of thinness and lower water absorption rate, and further higher requirements are provided for ceramic tile bonding materials. The ceramic tile glue on the market at present is various, but still has the following problems: (1) the ceramic tile has long cementing and fixing time, the general ceramic tile adhesive can be finally solidified after at least 12 hours, and the subsequent construction operation can be carried out after at least 48 hours after the ceramic tile is pasted, so that the construction period of the project is prolonged, and the construction requirement can not be met particularly in the project which urgently needs to be finished; (2) most tile glue contains volatile organic components, which can cause environmental pollution and certain harm to constructors and users.
The application of the novel tile adhesive is still in the starting stage, and the problem of tile slippage and falling is less concerned. For example, ZL201110422942.5 proposes a ceramic tile adhesive powder, but because of the cost problem, the adhesive strength is obviously low, and the ceramic tile adhesive powder is not suitable for paving exterior wall ceramic tiles. ZL20111.332087.9A high-strength tile adhesive is proposed, which greatly increases the usage amount of adhesive powder, but does not consider the problem of slippage and falling off in the initial stage of laying heavy tiles in an exterior wall environment, and has higher application cost.
Therefore, a new tile glue is urgently needed to be developed to meet the requirements of people.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems of long cementing and fixing time and low bonding strength of the existing common ceramic tile, the preparation method of the quick-drying high-bonding-strength ceramic tile adhesive is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of quick-drying high-bonding-strength tile glue specifically comprises the following steps:
(1) at the temperature of 30-45 ℃, according to the mass ratio of 1: 2-4: 15-25, mixing and stirring carboxymethyl chitosan, guar gum and an acetic acid solution to obtain a mixed gum solution, adding auxiliary materials accounting for 6-10% of the mass of the mixed gum solution into the mixed gum solution, mixing, and adjusting the pH value to obtain a pre-treated gum solution for later use;
(2) according to the mass parts, 2-5 parts of tetrabutyl titanate, 8-12 parts of absolute ethyl alcohol and 25-35 parts of ammonium chloride solution are mixed to obtain a mixed solution, and the mixed solution is taken according to the weight ratio of 12-25: 1-4, adding modified graphene, mixing, performing ultrasonic treatment to obtain a treatment material, and taking the treatment material according to a weight ratio of 15-25: 2-4, adding sugar calcium, mixing, adjusting the pH, reacting at 120-140 ℃ under heat preservation to obtain a reaction material,
(3) taking a reaction material for suction filtration, collecting filter residues, drying to obtain a dry substance, mixing and stirring 2-5 parts of an additive, 4-8 parts of the dry substance, 1-3 parts of sodium alginate, 0.01-0.04 part of bentonite and 20-30 parts of water according to parts by weight to obtain a suspension, adding a calcium chloride solution with the mass of 25-35% of that of the suspension into the suspension, mixing, shearing and dispersing to obtain a bulk material, and taking a dispersed material for reduced pressure evaporation to obtain a concentrated material for later use;
(4) at 35-55 ℃, according to the weight ratio of 4-8: 1: mixing and stirring metakaolin, trimethylchlorosilane and water, cooling, filtering, collecting filter residues, mixing 30-50 parts of nutrient base solution, 0.1-0.3 part of lactobacillus bulgaricus powder, 4-8 parts of glucose, 3-7 parts of oleic acid and 5-10 parts of filter residues in parts by weight, carrying out shaking culture at 25-32 ℃, sterilizing, discharging, filtering, and collecting filter cakes according to the weight ratio of 10-15: 1-3: 1, adding dodecyl dimethyl betaine and fatty acid diethanolamide, and mixing to obtain a fermentation treatment material;
(5) according to the weight parts, 30-50 parts of standby pretreatment glue solution, 10-14 parts of standby concentrated material, 4-8 parts of pretreatment fly ash, 6-10 parts of oiliness agent, 5-8 parts of fermentation treatment material, 0.2-0.5 part of anticorrosive material, 0.3-0.7 part of thickening agent, 0.1-0.3 part of polydimethylsiloxane and 60-80 parts of water are mixed, stirred and evaporated under reduced pressure, and the quick-drying high-bonding-strength tile glue is obtained.
The auxiliary materials in the step (1) are as follows: according to the weight ratio of 7-12: 3 mixing glycerol and glutaraldehyde to obtain adjuvants.
The modified graphene in the step (2): according to the mass ratio of 6-10: 1: 1, mixing and grinding graphene, polyvinyl alcohol and glycerol to obtain the modified graphene.
The additive in the step (3): according to the weight ratio of 1: and 1-3, mixing sodium dodecyl benzene sulfonate and ammonium chloride to obtain the additive.
