CN108707441B - Waterproof corrosion-resistant binder and preparation method thereof - Google Patents

Waterproof corrosion-resistant binder and preparation method thereof Download PDF

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CN108707441B
CN108707441B CN201810650552.5A CN201810650552A CN108707441B CN 108707441 B CN108707441 B CN 108707441B CN 201810650552 A CN201810650552 A CN 201810650552A CN 108707441 B CN108707441 B CN 108707441B
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agent
corrosion
mixture
waterproof
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CN108707441A (en
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李靖靖
孙浩冉
郭林
谢光辉
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Zhengzhou Institute of Technology
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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
    • C09J133/00—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 at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • 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
    • 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
    • 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
    • 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
    • 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
    • C08K2003/2262—Oxides; Hydroxides of metals of manganese
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Sealing Material Composition (AREA)

Abstract

The invention provides a waterproof corrosion-resistant binder, which belongs to the technical field of binders and is prepared from the following raw materials in parts by weight: 40-48 parts of trichloropropane, 25-30 parts of modified acrylic resin, 7-10 parts of a waterproof agent, 12-16 parts of a corrosion resistant agent, 5-8 parts of a filler and 6-8 parts of an auxiliary agent. The invention modifies acrylic resin, has obvious synergistic effect with a waterproof agent, a corrosion-resistant agent, a filler and an auxiliary agent, organically combines various materials to prepare the binder for the ceramic material, can improve the corrosion resistance and the water resistance of the material, has good mechanical property and aging resistance, has excellent comprehensive performance, meets the bonding requirements of the ceramic materials such as glass, ceramic tiles and the like, has good bonding property, and can be used for a long time under the severe environment condition.

Description

Waterproof corrosion-resistant binder and preparation method thereof
Technical Field
The invention relates to the technical field of binders, in particular to a waterproof and corrosion-resistant binder and a preparation method thereof.
Background
Ceramic materials such as glass, ceramic tiles and the like are often used by bonding a plurality of pieces of glass or ceramic tiles together under many conditions, so the using effect of a later product is greatly influenced by the performance of the bonding agent, and the ceramic products are not well bonded firmly, so that unnecessary problems are brought to the later use, and the normal production life is seriously influenced. Moreover, the ceramic material needs to have waterproof and corrosion-resistant effects in the using process, and the traditional adhesive is easy to have the defects of aging, cracking, deformation and the like after being corroded by water or acid and alkali. Therefore, it is of great significance to provide an adhesive which has good adhesive property, can bond ceramic materials well and has good waterproof and corrosion-resistant effects.
Patent document with publication number CN105950062A discloses a high-efficiency waterproof adhesive and a preparation method thereof, wherein the adhesive comprises the following raw materials in parts by weight: 50-70 parts of natural latex, 35-55 parts of phenolic resin, 10-15 parts of glass fiber, 4-5 parts of sodium laurate, 30-40 parts of wollastonite powder, 6-8 parts of nano zinc oxide, 5-10 parts of sawdust powder, 5-4 parts of anti-aging agent RD2, 10101-3 parts of antioxidant, 2-4 parts of triethyl citrate, 3-4 parts of acrylic acid, 1-2 parts of fatty acid amide and 600-800 parts of deionized water. The adhesive has stable performance, is prepared by compounding various organic and inorganic materials, has certain waterproof, thermal stability, corrosion resistance and ageing resistance, but in practical application, the invention has poor corrosion resistance, ageing resistance and alkali resistance, can have the defects of ageing, dry cracking and the like after being used for a period of time, and has short service life.
Patent No. CN101798494B discloses a normal temperature curing epoxy waterproof adhesive for bridge deck. The adhesive is prepared by mixing a mixture of a group A and a group B according to the weight ratio of 2: 1 at normal temperature, wherein the mixture of the group A comprises the following components in parts by weight: 80-100 parts of epoxy resin, 10-18 parts of toughening agent and 5-7 parts of epoxy active diluent, wherein the components are mixed at normal temperature to form a group A mixture; the component B comprises the following components in parts by weight: 40-50 parts of curing agent, 1-2 parts of trimerization catalyst and 1-2 parts of organic siloxane coupling agent KH-550, and the components are mixed at normal temperature to form a group B mixture. The waterproof adhesive has super strong adhesive capacity, stable performance in the temperature variation range of the bridge deck, good high-temperature flow resistance, compact and waterproof structure and certain deformation resistance. However, when the adhesive is used for bonding ceramic materials, the comprehensive performance is poor, the waterproof effect is not ideal, the corrosion resistance is poor, the tensile strength needs to be improved, and the use requirement of the bonded ceramic materials cannot be met.
