CN112778450A - Ceramic tile back glue emulsion with high initial adhesion and high bonding strength and preparation method thereof - Google Patents
Ceramic tile back glue emulsion with high initial adhesion and high bonding strength and preparation method thereof Download PDFInfo
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- CN112778450A CN112778450A CN202011632554.5A CN202011632554A CN112778450A CN 112778450 A CN112778450 A CN 112778450A CN 202011632554 A CN202011632554 A CN 202011632554A CN 112778450 A CN112778450 A CN 112778450A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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- C09J143/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Adhesives based on derivatives of such polymers
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Abstract
The invention discloses a ceramic tile back glue emulsion with high initial adhesion and high bonding strength and a preparation method thereof, wherein the ceramic tile back glue emulsion comprises the following components in parts by weight: 92.5-100 parts of deionized water; 1-5 parts of tridecyl methacrylate; 95-105 parts of butyl acrylate; 5-10 parts of 2-ethylhexyl acrylate; 1-3 parts of acrylic acid; 1.8-2.8 parts of hydroxyethyl acrylate; 0.1-0.5 part of vinyl trimethoxy silane; 0.1-0.5 part of methacrylamide ethyl ethylene urea; 1-3 parts of an emulsifier; 0.5-2 parts of an initiator; 0.1-1 part of sodium hydroxide; 0.4-1 part of bactericide; 0.05-0.2 part of defoaming agent. The ceramic tile back glue emulsion obtained by using the formula has excellent water resistance and low odor (low VOC content), does not contain APEO (alkylphenol ethoxylates) and formaldehyde, simultaneously has high initial viscosity and high bonding strength, has better performance compared with the prior ceramic tile back glue emulsion, and can be directly used as a ceramic tile back glue product.
Description
Technical Field
The invention relates to the technical field of ceramic tile back glue, in particular to ceramic tile back glue emulsion with high initial adhesion and high bonding strength and a preparation method thereof.
Background
The existing acrylic acid single-component ceramic tile back glue has various types, but has the problem that the characteristics of high initial viscosity and high bonding strength cannot be simultaneously considered, for example, the ceramic tile back glue of a modified pressure-sensitive adhesive system has high initial viscosity, but the bonding strength of the back glue is poor; the existing ceramic tile back glue with high bonding strength has general initial viscosity, and due to strong rigidity and poor vibration resisting effect, the ceramic tile back glue is poor in tile smashing effect, and after being paved, if holes are punched in decoration, the ceramic tile back glue is easy to fall off.
Some tile back glue products with medium initial viscosity (initial adhesive ball number is 10-16 balls) and medium adhesive strength (adhesive strength is 0.4-0.6MPa) are also provided in the existing market, but because acrylic resin has the characteristics of hot adhesion and cold brittleness, acrylic single-component back glue products with high initial viscosity and adhesive strength are still rarely available in the market. If the glass transition temperature of the acrylic emulsion is less than or equal to minus 40 ℃, the rigidity of a macromolecular chain is not enough, and the back glue of the ceramic tile is difficult to achieve high bonding strength; if the glass transition temperature is increased, the bonding strength of the tile back adhesive is increased, but the initial adhesion is decreased, which makes it difficult to simultaneously have high initial adhesion and high bonding strength in the tile back adhesive.
It is seen that improvements and enhancements to the prior art are needed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide the ceramic tile back glue emulsion with high initial adhesion and high bonding strength and the preparation method thereof, and aims to solve the problem that the initial adhesion performance and the bonding strength of the existing ceramic tile back glue product cannot be improved at the same time.
In order to achieve the purpose, the invention adopts the following technical scheme:
the ceramic tile back glue emulsion with high initial adhesion and high bonding strength comprises the following raw materials in parts by weight:
in the ceramic tile back glue emulsion with high initial adhesion and high strength, the raw materials also comprise the following components in parts by weight:
0.1-0.5 part of tert-butyl hydroperoxide;
0.1 to 0.4 portion of sodium bisulfite.
In the high initial adhesion and high strength tile back glue emulsion, the emulsifier comprises an anionic emulsifier and a nonionic emulsifier; the ratio of the anionic emulsifier to the nonionic emulsifier is 1-6:1 in parts by weight.
In the high-initial-viscosity high-strength ceramic tile back glue emulsion, the anionic emulsifier is one or more of sodium dodecyl diphenyl ether disulfonate, sodium allyloxy hydroxypropyl sulfonate and sodium tridecyl ether sulfate.
In the ceramic tile back glue emulsion with high initial adhesion and high strength, the nonionic emulsifier is one or two of fatty alcohol polyoxyethylene (7) ether and isomeric C13 fatty alcohol polyoxyethylene (40) ether.
In the high-initial-adhesion high-strength ceramic tile back glue emulsion, the initiator is one or two of ammonium persulfate and sodium persulfate.
