CN107974143B - Corrosion-resistant glass flake resin - Google Patents
Corrosion-resistant glass flake resin Download PDFInfo
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- CN107974143B CN107974143B CN201710666014.0A CN201710666014A CN107974143B CN 107974143 B CN107974143 B CN 107974143B CN 201710666014 A CN201710666014 A CN 201710666014A CN 107974143 B CN107974143 B CN 107974143B
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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
- C09D141/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a bond to sulfur or by a heterocyclic ring containing sulfur; Coating compositions based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F216/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F216/12—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an ether radical
- C08F216/14—Monomers containing only one unsaturated aliphatic radical
- C08F216/1416—Monomers containing oxygen in addition to the ether oxygen, e.g. allyl glycidyl ether
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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
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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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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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Abstract
The corrosion-resistant glass flake resin comprises a component A and a component B, wherein the component A is prepared from the following raw materials: allyl glycidyl ether, vinyl thiophene, mercaptosilane, aminosilane, vinyl benzimidazole, glass flake, titanium dioxide, methyl isobutyl ketone, calcium carbonate and dimethyl silicone oil; the preparation raw materials of the component B comprise: pentaerythritol glycidyl ether, 2-aminomethyl-15-crown-5, tetrahydrofurfuryl alcohol; the weight ratio of the component A to the component B is 1: (0.2-0.4).
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to corrosion-resistant glass flake resin.
Background
In the modern society, scientific technology is rapidly advanced, global economy is rapidly developed, the requirements of people on the quality of industrial equipment, machines, buildings and the like are higher and higher, and more metal materials are widely applied to the fields of buildings, petroleum, aerospace, pipelines and the like. However, they are inevitably corrosive when used in various environments. Equipment failure, machine stall, etc. caused by corrosion of metallic materials can cause great accidents. Particularly, in the equipment for desulfurization and denitrification treatment, the corrosion of sulfuric acid and nitric acid exists for a long time, and the aging and the failure of the pipeline are accelerated.
The damage caused by the chemical and electrochemical action between the surface of the metal material and the medium in the surrounding environment is called metal corrosion, and the combined action of the above factors and mechanical factors or biological factors is included. Metal corrosion is a reaction system in which it involves the interaction of a metallic material with a corrosive medium under certain conditions (pressure, temperature, flow rate of the medium, etc.). Therefore, general mechanical damage (such as the breakage of an iron cable and the abrasion of mechanical parts) of the metal material and the metal alloy is not the metal corrosion, which is the damage caused by the performance failure of the metal material.
Most metals exist in a compound state in natural ores, oxides in the compound state cannot be utilized in production or life, and the metals can be widely applied only by converting the metals from the compound state into a free state through smelting. However, most of the metals in a free state except for a few inactive metals (such as gold, uranium, etc.) are chemically highly active in nature and in an unstable state, and they react with a medium such as water, oxygen, etc. in the surrounding environment to generate oxides, and the metal materials are gradually corroded and destroyed.
When a metal corrodes, since a corrosive medium first comes into contact with the surface of the metal material when the metal material corrodes, the surface of the metal material is first damaged and then the damage penetrates into the metal material. As the metal material corrodes, rust spots and cracks are generated on the surface of the metal material, and reaction substances are generated. When the metal material is corroded to a certain degree, the metal material becomes brittle, the mechanical strength is reduced, and the structure undergoes phase change. Before the metallic material is not sufficiently corroded to fail, it may cause machine failure or personal injury.
The glass flakes are prepared from molten medium-alkali glass with the temperature of over 1200 ℃ by the process steps of bubbling, cooling, crushing, screening, grinding and the like. The anticorrosive coating using the glass flake as filler has high binding power and excellent chemical resistance and ageing resistance.