Disclosure of Invention
In view of the above, the invention provides a waterproof and corrosion-resistant adhesive for ceramic materials, which has good mechanical properties, is waterproof and corrosion-resistant, and a preparation method thereof.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the waterproof corrosion-resistant binder is prepared from the following raw materials in parts by weight: 40-48 parts of trichloropropane, 25-30 parts of modified acrylic resin, 7-10 parts of a waterproof agent, 12-16 parts of a corrosion resistant agent, 5-8 parts of a filler and 6-8 parts of an auxiliary agent.
Preferably, the modified acrylic resin is prepared from the following components in parts by weight: 60-65 parts of acrylic resin, 1.5-2.2 parts of silane coupling agent, 1.8-2.6 parts of zinc oxide, 18-21 parts of polyvinyl acetate, 9-13 parts of polyvinylidene fluoride and 20-24 parts of tetrahydrofuran.
Preferably, the waterproof agent is a mixture of sodium methylsiliconate and zinc stearate, and the weight ratio of sodium methylsiliconate: the ratio of zinc stearate is 5-7: 1.
Preferably, the corrosion resistant agent is one or two of sodium chromate and cinnamaldehyde.
Preferably, the corrosion resistant agent is a mixture of sodium chromate and cinnamaldehyde, and the weight ratio of sodium chromate: the cinnamaldehyde accounts for 1: 3-4.
Preferably, the filler is: the mixture of the vermiculite powder, the manganese oxide and the titanium dioxide comprises the following components in percentage by weight: manganese sesquioxide: the ratio of titanium dioxide is 1:2.5-3.5: 4-6.
Preferably, the auxiliary agent is a mixture of dimethyl tetrachloroterephthalate, polyoxyethylene nonyl phenyl ether and p-toluenesulfonic acid, and the weight ratio of dimethyl tetrachloroterephthalate: polyoxyethylene nonyl phenyl ether: the ratio of p-toluenesulfonic acid is 1:5-6: 3.5-5.
Preferably, the auxiliary agent is a mixture of dimethyl tetrachloroterephthalate, polyoxyethylene nonyl phenyl ether and p-toluenesulfonic acid, and the weight ratio of dimethyl tetrachloroterephthalate: polyoxyethylene nonyl phenyl ether: the ratio of p-toluenesulfonic acid was 1:5.5: 4.
Preferably, the preparation method of the modified acrylic resin comprises the following steps: mixing acrylic resin and tetrahydrofuran, and then placing the mixture in a magnetic stirrer to stir for 10-20min at the temperature of 20-25 ℃, wherein the rotating speed is 200-300 r/min; keeping the rotating speed unchanged, adding a silane coupling agent and zinc oxide, and continuously stirring for 30-40 min; adding polyvinyl acetate and polyvinylidene fluoride, adjusting the rotating speed to be 500-ion 600r/min, stirring for 1-1.5h, and then putting into an ultrasonic oscillator with the frequency of 30kHz, the power of 500W and the oscillation time of 45-60 mim.
Preferably, the preparation method of the waterproof and corrosion-resistant adhesive comprises the following steps:
s1: mixing the modified acrylic resin and trichloropropane, and then placing the mixture in a reaction kettle, stirring the mixture for 10 to 20min at the normal temperature of between 20 and 25 ℃, wherein the rotating speed is 400-;
s2: raising the temperature of the reaction kettle in the step S1 to 60-80 ℃, adding a waterproof agent and an anticorrosive agent, adjusting the rotation speed to 200-;
s3: adding the filler and the auxiliary agent into the mixture I obtained in the step S2, placing the mixture in a magnetic stirrer, and stirring for 40-50min at the rotating speed of 600-800r/min to obtain a mixture II;
s4: and refluxing the mixture II obtained in the step S3 at the temperature of 160-165 ℃ for 10-12 h.
The invention has the beneficial effects that: the invention takes modified acrylic resin as main material and trichloropropane as organic solvent to be mixed with the modified acrylic resin. The modified acrylic resin is prepared by adding silane coupling agent, zinc oxide, polyvinyl acetate and polyvinylidene fluoride into acrylic resin by taking tetrahydrofuran as an organic solvent.
