CN114958264A - Epoxy joint paste not prone to cracking and preparation method thereof - Google Patents
Epoxy joint paste not prone to cracking and preparation method thereof Download PDFInfo
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- CN114958264A CN114958264A CN202210536598.0A CN202210536598A CN114958264A CN 114958264 A CN114958264 A CN 114958264A CN 202210536598 A CN202210536598 A CN 202210536598A CN 114958264 A CN114958264 A CN 114958264A
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5006—Amines aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/66—Mercaptans
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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
- C09J11/08—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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The application relates to the field of joint paste, in particular to epoxy joint paste not prone to cracking and a preparation method thereof. The epoxy jointing paste not easy to crack comprises the following components in parts by weight of 1.5-2.5: 1, component one and component two; the component one comprises bisphenol F epoxy resin, bisphenol A epoxy resin, hydroxymethyl epoxy resin, trimethylolpropane triglycidyl ether, organic silicon polyether copolymer, asbestos powder, heavy calcium, organic silicon bentonite, gas-phase silicon dioxide, a thixotropic stabilizer, a bulking agent, a toughening agent and an anti-wear agent; the second component comprises polythiol curing agent, fatty amine curing agent, curing accelerator, N-isopropyl benzylamine and fumed silica. This application utilizes the seam cream that component one and component two mix made, and the adhesion is good, and comprehensive mechanical properties and temperature resistant degeneration are excellent for the product is lighter, difficult stream weighs down, does not tell yellow, changes and fills in little gap, and the construction is more convenient, and the off-the-shelf wear resistance that improves simultaneously reduces the fracture problem.
Description
Technical Field
The application relates to the technical field of joint paste, in particular to epoxy joint paste not prone to cracking and a preparation method thereof.
Background
In the indoor and outdoor decoration, the decoration material often generates gaps and parts easy to crack, and in order to achieve the effects of attractiveness, safety and prevention of dirt collection and dirt collection, the parts have to be treated, so that various seam filling products are derived, and the products are roughly divided into two main types, namely cement-based products and resin-based products according to different constituent materials of the products. The epoxy resin adhesive has outstanding technological performance, convenient construction and smooth and porcelain-like surface after being cured, and is widely applied in various fields.
The epoxy resin adhesives with various performance indexes are designed and developed by a producer through selection and blending of epoxy resin and a curing agent, and the common epoxy resin adhesive generates larger shrinkage stress during curing, and is characterized by brittleness, low strength and elongation, easy cracking and debonding and poor surface wear resistance.
Disclosure of Invention
Additional features and advantages of the application will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the application. The objectives and other advantages of the application may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as from the other detailed description.
The application aims to overcome the defects and provide the epoxy jointing paste which is not easy to crack and the preparation method thereof so as to solve the problems of brittleness, easy cracking, debonding and poor wear resistance of the existing jointing paste.
In order to achieve the purpose, the technical solution of the application is as follows: the epoxy joint compound not easy to crack comprises a first component and a second component, wherein the weight ratio of the first component to the second component is 1.5-2.5: 1;
the component one comprises the following raw materials in parts by weight: 55-65 parts of bisphenol F epoxy resin, 45-55 parts of bisphenol A epoxy resin, 40-50 parts of hydroxymethyl epoxy resin, 45-55 parts of trimethylolpropane triglycidyl ether, 11-15 parts of organic silicon polyether copolymer, 25-35 parts of asbestos powder, 55-65 parts of triple superphosphate, 64-75 parts of organic silicon bentonite, 12-14 parts of fumed silica, 1.2-1.3 parts of thixotropic stabilizer, 1.2-2.4 parts of bulking agent, 2-5 parts of toughening agent, 2-5 parts of wear-resisting agent, 10-20 parts of linseed oil emulsion and 5-8 parts of calcium carbonate powder;
the component II comprises the following raw materials in parts by weight: 23-28 parts of polythiol curing agent, 20-25 parts of aliphatic amine curing agent, 1.5-2.5 parts of curing accelerator, 6-10 parts of N-isopropylaniline and 10-12 parts of fumed silica.
In some embodiments, the thixotropic stabilizer is comprised of one or more of thixotropic stabilizer BYK-R605, thixotropic stabilizer PR600, or thixotropic stabilizer 1065.
In some embodiments, the toughening agent is one or more of a core-shell toughening agent, a carboxyl-terminated liquid nitrile rubber, a polyamide resin, polyazelaic anhydride, or a liquid polysulfide compound.
In some embodiments, the anti-wear agent is a mixture of silicone oil and one or more of nano aluminum oxide, nano silicon dioxide or nano zirconium dioxide.
In some embodiments, the nano aluminum oxide, nano silicon dioxide and nano zirconium dioxide all have a particle size of 2-5 nm.
In some embodiments, the polythiol curing agent is a polyglycerol thiol epoxy curing agent.
In some embodiments, the aliphatic amine curing agent is one or more of ethylenediamine curing agent, hexamethylenediamine curing agent, diethylenetriamine curing agent, and triethylenetetramine curing agent.