The anticorrosive paint for glass flakes is a thick paste type paint which is composed of anticorrosive resin as a main film forming substance, fine flaky glass powder as an aggregate and various additives. The coating can be thickly coated, and has good anti-seepage effect on water, water vapor, electrolyte and oxygen due to great isolation effect of the flaky glass powder, so the coating is an excellent heavy anti-corrosion coating.
The glass scale is far less permeated by media, gas and water vapor than the common glass fiber reinforced plastics. Medium diffusion is not easy to generate, and physical damage such as bottom corrosion, dispersion, bubbling, stripping and the like can be effectively avoided. And the shrinkage rate is small when the resin is hardened. Because the stress is dispersed by the glass flakes, the residual stress of each contact surface is small, the thermal expansion coefficient is also small, so the bonding strength cannot be attenuated due to thermal expansion, and the thermal stability is good. The wear resistance and the scratch resistance are strong, the mechanical damage is only limited to local parts, and the diffusion tendency is small. After several years of use, the damaged part can be repaired by simple treatment. Has strong adaptability to the protective surface and is suitable for the corrosion prevention of complex surfaces. The scale can be applied by spraying, rolling, scraping and other methods, the integrity is good, the on-site burdening is convenient, and the scale can be cured at room temperature and thermally.
However, the glass flake coating still has some problems, such as that the glass flake is an inorganic material, has great brittleness, poor compatibility with organic polymers, low glass thermal conductivity, and is not beneficial to improving the heat resistance of the coating, poor weather resistance and the like. Particularly poor corrosion resistance to fluorine.
Disclosure of Invention
In order to solve the problems of the prior art, the first aspect of the invention provides a corrosion-resistant glass flake resin, which comprises a component A and a component B, wherein the component A is prepared from the following raw materials: allyl glycidyl ether, vinyl thiophene, mercaptosilane, aminosilane, vinyl benzimidazole, glass flake, titanium dioxide, methyl isobutyl ketone, calcium carbonate and dimethyl silicone oil; the preparation raw materials of the component B comprise: pentaerythritol glycidyl ether, 2-aminomethyl-15-crown-5, tetrahydrofurfuryl alcohol; the weight ratio of the component A to the component B is 1: (0.2-0.4).
In some embodiments, component a is prepared from raw materials comprising, in parts by weight: 40-60 parts of allyl glycidyl ether, 20-30 parts of vinyl thiophene, 4-6 parts of mercaptosilane, 2-6 parts of aminosilane, 10-20 parts of vinyl benzimidazole, 20-30 parts of glass flake, 0.5-2 parts of titanium dioxide, 10-16 parts of methyl isobutyl ketone, 0.5-2 parts of calcium carbonate and 0.01-0.1 part of dimethyl silicone oil.
In some embodiments, component B is prepared from raw materials comprising, in parts by weight: 1-4 parts of pentaerythritol glycidyl ether, 56-10 parts of 2-aminomethyl-15-crown ether and 2-4 parts of tetrahydrofurfuryl alcohol.
In some embodiments, the vinyl thiophene is selected from 2-vinyl thiophene or 3-vinyl thiophene.
In some embodiments, the mercaptosilane is selected from 2-mercaptoethyltriethoxysilane or (mercaptomethyl) triethoxysilane.
In some embodiments, the aminosilane is selected from 3-aminopropyltrimethoxysilane or N-methyl-3-aminopropyltrimethoxysilane.
In some embodiments, the vinylbenzimidazole is selected from one of (5-vinyl-1H-benzimidazol-2-yl) methanethiol, 2-methyl-5-vinyl-1H-benzimidazole, 1-vinyl-1, 3-dihydro-2H-benzimidazole-2-thione.
In some embodiments, the glass flakes have a particle size of 350-400 mesh.
In some embodiments, the calcium carbonate is precipitated calcium carbonate.
