CN110804369A - Synthetic method of solvent-type organic silicon modified epoxy resin coating - Google Patents
Synthetic method of solvent-type organic silicon modified epoxy resin coating Download PDFInfo
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- CN110804369A CN110804369A CN201911129083.3A CN201911129083A CN110804369A CN 110804369 A CN110804369 A CN 110804369A CN 201911129083 A CN201911129083 A CN 201911129083A CN 110804369 A CN110804369 A CN 110804369A
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions 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
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
- C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
Abstract
The invention relates to the technical field of epoxy resin, and discloses a synthetic method of a solvent-type organic silicon modified epoxy resin coating, which comprises the following steps: s1, adding a solvent, a water removing agent, a defoaming agent, a flatting agent and a storage stabilizer into the reaction kettle, and stirring for 10-60 minutes, wherein the weight ratio of S2: adding epoxy resin, fully stirring and dissolving, and performing S3: adding a silane coupling agent, and raising the temperature to 55-95 ℃, S4: keeping the temperature for 4 to 8 hours to obtain a transparent or light yellow product. According to the synthesis method of the solvent-type organic silicon modified epoxy resin coating, the aminosilane coupling agent is utilized to perform an open loop reaction before epoxy resin to form a prepolymer, so that the epoxy resin can be conveniently subjected to full open loop grafting, and silicon-oxygen bonds with excellent chemical resistance are grafted on the epoxy resin, so that various performances of the epoxy resin are greatly improved, and the aims of full curing, solvent resistance, wear resistance, acid-base corrosion resistance and weather resistance, especially ultraviolet light aging resistance are fulfilled.
Description
Technical Field
The invention relates to the technical field of epoxy resin, in particular to a synthetic method of a solvent-type organic silicon modified epoxy resin coating.
Background
At present, the epoxy resin is widely applied to various aspects such as machinery, buildings, electronics, automobiles, ships and the like as a coating, and is mainly used as a curing method for corrosion prevention, wear resistance, pollution leakage prevention and the like. However, its disadvantages are also evident, mainly manifested as: the paint is not completely cured, and as a cement product and stone finishing paint, the paint has quite common solvent resistance because the curing is not sufficient, and common solvents such as acetone, ethyl acetate, toluene, alcohol, butanone and the like can easily swell a coating, so that the coating loses the effects of corrosion prevention and the like, the hardness is not enough, only about 2H is needed, the hardness is improved, the wear resistance is improved, and the paint is required to be added with fillers, so that the adhesive force is reduced; the method for synthesizing the solvent-type organic silicon modified epoxy resin coating has the advantages of full curing, solvent resistance, wear resistance, acid-base corrosion resistance and weather resistance, particularly ultraviolet light aging resistance.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a synthesis method of a solvent-type organic silicon modified epoxy resin coating, which has the advantages of full curing, solvent resistance, wear resistance, acid-base corrosion resistance, weather resistance, ultraviolet light aging resistance and the like, and solves the problems of incomplete curing, loss of corrosion resistance of a coating, insufficient hardness, increased wear resistance, cracking of carbon-carbon single bonds due to exposure to ultraviolet light, oxidation of carbon-carbon double bonds, embrittlement of the coating, loss of a corrosion resistance function and the like.
(II) technical scheme
In order to realize the purposes of full curing, solvent resistance, wear resistance, acid-base corrosion resistance and weather resistance, particularly ultraviolet light aging resistance, the invention provides the following technical scheme: a synthetic method of a solvent-type organic silicon modified epoxy resin coating comprises the following steps:
and S1, adding the solvent, the water removing agent, the defoaming agent, the flatting agent and the storage stabilizer into the reaction kettle, and stirring for 10-60 minutes.
S2: the epoxy resin was added and dissolved by stirring thoroughly.
S3: the silane coupling agent is added and the temperature is raised to 55-95 degrees.
S4: keeping the temperature for 4 to 8 hours to obtain a transparent or light yellow product.
