CN112574637A - Preparation method of nano modified solvent-free epoxy ceramic coating - Google Patents
Preparation method of nano modified solvent-free epoxy ceramic coating Download PDFInfo
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- 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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- 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
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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
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/61—Additives non-macromolecular inorganic
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- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a preparation method of a nano modified solvent-free epoxy ceramic coating, which comprises a component A and a component B, wherein the component A is a main material, the component A comprises liquid epoxy resin, silicon carbide, precipitated barium sulfate, ceramic micro powder, nano modified epoxy resin and a defoaming agent, and the percentages of the liquid epoxy resin, the silicon carbide, the precipitated barium sulfate ceramic micro powder, the nano modified epoxy resin and the defoaming agent are respectively 35-70%, 11-27%, 15-25%, 2-7%, 1.6-5% and 0.4-1.0%. The invention improves the prior art in a breakthrough manner, the nano modified solvent-free epoxy resin is formed by uniformly dispersing the nano modified epoxy resin into the liquid epoxy resin, and the nano modified solvent-free epoxy resin is prepared into the nano modified solvent-free epoxy ceramic coating.
Description
Technical Field
The invention relates to the technical field of solvent-free epoxy materials, in particular to a preparation method of a nano modified solvent-free epoxy ceramic coating.
Background
Products prepared from the coating and the adhesive prepared from the epoxy resin are widely applied to the fields of national defense, petrochemical industry, machinery, electronics and the like. In actual use, Volatile Solvents (VOCs) are used for dissolving, the Volatile Solvents (VOCs) cause environmental pollution, and potential safety hazards are easily generated in production and use; due to the use of an emulsifier, the waterborne epoxy resin has poor comprehensive corrosion resistance and protective performance, and the application field of the waterborne epoxy resin is limited. Thus, solventless epoxy materials are very important and preferred.
Chinese patent ZL 02155418.8 discloses a solvent-free epoxy ceramic coating, which is prepared by taking epoxy resin as a main material and adding quartz powder and an auxiliary agent, wherein a polyamine curing agent is used as a curing agent and added with the quartz powder and the auxiliary agent.
Chinese patent ZL 200410088518 discloses a solvent-free epoxy ceramic paint, which comprises a component A consisting of modified epoxy resin, quartz powder, an anti-settling agent, a thickening agent, a flatting agent and a foam inhibitor; the component B consists of a curing agent, quartz powder, an anti-settling agent, a toughening agent, a flatting agent, an accelerant and a defoaming agent. The A, B components are mixed evenly in site in a mass ratio of 1: 1 to form the two-component epoxy ceramic paint.
As shown in the above patent for the solvent-free epoxy ceramic paint, the domestic solvent-free epoxy ceramic paint is mainly prepared by taking epoxy resin as a main material and adding quartz powder, an anti-settling agent, a thickening agent, a leveling agent and a foam inhibitor, and the curing agent is prepared by adding a polyamine curing agent into auxiliary agents such as quartz powder, an anti-settling agent, a thickening agent, a leveling agent, a foam inhibitor and the like. As the quartz powder is added into the ceramic coating, the strength of the ceramic coating is improved, but the flexibility of the coating is reduced and the brittleness is increased. In addition, the auxiliaries such as the anti-settling agent, the thickening agent, the flatting agent and the foam inhibitor are mainly surfactants, and the addition of various auxiliaries can reduce the corrosion resistance and the protective performance of the coating film.
The epoxy resin coating has excellent performance, is difficult to construct due to larger viscosity, has good leveling property and is easy to sag, so the solvent-free epoxy coating has the difficulty of solving the problem of low viscosity of the construction performance, and simultaneously ensures that the sagging is not generated under the condition of larger coating thickness. The current solution to these problems is mainly to use auxiliaries, which in turn reduce the corrosion and protective properties of the coating.
Disclosure of Invention
The invention aims to provide a preparation method of a nano modified solvent-free epoxy ceramic coating, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a nano modified solvent-free epoxy ceramic coating comprises a component A and a component B, wherein the component A is a main material, the component A comprises liquid epoxy resin, silicon carbide, precipitated barium sulfate, ceramic micro powder, nano modified epoxy resin and a defoaming agent, the percentages of the liquid epoxy resin, the silicon carbide, the precipitated barium sulfate ceramic micro powder, the nano modified epoxy resin and the defoaming agent are respectively 35-70%, 11-27%, 15-25%, 2-7%, 1.6-5% and 0.4-1.0%, the component B is a curing agent, and the component B is an aliphatic polyamine compound.