The nutrient base solution in the step (4): according to the mass parts, 20-30 parts of peptone, 6-10 parts of yeast powder, 0.1-0.4 part of potassium chloride, 0.2-0.5 part of magnesium sulfate, 1-3 parts of monopotassium phosphate, 1-4 parts of casein and 100-130 parts of water are mixed and sterilized to obtain the nutrient base solution.
The pretreatment fly ash in the step (5): according to the mass ratio of 3-7: and 18, mixing and stirring the fly ash and the HCl solution, filtering, and taking filter residues according to the mass ratio of 7-12: 1: 1, adding epoxidized soybean oil and lecithin, and mixing to obtain the pretreated fly ash.
The oily agent in the step (5): at 45-60 ℃, according to the weight ratio of 3-7: 1: 0.3: and 5, mixing methyl gallate, formic acid, cottonseed oil and a hydrogen peroxide solution, preserving heat, standing, collecting an upper oil phase, washing with a sodium bicarbonate solution to obtain an oil material, mixing and stirring 12-20 parts by weight of the oil material, 8-14 parts by weight of pentaerythritol and 0.1-0.3 part by weight of a catalyst, heating to 80-95 ℃, preserving heat, and washing with a sodium hydroxide solution to obtain the oily agent.
The catalyst comprises the following components: according to the weight ratio of 1: and 2-4, mixing stannous octoate and D001 resin to obtain the catalyst.
The thickening agent in the step (5): according to the weight ratio of 1: and 1-3, mixing hydroxypropyl methyl cellulose and polyacrylamide to obtain the thickening agent.
The anticorrosive material in the step (5): according to the weight ratio of 1: and 2-5, mixing the sodium benzoate and the methyl p-hydroxybenzoate to obtain the preservative.
Compared with other methods, the method has the beneficial technical effects that:
(1) in the process, graphene and macromolecular alcohol are ground and modified, so that the dispersibility of the graphene is improved, the titanium dioxide generated by taking tetrabutyl titanate as a raw material can be wrapped, a catalytic drying effect is provided, more hydrophilic groups are mixed to improve the dispersion stability of the tile glue properly and provide good bonding strength, more oily components are added subsequently, the quick-drying effect of the tile glue can be improved, the added sodium alginate also has the function of thickening a matrix, calcium saccharate is added to facilitate the internal polymerization, the addition of calcium chloride can promote the crosslinking, and calcium ions can be combined with the sodium alginate to mask part of hydrophilic groups, a stable egg box structure is formed to provide the function of separating water, so that the time required by solidification is conveniently shortened, and the bonding strength is kept for a long time;
(2) the invention adopts trimethylchlorosilane to modify metakaolin, constructs a hydrophobic membrane on the surface of the metakaolin, improves the oleophylic property of the metakaolin, enables partial methyl to successfully replace hydroxyl in the blending process, reduces the number of hydrophilic silicon hydroxyl, increases the electron cloud density around silicon atoms, enhances the shielding effect, reduces the binding energy of the silicon atoms and oxygen atoms, enhances the interaction between particles by the modified methyl, improves the compatibility with sizing materials,
meanwhile, metakaolin with a layered silicate structure can reach a high degree through fermentation for 5-8 days in the subsequent fermentation process, is metabolized by lactic acid bacteria to open the interlayer, and residual micro fibers provide the effect of dredging water, and then is blended and compounded with dodecyl dimethyl betaine and fatty acid diethanolamide to provide the wetting and penetrating effect, reduce the interfacial tension of the rubber material and the ground and the ceramic tile, and also provide the emulsification and compatibilization effect, so that the rubber material is partially dispersed among the metakaolin layers, the aggregation of viscous components is avoided, the bonding strength of the ceramic tile adhesive is stably maintained, the aging resistance is good, and the bonding effect is durable;
(3) the invention aims at the problems of long cementing time and low bonding strength of the existing common ceramic tile, has obvious quick drying effect and has good application prospect.
Detailed Description
Auxiliary materials: according to the weight ratio of 7-12: 3 mixing glycerol and glutaraldehyde to obtain adjuvants.
Pretreating fly ash: according to the mass ratio of 3-7: mixing and stirring the fly ash and 12% by mass of HCl solution for 30-45 min, filtering, and taking filter residues according to the mass ratio of 7-12: 1: 1, adding epoxidized soybean oil and lecithin, and uniformly mixing to obtain the pretreated fly ash.
Additive: according to the weight ratio of 1: and 1-3, mixing sodium dodecyl benzene sulfonate and ammonium chloride to obtain the additive.
Modified graphene: according to the mass ratio of 6-10: 1: and 1, mixing and grinding graphene, polyvinyl alcohol and glycerol in a mortar for 1-3 hours to obtain the modified graphene.