The second aspect of the invention provides a preparation method of corrosion-resistant glass flake resin, which comprises the following steps:
(1) preparation of component A: stirring the glass flakes, calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding mercaptosilane and aminosilane, and stirring for 1 h; then adding allyl glycidyl ether, vinyl thiophene and vinyl benzimidazole into a reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12 hours, cooling to room temperature, adding dimethyl silicone oil, stirring uniformly, and aging for 24 hours to obtain a component A;
(2) preparation of component B: uniformly stirring pentaerythritol glycidyl ether, 2-aminomethyl-15-crown ether-5 and tetrahydrofurfuryl alcohol at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
The glass flakes are made by spraying the molten glass at 1700 deg.C from the inner surface of a rotary drum, and breaking the formed glass film by the action of centrifugal force, or by making the molten glass into thin tube shape and charging air, then breaking the thin tube wall into glass flakes, then winnowing, crushing and screening to obtain irregular flake fillers with different granularities. The ability of glass to resist attack by gases, water, acids, bases, salts and various chemical agents is called chemical stability and can be divided into water resistance, acid resistance, and alkali resistance.
The silicate glass is attacked by water. Glass has strong acid resistance, but except hydrofluoric acid, common acid attacks the glass through the action of water, and the concentration of the acid is high, which means that the content of the water is low, so the glass attacking action of concentrated acid is lower than that of dilute acid. One of the corrosion products of silicate glass by water is metal oxide, which is neutralized by an acid. The neutralization has two opposite effects, namely accelerating the ion exchange reaction between the glass and the aqueous solution to increase the weight loss of the glass, and reducing the pH value of the solution to enable Si (OH)4And thus reduces the weight loss of the glass. When R in the glass2The former effect is predominant when the content of O is high, when Si is present2The latter effect is predominant at higher O contents. The acid resistance of the high alkali glass is less than the water resistance, and the acid resistance of the high silica glass is greater than the water resistance.
Silicate glass is generally not alkali-resistant, and the corrosion of alkali to glass is realized by destroying silica framework through hydroxide ions to ensure that SiO2Dissolved in the solution. Therefore, in the glass erosion process, the silicon gel film is not formed, the surface layer of the glass is completely peeled off, and the erosion degree of the glass is in a linear relation with the erosion time.
The erosion of glass by atmosphere is essentially water vapor and CO2、SO2Equal pairThe sum of the glass surface attacks. The process of attacking glass by a humid atmosphere begins with the adsorption of atmospheric water molecules by certain ions on the surface of the glass, which are coated on the surface of the glass in the form of hydroxide ion groups, forming a thin layer. If K is in the chemical composition of the glass2O、Na2The content of O and CaO is low and the formation of such a thin layer does not progress. If the glass chemical composition contains a large amount of alkali hydroxide, the adsorbed water film becomes a solution of alkali hydroxide. The released alkali is accumulated on the surface of the glass continuously, the concentration is higher and higher, the pH value is increased rapidly, and finally the corrosion of the glass is intensified similarly to the corrosion of the alkali to the glass.
The invention provides a corrosion-resistant glass flake resin, which comprises a component A and a component B, wherein the component A is prepared from the following raw materials: allyl glycidyl ether, vinyl thiophene, mercaptosilane, aminosilane, vinyl benzimidazole, glass flake, titanium dioxide, methyl isobutyl ketone, calcium carbonate and dimethyl silicone oil; the preparation raw materials of the component B comprise: pentaerythritol glycidyl ether, 2-aminomethyl-15-crown-5, tetrahydrofurfuryl alcohol; the weight ratio of the component A to the component B is 1: (0.2-0.4).
In some embodiments, component a is prepared from raw materials comprising, in parts by weight: 40-60 parts of allyl glycidyl ether, 20-30 parts of vinyl thiophene, 4-6 parts of mercaptosilane, 2-6 parts of aminosilane, 10-20 parts of vinyl benzimidazole, 20-30 parts of glass flake, 0.5-2 parts of titanium dioxide, 10-16 parts of methyl isobutyl ketone, 0.5-2 parts of calcium carbonate and 0.01-0.1 part of dimethyl silicone oil.