Preferably, the epoxy resin in the S2 is a polycondensation product of epichlorohydrin and bisphenol a, and accounts for 16% to 76% of the total weight of the system, the S3 silane coupling agent is butadiene-based triethoxysilane, and accounts for 15% to 59% of the total weight of the system, and the weight ratio of the epoxy resin to the silane coupling agent is 1: 0.2-3.8.
Preferably, the solvent in S1 is selected from any one of alcohols, ketones, ethers and aromatic hydrocarbons, and the defoaming agent is a higher alcohol fatty acid ester compound and accounts for 1-5% of the total weight of the system.
Preferably, the leveling agent in S1 adopts an acrylate leveling agent and accounts for 1-5% of the total weight of the system.
Preferably, the water removing agent in S1 is ALT-201 water removing agent, and the total weight of the system is 5-10%.
Preferably, the storage stabilizer in S1 adopts organotin, and accounts for 2-5% of the total weight of the system.
Compared with the prior art, the invention provides a synthetic method of a solvent-type organic silicon modified epoxy resin coating, which has the following beneficial effects:
1. the synthetic method of the solvent-type organic silicon modified epoxy resin coating utilizes the aminosilane coupling agent to perform ring-opening reaction before the epoxy resin to form a prepolymer, thereby facilitating the full ring-opening grafting of the epoxy resin, further avoids the situation that the conventional two-component curing is not complete, and by adopting the silane active group with the terminal group being unhydrolyzed and crosslinked, the curing condition is normal temperature, thereby facilitating the site construction without special requirements such as temperature and pressure, and after the method determines the synthetic scheme, the process synthesis is relatively simple and uncomplicated, is environment-friendly and has no waste, and various performances of the epoxy resin are greatly improved by grafting silicon-oxygen bonds with excellent chemical resistance on the epoxy resin, the resin with corresponding performance is selected according to different performance requirements, so that the aims of full curing, solvent resistance, wear resistance, acid-base corrosion resistance and weather resistance, particularly ultraviolet light aging resistance are fulfilled.
Detailed Description
The first embodiment is as follows:
a synthetic method of a solvent-type organic silicon modified epoxy resin coating comprises the following steps:
s1, adding a solvent into a reaction kettle, wherein the solvent is selected from any one of alcohols, ketones, ethers and aromatic hydrocarbon solvents, a water removal agent, the water removal agent adopts ALT-201 water removal agent, the total weight of the system is 5%, the ALT-201 is a low-toxicity mono-oxazolidine drying agent and a moisture removal agent, the functionality of the indirect reaction with isocyanate is 2, water and a defoaming agent in the system are removed by decomposing water-sensitive oxazolidine and consuming water, the defoaming agent adopts a high-alcohol fatty acid ester compound and accounts for 1% of the total weight of the system, the mechanism is that higher alcohol or vegetable oil is scattered on foam, when the foam is dissolved in foam liquid, the surface tension of the foam is remarkably reduced, because the substances generally have low water solubility, the reduction of the surface tension is limited to the local part of the foam, the surface tension around the foam is hardly changed, and the part with the reduced surface tension is strongly pulled around the foam, Extending, finally breaking and leveling agent, wherein the leveling agent is an acrylate leveling agent and accounts for 1% of the total weight of the system, the controllability of the acrylate leveling agent is realized by changing the molecular weight and the polarity, the compatibility of a homopolymer is not good as that of a copolymer, for example, homopolymerized acrylic acid is generally poor in compatibility with resin used by epoxy, polyester, polyurethane and other coatings, and a dull coating film with a poor surface state is formed if the homopolymerized acrylic acid is mixed by a physical method, so that the acrylate homopolymer is not suitable for being used as the leveling agent, the ideal leveling agent mostly adopts a copolymer, can be a terpolymer or a modified copolymer, only the copolymer can change the polarity of the polymer through different monomers, and the glass flower temperature and the storage stabilizer are both high, the storage stabilizer adopts organic tin and accounts for 2% of the total weight of the system, and the highest advantage of the excellent transparent organic tin stabilizer is that the excellent transparency is realized, the use of organotin stabilizers in PVC formulations allows the production of crystalline articles, and as such, organotin is the preferred stabilizer for rigid PVC, and for flexible articles, including all PVC homopolymers such as emulsion, suspension and bulk PVC, and copolymers, graft and blend polymers of vinyl chloride, for which the majority of organotin stabilizers are non-toxic, and which have minimal migration in rigid PVC, and thus are preferred heat stabilizers for food contact PVC, and which are agitated for 20 minutes.