Preferably, the amine value of the aliphatic polyamine compound in the component B is between 300 and 400 mgKOH/g.
Preferably, the mass ratio of the component A to the component B is 3-5: 1.
Preferably, the preparation steps of the nano modified solvent-free epoxy ceramic coating are as follows:
step S1: 60-70% of hexadecyl trimethyl ammonium bromide and liquid epoxy resin at room temperature: 30-40% (mass ratio) mixing;
step S2: heating 87 parts of deionized water, 1-4 parts of isopropanol and 1-4 parts of N-methyl pyrrolidone to 45-55 ℃, adding 8 parts of the mixture under stirring (80-200 revolutions per minute), and continuing stirring for 30min after the addition is finished;
step S3: adding 20 parts of sodium-based montmorillonite (the particle size is less than 200 meshes) into the liquid, and reacting at 60-75 ℃ for 150-180 min;
step S4: and filtering the reactants, washing the ground by deionized water, dehydrating, drying at 100 ℃, and grinding to obtain the nano modified epoxy resin.
Preferably, the epoxy equivalent of the liquid epoxy resin used in step S1 is between 160-200.
Preferably, the isopropanol and the N-methylpyrrolidone used in the step S1 are complex intercalation aids.
Preferably, in the step S2, a thermometer and a time switch are provided in the process of heating 87 parts of deionized water, 1-4 parts of isopropanol and 1-4 parts of N-methylpyrrolidone to 45-55 ℃.
Preferably, in the step S3, 20 parts of sodium-based montmorillonite (the particle size is less than 200 meshes) is added into the liquid, and an insulation board is arranged outside the equipment container in the process of reacting at 60-75 ℃ for 150-180 min.
Preferably, in the step S4, the two filter screens with different filter diameters are arranged in the process of filtering the reactant, washing the ground with deionized water, dehydrating, drying at 100 ℃, and grinding to obtain the nano modified epoxy resin.
Preferably, the application method of the nano modified solvent-free epoxy ceramic coating is as follows:
the first step is as follows: adding the nano modified epoxy resin into the liquid solvent-free epoxy resin under stirring at room temperature, and stirring for 30min at 1000-1200 rpm to ensure uniform mixing;
the second step is that: adding silicon carbide, precipitated barium sulfate, ceramic micro powder and a defoaming agent into the mixture at room temperature under stirring, and uniformly stirring and grinding to obtain a component A;
the third step: and adding the component B into the component A, and fully and uniformly mixing to obtain the product.
Compared with the prior art, the invention has the beneficial effects that:
the invention improves the prior art in a breakthrough way, the nano modified solvent-free epoxy resin is formed by uniformly dispersing the nano modified epoxy resin into the liquid epoxy resin, and the nano modified solvent-free epoxy resin is prepared into the nano modified solvent-free epoxy ceramic coating.
Drawings
FIG. 1 is a flow chart of a method for preparing a nano-modified solvent-free epoxy ceramic coating according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a nano modified solvent-free epoxy ceramic coating comprises a component A and a component B, wherein the component A is a main material, the component A comprises liquid epoxy resin, silicon carbide, precipitated barium sulfate, ceramic micro powder, nano modified epoxy resin and a defoaming agent, the percentages of the liquid epoxy resin, the silicon carbide, the precipitated barium sulfate ceramic micro powder, the nano modified epoxy resin and the defoaming agent are respectively 35-70%, 11-27%, 15-25%, 2-7%, 1.6-5% and 0.4-1.0%, the component B is a curing agent, and the component B is an aliphatic polyamine compound.
The amine value of the aliphatic polyamine compound in the component B of the present invention is between 300 and 400 mgKOH/g.
The mass ratio of the component A to the component B is 3-5: 1.
1. Preparation of nano modified epoxy resin
Step S1: uniformly mixing 20g of hexadecyl trimethyl ammonium bromide and 12g of liquid epoxy resin at room temperature;
step S2: heating 348g of deionized water, 12g of isopropanol and 8g of N-methylpyrrolidone to 45-55 ℃, adding 32g of the mixture under stirring (80-200 revolutions per minute), and continuing stirring for 30min after the addition is finished;
step S3: adding 40g of sodium-based montmorillonite (the particle size is less than 200 meshes) into the liquid, and reacting at 60-75 ℃ for 150-180 min;
step S4: and filtering the reactants, washing the ground by deionized water, dehydrating, drying at 100 ℃, and grinding to obtain the nano modified epoxy resin.