In some embodiments, the cure accelerator is composed of one or more of 2-methylimidazole, 2-ethyl-4-methylimidazole, 2-heptadecylimidazole, and 2-isopropylimidazole.
The application also provides a preparation method of the epoxy jointing paste which is not easy to crack, comprising the following steps,
preparation of component one: weighing bisphenol F epoxy resin, bisphenol A epoxy resin, hydroxymethyl epoxy resin, trimethylolpropane triglycidyl ether, organic silicon polyether copolymer, asbestos powder, heavy calcium carbonate, organic silicon bentonite, gas-phase silicon dioxide, a thixotropic stabilizer, a bulking agent, a toughening agent, an anti-wear agent, a linseed oil emulsion and calcium carbonate powder according to the weight ratio, adding the bisphenol F epoxy resin, the bisphenol A epoxy resin and the hydroxymethyl epoxy resin into a reaction kettle, heating for 5-8 minutes at the temperature of 85-95 ℃, adding the trimethylolpropane triglycidyl ether, mixing and stirring the organic silicon polyether copolymer at the rotating speed of 50-60rpm, naturally cooling to 60-70 ℃, and finally, weighing the asbestos powder, the heavy calcium carbonate, the organic silicon bentonite, the gas-phase silicon dioxide, the thixotropic stabilizer, the bulking agent, the toughening agent, the anti-wear agent and the linseed oil emulsion, adding calcium carbonate powder into a reaction kettle, increasing the rotating speed to 200-300rpm for mixing and stirring, vacuumizing and maintaining the rotating speed for stirring for 20-40min to obtain a component I;
preparation of component two: weighing polythiol curing agent, fatty amine curing agent, curing accelerator, N-isopropyl benzylamine and fumed silica according to the weight ratio, adding polythiol curing agent, fatty amine curing agent, curing accelerator, N-isopropyl benzylamine and fumed silica into a stirring barrel at normal temperature and normal pressure, and stirring at the rotating speed of 100-120rpm for 20-30min to obtain a second component;
preparation of the joint paste: weighing the first component and the second component according to the weight ratio, and adding the first component and the second component into a mixing container to be uniformly mixed to obtain the jointing paste.
Through adopting foretell technical scheme, the beneficial effect of this application is:
1. the component I is mainly obtained by mixing bisphenol F epoxy resin, bisphenol A epoxy resin, hydroxymethyl epoxy resin, trimethylolpropane triglycidyl ether, organic silicon polyether copolymer, asbestos powder, heavy calcium, organic silicon bentonite, fumed silica, a thixotropic stabilizer, a bulking agent, a toughening agent, an anti-wear agent, a flax oil emulsion and calcium carbonate powder, and has the advantages of high toughness, good heat resistance, corrosion resistance, pollution resistance, good wear resistance and difficult dilution after long-term storage, wherein the flax oil emulsion can be mixed with dispersed calcium carbonate powder to form a protective film, so that the anti-cracking effect can be achieved;
2. the second component is mainly prepared by mixing a polythiol curing agent, a fatty amine curing agent, a curing accelerator, N-isopropylaniline and fumed silica, has a great influence on the curing effect of the joint paste, and can accelerate the curing speed of the first component;
3. the joint paste made by mixing the first component and the second component has good bonding force, excellent comprehensive mechanical property and temperature resistance, and the epoxy resin component has the capability of being synchronously cured at medium and low temperature, so that the product is lighter, is not easy to flow and fall, is not yellow in spitting, is easier to flow into a small gap, is more convenient to construct, and simultaneously has improved wear resistance and reduces the cracking problem.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.
These and other objects, features and advantages of the present application will become more readily apparent from the following detailed description of one or more preferred embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the present application is further described in detail with reference to the following detailed description. It should be understood that the detailed description and specific examples, while indicating the present application, are given by way of illustration only.
According to some embodiments of the present application, the present application provides an epoxy joint compound not prone to cracking, which includes a first component and a second component, wherein the weight ratio of the first component to the second component is 1.5-2.5: 1;
the component one comprises the following raw materials in parts by weight: 55-65 parts of bisphenol F epoxy resin, 45-55 parts of bisphenol A epoxy resin, 40-50 parts of hydroxymethyl epoxy resin, 45-55 parts of trimethylolpropane triglycidyl ether, 11-15 parts of organic silicon polyether copolymer, 25-35 parts of asbestos powder, 55-65 parts of triple superphosphate, 64-75 parts of organic silicon bentonite, 12-14 parts of fumed silica, 1.2-1.3 parts of thixotropic stabilizer, 1.2-2.4 parts of bulking agent, 2-5 parts of toughening agent, 2-5 parts of wear-resisting agent, 10-20 parts of linseed oil emulsion and 5-8 parts of calcium carbonate powder; the component II comprises the following raw materials in parts by weight: 23-28 parts of polythiol curing agent, 20-25 parts of aliphatic amine curing agent, 1.5-2.5 parts of curing accelerator, 6-10 parts of N-isopropylaniline and 10-12 parts of fumed silica.