In some embodiments, component B is prepared from raw materials comprising, in parts by weight: 1-4 parts of pentaerythritol glycidyl ether, 56-10 parts of 2-aminomethyl-15-crown ether and 2-4 parts of tetrahydrofurfuryl alcohol.
The CAS number for 2-aminomethyl-15-crown-5 is 83585-56-2.
In some embodiments, the vinyl thiophene is selected from 2-vinyl thiophene or 3-vinyl thiophene.
The CAS number for 2-vinylthiophene is 1918-82-7, and the CAS number for 3-vinylthiophene is 13679-64-6.
In some embodiments, the vinylbenzimidazole is selected from one of (5-vinyl-1H-benzimidazol-2-yl) methanethiol, 2-methyl-5-vinyl-1H-benzimidazole, 1-vinyl-1, 3-dihydro-2H-benzimidazole-2-thione.
CAS number for (5-vinyl-1H-benzimidazol-2-yl) methanethiol is 87765-90-0, CAS number for 2-methyl-5-vinyl-1H-benzimidazole is 84170-66-1, 1-vinyl-1, 3-dihydro-2H-benzimidazole-2-thione is 58536-65-5.
The vinylbenzimidazole is preferably a sulfur-containing vinylbenzimidazole.
In the glass flake resin provided by the invention, allyl glycidyl ether is used as a matrix and provides basic crosslinking points, and vinyl thiophene and vinyl benzimidazole are both arranged on the main chain of a molecular chain and provide more types of crosslinking points. The hydrosulphonyl silane and amino silane can connect the scales with the matrix, on one hand, the adhesive force between the glass scales and the matrix is improved, on the other hand, the hydrosulphonyl silane and vinyl benzimidazole in the molecular chain generate the multi-crosslinking effect, the soaking blank between the scales is reduced, and the permeability resistance is improved. The pentaerythritol glycidyl ether introduces a branched system in the system, and the tetrahydrofurfuryl alcohol and the 2-aminomethyl-15-crown ether-5 have the functions of end capping and crosslinking, so that the corrosion resistance of the glass flake resin coating, particularly the corrosion resistance to fluorine, is improved together.
In some embodiments, the mercaptosilane is selected from 2-mercaptoethyltriethoxysilane or (mercaptomethyl) triethoxysilane.
The CAS number for 2-mercaptoethyltriethoxysilane is 18236-15-2, and for (mercaptomethyl) triethoxysilane is 60764-83-2.
In some embodiments, the aminosilane is selected from 3-aminopropyltrimethoxysilane or N-methyl-3-aminopropyltrimethoxysilane.
3-aminopropyltrimethoxysilane had a CAS number of 13822-56-5 and N-methyl-3-aminopropyltrimethoxysilane had a CAS number of 3069-25-8.
In the process of manufacturing the coating, hydrophilic polar substances such as fillers, pigments and the like are required to be dispersed into non-polar substances which are hydrophobic. The dispersion condition of the inorganic filler and the auxiliary agent in the high molecular film-forming substance is an important factor influencing the performance of the coating. The surface modification treatment of the inorganic filler can effectively disperse the inorganic filler, and the inorganic filler is tightly combined with the polymer base material, so that the corrosion resistance and the decoration are improved. The coupling agent is coupled and combined with the surface of the inorganic pigment and filler through the actions of physical adsorption and chemical reaction.
The mercapto and amino groups in the mercaptosilane and the aminosilane adopted by the invention can form a space network structure with vinyl thiophene and vinyl benzimidazole in a molecular chain, so that the permeability resistance is improved. In addition, the viscosity of the system can be adjusted by the length of the molecule.
In some embodiments, the glass flakes have a particle size of 350-400 mesh.
In some embodiments, the calcium carbonate is precipitated calcium carbonate.