Nutrient base solution: according to the mass parts, 20-30 parts of peptone, 6-10 parts of yeast powder, 0.1-0.4 part of potassium chloride, 0.2-0.5 part of magnesium sulfate, 1-3 parts of monopotassium phosphate, 1-4 parts of casein and 100-130 parts of water are mixed and sterilized to obtain the nutrient base solution.
An oiliness agent: at 45-60 ℃, according to the weight ratio of 3-7: 1: 0.3: and 5, mixing methyl gallate, formic acid, cottonseed oil and a hydrogen peroxide solution with the volume fraction of 16%, preserving heat for 1-3 h, standing for 2-4 h, collecting an upper oil phase, washing for 2-4 times by using a sodium bicarbonate solution with the mass fraction of 8% to obtain an oil material, mixing 12-20 parts of the oil material, 8-14 parts of pentaerythritol and 0.1-0.3 part of a catalyst in a reaction kettle in parts by mass, stirring for 25-50 min at the speed of 350-550 r/min, heating to 80-95 ℃, preserving heat for 1-3 h, and then washing for 2-4 times by using a sodium hydroxide solution with the mass fraction of 5% to obtain the oiliness agent.
Catalyst: according to the weight ratio of 1: and 2-4, mixing stannous octoate and D001 resin to obtain the catalyst.
Anticorrosive material: according to the weight ratio of 1: and 2-5, mixing the sodium benzoate and the methyl p-hydroxybenzoate to obtain the preservative.
Thickening agent: according to the weight ratio of 1: and 1-3, mixing hydroxypropyl methyl cellulose and polyacrylamide to obtain the thickening agent.
A preparation method of quick-drying high-bonding-strength tile glue comprises the following steps:
(1) at the temperature of 30-45 ℃, according to the mass ratio of 1: 2-4: 15-25, mixing carboxymethyl chitosan, guar gum and 5% by mass of acetic acid solution, magnetically stirring for 40-60 min at a speed of 350-550 r/min to obtain a mixed gum solution, adding an auxiliary material accounting for 6-10% by mass of the mixed gum solution into the mixed gum solution, mixing, and adjusting the pH to 4.7-5.3 by using 15% by mass of HCl solution to obtain a pre-treated gum solution for later use;
(2) according to the mass parts, 2-5 parts of tetrabutyl titanate, 8-12 parts of absolute ethyl alcohol and 25-35 parts of 15% ammonium chloride solution are mixed to obtain a mixed solution, and the mixed solution is prepared from the following raw materials in parts by weight: 1-4, adding modified graphene, mixing in an ultrasonic oscillator, carrying out ultrasonic treatment for 12-25 min at a frequency of 45-55 kHz to obtain a treated material, and taking the treated material according to a weight ratio of 15-25: 2-4, adding sugar calcium, mixing, adjusting the pH to 8.1-8.4 by using an ammonia water solution with the concentration of 2mol/L, reacting for 1-3 h at the temperature of 120-140 ℃ to obtain a reaction material,
(3) taking a reaction material for suction filtration, collecting filter residues and drying to obtain a dry matter, mixing and stirring 2-5 parts of an additive, 4-8 parts of the dry matter, 1-3 parts of sodium alginate, 0.01-0.04 part of bentonite and 20-30 parts of water for 25-45 min by mass to obtain a suspension, adding the suspension into a 1.2mol/L calcium chloride solution with the mass of 25-35% of the suspension for mixing, shearing and dispersing for 25-45 min at 2000-4000 r/min to obtain a bulk material, taking a dispersion material, and evaporating under reduced pressure to 25-35% of the original volume to obtain a concentrated material for later use;
(4) at 35-55 ℃, according to the weight ratio of 4-8: 1: mixing and stirring metakaolin, trimethylchlorosilane and water, naturally cooling to room temperature, filtering, collecting filter residues, mixing 30-50 parts of nutrient base solution, 0.1-0.3 part of lactobacillus bulgaricus powder, 4-8 parts of glucose, 3-7 parts of oleic acid and 5-10 parts of filter residues in parts by weight in a fermentation tank, carrying out shaking culture at the temperature of 25-32 ℃ at 150-220 r/min for 5-8 days, sterilizing, discharging, filtering, and collecting the filter cakes according to the weight ratio of 10-15: 1-3: 1, adding dodecyl dimethyl betaine and fatty acid diethanolamide, and uniformly mixing to obtain a fermentation treatment material;
(5) according to the weight parts, 30-50 parts of standby pretreatment glue solution, 10-14 parts of standby concentrated material, 4-8 parts of pretreatment fly ash, 6-10 parts of oiliness agent, 5-8 parts of fermentation treatment material, 0.2-0.5 part of anticorrosive material, 0.3-0.7 part of thickening agent, 0.1-0.3 part of polydimethylsiloxane and 60-80 parts of water are mixed in a reaction kettle, and are magnetically stirred for 40-60 min at 500-800 r/min, and are evaporated under reduced pressure to 25-35% of the original volume, so that the quick-drying high-bonding-strength tile glue is obtained.