The invention also provides a preparation method of the ceramic tile back glue emulsion with high initial adhesion and high strength, which comprises the following steps:
adding 0.4-0.8 weight part of emulsifier and 30.5-34 weight parts of deionized water into a polymerization kettle with a stirrer, a condenser and a constant flow pump heating device to prepare a base solution, and raising the temperature in the polymerization kettle to 80-83 ℃;
adding tridecyl methacrylate, butyl acrylate, 2-ethylhexyl acrylate, acrylic acid, hydroxyethyl acrylate, vinyl trimethoxy silane, methacrylamide ethyl ethylene urea, 0.6-2.2 parts by weight of emulsifier and 34-39 parts by weight of deionized water into a pre-emulsification tank with a monomer metering tank and a stirrer at normal temperature and normal pressure, and stirring and mixing uniformly to prepare a pre-emulsion;
preparing an initiator solution A: adding 0.1-0.8 part of initiator and 8-15 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the initiator and the deionized water are completely dissolved for later use;
preparing an initiator solution B: adding 0.4-1.2 parts of initiator and 2 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the initiator and the deionized water are completely dissolved for later use;
fifthly, when the temperature in the polymerization kettle reaches 80-83 ℃, adding 4-7 percent of the total amount of the pre-emulsion and the initiator solution B into the bottom liquid in the kettle at one time, reacting for 15-25min, preparing a seed emulsion, then simultaneously dropwise adding the rest pre-emulsion and the initiator solution A into the polymerization kettle through a constant flow pump feeding device and a constant current dropwise adding metering device, wherein the dropwise adding speed is constant, the dropwise adding time is controlled to be 3-3.5h, and the dropwise adding of the initiator solution A is finished 5-10min later than that of the pre-emulsion;
sixthly, after the initiator solution A and the pre-emulsion are dripped, controlling the temperature in the polymerization kettle to be 80-83 ℃, and keeping the temperature for 1-1.5 h; after the heat preservation is finished, reducing the temperature in the polymerization kettle to be below 50 ℃, and adjusting the pH of the liquid in the kettle to 7-8 by using sodium hydroxide; after pH is adjusted, adding a defoaming agent, a bactericide and 2.5-18 parts by weight of deionized water, and stirring the liquid in the kettle for 0.5-1 h; and after stirring, filtering the liquid in the kettle to obtain the ceramic tile back glue emulsion with high initial adhesion and high bonding strength.
The preparation method of the ceramic tile back glue emulsion with high initial adhesion and high strength further comprises the following steps:
adding 0.1-0.5 part of tert-butyl hydroperoxide and 3.5 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the tert-butyl hydroperoxide and the deionized water are completely dissolved for later use;
adding 0.1-0.4 part of sodium bisulfite and 4 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the sodium bisulfite and the deionized water are completely dissolved for later use;
thirdly, keeping the temperature in the polymerization kettle at 80-83 ℃, keeping the temperature for 1-1.5h, then cooling the temperature in the polymerization kettle to 70-75 ℃, and simultaneously dropwise adding a tert-butyl hydroperoxide solution and a sodium bisulfite solution into the polymerization kettle, wherein the dropwise adding time is controlled to be 1-1.5 h; after the dropwise addition is finished, the temperature in the polymerization kettle is reduced to below 50 ℃, and the pH of the liquid in the kettle is adjusted to 7-8 by using sodium hydroxide.
Has the advantages that:
the invention provides a ceramic tile back glue emulsion with high initial adhesion and high bonding strength and a preparation method thereof, compared with the prior art, the ceramic tile back glue emulsion has the following advantages:
(1) according to the invention, the tridecyl methacrylate, the butyl acrylate and the 2-ethylhexyl acrylate are used as main monomers, so that the glass transition temperature of the emulsion main body can be reduced, the flexibility of a macromolecular chain (emulsion main body) of a high polymer can be fully ensured, and the tile back glue emulsion can be ensured to have high initial adhesion performance and large adjustment space of the initial adhesion performance and also have certain bonding strength and water resistance;
(2) according to the invention, the seed emulsion is prepared in advance in the synthesis reaction process of the emulsion, so that the particle size distribution of the obtained emulsion is more uniform, the distribution of functional groups in the ceramic tile back glue emulsion is effectively controlled, and the permeability and the density of the ceramic tile back glue emulsion after film forming are improved;
(3) functional monomers of acrylic acid, hydroxyethyl acrylate, vinyl trimethoxy silane and methacrylamide ethyl ethylene urea are introduced; functional groups such as carboxyl, hydroxyl, carbamido, amino and the like can be grafted on the macromolecular chain of the emulsion main body, so that the adhesive property of the ceramic tile back glue emulsion is obviously improved;
(4) according to the invention, by introducing the oxidant and the reducing agent, the residual monomer can be treated, the odor of the ceramic tile gum emulsion can be reduced, and the environment-friendly ceramic tile gum emulsion can improve the body health of a constructor.