The second aspect of the invention provides a preparation method of corrosion-resistant glass flake resin, which comprises the following steps:
(1) preparation of component A: stirring the glass flakes, calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding mercaptosilane and aminosilane, and stirring for 1 h; then adding allyl glycidyl ether, vinyl thiophene and vinyl benzimidazole into a reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12 hours, cooling to room temperature, adding dimethyl silicone oil, stirring uniformly, and aging for 24 hours to obtain a component A;
(2) preparation of component B: uniformly stirring pentaerythritol glycidyl ether, 2-aminomethyl-15-crown ether-5 and tetrahydrofurfuryl alcohol at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
The invention is further illustrated by the following specific examples.
Example 1
The corrosion-resistant glass flake resin comprises a component A and a component B, wherein the component A comprises the following preparation raw materials in parts by weight: 50 parts of allyl glycidyl ether, 25 parts of 2-vinyl thiophene, 5 parts of 2-mercaptoethyltriethoxysilane, 4 parts of N-methyl-3-aminopropyltrimethoxysilane, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan, 380-mesh 25 parts of glass flakes, 1 part of titanium dioxide, 12 parts of methyl isobutyl ketone, 1 part of light calcium carbonate and 0.05 part of dimethyl silicone oil;
the component B comprises the following preparation raw materials in parts by weight: 2 parts of pentaerythritol glycidyl ether, 58 parts of 2-aminomethyl-15-crown ether and 3 parts of tetrahydrofurfuryl alcohol;
the weight ratio of the component A to the component B is 1: 0.3;
the preparation method comprises the following steps:
(1) preparation of component A: stirring 380-mesh glass flakes, light calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding 2-mercaptoethyltriethoxysilane and N-methyl-3-aminopropyltrimethoxysilane, and stirring for 1 h; then adding allyl glycidyl ether, 2-vinyl thiophene, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan into the reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12 hours, cooling to room temperature, adding dimethyl silicone oil, uniformly stirring, and aging for 24 hours to obtain a component A;
(2) preparation of component B: uniformly stirring pentaerythritol glycidyl ether, 2-aminomethyl-15-crown ether-5 and tetrahydrofurfuryl alcohol at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
Example 2
The corrosion-resistant glass flake resin comprises a component A and a component B, wherein the component A comprises the following preparation raw materials in parts by weight: 50 parts of allyl glycidyl ether, 25 parts of 3-vinyl thiophene, 5 parts of 2-mercaptoethyltriethoxysilane, 4 parts of N-methyl-3-aminopropyltrimethoxysilane, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan, 380-mesh 25 parts of glass flakes, 1 part of titanium dioxide, 12 parts of methyl isobutyl ketone, 1 part of light calcium carbonate and 0.05 part of simethicone;
the component B comprises the following preparation raw materials in parts by weight: 2 parts of pentaerythritol glycidyl ether, 58 parts of 2-aminomethyl-15-crown ether and 3 parts of tetrahydrofurfuryl alcohol;
the weight ratio of the component A to the component B is 1: 0.3;
the preparation method comprises the following steps:
(1) preparation of component A: stirring 380-mesh glass flakes, light calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding 2-mercaptoethyltriethoxysilane and N-methyl-3-aminopropyltrimethoxysilane, and stirring for 1 h; then adding allyl glycidyl ether, 3-vinyl thiophene, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan into a reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12 hours, cooling to room temperature, adding dimethyl silicone oil, uniformly stirring, and aging for 24 hours to obtain a component A;
(2) preparation of component B: uniformly stirring pentaerythritol glycidyl ether, 2-aminomethyl-15-crown ether-5 and tetrahydrofurfuryl alcohol at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
Example 3