Silane coupling agent is combined with zinc oxide to connect organic functional group to the surface of zinc oxide, so as to raise its compatibility and dispersibility with organic matter. The zinc oxide not only has good antibacterial performance, but also can improve the corrosion resistance of the binder. The polyvinyl acetate enhances the adhesive force, and the polyvinylidene fluoride improves the impact strength and toughness of the adhesive and enhances the wear resistance. The modified acrylic resin has better adhesive force and mechanical property.
The waterproof agent improves the waterproof performance of the adhesive, has long waterproof life, resists corrosion and acid and alkali, enhances the aging resistance of the adhesive, and ensures that the crystal phase structure of the adhesive is not easy to damage. The filler reduces the adverse effects of volume shrinkage, loose bonding layer structure, weak bonding strength of bonding interface and the like caused by pyrolysis weight loss of the organic matrix, and improves the performance of the bonding agent.
The auxiliary agent is a mixture of dimethyl tetrachloroterephthalate, nonylphenol polyoxyethylene ether and p-toluenesulfonic acid, the dimethyl tetrachloroterephthalate improves the heat resistance of the adhesive, the nonylphenol polyoxyethylene ether improves the surface activity and the wettability of the adhesive, the p-toluenesulfonic acid has a curing effect, and the surface drying time of the adhesive is further shortened.
According to the invention, the acrylic resin is modified, and has a remarkable synergistic effect with a waterproof agent, a corrosion-resistant agent, a filler and an auxiliary agent, various materials are organically combined, and the synergistic effect of each component is exerted, so that the adhesive for the ceramic material is prepared, the corrosion resistance and the water resistance of the material can be improved, the mechanical property and the aging resistance are good, the comprehensive performance is excellent, the bonding requirements of the ceramic materials such as glass, ceramic tiles and the like are met, the adhesion is good, and the adhesive can be used for a long time under the severe environment condition.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention are clearly and completely described below. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention, are within the scope of the invention.
Example 1
The embodiment provides a waterproof and corrosion-resistant binder which is prepared from the following raw materials in parts by weight: 40 parts of trichloropropane, 25 parts of modified acrylic resin, 7 parts of a waterproof agent, 12 parts of a corrosion resistant agent, 5 parts of a filler and 6 parts of an auxiliary agent.
The modified acrylic resin is prepared from the following components in parts by weight: 60 parts of acrylic resin, 1.5 parts of silane coupling agent, 1.8 parts of zinc oxide, 18 parts of polyvinyl acetate, 9 parts of polyvinylidene fluoride and 20 parts of tetrahydrofuran.
The waterproof agent is a mixture of sodium methyl silanol and zinc stearate, and the weight ratio of the sodium methyl silanol to the zinc stearate is as follows: the zinc stearate is 5: 1.
The corrosion resistant agent is sodium chromate.
The filler is a mixture of vermiculite powder, manganese oxide and titanium dioxide, and the weight ratio of the vermiculite powder to the filler is as follows: manganese sesquioxide: the ratio of titanium dioxide is 1:2.5: 4.
The auxiliary agent is a mixture of dimethyl tetrachloroterephthalate, nonylphenol polyoxyethylene ether and p-toluenesulfonic acid, and the weight ratio of dimethyl tetrachloroterephthalate: polyoxyethylene nonyl phenyl ether: the ratio of p-toluenesulfonic acid is 1:5: 3.5.
The preparation method of the modified acrylic resin comprises the following steps: mixing acrylic resin and tetrahydrofuran, and then placing the mixture in a magnetic stirrer to stir at 20-25 ℃ for 10min at the rotating speed of 300 r/min; keeping the rotating speed unchanged, adding a silane coupling agent and zinc oxide, and continuously stirring for 30 min; adding polyvinyl acetate and polyvinylidene fluoride, adjusting the rotating speed to 600r/min, stirring for 1h, and then putting into an ultrasonic oscillator, wherein the frequency is 30kHz, the power is 500W, and the oscillation time is 45 mm.