S2: adding epoxy resin which is a polycondensation product of epoxy chloropropane and bisphenol A and accounts for 76% of the total weight of the system, and fully stirring and dissolving the epoxy resin.
S3: adding a silane coupling agent, wherein the silane coupling agent is butadiene-based triethoxysilane and accounts for 15% of the total weight of the system, and the weight ratio of the epoxy resin to the silane coupling agent is 1: 0.2, and the temperature is raised to 55 degrees.
S4: preserving the temperature for 4 hours to obtain a transparent product.
Example two:
a synthetic method of a solvent-type organic silicon modified epoxy resin coating comprises the following steps:
s1, adding a solvent into a reaction kettle, wherein the solvent is selected from any one of alcohols, ketones, ethers and aromatic hydrocarbon solvents, a water removal agent, the water removal agent adopts ALT-201 water removal agent, 6% of the total weight of the system, the ALT-201 is a low-toxicity mono-oxazolidine drying agent and a moisture removal agent, the functionality of the indirect reaction with isocyanate is 2, water and a defoaming agent in the system are removed by decomposing water-sensitive oxazolidine and consuming water, the defoaming agent adopts a high-alcohol fatty acid ester compound and accounts for 2% of the total weight of the system, the mechanism is that higher alcohol or vegetable oil is scattered on foam, when the foam is dissolved in foam liquid, the surface tension of the foam is remarkably reduced, because the substances generally have low water solubility, the reduction of the surface tension is limited to the local part of the foam, the surface tension around the foam is hardly changed, and the part with the reduced surface tension is strongly pulled around the foam, Extending, finally breaking and leveling agent, the leveling agent is an acrylate leveling agent and accounts for 3% of the total weight of the system, the controllability of the acrylate leveling agent is realized by changing the molecular weight and the polarity, the compatibility of a homopolymer is not good as that of a copolymer, for example, homopolymerized acrylic acid is generally poor in compatibility with resin used by epoxy, polyester, polyurethane and other coatings, and a dull coating film with poor surface state is formed if the homopolymerized acrylic acid is mixed by a physical method, so the acrylate homopolymer is not suitable for being used as the leveling agent, the ideal leveling agent mostly adopts a copolymer, can be a terpolymer or a modified copolymer, only the copolymer can change the polarity of the polymer through different monomers, and the glass flower temperature and the storage stabilizer adopt organic tin, account for 3% of the total weight of the system, and the most excellent transparent organic tin stabilizer has the advantage of excellent transparency, the use of organotin stabilizers in PVC formulations allows the production of crystalline articles, and as such, organotin is the preferred stabilizer for rigid PVC, and for flexible articles, including all PVC homopolymers such as emulsion, suspension and bulk PVC, and copolymers, graft and blend polymers of vinyl chloride, for which the majority of organotin stabilizers are non-toxic, and which are preferred for food contact PVC, stirring for 40 minutes.
S2: adding epoxy resin which is a polycondensation product of epoxy chloropropane and bisphenol A and accounts for 43 percent of the total weight of the system, and fully stirring and dissolving the epoxy resin.
S3: adding a silane coupling agent which is butadiene-triethoxy silane and accounts for 43 percent of the total weight of the system, wherein the weight ratio of the epoxy resin to the silane coupling agent is 1: 1 and the temperature is raised to 75 degrees.
S4: and preserving the heat for 6 hours to obtain a transparent product.