Detailed Description
The invention provides a ceramic tile back glue emulsion with high initial adhesion and high bonding strength and a preparation method thereof, and in order to make the purpose, technical scheme and effect of the invention clearer and more clear, the invention is further described in detail by taking examples as follows. 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 ceramic tile back glue emulsion with high initial adhesion and high bonding strength comprises the following raw materials in parts by weight:
in the formula, the tridecyl methacrylate, the butyl acrylate and the 2-ethylhexyl acrylate are all main monomers; the glass transition temperature of the three main monomers is very low, the flexibility of a macromolecular chain (emulsion main body) of a high polymer can be fully ensured, the ceramic tile back glue emulsion is ensured to have high initial viscosity and the adjustment space of the viscosity is larger, and meanwhile, the ceramic tile back glue emulsion can also be ensured to have certain bonding strength and water resistance. When butyl acrylate and acrylic acid-2-ethyl hexyl ester are used as main monomers, although the initial viscosity of the ceramic tile back glue emulsion can be improved, the bonding strength is not greatly improved, and the modification of other monomers to the emulsion main body is not facilitated; the tridecyl methacrylate has methyl and tridecyl long-chain side groups, the steric hindrance effect of the two side groups strengthens the rigidity of the macromolecular chain of the emulsion main body, and meanwhile, the tridecyl long-chain side group has longer length and large flexibility and can not greatly lose the initial viscosity performance of the emulsion; compared with butyl acrylate and 2-ethylhexyl acrylate, the water resistance and the bonding property of the ceramic tile back glue emulsion are improved after the emulsion is modified with a main macromolecular chain of the emulsion.
In the formula, the acrylic acid, the hydroxyethyl acrylate, the vinyl trimethoxy silane and the methacrylamide ethyl ethylene urea are all functional monomers. The acrylic acid can provide carboxyl for the ceramic tile back glue emulsion, and when the ceramic tile back glue emulsion is used, the carboxyl can form a hydrogen bond with the surface of a ceramic tile and ceramic tile glue and can be chelated with metal ions; the ethyl acrylate can provide hydroxyl for the ceramic tile back glue emulsion, and when the ceramic tile back glue emulsion is used, the hydroxyl can also form a hydrogen bond with the surface of the ceramic tile and the ceramic tile glue; after vinyl trimethoxy silane is grafted to the emulsion main body and the pH value of the emulsion is adjusted by sodium hydroxide, a silanol bond can be provided for the ceramic tile back glue emulsion, and after the emulsion forms a film, a covalent bond and a hydrogen bond can be formed with the surface of a ceramic tile, so that the bonding strength of the ceramic tile back glue emulsion is greatly improved; after the methacrylamide ethyl ethylene urea participates in the polymerization reaction, urea bonds can be introduced into the tile back glue emulsion, and the urea bonds can improve the bonding strength of the tile back glue emulsion, the tiles and the tile glue through dipole-dipole and hydrogen bond actions. The four functional monomers can improve the rigidity and intermolecular acting force of the ceramic tile back glue emulsion, so that the bonding strength of the ceramic tile back glue emulsion is further improved; however, the four functional monomers can achieve the effect of improving the bonding strength of the ceramic tile back glue emulsion through the synergistic effect of the monomers in a specific ratio. Too much introduction of any one functional monomer can improve the branching degree or crosslinking degree of a macromolecular chain of the emulsion main body, so that the initial viscosity of the ceramic tile back glue emulsion is reduced, and the initial viscosity of the ceramic tile back glue emulsion cannot meet the use requirement; meanwhile, the functional monomer is introduced too much, so that the phenomenon that functional groups in latex particles are embedded in the emulsion can occur, the number of effective functional groups for generating molecular acting force by the gum, the ceramic tile and the ceramic tile glue is reduced, and the improvement of the bonding strength of the ceramic tile gum emulsion is limited. Therefore, it is necessary to accurately control the amount of each functional monomer so that the effects of the other functional monomers are not reduced by introducing an excessive amount of any one of the functional monomers.
The tile back glue emulsion obtained by using the formula has excellent water resistance and low odor (low VOC content), does not contain APEO (alkylphenol ethoxylates) and formaldehyde, and simultaneously has the characteristics of high initial adhesion and high bonding strength. The ceramic tile back adhesive emulsion is tested according to the GB/T4852-2002 pressure-sensitive adhesive tape initial adhesion test method (ball rolling method) and the JC/T547-2017 ceramic tile adhesive standard (the single-component emulsion back adhesive has no national standard temporarily, so the bonding strength test is carried out according to the JC/T547-2017 ceramic tile adhesive standard), and the detection result shows that the high initial adhesion and the high bonding strength of the ceramic tile back adhesive emulsion can be simultaneously considered, so that the product performance is better compared with the existing ceramic tile back adhesive product, and the ceramic tile back adhesive emulsion can be directly used as the ceramic tile back adhesive product.
Specifically, the emulsifier includes an anionic emulsifier and a nonionic emulsifier; the stability of the emulsion can be improved by the double-layer electrostatic repulsion of the anionic emulsifier and the steric hindrance of the nonionic emulsifier. Preferably, when the proportion of the anionic emulsifier and the nonionic emulsifier is 1-6:1 by weight and the total amount of the emulsifiers is 1-3 parts, the tile back glue emulsion has good emulsifying property and the stability of the emulsion is optimal.
Further, the anionic emulsifier is one or more of sodium dodecyl diphenyl ether disulfonate, sodium allyloxy hydroxypropyl sulfonate and sodium tridecyl ether sulfate. The sodium dodecyl diphenyl ether disulfonate can better emulsify a reaction monomer, improve the hydroxyl group of the emulsion and effectively reduce the gel rate; the emulsifier allyloxy hydroxypropyl sodium sulfonate can polymerize substances with surface activity to the molecular chain of the emulsion main body, so that the water resistance of the tile back glue emulsion can be improved; when the dosage of the emulsifier sodium tridecyl ether sulfate in the formula is less, the emulsifying effect can be improved, so that the influence on the overall performance of the emulsion is less.