The epoxy equivalent of the liquid epoxy resin used in step S1 of the present invention is between 160-200.
Isopropanol and N-methyl pyrrolidone used in step S1 of the present invention are complex intercalation aids.
In step S2, 87 parts of deionized water, 1-4 parts of isopropanol and 1-4 parts of N-methyl pyrrolidone are heated to 45-55 ℃, and a thermometer and a timing switch are arranged.
In the step S3, 20 parts of sodium montmorillonite (the particle size is less than 200 meshes) is added into the liquid, and a heat insulation plate is arranged outside the equipment container in the process of reacting at 60-75 ℃ for 150-180 min.
In the step S4, the reactants are filtered, washed with deionized water, dehydrated, dried at 100 ℃ and ground, and two filter screens with different filter diameters are arranged in the process of obtaining the nano modified epoxy resin.
2. Preparation of nano modified solvent-free epoxy ceramic coating component A
60g of the prepared nano modified epoxy resin is added into 500g of liquid solvent-free epoxy resin at normal temperature, dispersed at high speed of 1000-1200 rpm for 30min, then added with 180g of silicon carbide, 210g of precipitated barium sulfate, 50g of ceramic micropowder and 5g of defoaming agent under stirring, and ground uniformly.
3. Preparation of component B
The component B is 340-350mgKOH/g aliphatic polyamine compound.
4. Preparation of the product
The invention relates to a nano modified solvent-free epoxy ceramic coating, which comprises the following steps:
the first step is as follows: adding the nano modified epoxy resin into the liquid solvent-free epoxy resin under stirring at room temperature, and stirring for 30min at 1000-1200 rpm to ensure uniform mixing;
the second step is that: adding silicon carbide, precipitated barium sulfate, ceramic micro powder and a defoaming agent into the mixture at room temperature under stirring, and uniformly stirring and grinding to obtain a component A;
the third step: the component A and the component B are mixed and stirred uniformly according to the ratio of 4:1 to obtain the product of the invention.
Example 2
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a nano modified solvent-free epoxy ceramic coating comprises a component A and a component B, wherein the component A is a main material, the component A comprises liquid epoxy resin, silicon carbide, precipitated barium sulfate, ceramic micro powder, nano modified epoxy resin and a defoaming agent, the percentages of the liquid epoxy resin, the silicon carbide, the precipitated barium sulfate ceramic micro powder, the nano modified epoxy resin and the defoaming agent are respectively 35-70%, 11-27%, 15-25%, 2-7%, 1.6-5% and 0.4-1.0%, the component B is a curing agent, and the component B is an aliphatic polyamine compound.
The amine value of the aliphatic polyamine compound in the component B of the present invention is between 300 and 400 mgKOH/g.
The mass ratio of the component A to the component B is 3-5: 1.
1. Preparation of stone nano modified epoxy resin
Step S1: mixing 22g of hexadecyl trimethyl ammonium bromide and 10g of liquid epoxy resin uniformly at room temperature;
step S2: heating 348g of deionized water, 10g of isopropanol and 6g of N-methylpyrrolidone to 45-55 ℃, adding 32g of the mixture under stirring (80-200 revolutions per minute), and continuing stirring for 30min after the addition is finished;
step S3: adding 40g of sodium-based montmorillonite (the particle size is less than 200 meshes) into the liquid, and reacting at 60-75 ℃ for 150-180 min;
step S4: and filtering the reactants, washing the ground by deionized water, dehydrating, drying at 100 ℃, and grinding to obtain the nano modified epoxy resin.
The epoxy equivalent of the liquid epoxy resin used in step S1 of the present invention is between 160-200.
Isopropanol and N-methyl pyrrolidone used in step S1 of the present invention are complex intercalation aids.
In step S2, 87 parts of deionized water, 1-4 parts of isopropanol and 1-4 parts of N-methyl pyrrolidone are heated to 45-55 ℃, and a thermometer and a timing switch are arranged.
In the step S3, 20 parts of sodium montmorillonite (the particle size is less than 200 meshes) is added into the liquid, and a heat insulation plate is arranged outside the equipment container in the process of reacting at 60-75 ℃ for 150-180 min.