Example 1
Auxiliary materials: according to the weight ratio of 7: 3 mixing glycerol and glutaraldehyde to obtain adjuvants.
Pretreating fly ash: according to the mass ratio of 3: mixing and stirring the fly ash and 12% by mass of HCl solution for 30-45 min, filtering, and taking filter residues according to the mass ratio of 7: 1: 1, adding epoxidized soybean oil and lecithin, and uniformly mixing to obtain the pretreated fly ash.
Additive: according to the weight ratio of 1: 1, mixing sodium dodecyl benzene sulfonate and ammonium chloride to obtain the additive.
Modified graphene: according to the mass ratio of 6: 1: and 1, mixing and grinding graphene, polyvinyl alcohol and glycerol in a mortar for 1-3 hours to obtain the modified graphene.
Nutrient base solution: according to the mass parts, 20 parts of peptone, 6 parts of yeast powder, 0.1 part of potassium chloride, 0.2 part of magnesium sulfate, 1 part of monopotassium phosphate, 1 part of casein and 100 parts of water are mixed and sterilized to obtain the nutrient base solution.
An oiliness agent: at 45 ℃, according to the weight ratio of 3: 1: 0.3: and 5, mixing methyl gallate, formic acid, cottonseed oil and a hydrogen peroxide solution with the volume fraction of 16%, preserving heat for 1h, standing for 2h, collecting an upper oil phase, washing for 2 times by using a sodium bicarbonate solution with the mass fraction of 8% to obtain an oil material, mixing 12-20 parts of the oil material, 8 parts of pentaerythritol and 0.1 part of a catalyst in parts by mass in a reaction kettle, stirring for 25min at the speed of 350r/min, heating to 80 ℃, preserving heat for 1h, and then washing for 2 times by using a sodium hydroxide solution with the mass fraction of 5% to obtain the oiliness agent.
Catalyst: according to the weight ratio of 1: and 2, mixing stannous octoate and D001 resin to obtain the catalyst.
Anticorrosive material: according to the weight ratio of 1: 2, mixing the sodium benzoate and the methyl p-hydroxybenzoate to obtain the preservative.
Thickening agent: according to the weight ratio of 1: 1, mixing hydroxypropyl methylcellulose and polyacrylamide to obtain the thickening agent.
A preparation method of quick-drying high-bonding-strength tile glue comprises the following steps:
(1) at 30 ℃, according to the mass ratio of 1: 2: mixing carboxymethyl chitosan, guar gum and 5% by mass of acetic acid solution, magnetically stirring for 40min at the speed of 350r/min to obtain a mixed gum solution, adding auxiliary materials accounting for 6% by mass of the mixed gum solution into the mixed gum solution, mixing, and adjusting the pH to 4.7 by using 15% by mass of HCl solution to obtain a pre-treated gum solution for later use;
(2) according to the mass parts, 2 parts of tetrabutyl titanate, 8 parts of absolute ethyl alcohol and 25 parts of ammonium chloride solution with the mass fraction of 15% are mixed to obtain a mixed solution, and the mixed solution is prepared from the following raw materials in parts by weight: 1, adding modified graphene, mixing in an ultrasonic oscillator, carrying out ultrasonic treatment for 12min at the frequency of 45kHz to obtain a treated material, and taking the treated material according to the weight ratio of 15: 2 adding sugar calcium, mixing, adjusting pH to 8.1 with 2mol/L ammonia water solution, reacting at 120 deg.C for 1h to obtain reaction material,
(3) taking a reaction material, carrying out suction filtration, collecting filter residues, drying to obtain a dry substance, mixing and stirring 2 parts of an additive, 4 parts of the dry substance, 1 part of sodium alginate, 0.01 part of bentonite and 20 parts of water for 25min by mass to obtain a suspension, adding the suspension into a 1.2mol/L calcium chloride solution with the mass of 25% of the suspension, mixing, shearing and dispersing for 25min at 2000r/min to obtain a dispersing material, and carrying out reduced pressure evaporation on the dispersing material to 25% of the original volume to obtain a concentrated material for later use;
(4) at 35 ℃, according to the weight ratio of 4: 1: mixing and stirring metakaolin, trimethylchlorosilane and water, naturally cooling to room temperature, filtering, collecting filter residues, mixing 30 parts of nutrient base solution, 0.1 part of lactobacillus bulgaricus powder, 4 parts of glucose, 3 parts of oleic acid and 5 parts of filter residues in parts by weight in a fermentation tank, carrying out shaking culture at 25 ℃ at 150r/min for 5 days, sterilizing, discharging, filtering, and collecting filter cakes according to a weight ratio of 10: 1: 1, adding dodecyl dimethyl betaine and fatty acid diethanolamide, and uniformly mixing to obtain a fermentation treatment material;
(5) according to the weight parts, 30 parts of standby pretreatment glue solution, 10 parts of standby concentrated material, 4 parts of pretreatment fly ash, 6 parts of oiliness agent, 5 parts of fermentation treatment material, 0.2 part of anticorrosive material, 0.3 part of thickening agent, 0.1 part of polydimethylsiloxane and 60 parts of water are mixed in a reaction kettle, and are magnetically stirred for 40min at 500r/min, and are evaporated under reduced pressure to 25% of the original volume, so that the quick-drying high-bonding-strength tile glue is obtained.