Further, the nonionic emulsifier is one or two of fatty alcohol polyoxyethylene (7) ether and isomeric C13 fatty alcohol polyoxyethylene (40) ether. The emulsifier fatty alcohol polyoxyethylene (7) ether has 7 ethoxy groups, and is good in water resistance, hydrophobic, excellent in emulsifying effect and wettability; the emulsifier isomeric C13 fatty alcohol polyoxyethylene (40) ether has 40 ethoxy groups in the molecular structure, is less in dosage in the formula, and has better wettability and emulsification protection than fatty alcohol polyoxyethylene (7) ether.
Specifically, the initiator is one or two of ammonium persulfate and sodium persulfate.
In addition, the ceramic tile back glue emulsion with high initial adhesion and high strength provided by the invention also comprises the following components in parts by weight:
0.1-0.5 part of tert-butyl hydroperoxide;
0.1 to 0.4 portion of sodium bisulfite.
The tert-butyl hydroperoxide is an oxidizing agent, the sodium bisulfite is a reducing agent, and the sodium bisulfite is used for treating residual monomers in the ceramic tile back glue emulsion respectively, so that the conversion rate of the main monomer and the functional monomer is improved, the pungent smell is eliminated, the smell of the ceramic tile back glue emulsion is reduced, and the environmental protection is realized while the body health of a constructor is improved.
The invention also provides a preparation method of the ceramic tile back glue emulsion with high initial adhesion and high strength, which comprises the following steps:
adding 0.4-0.8 weight part of emulsifier and 30.5-34 weight parts of deionized water into a polymerization kettle with a stirrer, a condenser and a constant flow pump heating device to prepare a base solution, and raising the temperature in the polymerization kettle to 80-83 ℃;
adding tridecyl methacrylate, butyl acrylate, 2-ethylhexyl acrylate, acrylic acid, hydroxyethyl acrylate, vinyl trimethoxy silane, methacrylamide ethyl ethylene urea, 0.6-2.2 parts by weight of emulsifier and 34-39 parts by weight of deionized water into a pre-emulsification tank with a monomer metering tank and a stirrer at normal temperature and normal pressure, and stirring and mixing uniformly to prepare a pre-emulsion;
preparing an initiator solution A: adding 0.1-0.8 part of initiator and 8-15 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the initiator and the deionized water are completely dissolved for later use;
preparing an initiator solution B: adding 0.4-1.2 parts of initiator and 2 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the initiator and the deionized water are completely dissolved for later use;
fifthly, when the temperature in the polymerization kettle reaches 80-83 ℃, adding 4-7 percent of the total amount of the pre-emulsion and the initiator solution B into the bottom liquid in the kettle at one time, reacting for 15-25min, preparing a seed emulsion, then simultaneously dropwise adding the rest pre-emulsion and the initiator solution A into the polymerization kettle through a constant flow pump feeding device and a constant current dropwise adding metering device, wherein the dropwise adding speed is constant, the dropwise adding time is controlled to be 3-3.5h, and the dropwise adding of the initiator solution A is finished 5-10min later than that of the pre-emulsion;
in the step, the seed emulsion is prepared in advance in the synthesis reaction process of the emulsion, so that part of emulsion main bodies can be synthesized in advance, the condition that the emulsion main bodies are aggregated due to too high monomer concentration in a reaction system during emulsion synthesis by a one-step method can be avoided, the particle size distribution of the obtained emulsion is more uniform, the distribution of functional groups in the ceramic tile back adhesive emulsion is effectively controlled, and the quality of the ceramic tile back adhesive emulsion is ensured;
in addition, when the seed emulsion is prepared, as the concentration of polymerizable monomers at the bottom of the polymerization kettle is low in the early stage of reaction, the probability of collision between the initiator and monomer molecules can be improved by adding more initiators, the initiation speed of the monomers is accelerated, and the using amount of the initiators is more; and in the later stage of the reaction, in order to reduce the chain termination probability and improve the molecular weight of the polymer, the using amount of the initiator can be reduced, so that the toughness of the macromolecular chain of the emulsion main body is high, and the adhesive strength of the ceramic tile back adhesive emulsion is improved while the ceramic tile back adhesive emulsion still has better initial adhesive property.
Sixthly, after the initiator solution A and the pre-emulsion are dripped, controlling the temperature in the polymerization kettle to be 80-83 ℃, and keeping the temperature for 1-1.5 h; after the heat preservation is finished, reducing the temperature in the polymerization kettle to be below 50 ℃, and adjusting the pH of the liquid in the kettle to be 7-8 by using sodium hydroxide to enable the emulsion to have a silanol bond capable of generating acting force with the surface of the ceramic tile and the ceramic tile glue; after pH is adjusted, adding a defoaming agent, a bactericide and 2.5-18 parts by weight of deionized water, and stirring the liquid in the kettle for 0.5-1 h; and after stirring, filtering the liquid in the kettle to obtain the ceramic tile back glue emulsion with high initial adhesion and high bonding strength.