The preparation method of the waterproof and corrosion-resistant binder comprises the following steps:
s1: mixing the modified acrylic resin and trichloropropane, placing the mixture in a reaction kettle, stirring the mixture for 10min at the normal temperature of 20-25 ℃, and the rotating speed of 500 r/min;
s2: raising the temperature of the reaction kettle in the step S1 to 60-80 ℃, adding a waterproof agent and a corrosion resistant agent, adjusting the rotation speed to 300r/min, and stirring for 30min to obtain a first mixture;
s3: adding the filler and the auxiliary agent into the mixture I obtained in the step S2, placing the mixture in a magnetic stirrer, and stirring for 40min at the rotating speed of 800r/min to obtain a mixture II;
s4: and refluxing the mixture II obtained in the step S3 at the temperature of 160-165 ℃ for 10 h.
Example 2
The embodiment provides a waterproof and corrosion-resistant binder, which comprises the same raw materials and parts by weight as those in embodiment 1, and is different from embodiment 1 in that the corrosion-resistant agent adopted in the embodiment is cinnamaldehyde, and the modified acrylic resin comprises the same raw materials and parts by weight as those in embodiment 1.
The preparation method of the modified acrylic resin comprises the following steps: mixing acrylic resin and tetrahydrofuran, and then placing the mixture in a magnetic stirrer to stir at 20-25 ℃ for 20min, wherein the rotating speed is 200 r/min; keeping the rotating speed unchanged, adding a silane coupling agent and zinc oxide, and continuously stirring for 40 min; adding polyvinyl acetate and polyvinylidene fluoride, adjusting the rotating speed to be 500r/min, stirring for 1.5h, and then putting into an ultrasonic oscillator, wherein the frequency is 30kHz, the power is 500W, and the oscillation time is 45 mm.
The preparation method of the waterproof and corrosion-resistant binder comprises the following steps:
s1: mixing the modified acrylic resin and trichloropropane, placing the mixture in a reaction kettle, stirring the mixture for 10min at the normal temperature of 20-25 ℃, and the rotating speed of 500 r/min;
s2: raising the temperature of the reaction kettle in the step S1 to 60-80 ℃, adding a waterproof agent and a corrosion resistant agent, adjusting the rotation speed to 200r/min, and stirring for 40min to obtain a first mixture;
s3: adding the filler and the auxiliary agent into the mixture I obtained in the step S2, placing the mixture in a magnetic stirrer, and stirring for 50min at the rotating speed of 600r/min to obtain a mixture II;
s4: and refluxing the mixture II obtained in the step S3 at the temperature of between 160 ℃ and 165 ℃ for 12 h.
Example 3
The embodiment provides a waterproof and corrosion-resistant binder which is prepared from the following raw materials in parts by weight: 43 parts of trichloropropane, 26 parts of modified acrylic resin, 8 parts of a waterproof agent, 13 parts of a corrosion resistant agent, 6 parts of a filler and 7 parts of an auxiliary agent.
The components and parts by weight of the modified acrylic resin are the same as those in example 1.
The waterproof agent is a mixture of sodium methylsilanolate and zinc stearate, and the weight ratio of sodium methylsilanolate to zinc stearate is as follows: the zinc stearate is 5: 1.
The corrosion resistant agent is as follows: sodium chromate.
The filler is as follows: the mixture of the vermiculite powder, the manganese oxide and the titanium dioxide comprises the following components in percentage by weight: manganese sesquioxide: the ratio of titanium dioxide is 1:2.5: 6.
The auxiliary agent is: the mixture of tetrachloro terephthalic acid dimethyl ester, nonyl phenol polyethenoxy ether and p-toluenesulfonic acid, the weight ratio of tetrachloro terephthalic acid dimethyl ester: polyoxyethylene nonyl phenyl ether: the ratio of p-toluenesulfonic acid is 1:5: 4.
The preparation method of the modified acrylic resin comprises the following steps: mixing acrylic resin and tetrahydrofuran, and then placing the mixture in a magnetic stirrer to stir for 15min at the normal temperature of 20-25 ℃ at the rotating speed of 300 r/min; keeping the rotating speed unchanged, adding a silane coupling agent and zinc oxide, and continuously stirring for 40 min; adding polyvinyl acetate and polyvinylidene fluoride, adjusting the rotating speed to be 500r/min, stirring for 1.5h, and then putting into an ultrasonic oscillator, wherein the frequency is 30kHz, the power is 500W, and the oscillation time is 50 mim.