Bisphenol F epoxy resin is also called bisphenol F diglycidyl ether, BPF for short, and is prepared by reacting phenol with formaldehyde under acidic catalysis to generate bisphenol F, and then carrying out polycondensation reaction with epichlorohydrin in the presence of sodium hydroxide, and is liquid bisphenol F epoxy resin obtained by reacting bisphenol F (diphenolylmethane) with epichlorohydrin under the action of NaOH.
Bisphenol a epoxy resins refer to those resin compounds that contain at least two reactive epoxy groups in the molecule; is a high molecular compound prepared by condensation of bisphenol A and epichlorohydrin under alkaline condition, water washing and solvent removal.
The hydroxymethyl epoxy resin is a generic name of a polymer containing a hydroxymethyl group and more than two epoxy groups in a molecule.
Trimethylolpropane triglycidyl ether is an organic compound of formula C15H26O 6.
The organic silicon polyether copolymer consists of polysiloxane, polyether copolymer and efficient dispersant.
Asbestos powder is a powdery non-metallic material containing asbestos fibers.
The heavy calcium is prepared by grinding natural carbonate minerals such as calcite, marble, and limestone. The inorganic filler is a common powdery inorganic filler and has the advantages of high chemical purity, high inertia, difficult chemical reaction, good thermal stability, no decomposition at the temperature of below 400 ℃, high whiteness, low oil absorption rate, low refractive index, soft quality, dryness, no crystal water, low hardness, low abrasion value, no toxicity, no odor, good dispersibility and the like.
The organic silicon bentonite and the organic bentonite are inorganic mineral/organic ammonium compounds, the bentonite is used as a raw material, the lamellar structure of montmorillonite in the bentonite and the characteristic that the montmorillonite can be swelled and dispersed into colloidal clay are utilized, and the organic silicon covering agent is inserted into the organic silicon bentonite and the organic bentonite through an ion exchange technology, so that the organic silicon bentonite and the organic bentonite have good thickening property, thixotropy, suspension stability, high-temperature stability, lubricity, film-forming property, water resistance and chemical stability.
The fumed silica is nano white powder generated by high-temperature hydrolysis of silicon halide in oxyhydrogen flame, is commonly called fumed silica, is an amorphous silica product, has a primary particle size of 7-40 nm, an aggregate particle size of about 200-500 nm, a specific surface area of 100-400 m2/g, high purity and a SiO2 content of not less than 99.8%. The surface-untreated fumed silica aggregates contain a plurality of silicon hydroxyl groups.
The thixotropic stabilizer is a colorless transparent liquid which contains active oxygen groups and can improve the performance of fumed silica, does not break an outlet network, contains epoxy groups, improves the crosslinking density, is used together with epoxy resin, and can ensure that oxygen silicon can obtain lasting and stable thixotropy.
The loosening agent contains a large amount of active groups, can improve gas-phase carbon dioxide, can ensure that the epoxy resin obtains lasting and stable thixotropy, and can form hydrogen bonds with gas-phase silicon dioxide to achieve the natural increase of viscosity, and can be used on the premise of not losing the application performance of the epoxy resin, thereby reducing the use cost of raw materials and improving the product quality.
The toughening agent is a substance capable of increasing the flexibility of the adhesive film layer.
The main component of the wear-resistant agent is a silicone oil component, so that the wear resistance and scratch resistance of the product can be improved, and the self-cleaning performance of the product can be improved.
The main component of the flax oil emulsion is flax oil.
Calcium carbonate powder is an inorganic compound of the chemical formula CaCO3, is basic and is substantially insoluble in water.
The polythiol curing agent is polythiol, can be prepared by reacting beta-mercaptopropionic acid with pentaerythritol to generate polythiol ester, and then carrying out heating chain extension reaction with a small amount of E51 epoxy resin, is a room-temperature or low-temperature rapid curing agent, takes tertiary amine as an accelerator, and can cure the epoxy resin within 1-5 min.
The aliphatic amine curing agent refers to an alicyclic amine modified epoxy resin curing agent, and has the advantages of mild curing speed, high permeability, high strength, high gloss and good water resistance.
The curing accelerator can greatly accelerate the reaction between the thermosetting resin and the curing agent.
N-isopropylamine is a chemical substance with the molecular formula of C10H 16N.
Therefore, the main raw materials of the epoxy joint compound which is not easy to crack are bisphenol F epoxy resin, bisphenol A epoxy resin, hydroxymethyl epoxy resin, trimethylolpropane triglycidyl ether, organic silicon polyether copolymer, asbestos powder, heavy calcium, organic silicon bentonite, fumed silica, thixotropic stabilizer, bulking agent, toughening agent and wear-resisting agent, and the component I which is high in toughness, good in heat resistance, corrosion-resistant, anti-fouling and wear-resisting properties and not easy to thin after long-term storage is obtained by mixing; in the second component, polythiol curing agent, fatty amine curing agent, curing accelerator, N-isopropylaniline and fumed silica are adopted, and the mass ratio of the polythiol curing agent to the fatty amine curing agent has great influence on the curing effect of the joint compound. If the polythiol curing agent is too much, the bonding strength and toughness of the joint paste can be reduced; if the fatty amine curing agent is too much, the heat resistance and stability of the joint compound are reduced; the joint paste prepared by mixing the component I and the component II has good bonding force and excellent comprehensive mechanical property and temperature change resistance, and the epoxy resin component has the capability of being synchronously cured at medium and low temperature, so that the product is lighter, is not easy to flow and fall, is not yellow in spitting, is easier to fill small gaps, is more convenient to construct, and simultaneously improves the wear resistance of the finished product and reduces the cracking problem.