Further, the preparation method of the ceramic tile back glue emulsion with high initial adhesion and high strength further comprises the following steps:
adding 0.1-0.5 part of tert-butyl hydroperoxide and 3.5 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the tert-butyl hydroperoxide and the deionized water are completely dissolved for later use;
adding 0.1-0.4 part of sodium bisulfite and 4 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the sodium bisulfite and the deionized water are completely dissolved for later use;
thirdly, keeping the temperature in the polymerization kettle at 80-83 ℃, keeping the temperature for 1-1.5h, then cooling the temperature in the polymerization kettle to 70-75 ℃, and simultaneously dropwise adding a tert-butyl hydroperoxide solution and a sodium bisulfite solution into the polymerization kettle to treat residual monomers, wherein the dropwise adding time is controlled to be 1-1.5 h; after the dropwise addition is finished, the temperature in the polymerization kettle is reduced to below 50 ℃, and the pH of the liquid in the kettle is adjusted to 7-8 by using sodium hydroxide.
To further illustrate the high tack high bond strength tile backsize emulsion and method of making the same provided by the present invention, the following examples are provided:
example 1:
the ceramic tile back glue emulsion with high initial adhesion and high bonding strength comprises the following components in parts by weight:
100 parts of deionized water; 1 part of tridecyl methacrylate; 105 parts of butyl acrylate; 9.9 parts of 2-ethylhexyl acrylate; 1.2 parts of acrylic acid; 2.4 parts of hydroxyethyl acrylate; 0.3 part of vinyl trimethoxy silane; 0.2 part of methacrylamide ethyl ethylene urea; 2.3 parts of an emulsifier; 0.5 part of ammonium persulfate; 0.2 part of tert-butyl hydroperoxide; 0.15 part of sodium bisulfite; 0.3 part of sodium hydroxide; 0.5 part of a bactericide; 0.1 part of defoaming agent.
The emulsifier consists of mixed anionic emulsifier and non-ionic emulsifier, and the anionic emulsifier comprises 1.2 parts by weight of sodium dodecyl diphenyl ether disulfonate and 0.8 part by weight of sodium allyloxy hydroxypropyl sulfonate; the nonionic emulsifier comprises 0.3 part by weight of fatty alcohol polyoxyethylene (7) ether.
Further, a preparation method of the ceramic tile back glue emulsion with high initial adhesion and high bonding strength is provided, and comprises the following steps:
adding 0.5 weight part of emulsifier and 33 weight parts of deionized water into a polymerization kettle with a stirrer, a condenser and a constant flow pump heating device to prepare a bottom solution, and raising the temperature in the polymerization kettle to 80 ℃;
adding tridecyl methacrylate, butyl acrylate, 2-ethylhexyl acrylate, acrylic acid, hydroxyethyl acrylate, vinyl trimethoxy silane, methacrylamide ethyl ethylene urea, 1.8 parts by weight of emulsifier and 36 parts by weight of deionized water into a pre-emulsification tank with a monomer metering tank and a stirrer at normal temperature and normal pressure, and stirring and mixing uniformly to prepare a pre-emulsion; stirring the pre-emulsion for 30min for later use;
preparing an initiator solution A: adding 0.2 part of ammonium persulfate and 9 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the ammonium persulfate and the deionized water are completely dissolved for later use;
preparing an initiator solution B: adding 0.4 part of ammonium persulfate and 2 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the ammonium persulfate and the deionized water are completely dissolved for later use;
adding tert-butyl hydroperoxide and 3.5 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the tert-butyl hydroperoxide and the deionized water are completely dissolved for later use;
adding 4 parts of sodium bisulfite and deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the sodium bisulfite and the deionized water are completely dissolved for later use;
when the temperature in the polymerization kettle reaches 80 ℃, adding 4% of the total amount of the pre-emulsion and the initiator solution B into the bottom liquid in the kettle at one time, reacting for 15min, preparing a seed emulsion, then simultaneously dropwise adding the rest pre-emulsion and the initiator solution A into the polymerization kettle through a constant flow pump feeding device and a constant flow dropwise adding metering device, wherein the dropwise adding speed is constant, the dropwise adding time is controlled to be 3h, and the dropwise adding of the initiator solution A is finished 5min later than that of the pre-emulsion;
after the initiator solution A and the pre-emulsion are dripped, controlling the temperature in the polymerization kettle to enable the temperature in the kettle to be at 80 ℃, and preserving the temperature for 1 h; after the heat preservation is finished, reducing the temperature in the polymerization kettle to 70 ℃, and simultaneously dropwise adding tert-butyl hydroperoxide and sodium bisulfite solution into the polymerization kettle for 1 h; after the residual monomer is treated, cooling the temperature in the polymerization kettle to below 50 ℃, and adjusting the pH of the liquid in the kettle to 7-7.5 by using sodium hydroxide; after the pH value is adjusted, adding a defoaming agent, a bactericide and 12.5 parts by weight of deionized water, and stirring the liquid in the kettle for 0.5 h; and after stirring, filtering the liquid in the kettle to obtain the ceramic tile back glue emulsion with high initial adhesion and high bonding strength.