Example 2
Auxiliary materials: according to the weight ratio of 12: 3 mixing glycerol and glutaraldehyde to obtain adjuvants.
Pretreating fly ash: according to the mass ratio of 7: 18, mixing and stirring the fly ash and the HCl solution with the mass fraction of 12% for 45min, filtering, and taking filter residues according to the mass ratio of 12: 1: 1, adding epoxidized soybean oil and lecithin, and uniformly mixing to obtain the pretreated fly ash.
Additive: according to the weight ratio of 1: 3 mixing sodium dodecyl benzene sulfonate and ammonium chloride to obtain the additive.
Modified graphene: according to the mass ratio of 10: 1: and 1, mixing and grinding graphene, polyvinyl alcohol and glycerol in a mortar for 1-3 hours to obtain the modified graphene.
Nutrient base solution: according to the mass parts, 30 parts of peptone, 10 parts of yeast powder, 0.4 part of potassium chloride, 0.5 part of magnesium sulfate, 3 parts of monopotassium phosphate, 4 parts of casein and 130 parts of water are mixed and sterilized to obtain the nutrient base solution.
An oiliness agent: at 60 ℃, according to the weight ratio of 7: 1: 0.3: and 5, mixing methyl gallate, formic acid, cottonseed oil and a hydrogen peroxide solution with the volume fraction of 16%, preserving heat for 3h, standing for 4h, collecting an upper oil phase, washing for 4 times by using a sodium bicarbonate solution with the mass fraction of 8% to obtain an oil material, mixing 20 parts of the oil material, 14 parts of pentaerythritol and 0.3 part of a catalyst in parts by mass in a reaction kettle, stirring for 50min at 550r/min, heating to 95 ℃, preserving heat for 3h, and then washing for 4 times by using a sodium hydroxide solution with the mass fraction of 5% to obtain the oiliness agent.
Catalyst: according to the weight ratio of 1: and 4, mixing stannous octoate and D001 resin to obtain the catalyst.
Anticorrosive material: according to the weight ratio of 1: 5 mixing sodium benzoate and methyl p-hydroxybenzoate to obtain antiseptic.
Thickening agent: according to the weight ratio of 1: 3 mixing hydroxypropyl methyl cellulose and polyacrylamide to obtain the thickening agent.
A preparation method of quick-drying high-bonding-strength tile glue comprises the following steps:
(1) at 45 ℃, mixing the components in a mass ratio of 1: 4: 25 mixing carboxymethyl chitosan, guar gum and 5% by mass of acetic acid solution, magnetically stirring for 60min at 550r/min to obtain mixed gum solution, adding 10% by mass of auxiliary materials into the mixed gum solution, mixing, and adjusting the pH to 5.3 by using 15% by mass of HCl solution to obtain a pre-treated gum solution for later use;
(2) according to the mass parts, 5 parts of tetrabutyl titanate, 12 parts of absolute ethyl alcohol and 35 parts of ammonium chloride solution with the mass fraction of 15% are mixed to obtain a mixed solution, and the mixed solution is prepared from the following components in parts by weight: 4, adding the modified graphene, mixing the modified graphene in an ultrasonic oscillator, carrying out ultrasonic treatment for 25min at the frequency of 55kHz to obtain a treated material, and taking the treated material according to the weight ratio of 25: 4 adding sugar calcium, mixing, adjusting the pH to 8.4 by using an ammonia water solution with the concentration of 2mol/L, keeping the temperature at 140 ℃ for reaction for 3 hours to obtain a reaction material,
(3) taking a reaction material for suction filtration, collecting filter residues, drying to obtain a dry substance, mixing and stirring 5 parts of an additive, 8 parts of the dry substance, 3 parts of sodium alginate, 0.04 part of bentonite and 30 parts of water for 45min by mass to obtain a suspension, adding the suspension into a calcium chloride solution with the concentration of 1.2mol/L and the mass of 35% of the suspension for mixing, shearing and dispersing for 45min at 4000r/min to obtain a bulk material, and taking a dispersed material for reduced pressure evaporation to 35% of the original volume to obtain a concentrated material for later use;