According to some embodiments of the present application, optionally, the thixotropic stabilizer is one or more of a thixotropic stabilizer BYK-R605, a thixotropic stabilizer PR600, or a thixotropic stabilizer 1065. By adding these types of thixotropic stabilizers, the oxygen-containing silicon can be made to have a long-lasting, stable thixotropy.
Thixotropic stabilizer 1065 is produced by Xiamen Baianxing New materials Co.
According to some embodiments of the present application, optionally, the toughening agent is one or more of a core shell toughening agent, a carboxyl-terminated liquid nitrile rubber, a polyamide resin, polyazelaic anhydride, or a liquid polysulfide compound. By adding these types of toughening agents, the toughness of the final product is increased to reduce cracking problems.
The core-shell toughening agent refers to a Japanese clockwork epoxy resin toughening agent MX-153.
The carboxyl-terminated liquid nitrile rubber refers to nitrile rubber of which two ends of a molecular chain are carboxyl groups with active functional groups.
The polyamide resin is a polycondensation type high molecular compound having a CONH structure in the molecule, and is usually obtained by polycondensation of a dibasic acid and a diamine.
Polyazelaic anhydride is called PAPA for short, when the polyazelaic anhydride is placed in air for a long time or in a sealed bottle for more than half a year, the surface becomes whitish, the melting point is obviously increased, because the water in the air is absorbed, the PAPA is partially hydrolyzed into azelaic acid, and the melting point is 106.5 ℃.
The liquid polysulfide compounds include ethyl formal polysulfide compound and butyl formal polysulfide compound.
According to some embodiments of the present application, optionally, the anti-wear agent is a mixture of silicone oil and one or more of nano alumina, nano silica, or nano zirconia. The anti-wear agent is arranged, so that the finished product has certain wear resistance after indication, and the service life of the finished product is prolonged.
Silicone oil refers to a linear polysiloxane product that remains in a liquid state at room temperature.
The nano alumina is an inorganic substance with a chemical formula of Al2O3, and is white crystalline powder.
The nano silicon dioxide is superfine nano and has the size range of 1-100 nm, so that the nano silicon dioxide has a plurality of unique properties, such as optical performance of resisting ultraviolet rays, and the ageing resistance, strength and chemical resistance of other materials can be improved.
The nanometer zirconium dioxide is nontoxic and tasteless white powder, can be divided into monoclinic phase, tetragonal phase and cubic phase according to different sintering temperatures and contents of stabilizing substances such as yttrium oxide and the like, and is dissolved in sulfuric acid and hydrofluoric acid; the nano zirconia has the advantages of good thermochemical stability, high-temperature conductivity, higher strength and toughness, good mechanical, thermal, electrical and optical properties, small particle size of nano zirconia, strong stability, acid resistance, alkali resistance, corrosion resistance and high temperature resistance.
According to some embodiments of the present application, optionally, the nano alumina, the nano silica and the nano zirconia each have a particle size of 2 to 5 nm. The grain sizes of the nano aluminum oxide, the nano silicon dioxide and the nano zirconium dioxide are set, so that the grain sizes are uniform, and the uneven mixing is avoided.
According to some embodiments of the present application, optionally, the polythiol curing agent is a polyglycerol thiol epoxy curing agent. The polythiol curing agent can increase the curing rate of the epoxy resin.
The polyglycerol mercaptan epoxy resin curing agent is chemically reacted with epoxy resin to form a net-shaped three-dimensional polymer.
According to some embodiments of the present application, optionally, the aliphatic amine curing agent is one or more of ethylenediamine curing agent, hexamethylenediamine curing agent, diethylenetriamine curing agent, and triethylenetetramine curing agent. The aliphatic amine curing agent can increase the curing rate of the epoxy resin.
The ethylene diamine curing agent, which has the chemical formula of C2H8N2, is a typical aliphatic diamine, is colorless or yellowish oily or water-like transparent liquid, generates smoke in air, has an odor similar to ammonia, and is hygroscopic.
The hexamethylene diamine curing agent has a chemical formula of C6H16N2, is an organic compound, is white crystalline powder, is easily soluble in water, and is slightly soluble in ethanol, benzene and diethyl ether.
The diethylenetriamine curing agent is yellow transparent viscous liquid with hygroscopicity, has irritant ammonia odor, is combustible and is strong in alkalinity.
Triethylene tetramine curing agent, molecular formula is C6H18N4, and has light yellow liquid with strong basicity and medium viscosity.