The preparation method of the waterproof and corrosion-resistant binder comprises the following steps:
s1: mixing the modified acrylic resin and trichloropropane, placing the mixture in a reaction kettle, stirring the mixture for 15min at the normal temperature of 20-25 ℃, and the rotating speed of 500 r/min;
s2: raising the temperature of the reaction kettle in the step S1 to 60-80 ℃, adding a waterproof agent and a corrosion resistant agent, adjusting the rotation speed to 300r/min, and stirring for 35min to obtain a first mixture;
s3: adding the filler and the auxiliary agent into the mixture I obtained in the step S2, placing the mixture in a magnetic stirrer, and stirring for 45min at the rotating speed of 700r/min to obtain a mixture II;
s4: and refluxing the mixture II obtained in the step S3 at the temperature of between 160 ℃ and 165 ℃ for 11 h.
Example 4
The embodiment provides a waterproof and corrosion-resistant binder, which comprises the same raw materials and weight parts as those in embodiment 3, and is different from embodiment 3 in that cinnamaldehyde is used as a corrosion-resistant agent.
The modified acrylic resin is prepared from the following components in parts by weight: 63 parts of acrylic resin, 2 parts of silane coupling agent, 2 parts of zinc oxide, 20 parts of polyvinyl acetate, 11 parts of polyvinylidene fluoride and 22 parts of tetrahydrofuran.
The preparation method of the modified acrylic resin is the same as that in example 3, and the preparation method of the waterproof and corrosion-resistant adhesive is the same as that in example 3.
Example 5
The waterproof corrosion-resistant binder is prepared from the following raw materials in parts by weight: 45 parts of trichloropropane, 28 parts of modified acrylic resin, 9 parts of a waterproof agent, 15 parts of a corrosion resistant agent, 7 parts of a filler and 7 parts of an auxiliary agent.
The components and parts by weight of the modified acrylic resin are the same as those in example 4.
The waterproof agent is a mixture of sodium methyl silanol and zinc stearate, and the weight ratio of the sodium methyl silanol to the zinc stearate is as follows: the zinc stearate is 6: 1.
The corrosion resistant agent is as follows: sodium chromate, cinnamaldehyde, sodium chromate: the cinnamaldehyde is 1: 4.
The filler is as follows: the mixture of the vermiculite powder, the manganese oxide and the titanium dioxide comprises the following components in percentage by weight: manganese sesquioxide: the ratio of titanium dioxide is 1:3: 5.
The auxiliary agent is: the mixture of tetrachloro terephthalic acid dimethyl ester, nonyl phenol polyethenoxy ether and p-toluenesulfonic acid, the weight ratio of tetrachloro terephthalic acid dimethyl ester: polyoxyethylene nonyl phenyl ether: the ratio of p-toluenesulfonic acid was 1:5.5: 4.
The preparation method of the modified acrylic resin is the same as that in example 3, and the preparation method of the waterproof and corrosion-resistant adhesive is the same as that in example 3.
Example 6
The embodiment provides a waterproof and corrosion-resistant binder, which comprises the same raw materials and weight parts as those in embodiment 5, and is different from embodiment 5 in that the waterproof agent adopted in the embodiment is a mixture of sodium methylsiliconate and zinc stearate, and the weight ratio of sodium methylsiliconate: zinc stearate is 7: 1; the corrosion resistant agent is: sodium chromate, cinnamaldehyde, sodium chromate: the cinnamaldehyde is 1:3. The auxiliary agent is: the mixture of dimethyl tetrachloroterephthalate, polyoxyethylene nonyl phenyl ether, p-toluenesulfonic acid and sodium benzoate, wherein the weight ratio of dimethyl tetrachloroterephthalate: polyoxyethylene nonyl phenyl ether: p-toluenesulfonic acid: sodium benzoate is 1:5.5: 4: 0.8.
the preparation method of the modified acrylic resin is the same as that in example 1, and the preparation method of the waterproof and corrosion-resistant adhesive is the same as that in example 1.
Example 7
The waterproof corrosion-resistant binder is prepared from the following raw materials in parts by weight: 48 parts of trichloropropane, 30 parts of modified acrylic resin, 10 parts of a waterproof agent, 16 parts of a corrosion resistant agent, 8 parts of a filler and 8 parts of an auxiliary agent.
The components and parts by weight of the modified acrylic resin are the same as those in example 1.
The waterproof agent is a mixture of sodium methyl silanol and zinc stearate, and the weight ratio of the sodium methyl silanol to the zinc stearate is as follows: the zinc stearate is 6: 1.