(4) at 55 ℃, according to the weight ratio of 8: 1: mixing and stirring metakaolin, trimethylchlorosilane and water, naturally cooling to room temperature, filtering, collecting filter residues, mixing 50 parts of nutrient base solution, 0.3 part of lactobacillus bulgaricus powder, 8 parts of glucose, 7 parts of oleic acid and 10 parts of filter residues in parts by weight in a fermentation tank, carrying out shaking culture at 32 ℃ at 220r/min for 8 days, sterilizing, discharging, filtering, and collecting filter cakes according to a weight ratio of 15: 3: 1, adding dodecyl dimethyl betaine and fatty acid diethanolamide, and uniformly mixing to obtain a fermentation treatment material;
(5) taking 50 parts by weight of standby pretreatment glue solution, 14 parts by weight of standby concentrated material, 8 parts by weight of pretreatment fly ash, 10 parts by weight of oiliness agent, 5-8 parts by weight of fermentation treatment material, 0.5 part by weight of anticorrosive material, 0.7 part by weight of thickening agent, 0.3 part by weight of polydimethylsiloxane and 80 parts by weight of water, mixing in a reaction kettle, magnetically stirring for 60min at 800r/min, and evaporating under reduced pressure to 35% of the original volume to obtain the quick-drying high-bonding-strength ceramic tile glue.
Example 3
Auxiliary materials: according to the weight ratio of 9: 3 mixing glycerol and glutaraldehyde to obtain adjuvants.
Pretreating fly ash: according to the mass ratio of 5: and 18, mixing and stirring the fly ash and the HCl solution with the mass fraction of 12% for 30min, filtering, and taking filter residues according to the mass ratio of 8: 1: 1, adding epoxidized soybean oil and lecithin, and uniformly mixing to obtain the pretreated fly ash.
Additive: according to the weight ratio of 1: 3 mixing sodium dodecyl benzene sulfonate and ammonium chloride to obtain the additive.
Modified graphene: according to the mass ratio of 10: 1: 1, mixing and grinding graphene, polyvinyl alcohol and glycerol in a mortar for 1 hour to obtain the modified graphene.
Nutrient base solution: according to the mass parts, 20 parts of peptone, 6 parts of yeast powder, 0.1 part of potassium chloride, 0.2 part of magnesium sulfate, 1 part of monopotassium phosphate, 1 part of casein and 100 parts of water are mixed and sterilized to obtain the nutrient base solution.
An oiliness agent: at 50 ℃, according to the weight ratio of 5: 1: 0.3: and 5, mixing methyl gallate, formic acid, cottonseed oil and a hydrogen peroxide solution with the volume fraction of 16%, preserving heat for 2h, standing for 3h, collecting an upper oil phase, washing for 3 times by using a sodium bicarbonate solution with the mass fraction of 8% to obtain an oil material, mixing 16 parts of the oil material, 11 parts of pentaerythritol and 0.2 part of a catalyst in parts by mass in a reaction kettle, stirring for 40min at 450r/min, heating to 85 ℃, preserving heat for 2h, and then washing for 3 times by using a sodium hydroxide solution with the mass fraction of 5% to obtain the oiliness agent.
Catalyst: according to the weight ratio of 1: and 3, mixing stannous octoate and D001 resin to obtain the catalyst.
Anticorrosive material: according to the weight ratio of 1: 4 mixing sodium benzoate and methyl p-hydroxybenzoate to obtain antiseptic.
Thickening agent: according to the weight ratio of 1: 2 mixing hydroxypropyl methylcellulose and polyacrylamide to obtain the thickening agent.