According to some embodiments of the present application, optionally, the cure accelerator is one or more of 2-methylimidazole, 2-ethyl-4-methylimidazole, 2-heptadecylimidazole, and 2-isopropylimidazole. The cure accelerator may increase the rate of cure.
2-methylimidazole is an organic compound of the formula C4H6N 2.
2-Ethyl-4-methylimidazole is an organic compound of formula C6H10N 2.
2-heptadecylimidazole is an organic compound of formula C20H38N 2.
2-isopropylimidazole is an organic compound of formula C6H10N 2.
The application also provides a preparation method of the epoxy jointing paste which is not easy to crack, comprising the following steps,
preparation of component one: weighing bisphenol F epoxy resin, bisphenol A epoxy resin, hydroxymethyl epoxy resin, trimethylolpropane triglycidyl ether, organic silicon polyether copolymer, asbestos powder, heavy calcium carbonate, organic silicon bentonite, fumed silica, a thixotropic stabilizer, a bulking agent, a toughening agent, an anti-wear agent, flax oil emulsion and calcium carbonate powder according to the weight ratio, adding the bisphenol F epoxy resin, the bisphenol A epoxy resin and the hydroxymethyl epoxy resin into a reaction kettle, heating for 5-8 minutes at the temperature of 85-95 ℃, adding the trimethylolpropane triglycidyl ether, mixing and stirring the organic silicon polyether copolymer at the rotating speed of 50-60rpm, naturally cooling to 60-70 ℃, and finally, adding the asbestos powder, the heavy calcium carbonate, the organic silicon bentonite, the fumed silica, the thixotropic stabilizer, the bulking agent, the toughening agent, the anti-wear agent and the flax oil emulsion, adding calcium carbonate powder into a reaction kettle, increasing the rotating speed to 200-300rpm for mixing and stirring, vacuumizing and keeping the rotating speed for stirring for 20-40min to obtain a component I;
preparation of component two: weighing polythiol curing agent, fatty amine curing agent, curing accelerator, N-isopropyl benzylamine and fumed silica according to the weight ratio, adding polythiol curing agent, fatty amine curing agent, curing accelerator, N-isopropyl benzylamine and fumed silica into a stirring barrel at normal temperature and normal pressure, and stirring at the rotating speed of 100-120rpm for 20-30min to obtain a second component;
preparation of the joint paste: weighing the first component and the second component according to the weight ratio, and adding the first component and the second component into a mixing container to be uniformly mixed to obtain the jointing paste. The joint paste is prepared by the method, so that the joint paste is simpler and quicker to manufacture, meanwhile, when the joint paste is not used, the component I and the component II can be separately placed, and when the joint paste is used, the component I and the component II are uniformly mixed to obtain the newly-prepared joint paste.
Example 1
The application provides epoxy joint paste not prone to cracking, which comprises a first component and a second component, wherein the weight ratio of the first component to the second component is 1.5-2: 1;
the component one comprises the following raw materials in parts by weight: 55-60 parts of bisphenol F epoxy resin, 45-50 parts of bisphenol A epoxy resin, 40-45 parts of hydroxymethyl epoxy resin, 45-50 parts of trimethylolpropane triglycidyl ether, 11-13 parts of organic silicon polyether copolymer, 25-30 parts of asbestos powder, 55-60 parts of triple superphosphate, 64-69.5 parts of organic silicon bentonite, 12-13 parts of fumed silica, 1.2-1.25 parts of thixotropic stabilizer, 1.2-1.8 parts of bulking agent, 2-3.5 parts of toughening agent, 2-3.5 parts of wear-resisting agent, 10-20 parts of linseed oil emulsion and 5-8 parts of calcium carbonate powder;
the component II comprises the following raw materials in parts by weight: 23-25.5 parts of polythiol curing agent, 20-22.5 parts of aliphatic amine curing agent, 1.5-2 parts of curing accelerator, 6-8 parts of N-isopropylaniline and 10-11 parts of fumed silica.
The thixotropic stabilizer is one of a thixotropic stabilizer BYK-R605, a thixotropic stabilizer PR600 or a thixotropic stabilizer 1065.
The toughening agent is one of carboxyl-terminated liquid nitrile rubber, polyamide resin, polyazelaic anhydride or liquid polysulfide compound.
The wear-resisting agent is one of silicone oil and nano aluminum oxide, nano silicon dioxide or nano zirconium dioxide.
The grain diameters of the nano aluminum oxide, the nano silicon dioxide and the nano zirconium dioxide are all 2-3.5 nm.
The polythiol curing agent is a polyglycerol mercaptan epoxy resin curing agent.
The aliphatic amine curing agent is one or more than two of ethylenediamine curing agent, hexamethylenediamine curing agent, diethylenetriamine curing agent and triethylene tetramine curing agent.
The curing accelerator is composed of one or more than two of 2-methylimidazole, 2-ethyl-4-methylimidazole, 2-heptadecylimidazole and 2-isopropylimidazole.