Example three:
a synthetic method of a solvent-type organic silicon modified epoxy resin coating comprises the following steps:
s1, adding a solvent into a reaction kettle, wherein the solvent is selected from any one of alcohols, ketones, ethers and aromatic hydrocarbon solvents, a water removal agent, the water removal agent adopts ALT-201 water removal agent, the total weight of the system is 8%, the ALT-201 is a low-toxicity mono-oxazolidine drying agent and a moisture removal agent, the functionality of the indirect reaction with isocyanate is 2, water and a defoaming agent in the system are removed by decomposing water-sensitive oxazolidine and consuming water, the defoaming agent adopts a high-alcohol fatty acid ester compound and accounts for 3% of the total weight of the system, the mechanism is that higher alcohol or vegetable oil is scattered on foam, when the foam is dissolved in foam liquid, the surface tension of the foam is remarkably reduced, because the substances generally have low water solubility, the reduction of the surface tension is limited to the local part of the foam, the surface tension around the foam is hardly changed, and the part with the reduced surface tension is strongly pulled around the foam, Extending, finally breaking and leveling agent, wherein the leveling agent is an acrylate leveling agent and accounts for 4% of the total weight of the system, the controllability of the acrylate leveling agent is realized by changing the molecular weight and polarity, the compatibility of a homopolymer is not good as that of a copolymer, for example, homopolymerized acrylic acid is generally poor in compatibility with resins used by epoxy, polyester, polyurethane and other coatings, and a dull coating film with a poor surface state is formed if the homopolymerized acrylic acid is mixed by a physical method, so that the acrylate homopolymer is not suitable for being used as the leveling agent, the ideal leveling agent mostly adopts a copolymer, can be a terpolymer or a modified copolymer, only the copolymer can change the polarity of the polymer through different monomers, and the glass flower temperature and the storage stabilizer are both storage stabilizers and organotin is adopted as the storage stabilizer and accounts for 4% of the total weight of the system, and the most remarkable advantage of the transparent organotin stabilizer is that the transparency is excellent, the use of organotin stabilizers in PVC formulations allows the production of crystalline articles, and as such, organotin is the preferred stabilizer for rigid PVC, and for flexible articles, including all PVC homopolymers such as emulsion, suspension and bulk PVC, and copolymers, graft and blend polymers of vinyl chloride, for which the majority of organotin stabilizers are non-toxic, and which are preferred for food contact PVC, stirring for 50 minutes.
S2: adding epoxy resin which is a polycondensation product of epoxy chloropropane and bisphenol A and accounts for 27% of the total weight of the system, and fully stirring and dissolving the epoxy resin.
S3: adding a silane coupling agent, wherein the silane coupling agent is butadiene-based triethoxysilane and accounts for 54% of the total weight of the system, and the weight ratio of the epoxy resin to the silane coupling agent is 1: 2 and the temperature is raised to 85 degrees.
S4: after the temperature is kept for 7 hours, a light yellow product can be obtained.