The corrosion resistant agent is as follows: sodium chromate, cinnamaldehyde, sodium chromate: the cinnamaldehyde is 1: 4.
The filler is as follows: the mixture of the vermiculite powder, the manganese oxide and the titanium dioxide comprises the following components in percentage by weight: manganese sesquioxide: the ratio of titanium dioxide is 1:3.5: 6.
The auxiliary agent is: the mixture of tetrachloro terephthalic acid dimethyl ester, nonyl phenol polyethenoxy ether and p-toluenesulfonic acid, the weight ratio of tetrachloro terephthalic acid dimethyl ester: polyoxyethylene nonyl phenyl ether: the ratio of p-toluenesulfonic acid is 1:6: 5.
The preparation method of the modified acrylic resin is the same as that of the embodiment 2, and the preparation method of the waterproof and corrosion-resistant adhesive is the same as that of the embodiment 2.
Example 8
The embodiment provides a waterproof and corrosion-resistant binder, which comprises the following raw materials in parts by weight as in embodiment 7, and is different from embodiment 7 in that the modified acrylic resin is prepared from the following components in parts by weight: 65 parts of acrylic resin, 2.2 parts of silane coupling agent, 2.6 parts of zinc oxide, 21 parts of polyvinyl acetate, 13 parts of polyvinylidene fluoride and 24 parts of tetrahydrofuran.
The preparation method of the modified acrylic resin is the same as that in example 3, and the preparation method of the waterproof and corrosion-resistant adhesive is the same as that in example 3.
Comparative example 1
This comparative example provides a waterproof and corrosion-resistant adhesive, similar to example 1, but different from example 1, in which a waterproofing agent and a filler are not added.
Comparative example 2
This comparative example provides a waterproof and corrosion-resistant adhesive, similar to example 2, but different from example 2, in which no corrosion-resistant agent and no auxiliary agent are added.
Comparative example 3
This comparative example provides a waterproof and corrosion-resistant adhesive, similar to example 5, but different from example 5, in which no acrylic resin was modified.
Comparative example 4
This comparative example provides a waterproof and corrosion-resistant adhesive, which is prepared by the same method as in example 3, but is different from example 3 in that step S4 is omitted.
Tensile strength of original adhesive, tensile strength of adhesive after soaking, tensile strength of original adhesive after thermal aging and shrinkage test: see JC/T547-2005.
Water resistance test
And (3) taking 30g of the adhesive in a glass culture dish, and naturally drying to prepare the film. The water resistance of the film was characterized by the water absorption, the film was cut into square test specimens of 15mm × 15mm, and the mass of the test specimens was weighed (to the nearest 0.001 g). Placing the membrane into a culture dish filled with distilled water, soaking the membrane on the upper surface of the membrane for 24h at room temperature, and taking out the membrane. The surface of the film was gently wiped off with filter paper and immediately weighed. The water absorption of the film was calculated according to equation 1-1, and each sample was tested 3 times and averaged.
W=(m1-m0)/m0×100% （1-1）
In the formula, the water absorption of the W-film,%;
m0-initial mass of the sample, g;
m1mass after water absorption of the sample, g.
Corrosion resistance test
Taking three clean beakers, respectively preparing 10% hydrochloric acid and 10% NaOH solutions, respectively soaking the adhesive sample in the two prepared solutions, keeping a sealed environment for 45 days, and taking out the adhesive sample to observe the corrosion condition of the surface of the film.
TABLE 1 test results of examples and comparative examples
Figure DEST_PATH_IMAGE002
As can be seen from table 1: examples 1 to 8 all show excellent tensile adhesive strength, and good water resistance and chemical corrosion resistance, which show that the adhesive has a reasonable formula and good process adaptability, the viscosity is between 2 Pa.s and 4Pa.s at normal temperature, and the acid-base resistance and the aging resistance of the adhesive are enhanced by adding sodium benzoate in example 6. Compared with the example 1, the comparative example 1 lacks the waterproof agent and the filler, the water resistance of the adhesive and the tensile adhesive strength after soaking are the worst, and the shrinkage rate is the largest, which shows that the filler and the waterproof agent have important influence on the waterproof performance and the shrinkage rate of the adhesive; comparative example 2 compared with example 2, the corrosion resisting agent and the auxiliary agent are absent, and the tensile adhesive strength and the corrosion resisting property of the corrosion resisting agent and the auxiliary agent are obviously reduced, which shows that the corrosion resisting agent and the auxiliary agent can improve the corrosion resisting property and the mechanical property of the adhesive; compared with the embodiment 5, the acrylic resin is not modified, all the performances of the adhesive are obviously reduced, particularly the tensile bond strength is the worst, and the modified acrylic resin can obviously improve the comprehensive performance of the adhesive; compared with the embodiment 3, the preparation process of the adhesive has no backflow, and the comprehensive performance of the adhesive is poor, which shows that the backflow can effectively improve the intermiscibility of the components and improve the purity of the adhesive. The raw materials of the invention supplement each other, and the performance of the adhesive can be obviously reduced by changing any one component or process step, which shows that the invention has reasonable formula and good process adaptability.