The application also provides a preparation method of the epoxy jointing paste which is not easy to crack, comprising the following steps,
preparation of component one: weighing bisphenol F epoxy resin, bisphenol A epoxy resin, hydroxymethyl epoxy resin, trimethylolpropane triglycidyl ether, organic silicon polyether copolymer, asbestos powder, heavy calcium carbonate, organic silicon bentonite, gas-phase silicon dioxide, a thixotropic stabilizer, a bulking agent, a toughening agent, an anti-wear agent, flax oil emulsion and calcium carbonate powder according to the weight ratio, adding the bisphenol F epoxy resin, the bisphenol A epoxy resin and the hydroxymethyl epoxy resin into a reaction kettle, heating for 5-6.5 minutes at the temperature of 85-90 ℃, adding the trimethylolpropane triglycidyl ether, mixing and stirring the organic silicon polyether copolymer at the rotating speed of 50-55rpm, naturally cooling to 60-65 ℃, and finally adding the asbestos powder, the heavy calcium carbonate, the organic silicon bentonite, the gas-phase silicon dioxide, the thixotropic stabilizer, the bulking toughening agent, the anti-wear agent and the flax oil emulsion, adding calcium carbonate powder into a reaction kettle, increasing the rotating speed to 200-250rpm for mixing and stirring, vacuumizing and keeping the rotating speed for stirring for 20-30min to obtain a component I;
preparation of component two: weighing polythiol curing agent, fatty amine curing agent, curing accelerator, N-isopropyl benzylamine and fumed silica according to the weight ratio, adding polythiol curing agent, fatty amine curing agent, curing accelerator, N-isopropyl benzylamine and fumed silica into a stirring barrel at normal temperature and normal pressure, and stirring at the rotating speed of 100 plus 110rpm for 20-25min to obtain a component II;
preparation of the joint paste: weighing the first component and the second component according to the weight ratio, and adding the first component and the second component into a mixing container to be uniformly mixed to obtain the jointing paste.
Example 2
The application provides epoxy joint compound not prone to cracking, which comprises a first component and a second component, wherein the weight ratio of the first component to the second component is 2-2.5: 1; the component one comprises the following raw materials in parts by weight: 55-65 parts of bisphenol F epoxy resin, 50-55 parts of bisphenol A epoxy resin, 45-50 parts of hydroxymethyl epoxy resin, 50-55 parts of trimethylolpropane triglycidyl ether, 13-15 parts of organic silicon polyether copolymer, 30-35 parts of asbestos powder, 60-65 parts of heavy calcium carbonate, 69.5-75 parts of organic silicon bentonite, 13-14 parts of fumed silica, 1.25-1.3 parts of thixotropic stabilizer, 1.8-2.4 parts of bulking agent, 3.5-5 parts of toughening agent and 3.5-5 parts of wear-resisting agent; the component II comprises the following raw materials in parts by weight: 25.5-28 parts of polythiol curing agent, 22.5-25 parts of fatty amine curing agent, 2-2.5 parts of curing accelerator, 8-10 parts of N-isopropylaniline, 11-12 parts of fumed silica, 10-20 parts of linseed oil emulsion and 5-8 parts of calcium carbonate powder.
The thixotropic stabilizer is prepared by mixing a thixotropic stabilizer BYK-R605, a thixotropic stabilizer PR600 and a thixotropic stabilizer 1065.
The toughening agent is prepared by mixing carboxyl-terminated liquid nitrile rubber, polyamide resin, polyazelaic anhydride and liquid polysulfide compound.
The wear-resisting agent is prepared by mixing silicone oil, nano aluminum oxide, nano silicon dioxide and nano zirconium dioxide.
The grain diameters of the nano aluminum oxide, the nano silicon dioxide and the nano zirconium dioxide are all 3.5-5 nm.
The polythiol curing agent is a polyglycerol mercaptan epoxy resin curing agent.
The aliphatic amine curing agent is prepared by mixing an ethylenediamine curing agent, a hexamethylenediamine curing agent, a diethylenetriamine curing agent and a triethylenetetramine curing agent.
The curing accelerator is prepared by mixing 2-methylimidazole, 2-ethyl-4-methylimidazole, 2-heptadecylimidazole and 2-isopropylimidazole.
The application also provides a preparation method of the epoxy jointing paste which is not easy to crack, comprising the following steps,
preparation of component one: weighing bisphenol F epoxy resin, bisphenol A epoxy resin, hydroxymethyl epoxy resin, trimethylolpropane triglycidyl ether, organic silicon polyether copolymer, asbestos powder, heavy calcium carbonate, organic silicon bentonite, fumed silica, a thixotropic stabilizer, a bulking agent, a toughening agent, an anti-wear agent, flax oil emulsion and calcium carbonate powder according to the weight ratio, adding the bisphenol F epoxy resin, the bisphenol A epoxy resin and the hydroxymethyl epoxy resin into a reaction kettle, heating for 6.5-8 minutes at the temperature of 90-95 ℃, adding the trimethylolpropane triglycidyl ether, mixing and stirring the organic silicon polyether copolymer at the rotating speed of 55-60rpm, naturally cooling to 65-70 ℃, and finally adding the asbestos powder, the heavy calcium carbonate, the organic silicon bentonite, the fumed silica, the thixotropic stabilizer, the bulking toughening agent, the anti-wear agent and the flax oil emulsion, adding calcium carbonate powder into a reaction kettle, increasing the rotating speed to 250-300rpm for mixing and stirring, vacuumizing and keeping the rotating speed for stirring for 30-40min to obtain a component I;
preparation of component two: weighing polythiol curing agent, fatty amine curing agent, curing accelerator, N-isopropyl benzylamine and fumed silica according to the weight ratio, adding polythiol curing agent, fatty amine curing agent, curing accelerator, N-isopropyl benzylamine and fumed silica into a stirring barrel at normal temperature and normal pressure, and stirring at the rotation speed of 110-120rpm for 25-30min to obtain a component II;
preparation of the joint paste: weighing the first component and the second component according to the weight ratio, and adding the first component and the second component into a mixing container to be uniformly mixed to obtain the jointing paste.