The corrosion-resistant glass flake resin comprises a component A and a component B, wherein the component A comprises the following preparation raw materials in parts by weight: 50 parts of allyl glycidyl ether, 25 parts of 2-vinyl thiophene, (5 parts of mercaptomethyl) triethoxysilane, 4 parts of N-methyl-3-aminopropyltrimethoxysilane, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan, 380-mesh 25 parts of glass flakes, 1 part of titanium dioxide, 12 parts of methyl isobutyl ketone, 1 part of light calcium carbonate and 0.05 part of simethicone;
the component B comprises the following preparation raw materials in parts by weight: 2 parts of pentaerythritol glycidyl ether, 58 parts of 2-aminomethyl-15-crown ether and 3 parts of tetrahydrofurfuryl alcohol;
the weight ratio of the component A to the component B is 1: 0.3;
the preparation method comprises the following steps:
(1) preparation of component A: stirring 380-mesh glass flakes, light calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding (mercaptomethyl) triethoxysilane and N-methyl-3-aminopropyltrimethoxysilane, and stirring for 1 h; then adding allyl glycidyl ether, 2-vinyl thiophene, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan into the reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12 hours, cooling to room temperature, adding dimethyl silicone oil, uniformly stirring, and aging for 24 hours to obtain a component A;
(2) preparation of component B: uniformly stirring pentaerythritol glycidyl ether, 2-aminomethyl-15-crown ether-5 and tetrahydrofurfuryl alcohol at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
Example 4
The corrosion-resistant glass flake resin comprises a component A and a component B, wherein the component A comprises the following preparation raw materials in parts by weight: 50 parts of allyl glycidyl ether, 25 parts of 2-vinyl thiophene, 5 parts of 2-mercaptoethyltriethoxysilane, 4 parts of 3-aminopropyltrimethoxysilane, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan, 380-mesh 25 parts of glass flakes, 1 part of titanium dioxide, 12 parts of methyl isobutyl ketone, 1 part of light calcium carbonate and 0.05 part of dimethyl silicone oil;
the component B comprises the following preparation raw materials in parts by weight: 2 parts of pentaerythritol glycidyl ether, 58 parts of 2-aminomethyl-15-crown ether and 3 parts of tetrahydrofurfuryl alcohol;
the weight ratio of the component A to the component B is 1: 0.3;
the preparation method comprises the following steps:
(1) preparation of component A: stirring 380-mesh glass flakes, light calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding 2-mercaptoethyltriethoxysilane and 3-aminopropyltrimethoxysilane, and stirring for 1 h; then adding allyl glycidyl ether, 2-vinyl thiophene, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan into the reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12 hours, cooling to room temperature, adding dimethyl silicone oil, uniformly stirring, and aging for 24 hours to obtain a component A;
(2) preparation of component B: uniformly stirring pentaerythritol glycidyl ether, 2-aminomethyl-15-crown ether-5 and tetrahydrofurfuryl alcohol at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
Example 5
The corrosion-resistant glass flake resin comprises a component A and a component B, wherein the component A comprises the following preparation raw materials in parts by weight: 50 parts of allyl glycidyl ether, 25 parts of 2-vinyl thiophene, 5 parts of 2-mercaptoethyltriethoxysilane, 4 parts of N-methyl-3-aminopropyltrimethoxysilane, 15 parts of 1-vinyl-1, 3-dihydro-2H-benzimidazole-2-thioketone, 380-mesh 25 parts of glass flakes, 1 part of titanium dioxide, 12 parts of methyl isobutyl ketone, 1 part of light calcium carbonate and 0.05 part of simethicone;
the component B comprises the following preparation raw materials in parts by weight: 2 parts of pentaerythritol glycidyl ether, 58 parts of 2-aminomethyl-15-crown ether and 3 parts of tetrahydrofurfuryl alcohol;
the weight ratio of the component A to the component B is 1: 0.3;
the preparation method comprises the following steps:
(1) preparation of component A: stirring 380-mesh glass flakes, light calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding 2-mercaptoethyltriethoxysilane and N-methyl-3-aminopropyltrimethoxysilane, and stirring for 1 h; then adding allyl glycidyl ether and 1-vinyl-1, 3-dihydro-2H-benzimidazole-2-thioketone into a reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12H, cooling to room temperature, adding simethicone, uniformly stirring, and aging for 24H to obtain a component A;