In the step S4, the reactants are filtered, washed with deionized water, dehydrated, dried at 100 ℃ and ground, and two filter screens with different filter diameters are arranged in the process of obtaining the nano modified epoxy resin.
2. Preparation of nano modified solvent-free epoxy ceramic coating component A
40g of the prepared nano modified epoxy resin is added into 380g of liquid solvent-free epoxy resin at normal temperature, dispersed at high speed of 1000-1200 rpm for 30min, then added with 265g of silicon carbide, 242g of precipitated barium sulfate, 65g of ceramic micropowder and 8g of defoaming agent under stirring, and ground uniformly.
3. Preparation of component B
The component B is 340-350mgKOH/g aliphatic polyamine compound.
4. Preparation of the product
The invention relates to a nano modified solvent-free epoxy ceramic coating, which comprises the following steps:
the first step is as follows: adding the nano modified epoxy resin into the liquid solvent-free epoxy resin under stirring at room temperature, and stirring for 30min at 1000-1200 rpm to ensure uniform mixing;
the second step is that: adding silicon carbide, precipitated barium sulfate, ceramic micro powder and a defoaming agent into the mixture at room temperature under stirring, and uniformly stirring and grinding to obtain a component A;
the third step: the component A and the component B are mixed and stirred uniformly according to the proportion of 5:1 to obtain the product of the invention.
Example 3
Referring to fig. 1, the present invention provides a technical solution: a preparation method of a nano modified solvent-free epoxy ceramic coating comprises a component A and a component B, wherein the component A is a main material, the component A comprises liquid epoxy resin, silicon carbide, precipitated barium sulfate, ceramic micro powder, nano modified epoxy resin and a defoaming agent, the percentages of the liquid epoxy resin, the silicon carbide, the precipitated barium sulfate ceramic micro powder, the nano modified epoxy resin and the defoaming agent are respectively 35-70%, 11-27%, 15-25%, 2-7%, 1.6-5% and 0.4-1.0%, the component B is a curing agent, and the component B is an aliphatic polyamine compound.
The amine value of the aliphatic polyamine compound in the component B of the present invention is between 300 and 400 mgKOH/g.
The mass ratio of the component A to the component B is 3-5: 1.
1. Preparation of nano modified epoxy resin
Step S1: uniformly mixing 20g of hexadecyl trimethyl ammonium bromide and 12g of liquid epoxy resin at room temperature;
step S2: heating 348g of deionized water, 12g of isopropanol and 8g of N-methylpyrrolidone to 45-55 ℃, adding 32g of the mixture under stirring (80-200 revolutions per minute), and continuing stirring for 30min after the addition is finished;
step S3: adding 40g of sodium-based montmorillonite (the particle size is less than 200 meshes) into the liquid, and reacting at 60-75 ℃ for 150-180 min;
step S4: and filtering the reactants, washing the ground by deionized water, dehydrating, drying at 100 ℃, and grinding to obtain the nano modified epoxy resin.
The epoxy equivalent of the liquid epoxy resin used in step S1 of the present invention is between 160-200.
Isopropanol and N-methyl pyrrolidone used in step S1 of the present invention are complex intercalation aids.
In step S2, 87 parts of deionized water, 1-4 parts of isopropanol and 1-4 parts of N-methyl pyrrolidone are heated to 45-55 ℃, and a thermometer and a timing switch are arranged.
In the step S3, 20 parts of sodium montmorillonite (the particle size is less than 200 meshes) is added into the liquid, and a heat insulation plate is arranged outside the equipment container in the process of reacting at 60-75 ℃ for 150-180 min.
In the step S4, the reactants are filtered, washed with deionized water, dehydrated, dried at 100 ℃ and ground, and two filter screens with different filter diameters are arranged in the process of obtaining the nano modified epoxy resin.
2. Preparation of nano modified solvent-free epoxy ceramic coating component A
Adding 55g of the prepared nano modified epoxy resin into 650g of liquid solvent-free epoxy resin at normal temperature, dispersing at a high speed of 1200 rpm for 30min at 1000-.
4. Preparation of component B
The component B is 340-350mgKOH/g aliphatic polyamine compound.