Comparative example
The comparative example provides an epoxy joint compound, which comprises a first component and a second component, wherein the weight ratio of the first component to the second component is 1.5: 1; the component one comprises the following raw materials in parts by weight: 55-65 parts of bisphenol F epoxy resin, 50-55 parts of bisphenol A epoxy resin, 45-50 parts of hydroxymethyl epoxy resin, 50-55 parts of trimethylolpropane triglycidyl ether, 13-15 parts of organic silicon polyether copolymer, 30-35 parts of asbestos powder, 60-65 parts of heavy calcium carbonate and 69.5-75 parts of organic silicon bentonite; the component II comprises the following raw materials in parts by weight: 25.5-28 parts of polythiol curing agent, 22.5-25 parts of fatty amine curing agent, 2-2.5 parts of curing accelerator and 8-10 parts of N-isopropylbenzylamine.
The thixotropic stabilizer is a thixotropic stabilizer BYK-R605.
The polythiol curing agent is a polyglycerol mercaptan epoxy resin curing agent.
The aliphatic amine curing agent is an ethylenediamine curing agent.
The curing accelerator is 2-methylimidazole.
This comparative example provides a method of preparing an epoxy joint compound comprising the steps of,
preparation of component one: weighing bisphenol F epoxy resin, bisphenol A epoxy resin, hydroxymethyl epoxy resin, trimethylolpropane triglycidyl ether, organic silicon polyether copolymer, asbestos powder, heavy calcium and organic silicon bentonite according to the weight ratio, adding the bisphenol F epoxy resin, the bisphenol A epoxy resin and the hydroxymethyl epoxy resin into a reaction kettle, heating for 6.5-8 minutes at the temperature of 90-95 ℃, adding the trimethylolpropane triglycidyl ether, mixing and stirring the organic silicon polyether copolymer at the rotating speed of 55-60rpm, naturally cooling to 65-70 ℃, finally adding the asbestos powder, the heavy calcium and the organic silicon bentonite into the reaction kettle, increasing the rotating speed to 250-300rpm, mixing and stirring, vacuumizing, keeping the rotating speed and stirring for 30-40 minutes to obtain a component I;
preparation of a component II: weighing a polythiol curing agent, a fatty amine curing agent, a curing accelerator and N-isopropylbenzylamine according to the weight ratio, adding the polythiol curing agent, the fatty amine curing agent, the curing accelerator and the N-isopropylbenzylamine into a stirring barrel at normal temperature and normal pressure, and stirring at the rotating speed of 110-120rpm for 25-30min to obtain a component II;
preparation of the joint paste: weighing the first component and the second component according to the weight ratio, and adding the first component and the second component into a mixing container to be uniformly mixed to obtain the jointing paste.
Respectively taking the epoxy joint paste which is not easy to crack and is prepared in the embodiment 1-2 and the epoxy joint paste prepared in the comparative example, and measuring the viscosity according to GB/T2794-2013; the 180 DEG peeling force is measured according to GB/T2792-; tensile strength was determined according to GB/T528-; the elongation at break was determined according to GB/T528-; the wear resistance was measured in terms of the number of times of rubbing to wear. The specific data are as follows:
| test items | Example 1 | Example 2 | Comparative example |
| Viscosity (mPa) | 2.5 | 3.2 | 1.2 |
| 180 degree peel force (N/15mm) | 12 | 18 | 6 |
| Tensile strength (Mpa) | 11 | 14 | 4.5 |
| Elongation at Break (%) | 450 | 520 | 310 |
| Number of rubs (times) | 68 | 77 | 45 |
As can be seen from the above table, the performance indexes of the epoxy joint compound prepared in the embodiments 1-2 of the present invention are compared with the epoxy joint compound prepared in the comparative example, the epoxy joint compound prepared in the present invention has mechanical properties such as high adhesive strength, high tensile strength, high elongation at break, and good wear resistance.
It is to be understood that the embodiments disclosed herein are not limited to the particular process steps or materials disclosed herein, but rather, are extended to equivalents thereof as would be understood by those of ordinary skill in the relevant art. It is also to be understood that the terminology used herein is for the purpose of describing particular embodiments only, and is not intended to be limiting.