(2) preparation of component B: uniformly stirring pentaerythritol glycidyl ether, 2-aminomethyl-15-crown ether-5 and tetrahydrofurfuryl alcohol at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
Example 6
The corrosion-resistant glass flake resin comprises a component A and a component B, wherein the component A comprises the following preparation raw materials in parts by weight: 50 parts of allyl glycidyl ether, 25 parts of 2-vinyl thiophene, 5 parts of 2-mercaptoethyltriethoxysilane, 4 parts of N-methyl-3-aminopropyltrimethoxysilane, 15 parts of 2-methyl-5-vinyl-1H-benzimidazole, 380-mesh 25 parts of glass flakes, 1 part of titanium dioxide, 12 parts of methyl isobutyl ketone, 1 part of light calcium carbonate and 0.05 part of simethicone;
the component B comprises the following preparation raw materials in parts by weight: 2 parts of pentaerythritol glycidyl ether, 58 parts of 2-aminomethyl-15-crown ether and 3 parts of tetrahydrofurfuryl alcohol;
the weight ratio of the component A to the component B is 1: 0.3;
the preparation method comprises the following steps:
(1) preparation of component A: stirring 380-mesh glass flakes, light calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding 2-mercaptoethyltriethoxysilane and N-methyl-3-aminopropyltrimethoxysilane, and stirring for 1 h; then adding allyl glycidyl ether, 2-vinyl thiophene, 2-methyl-5-vinyl-1H-benzimidazole into the reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12H, cooling to room temperature, adding simethicone, stirring uniformly, and aging for 24H to obtain a component A;
(2) preparation of component B: uniformly stirring pentaerythritol glycidyl ether, 2-aminomethyl-15-crown ether-5 and tetrahydrofurfuryl alcohol at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
Example 7
The corrosion-resistant glass flake resin comprises a component A and a component B, wherein the component A comprises the following preparation raw materials in parts by weight: 50 parts of allyl glycidyl ether, 25 parts of 2-vinyl thiophene, 5 parts of 2-mercaptoethyltriethoxysilane, 4 parts of N-methyl-3-aminopropyltrimethoxysilane, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan, 25 parts of glass flakes, 1 part of titanium dioxide, 12 parts of methyl isobutyl ketone, 1 part of light calcium carbonate and 0.05 part of simethicone;
the component B comprises the following preparation raw materials in parts by weight: 2 parts of pentaerythritol glycidyl ether, 58 parts of 2-aminomethyl-15-crown ether and 3 parts of tetrahydrofurfuryl alcohol;
the weight ratio of the component A to the component B is 1: 0.3;
the preparation method comprises the following steps:
(1) preparation of component A: stirring 300 meshes of glass flakes, light calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding 2-mercaptoethyltriethoxysilane and N-methyl-3-aminopropyltrimethoxysilane, and stirring for 1 h; then adding allyl glycidyl ether, 2-vinyl thiophene, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan into the reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12 hours, cooling to room temperature, adding dimethyl silicone oil, uniformly stirring, and aging for 24 hours to obtain a component A;
(2) preparation of component B: uniformly stirring pentaerythritol glycidyl ether, 2-aminomethyl-15-crown ether-5 and tetrahydrofurfuryl alcohol at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
Example 8
The corrosion-resistant glass flake resin comprises a component A and a component B, wherein the component A comprises the following preparation raw materials in parts by weight: 50 parts of allyl glycidyl ether, 25 parts of 2-vinyl thiophene, 5 parts of 2-mercaptoethyltriethoxysilane, 4 parts of N-methyl-3-aminopropyltrimethoxysilane, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan, 380-mesh 25 parts of glass flakes, 1 part of titanium dioxide, 12 parts of methyl isobutyl ketone, 1 part of light calcium carbonate and 0.05 part of dimethyl silicone oil;
the component B comprises the following preparation raw materials in parts by weight: 2-aminomethyl-15-crown ether-58 parts and tetrahydrofurfuryl alcohol 3 parts;