Example 2
The ceramic tile back glue emulsion with high initial adhesion and high bonding strength comprises the following components in parts by weight:
100 parts of deionized water; 4 parts of tridecyl methacrylate; 99 parts of butyl acrylate; 5 parts of 2-ethylhexyl acrylate; 1.0 part of acrylic acid; 2.8 parts of hydroxyethyl acrylate; 0.5 part of vinyl trimethoxy silane; 0.1 part of methacrylamide ethyl ethylene urea; 1 part of an emulsifier; 1.2 parts of ammonium persulfate; 0.1 part of tert-butyl hydroperoxide; 0.1 part of sodium bisulfite; 0.1 part of sodium hydroxide; 1.0 part of a bactericide; 0.05 part of defoaming agent.
The emulsifier consists of mixed anionic emulsifier and non-ionic emulsifier, and the anionic emulsifier comprises 0.6 part by weight of sodium allyloxy hydroxypropyl sulfonate and 0.26 part by weight of sodium tridecyl ether sulfate; the non-ionic emulsifier comprises 0.14 part by weight of isomeric C13 fatty alcohol polyoxyethylene (40) ether.
Further, a preparation method of the ceramic tile back glue emulsion with high initial adhesion and high bonding strength is provided, and comprises the following steps:
adding 0.7 weight part of emulsifier and 32 weight parts of deionized water into a polymerization kettle with a stirrer, a condenser and a constant flow pump heating device to prepare a bottom solution, and raising the temperature in the polymerization kettle to 82 ℃;
adding tridecyl methacrylate, butyl acrylate, 2-ethylhexyl acrylate, acrylic acid, hydroxyethyl acrylate, vinyl trimethoxy silane, methacrylamide ethyl ethylene urea, 0.3 part by weight of emulsifier and 36 parts by weight of deionized water into a pre-emulsification tank with a monomer metering tank and a stirrer at normal temperature and normal pressure, and stirring and mixing uniformly to prepare a pre-emulsion; stirring the pre-emulsion for 30min for later use;
preparing an initiator solution A: adding 0.2 part of ammonium persulfate and 9 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the ammonium persulfate and the deionized water are completely dissolved for later use;
preparing an initiator solution B: adding 0.4 part of ammonium persulfate and 2 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the ammonium persulfate and the deionized water are completely dissolved for later use;
adding tert-butyl hydroperoxide and 3.5 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the tert-butyl hydroperoxide and the deionized water are completely dissolved for later use;
adding 4 parts of sodium bisulfite and deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the sodium bisulfite and the deionized water are completely dissolved for later use;
when the temperature in the polymerization kettle reaches 82 ℃, adding 5 percent of the total amount of the pre-emulsion and the initiator solution B into the bottom liquid in the kettle at one time, reacting for 20min, preparing a seed emulsion, then simultaneously dropwise adding the rest pre-emulsion and the initiator solution A into the polymerization kettle through a constant flow pump feeding device and a constant flow dropwise adding metering device, wherein the dropwise adding speed is constant, the dropwise adding time is controlled to be 3.2h, and the dropwise adding of the initiator solution A is finished 5min later than that of the pre-emulsion;
after the initiator solution A and the pre-emulsion are dripped, controlling the temperature in the polymerization kettle to ensure that the temperature in the kettle is 82 ℃, and preserving the heat for 1.2 hours; after the heat preservation is finished, the temperature in the polymerization kettle is reduced to 72 ℃, and meanwhile, tert-butyl hydroperoxide and sodium bisulfite solution are dripped into the polymerization kettle for 1.2 h; after the residual monomer is treated, cooling the temperature in the polymerization kettle to below 50 ℃, and adjusting the pH of the liquid in the kettle to 7-7.5 by using sodium hydroxide; after the pH value is adjusted, adding a defoaming agent, a bactericide and 13.5 parts by weight of deionized water, and stirring the liquid in the kettle for 0.5 h; and after stirring, filtering the liquid in the kettle to obtain the ceramic tile back glue emulsion with high initial adhesion and high bonding strength.
Example 3
The ceramic tile back glue emulsion with high initial adhesion and high bonding strength comprises the following components in parts by weight:
100 parts of deionized water; 5 parts of tridecyl methacrylate; 95 parts of butyl acrylate; 10 parts of 2-ethylhexyl acrylate; 3.0 parts of acrylic acid; 1.8 parts of hydroxyethyl acrylate; 0.1 part of vinyl trimethoxy silane; 0.5 part of methacrylamide ethyl ethylene urea; 3 parts of an emulsifier; 2.0 parts of sodium persulfate; 0.5 part of tert-butyl hydroperoxide; 0.4 part of sodium bisulfite; 1 part of sodium hydroxide; 0.4 part of a bactericide; 0.2 part of defoaming agent.
The emulsifier consists of mixed anionic emulsifier and non-ionic emulsifier, and the anionic emulsifier comprises 2 parts by weight of sodium dodecyl diphenyl ether disulfonate and 0.5 part by weight of allyloxy hydroxypropyl sodium sulfonate; the nonionic emulsifier comprises 0.5 part by weight of fatty alcohol polyoxyethylene (7) ether.