Reference in the specification to "an embodiment" means that a particular feature, or characteristic described in connection with the embodiment is included in at least one embodiment of the application. Thus, the appearances of the phrase or "an embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment.
Furthermore, the described features or characteristics may be combined in any other suitable manner in one or more embodiments. One skilled in the relevant art will recognize, however, that the application can be practiced without one or more of the specific details, or with other methods, components, materials, etc.
Claims (9)
1. The epoxy jointing paste is not easy to crack and is characterized in that: the adhesive comprises a first component and a second component, wherein the weight ratio of the first component to the second component is 1.5-2.5: 1;
the component one comprises the following raw materials in parts by weight: 55-65 parts of bisphenol F epoxy resin, 45-55 parts of bisphenol A epoxy resin, 40-50 parts of hydroxymethyl epoxy resin, 45-55 parts of trimethylolpropane triglycidyl ether, 11-15 parts of organic silicon polyether copolymer, 25-35 parts of asbestos powder, 55-65 parts of triple superphosphate, 64-75 parts of organic silicon bentonite, 12-14 parts of fumed silica, 1.2-1.3 parts of thixotropic stabilizer, 1.2-2.4 parts of bulking agent, 2-5 parts of toughening agent, 2-5 parts of wear-resisting agent, 10-20 parts of linseed oil emulsion and 5-8 parts of calcium carbonate powder;
the component II comprises the following raw materials in parts by weight: 23-28 parts of polythiol curing agent, 20-25 parts of aliphatic amine curing agent, 1.5-2.5 parts of curing accelerator, 6-10 parts of N-isopropylaniline and 10-12 parts of fumed silica.
2. The non-cracking epoxy joint compound of claim 1, wherein: the thixotropic stabilizer is one or more of a thixotropic stabilizer BYK-R605, a thixotropic stabilizer PR600 or a thixotropic stabilizer 1065.
3. The non-cracking epoxy joint compound of claim 1, wherein: the toughening agent is one or more than two of a core-shell toughening agent, carboxyl-terminated liquid nitrile rubber, polyamide resin, polyazelaic anhydride or liquid polysulfide compound.
4. The non-cracking epoxy joint compound of claim 1, wherein: the wear-resisting agent is formed by mixing silicone oil and one or more than two of nano aluminum oxide, nano silicon dioxide or nano zirconium dioxide.
5. The non-cracking epoxy jointing paste according to claim 4, wherein: the grain diameters of the nano aluminum oxide, the nano silicon dioxide and the nano zirconium dioxide are all 2-5 nm.
6. The non-cracking epoxy joint compound of claim 1, wherein: the polythiol curing agent is a polyglycerol mercaptan epoxy resin curing agent.
7. The non-cracking epoxy joint compound of claim 1, wherein: the aliphatic amine curing agent is one or more than two of ethylenediamine curing agent, hexamethylenediamine curing agent, diethylenetriamine curing agent and triethylene tetramine curing agent.
8. The non-cracking epoxy joint compound of claim 1, wherein: the curing accelerator is composed of one or more than two of 2-methylimidazole, 2-ethyl-4-methylimidazole, 2-heptadecylimidazole and 2-isopropylimidazole.
9. A method of preparing a non-cracking epoxy joint compound according to any one of claims 1 to 8, characterized in that: comprises the following steps of (a) carrying out,
preparation of component one: weighing bisphenol F epoxy resin, bisphenol A epoxy resin, hydroxymethyl epoxy resin, trimethylolpropane triglycidyl ether, organic silicon polyether copolymer, asbestos powder, heavy calcium carbonate, organic silicon bentonite, fumed silica, a thixotropic stabilizer, a bulking agent, a toughening agent, an anti-wear agent, a linseed oil emulsion and calcium carbonate powder according to the weight ratio, adding the weighed bisphenol F epoxy resin, bisphenol A epoxy resin and hydroxymethyl epoxy resin into a reaction kettle, heating for 5-8 minutes at the temperature of 85-95 ℃, adding the trimethylolpropane triglycidyl ether, mixing and stirring the organic silicon polyether copolymer at the rotating speed of 50-60rpm, naturally cooling to 60-70 ℃, and finally, adding the weighed asbestos powder, heavy calcium carbonate, organic silicon bentonite, fumed silica, the thixotropic stabilizer, the bulking agent, the toughening agent and the anti-wear agent, adding the calcium carbonate powder into a reaction kettle, increasing the rotating speed to 200-300rpm for mixing and stirring, vacuumizing and keeping the rotating speed for stirring for 20-40min to obtain a component I;
preparation of component two: weighing polythiol curing agent, fatty amine curing agent, curing accelerator, N-isopropyl benzylamine and fumed silica according to the weight ratio, adding polythiol curing agent, fatty amine curing agent, curing accelerator, N-isopropyl benzylamine and fumed silica into a stirring barrel at normal temperature and normal pressure, and stirring at the rotating speed of 100-120rpm for 20-30min to obtain a second component;
preparation of the joint paste: weighing the first component and the second component according to the weight ratio, and adding the first component and the second component into a mixing container to be uniformly mixed to obtain the jointing paste.
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