A preparation method of quick-drying high-bonding-strength tile glue comprises the following steps:
(1) at 35 ℃, according to the mass ratio of 1: 3: 20, mixing carboxymethyl chitosan, guar gum and 5% by mass of acetic acid solution, magnetically stirring for 50min at a speed of 400r/min to obtain a mixed gum solution, adding 8% by mass of auxiliary materials into the mixed gum solution, mixing, and adjusting the pH to 4.9 by using 15% by mass of HCl solution to obtain a pre-treated gum solution for later use;
(2) according to the mass portion, 3 portions of tetrabutyl titanate, 10 portions of absolute ethyl alcohol and 30 portions of ammonium chloride solution with the mass fraction of 15% are mixed to obtain mixed solution, and the mixed solution is prepared by mixing the following components in a weight ratio of 18: 3, adding the modified graphene, mixing the modified graphene in an ultrasonic oscillator, carrying out ultrasonic treatment for 18min at the frequency of 48kHz to obtain a treated material, and taking the treated material according to the weight ratio of 19: 3 adding sugar calcium, mixing, adjusting pH to 8.3 with 2mol/L ammonia water solution, reacting at 130 deg.C for 2h to obtain reaction material,
(3) taking a reaction material, carrying out suction filtration, collecting filter residues, drying to obtain a dry substance, mixing and stirring 3 parts of an additive, 6 parts of the dry substance, 2 parts of sodium alginate, 0.02 part of bentonite and 25 parts of water for 40min by mass to obtain a suspension, adding the suspension into a 1.2mol/L calcium chloride solution with the mass of 30% of the suspension, mixing, shearing and dispersing for 35min at 3000r/min to obtain a dispersing material, and carrying out reduced pressure evaporation on the dispersing material to 30% of the original volume to obtain a concentrated material for later use;
(4) at 45 ℃, the weight ratio of 6: 1: mixing and stirring metakaolin, trimethylchlorosilane and water, naturally cooling to room temperature, filtering, collecting filter residues, mixing 40 parts of nutrient base solution, 0.2 part of lactobacillus bulgaricus powder, 7 parts of glucose, 5 parts of oleic acid and 7 parts of filter residues in parts by weight in a fermentation tank, carrying out shaking culture at the temperature of 28 ℃ at 170r/min for 6 days, sterilizing, discharging, filtering, and collecting filter cakes according to the weight ratio of 13: 2: 1, adding dodecyl dimethyl betaine and fatty acid diethanolamide, and uniformly mixing to obtain a fermentation treatment material;
(5) taking 40 parts by weight of standby pretreatment glue solution, 12 parts by weight of standby concentrated material, 6 parts by weight of pretreatment fly ash, 8 parts by weight of oiliness agent, 6 parts by weight of fermentation treatment material, 0.4 part by weight of anticorrosive material, 0.5 part by weight of thickening agent, 0.2 part by weight of polydimethylsiloxane and 70 parts by weight of water, mixing in a reaction kettle, magnetically stirring for 50min at 600r/min, and evaporating under reduced pressure to 30% of the original volume to obtain the quick-drying high-bonding-strength tile glue.
Comparative example 1: the procedure was substantially the same as in example 3 except that the concentrate prepared in steps (1) to (3) was omitted.
Comparative example 2: the same preparation method as that of example 3 was followed except that the fermentation treatment material obtained in step (4) was absent.
Comparative example 3: the ceramic tile glue is produced by a certain company in the Wuxi market. (the main components are water glass, sodium silicate and sodium metasilicate pentahydrate).
The tile adhesive obtained in the above example and the tile adhesive of the comparative example are tested at 25 ℃ to respectively test the modulus, the surface dry time, the elongation at break and the tensile strength of each tile adhesive after one week of moisture curing and curing in air, and the test standard is JC/T547-2005, and the test results are shown in the following table 1.
In conclusion, the quick-drying high-bonding-strength ceramic tile adhesive disclosed by the invention is high in strength, high in surface drying speed and high in tensile strength. Compared with the products sold on the market, the product has better effect and is worth popularizing.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the subject matter of the invention is to be construed in all aspects and as broadly as possible, and all changes, equivalents and modifications that fall within the true spirit and scope of the invention are therefore intended to be embraced therein.