Further, a preparation method of the ceramic tile back glue emulsion with high initial adhesion and high bonding strength is provided, and comprises the following steps:
adding 0.8 weight part of emulsifier and 34 weight parts of deionized water into a polymerization kettle with a stirrer, a condenser and a constant flow pump heating device to prepare a bottom solution, and raising the temperature in the polymerization kettle to 83 ℃;
adding tridecyl methacrylate, butyl acrylate, 2-ethylhexyl acrylate, acrylic acid, hydroxyethyl acrylate, vinyl trimethoxy silane, methacrylamide ethyl ethylene urea, 2.2 parts by weight of emulsifier and 35 parts by weight of deionized water into a pre-emulsification tank with a monomer metering tank and a stirrer at normal temperature and normal pressure, and stirring and mixing uniformly to prepare a pre-emulsion; stirring the pre-emulsion for 40min for later use;
preparing an initiator solution A: adding 0.16 part of sodium persulfate and 9 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the sodium persulfate and the deionized water are completely dissolved for later use;
preparing an initiator solution B: adding 0.36 part of sodium persulfate and 2 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the sodium persulfate and the deionized water are completely dissolved for later use;
adding tert-butyl hydroperoxide and 3.5 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the tert-butyl hydroperoxide and the deionized water are completely dissolved for later use;
adding 4 parts of sodium bisulfite and deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the sodium bisulfite and the deionized water are completely dissolved for later use;
when the temperature in the polymerization kettle reaches 83 ℃, adding 7% of the total amount of the pre-emulsion and the initiator solution B into the bottom liquid in the kettle at one time, reacting for 25min, preparing a seed emulsion, then simultaneously dropwise adding the rest pre-emulsion and the initiator solution A into the polymerization kettle through a constant flow pump feeding device and a constant flow dropwise adding metering device, wherein the dropwise adding speed is constant, the dropwise adding time is controlled to be 3.5h, and the dropwise adding of the initiator solution A is finished 10min later than that of the pre-emulsion;
after the initiator solution A and the pre-emulsion are dripped, controlling the temperature in the polymerization kettle to enable the temperature in the kettle to be 83 ℃, and preserving the heat for 1.5 hours; after the heat preservation is finished, the temperature in the polymerization kettle is reduced to 75 ℃, and meanwhile, tert-butyl hydroperoxide and sodium bisulfite solution are dripped into the polymerization kettle for 1.5 h; after the residual monomer is treated, cooling the temperature in the polymerization kettle to below 50 ℃, and adjusting the pH of the liquid in the kettle to 7.5-8 by using sodium hydroxide; after the pH value is adjusted, adding a defoaming agent, a bactericide and 12.5 parts by weight of deionized water, and stirring the liquid in the kettle for 0.5 h; and after stirring, filtering the liquid in the kettle to obtain the ceramic tile back glue emulsion with high initial adhesion and high bonding strength.
The high initial adhesion and high bonding strength ceramic tile back adhesive emulsion prepared in the examples 1 to 3 and the commercially available ceramic tile back adhesive competitive products were respectively tested according to the GB/T4852-2002 pressure-sensitive adhesive tape initial adhesion test method (ball rolling method) standard and the JC/T547-2017 ceramic tile adhesive standard, and the test results are shown in the following tables.
From the test results in the table above, it can be seen that the tile back glue emulsions obtained in examples 1 to 3 have excellent initial adhesion performance, the initial adhesion ball number test is not less than 29 ball numbers, the distance between 14 ball number balls is not more than 1.6cm, and the adhesion strength is as follows: the tensile bonding strength is more than or equal to 0.9 MPa; the tensile bonding strength after soaking is more than or equal to 0.75 MPa; the tensile bonding strength after thermal aging is more than or equal to 1.0 MPa; the tensile bonding strength after freeze-thaw cycling is more than or equal to 0.83 MPa; the airing time is more than or equal to 20min, and the tensile bonding strength is more than or equal to 0.82 MPa. The ceramic tile back glue emulsion has excellent initial viscosity and high bonding strength. The initial adhesive performance and the adhesive strength of the commercially available tile back adhesive product cannot be simultaneously guaranteed, the adhesive strength is poor when the initial adhesive performance is good, and the initial adhesive performance is poor when the adhesive strength is high.
It should be understood that equivalents and modifications of the technical solution and inventive concept thereof may occur to those skilled in the art, and all such modifications and alterations should fall within the scope of the appended claims.
Claims (8)
1. The ceramic tile back glue emulsion with high initial adhesion and high bonding strength is characterized by comprising the following raw materials in parts by weight:
2. the ceramic tile gum emulsion with high initial adhesion and high strength as claimed in claim 1, wherein the raw materials further comprise the following components in parts by weight:
0.1-0.5 part of tert-butyl hydroperoxide;
0.1 to 0.4 portion of sodium bisulfite.
3. The high tack high strength tile backsize emulsion of claim 1, wherein said emulsifier comprises an anionic emulsifier and a nonionic emulsifier; the ratio of the anionic emulsifier to the nonionic emulsifier is 1-6:1 in parts by weight.
4. The high tack high strength tile backsize emulsion of claim 3, wherein the anionic emulsifier is one or more of sodium dodecyl diphenyl ether disulfonate, sodium allyloxy hydroxypropyl sulfonate, sodium tridecyl ether sulfate.
5. The high tack high strength tile backsize emulsion of claim 3, wherein said non-ionic emulsifier is one or both of fatty alcohol polyoxyethylene (7) ether, isomeric C13 fatty alcohol polyoxyethylene (40) ether.
6. The high tack high strength tile backsize emulsion of claim 1, wherein the initiator is one or both of ammonium persulfate and sodium persulfate.