4. Preparation of the product
The invention relates to a nano modified solvent-free epoxy ceramic coating, which comprises the following steps:
the first step is as follows: adding the nano modified epoxy resin into the liquid solvent-free epoxy resin under stirring at room temperature, and stirring for 30min at 1000-1200 rpm to ensure uniform mixing;
the second step is that: adding silicon carbide, precipitated barium sulfate, ceramic micro powder and a defoaming agent into the mixture at room temperature under stirring, and uniformly stirring and grinding to obtain a component A;
the third step: the component A and the component B are mixed and stirred uniformly according to the proportion of 5:1 to obtain the product of the invention.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A preparation method of a nano modified solvent-free epoxy ceramic coating comprises a component A and a component B, and is characterized in that: the component A is a main material and comprises 35-70% of liquid epoxy resin, 11-27% of silicon carbide, 2-7% of precipitated barium sulfate ceramic micro powder, 1.6-5% of nano modified epoxy resin and 0.4-1.0% of defoaming agent, 15-25% of silicon carbide, 2-7% of precipitated barium sulfate ceramic micro powder and 0.4-1.0% of fatty polyamine compound.
2. The preparation method of the nano-modified solvent-free epoxy ceramic coating according to claim 1, characterized in that: the amine value of the aliphatic polyamine compound in the component B is between 300 and 400 mgKOH/g.
3. The preparation method of the nano-modified solvent-free epoxy ceramic coating according to claim 1, characterized in that: the mass ratio of the component A to the component B is 3-5: 1.
4. The nano-modified solvent-free epoxy ceramic coating as claimed in claim 1, wherein the nano-modified epoxy resin is prepared by the following steps:
step S1: 60-70% of hexadecyl trimethyl ammonium bromide and liquid epoxy resin at room temperature: 30-40% (mass ratio) mixing;
step S2: heating 87 parts of deionized water, 1-4 parts of isopropanol and 1-4 parts of N-methyl pyrrolidone to 45-55 ℃, adding 8 parts of the mixture under stirring (80-200 revolutions per minute), and continuing stirring for 30min after the addition is finished;
step S3: adding 20 parts of sodium-based montmorillonite (the particle size is less than 200 meshes) into the liquid, and reacting at 60-75 ℃ for 150-180 min;
step S4: and filtering the reactants, washing the ground by deionized water, dehydrating, drying at 100 ℃, and grinding to obtain the nano modified epoxy resin.
5. The preparation method of the nano-modified solvent-free epoxy ceramic coating according to claim 4, characterized in that: the epoxy equivalent of the liquid epoxy resin used in the step S1 is between 160-200.
6. The preparation method of the nano-modified solvent-free epoxy ceramic coating according to claim 1, characterized in that: the isopropanol and the N-methyl pyrrolidone used in the step S1 are composite intercalation aids.
7. The preparation method of the nano-modified solvent-free epoxy ceramic coating according to claim 4, characterized in that: in the step S2, a thermometer and a timing switch are arranged in the process of heating 87 parts of deionized water, 1-4 parts of isopropanol and 1-4 parts of N-methyl pyrrolidone to 45-55 ℃.
8. The preparation method of the nano-modified solvent-free epoxy ceramic coating according to claim 4, characterized in that: in the step S3, 20 parts of sodium montmorillonite (the particle size is less than 200 meshes) is added into the liquid, and a heat insulation plate is arranged outside the equipment container in the process of reacting at 60-75 ℃ for 150-180 min.
9. The preparation method of the nano-modified solvent-free epoxy ceramic coating according to claim 4, characterized in that: and in the step S4, the reactant is filtered, the ground is washed by deionized water, the dehydrated, dried at 100 ℃ and ground, and two filter screens with different filter diameters are arranged in the process of obtaining the nano modified epoxy resin.
10. The nano-modified solvent-free epoxy ceramic coating as claimed in claims 1, 2, 3 and 4, which is prepared by the following steps:
the first step is as follows: adding the nano modified epoxy resin into the liquid solvent-free epoxy resin under stirring at room temperature, and stirring for 30min at 1000-1200 rpm to ensure uniform mixing;
the second step is that: adding silicon carbide, precipitated barium sulfate, ceramic micro powder and a defoaming agent into the mixture at room temperature under stirring, and uniformly stirring and grinding to obtain a component A;
the third step: and adding the component B into the component A, and fully and uniformly mixing to obtain the product.
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| CN113773720A (en) * | 2021-09-10 | 2021-12-10 | 南京卓煌工业技术有限公司 | Storage tank base composite anticorrosive material and method |
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