Finally, the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solutions of the present invention by those of ordinary skill in the art should be covered within the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solutions of the present invention.

Claims (4)

1. A waterproof and corrosion-resistant binder is characterized in that: the feed is prepared from the following raw materials in parts by weight: 40-48 parts of trichloropropane, 25-30 parts of modified acrylic resin, 7-10 parts of a waterproof agent, 12-16 parts of a corrosion resistant agent, 5-8 parts of a filler and 6-8 parts of an auxiliary agent;
the modified acrylic resin is prepared from the following components in parts by weight: 60-65 parts of acrylic resin, 1.5-2.2 parts of silane coupling agent, 1.8-2.6 parts of zinc oxide, 18-21 parts of polyvinyl acetate, 9-13 parts of polyvinylidene fluoride and 20-24 parts of tetrahydrofuran;
the filler is a mixture of vermiculite powder, manganese oxide and titanium dioxide, and the weight ratio of the vermiculite powder to the filler is as follows: manganese sesquioxide: titanium dioxide is 1:2.5-3.5:4-6 parts;
the auxiliary agent is: the mixture of tetrachloro terephthalic acid dimethyl ester, nonyl phenol polyethenoxy ether and p-toluenesulfonic acid, the weight ratio of tetrachloro terephthalic acid dimethyl ester: polyoxyethylene nonyl phenyl ether: p-toluenesulfonic acid 1:5.5: 4;
the preparation method of the modified acrylic resin comprises the following steps: mixing acrylic resin and tetrahydrofuran, and then placing the mixture in a magnetic stirrer to stir for 10-20min at the temperature of 20-25 ℃, wherein the rotating speed is 200-300 r/min; keeping the rotating speed unchanged, adding a silane coupling agent and zinc oxide, and continuously stirring for 30-40 min; adding polyvinyl acetate and polyvinylidene fluoride, adjusting the rotating speed to be 500-ion 600r/min, stirring for 1-1.5h, and then putting into an ultrasonic oscillator with the frequency of 30kHz, the power of 500W and the oscillation time of 45-60 mim;
the preparation method of the waterproof and corrosion-resistant binder comprises the following steps:
s1: mixing the modified acrylic resin and trichloropropane, and then placing the mixture in a reaction kettle, stirring the mixture for 10 to 20min at the normal temperature of between 20 and 25 ℃, wherein the rotating speed is 400-;
s2: raising the temperature of the reaction kettle in the step S1 to 60-80 ℃, adding a waterproof agent and an anticorrosive agent, adjusting the rotation speed to 200-;
s3: adding the filler and the auxiliary agent into the mixture I obtained in the step S2, placing the mixture in a magnetic stirrer, and stirring for 40-50min at the rotating speed of 600-800r/min to obtain a mixture II;
s4: and refluxing the mixture II obtained in the step S3 at the temperature of 160-165 ℃ for 10-12 h.
2. The waterproof, corrosion-resistant adhesive of claim 1, wherein: the waterproof agent is a mixture of sodium methyl silanol and zinc stearate, and the weight ratio of the sodium methyl silanol to the zinc stearate is as follows: the ratio of zinc stearate is 5-7: 1.
3. The waterproof, corrosion-resistant adhesive of claim 1, wherein: the corrosion resistant agent is one or two of sodium chromate and cinnamaldehyde.
4. The waterproof, corrosion-resistant adhesive of claim 3, wherein: the corrosion-resistant agent is a mixture of sodium chromate and cinnamaldehyde, and the weight ratio of the sodium chromate to the cinnamaldehyde is as follows: the cinnamaldehyde accounts for 1: 3-4.
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