7. A method for preparing the high initial adhesion and high strength tile backsize emulsion as claimed in any one of claims 1 to 6, which comprises the following steps:
adding 0.4-0.8 weight part of emulsifier and 30.5-34 weight parts of deionized water into a polymerization kettle with a stirrer, a condenser and a constant flow pump heating device to prepare a base solution, and raising the temperature in the polymerization kettle to 80-83 ℃;
adding tridecyl methacrylate, butyl acrylate, 2-ethylhexyl acrylate, acrylic acid, hydroxyethyl acrylate, vinyl trimethoxy silane, methacrylamide ethyl ethylene urea, 0.6-2.2 parts by weight of emulsifier and 34-39 parts by weight of deionized water into a pre-emulsification tank with a monomer metering tank and a stirrer at normal temperature and normal pressure, and stirring and mixing uniformly to prepare a pre-emulsion;
preparing an initiator solution A: adding 0.1-0.8 part of initiator and 8-15 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the initiator and the deionized water are completely dissolved for later use;
preparing an initiator solution B: adding 0.4-1.2 parts of initiator and 2 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the initiator and the deionized water are completely dissolved for later use;
fifthly, when the temperature in the polymerization kettle reaches 80-83 ℃, adding 4-7 percent of the total amount of the pre-emulsion and the initiator solution B into the bottom liquid in the kettle at one time, reacting for 15-25min, preparing a seed emulsion, then simultaneously dropwise adding the rest pre-emulsion and the initiator solution A into the polymerization kettle through a constant flow pump feeding device and a constant current dropwise adding metering device, wherein the dropwise adding speed is constant, the dropwise adding time is controlled to be 3-3.5h, and the dropwise adding of the initiator solution A is finished 5-10min later than that of the pre-emulsion;
sixthly, after the initiator solution A and the pre-emulsion are dripped, controlling the temperature in the polymerization kettle to be 80-83 ℃, and keeping the temperature for 1-1.5 h; after the heat preservation is finished, reducing the temperature in the polymerization kettle to be below 50 ℃, and adjusting the pH of the liquid in the kettle to 7-8 by using sodium hydroxide; after pH is adjusted, adding a defoaming agent, a bactericide and 2.5-18 parts by weight of deionized water, and stirring the liquid in the kettle for 0.5-1 h; and after stirring, filtering the liquid in the kettle to obtain the ceramic tile back glue emulsion with high initial adhesion and high bonding strength.
8. The preparation method of the ceramic tile back glue emulsion with high initial adhesion and high strength as claimed in claim 7, characterized by further comprising the following steps:
adding 0.1-0.5 part of tert-butyl hydroperoxide and 3.5 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the tert-butyl hydroperoxide and the deionized water are completely dissolved for later use;
adding 0.1-0.4 part of sodium bisulfite and 4 parts of deionized water into an initiator tank with a stirrer and a constant-current dropping device at normal temperature and normal pressure, and stirring until the sodium bisulfite and the deionized water are completely dissolved for later use;
thirdly, keeping the temperature in the polymerization kettle at 80-83 ℃ and keeping the temperature for 1-1.5h, then cooling the temperature in the polymerization kettle to 70-75 ℃, and simultaneously dropwise adding a tert-butyl hydroperoxide solution and a sodium bisulfite solution into the polymerization kettle, wherein the dropwise adding time is controlled to be 1-1.5 h; after the dropwise addition is finished, the temperature in the polymerization kettle is reduced to below 50 ℃, and the pH of the liquid in the kettle is adjusted to 7-8 by using sodium hydroxide.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114133482A (en) * | 2021-11-08 | 2022-03-04 | 广东华盛银洋环保新材料有限公司 | Emulsion for ceramic tile back glue, preparation method thereof and double-component ceramic tile back glue |
| CN114591462A (en) * | 2022-03-09 | 2022-06-07 | 广东巴德富新材料有限公司 | Hydrophobic high-strength high-viscosity composite ceramic tile back glue and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106590477A (en) * | 2016-11-18 | 2017-04-26 | 佛山市顺德区巴德富实业有限公司 | Acrylate tile back glue emulsion and preparation method thereof |
| CN111394023A (en) * | 2020-04-01 | 2020-07-10 | 上海保立佳新材料有限公司 | Water-whitening-resistant acrylate pressure-sensitive adhesive and preparation method thereof |
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2020
- 2020-12-31 CN CN202011632554.5A patent/CN112778450A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106590477A (en) * | 2016-11-18 | 2017-04-26 | 佛山市顺德区巴德富实业有限公司 | Acrylate tile back glue emulsion and preparation method thereof |
| CN111394023A (en) * | 2020-04-01 | 2020-07-10 | 上海保立佳新材料有限公司 | Water-whitening-resistant acrylate pressure-sensitive adhesive and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114133482A (en) * | 2021-11-08 | 2022-03-04 | 广东华盛银洋环保新材料有限公司 | Emulsion for ceramic tile back glue, preparation method thereof and double-component ceramic tile back glue |
| CN114591462A (en) * | 2022-03-09 | 2022-06-07 | 广东巴德富新材料有限公司 | Hydrophobic high-strength high-viscosity composite ceramic tile back glue and preparation method thereof |
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