Claims (10)
1. A preparation method of quick-drying high-bonding-strength tile glue is characterized by comprising the following steps:
(1) at the temperature of 30-45 ℃, according to the mass ratio of 1: 2-4: 15-25, mixing and stirring carboxymethyl chitosan, guar gum and an acetic acid solution to obtain a mixed gum solution, adding auxiliary materials accounting for 6-10% of the mass of the mixed gum solution into the mixed gum solution, mixing, and adjusting the pH value to obtain a pre-treated gum solution for later use;
(2) according to the mass parts, 2-5 parts of tetrabutyl titanate, 8-12 parts of absolute ethyl alcohol and 25-35 parts of ammonium chloride solution are mixed to obtain a mixed solution, and the mixed solution is taken according to the weight ratio of 12-25: 1-4, adding modified graphene, mixing, performing ultrasonic treatment to obtain a treatment material, and taking the treatment material according to a weight ratio of 15-25: 2-4, adding sugar calcium, mixing, adjusting the pH, reacting at 120-140 ℃ under heat preservation to obtain a reaction material,
(3) taking a reaction material for suction filtration, collecting filter residues, drying to obtain a dry substance, mixing and stirring 2-5 parts of an additive, 4-8 parts of the dry substance, 1-3 parts of sodium alginate, 0.01-0.04 part of bentonite and 20-30 parts of water according to parts by weight to obtain a suspension, adding a calcium chloride solution with the mass of 25-35% of that of the suspension into the suspension, mixing, shearing and dispersing to obtain a bulk material, and taking a dispersed material for reduced pressure evaporation to obtain a concentrated material for later use;
(4) at 35-55 ℃, according to the weight ratio of 4-8: 1: mixing and stirring metakaolin, trimethylchlorosilane and water, cooling, filtering, collecting filter residues, mixing 30-50 parts of nutrient base solution, 0.1-0.3 part of lactobacillus bulgaricus powder, 4-8 parts of glucose, 3-7 parts of oleic acid and 5-10 parts of filter residues in parts by weight, carrying out shaking culture at 25-32 ℃, sterilizing, discharging, filtering, and collecting filter cakes according to the weight ratio of 10-15: 1-3: 1, adding dodecyl dimethyl betaine and fatty acid diethanolamide, and mixing to obtain a fermentation treatment material;
(5) according to the weight parts, 30-50 parts of standby pretreatment glue solution, 10-14 parts of standby concentrated material, 4-8 parts of pretreatment fly ash, 6-10 parts of oiliness agent, 5-8 parts of fermentation treatment material, 0.2-0.5 part of anticorrosive material, 0.3-0.7 part of thickening agent, 0.1-0.3 part of polydimethylsiloxane and 60-80 parts of water are mixed, stirred and evaporated under reduced pressure, and the quick-drying high-bonding-strength tile glue is obtained.
2. The method for preparing quick-drying high-bonding-strength tile glue according to claim 1, wherein the auxiliary materials in the step (1) comprise: according to the weight ratio of 7-12: 3 mixing glycerol and glutaraldehyde to obtain adjuvants.
3. The preparation method of the quick-drying high-bonding-strength tile glue according to claim 1, wherein the modified graphene in the step (2): according to the mass ratio of 6-10: 1: 1, mixing and grinding graphene, polyvinyl alcohol and glycerol to obtain the modified graphene.
4. The method for preparing quick-drying high-bonding-strength tile glue according to claim 1, wherein the additives in the step (3): according to the weight ratio of 1: and 1-3, mixing sodium dodecyl benzene sulfonate and ammonium chloride to obtain the additive.
5. The method for preparing quick-drying high-bonding-strength tile glue according to claim 1, wherein the nutrient base solution in the step (4): according to the mass parts, 20-30 parts of peptone, 6-10 parts of yeast powder, 0.1-0.4 part of potassium chloride, 0.2-0.5 part of magnesium sulfate, 1-3 parts of monopotassium phosphate, 1-4 parts of casein and 100-130 parts of water are mixed and sterilized to obtain the nutrient base solution.
6. The method for preparing quick-drying high-bonding-strength tile glue according to claim 1, wherein the pre-treated fly ash in the step (5): according to the mass ratio of 3-7: and 18, mixing and stirring the fly ash and the HCl solution, filtering, and taking filter residues according to the mass ratio of 7-12: 1: 1, adding epoxidized soybean oil and lecithin, and mixing to obtain the pretreated fly ash.
7. The method for preparing quick-drying high-bonding-strength tile glue according to claim 1, wherein the oily agent in the step (5): at 45-60 ℃, according to the weight ratio of 3-7: 1: 0.3: and 5, mixing methyl gallate, formic acid, cottonseed oil and a hydrogen peroxide solution, preserving heat, standing, collecting an upper oil phase, washing with a sodium bicarbonate solution to obtain an oil material, mixing and stirring 12-20 parts by weight of the oil material, 8-14 parts by weight of pentaerythritol and 0.1-0.3 part by weight of a catalyst, heating to 80-95 ℃, preserving heat, and washing with a sodium hydroxide solution to obtain the oily agent.
8. The method for preparing a quick-drying high-bonding-strength tile adhesive according to claim 7, wherein the catalyst: according to the weight ratio of 1: and 2-4, mixing stannous octoate and D001 resin to obtain the catalyst.
9. The method for preparing quick-drying high-bonding-strength tile glue according to claim 1, wherein the thickening agent in the step (5): according to the weight ratio of 1: and 1-3, mixing hydroxypropyl methyl cellulose and polyacrylamide to obtain the thickening agent.
10. The method for preparing quick-drying high-bonding-strength tile glue according to claim 1, wherein the anticorrosive material in the step (5): according to the weight ratio of 1: and 2-5, mixing the sodium benzoate and the methyl p-hydroxybenzoate to obtain the preservative.
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