Example four:
a synthetic method of a solvent-type organic silicon modified epoxy resin coating comprises the following steps:
s1, adding a solvent into a reaction kettle, wherein the solvent is selected from any one of alcohols, ketones, ethers and aromatic hydrocarbon solvents, a water removal agent, the water removal agent adopts ALT-201 water removal agent, the total weight of the system is 10%, the ALT-201 is a low-toxicity mono-oxazolidine drying agent and a moisture removal agent, the functionality of the indirect reaction with isocyanate is 2, water and a defoaming agent in the system are removed by decomposing water-sensitive oxazolidine and consuming water, the defoaming agent adopts a high-alcohol fatty acid ester compound and accounts for 5% of the total weight of the system, the mechanism is that higher alcohol or vegetable oil is scattered on foam, when the foam is dissolved in foam liquid, the surface tension of the foam is remarkably reduced, because the substances generally have low water solubility, the reduction of the surface tension is limited to the local part of the foam, the surface tension around the foam is hardly changed, and the part with the reduced surface tension is strongly pulled around the foam, Extending, finally breaking and leveling agent, wherein the leveling agent is an acrylate leveling agent and accounts for 5% of the total weight of the system, the controllability of the acrylate leveling agent is realized by changing the molecular weight and polarity, the compatibility of a homopolymer is not good as that of a copolymer, for example, homopolymerized acrylic acid is generally poor in compatibility with resins used by epoxy, polyester, polyurethane and other coatings, and a dull coating film with a poor surface state is formed if the homopolymerized acrylic acid is mixed by a physical method, so that the acrylate homopolymer is not suitable for being used as the leveling agent, the ideal leveling agent mostly adopts a copolymer, can be a terpolymer or a modified copolymer, only the copolymer can change the polarity of the polymer through different monomers, and the glass flower temperature and the storage stabilizer are both storage stabilizers, the storage stabilizer adopts organic tin and accounts for 5% of the total weight of the system, and the most excellent transparent organic tin stabilizer has the advantage of excellent transparency, the use of organotin stabilizers in PVC formulations allows the production of crystalline articles, and as such, organotin is the preferred stabilizer for rigid PVC, and for flexible articles, including all PVC homopolymers such as emulsion, suspension and bulk PVC, and copolymers, graft and blend polymers of vinyl chloride, for which the majority of organotin stabilizers are non-toxic, and for which the migration of organotin stabilizers in rigid PVC is minimal, and which is the preferred stabilizer for food contact PVC, and which is stirred for 60 minutes.
S2: adding epoxy resin, a polycondensation product of epoxy chloropropane and bisphenol A, accounting for 16% of the total weight of the system, and fully stirring and dissolving the epoxy resin and the polycondensation product.
S3: adding a silane coupling agent which is butadiene-triethoxy silane and accounts for 59% of the total weight of the system, wherein the weight ratio of the epoxy resin to the silane coupling agent is 1: 3.7, and the temperature is raised to 95 ℃.
S4: keeping the temperature for 8 hours to obtain a light yellow product.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. A synthetic method of a solvent-type organic silicon modified epoxy resin coating comprises the following steps:
s1, adding a solvent, a water removing agent, a defoaming agent, a flatting agent and a storage stabilizer into the reaction kettle, and stirring for 10-60 minutes;
s2: adding epoxy resin, and fully stirring and dissolving the epoxy resin;
s3: adding a silane coupling agent, and raising the temperature to 55-95 ℃;
s4: keeping the temperature for 4 to 8 hours to obtain a transparent or light yellow product.
2. The method for synthesizing the solvent-type silicone modified epoxy resin coating according to claim 1, wherein the method comprises the following steps: the epoxy resin in the S2 is a polycondensation product of epoxy chloropropane and bisphenol A, and accounts for 16-76% of the total weight of the system, the S3 silane coupling agent is butadiene-based triethoxysilane, and accounts for 15-59% of the total weight of the system, and the weight ratio of the epoxy resin to the silane coupling agent is 1: 0.2-3.8.
3. The method for synthesizing the solvent-type silicone modified epoxy resin coating according to claim 1, wherein the method comprises the following steps: the solvent in the S1 is selected from any one of alcohols, ketones, ethers and aromatic hydrocarbon solvents, and the defoaming agent is a high-carbon alcohol fatty acid ester compound and accounts for 1-5% of the total weight of the system.
4. The method for synthesizing the solvent-type silicone modified epoxy resin coating according to claim 1, wherein the method comprises the following steps: the leveling agent in the S1 adopts an acrylate leveling agent and accounts for 1-5% of the total weight of the system.
5. The method for synthesizing the solvent-type silicone modified epoxy resin coating according to claim 1, wherein the method comprises the following steps: the water removing agent in the S1 is ALT-201 water removing agent, and the total weight of the system is 5-10%.
6. The method for synthesizing the solvent-type silicone modified epoxy resin coating according to claim 1, wherein the method comprises the following steps: the storage stabilizer in the S1 adopts organotin and accounts for 2-5% of the total weight of the system.
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Cited By (1)
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