the weight ratio of the component A to the component B is 1: 0.3;
the preparation method comprises the following steps:
(1) preparation of component A: stirring 380-mesh glass flakes, light calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding 2-mercaptoethyltriethoxysilane and N-methyl-3-aminopropyltrimethoxysilane, and stirring for 1 h; then adding allyl glycidyl ether, 2-vinyl thiophene, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan into the reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12 hours, cooling to room temperature, adding dimethyl silicone oil, uniformly stirring, and aging for 24 hours to obtain a component A;
(2) preparation of component B: uniformly stirring the 2-aminomethyl-15-crown ether-5 and the tetrahydrofurfuryl alcohol at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
Example 9
The corrosion-resistant glass flake resin comprises a component A and a component B, wherein the component A comprises the following preparation raw materials in parts by weight: 50 parts of allyl glycidyl ether, 25 parts of 2-vinyl thiophene, 5 parts of 2-mercaptoethyltriethoxysilane, 4 parts of N-methyl-3-aminopropyltrimethoxysilane, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan, 380-mesh 25 parts of glass flakes, 1 part of titanium dioxide, 12 parts of methyl isobutyl ketone, 1 part of light calcium carbonate and 0.05 part of dimethyl silicone oil;
the component B comprises the following preparation raw materials in parts by weight: 2 parts of pentaerythritol glycidyl ether and 3 parts of tetrahydrofurfuryl alcohol;
the weight ratio of the component A to the component B is 1: 0.3;
the preparation method comprises the following steps:
(1) preparation of component A: stirring 380-mesh glass flakes, light calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding 2-mercaptoethyltriethoxysilane and N-methyl-3-aminopropyltrimethoxysilane, and stirring for 1 h; then adding allyl glycidyl ether, 2-vinyl thiophene, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan into the reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12 hours, cooling to room temperature, adding dimethyl silicone oil, uniformly stirring, and aging for 24 hours to obtain a component A;
(2) preparation of component B: pentaerythritol glycidyl ether and tetrahydrofurfuryl alcohol are uniformly stirred at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
Example 10
The corrosion-resistant glass flake resin comprises a component A and a component B, wherein the component A comprises the following preparation raw materials in parts by weight: 50 parts of allyl glycidyl ether, 25 parts of 2-vinyl thiophene, 5 parts of 2-mercaptoethyltriethoxysilane, 4 parts of N-methyl-3-aminopropyltrimethoxysilane, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan, 380-mesh 25 parts of glass flakes, 1 part of titanium dioxide, 12 parts of methyl isobutyl ketone, 1 part of light calcium carbonate and 0.05 part of dimethyl silicone oil;
the component B comprises the following preparation raw materials in parts by weight: 2 parts of pentaerythritol glycidyl ether and 58 parts of 2-aminomethyl-15-crown ether;
the weight ratio of the component A to the component B is 1: 0.3;
the preparation method comprises the following steps:
(1) preparation of component A: stirring 380-mesh glass flakes, light calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding 2-mercaptoethyltriethoxysilane and N-methyl-3-aminopropyltrimethoxysilane, and stirring for 1 h; then adding allyl glycidyl ether, 2-vinyl thiophene, (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan into the reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12 hours, cooling to room temperature, adding dimethyl silicone oil, uniformly stirring, and aging for 24 hours to obtain a component A;
(2) preparation of component B: pentaerythritol glycidyl ether and 2-aminomethyl-15-crown ether-5 are uniformly stirred at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
Test method
1. Test for dielectric resistance
Examples 1-10 were each coated onto copper sheets to a dry film thickness of about 500 μm. Medium resistance was determined according to GB/T9274-1988. The medium is 15 wt% NaOH aqueous solution, and soaking for 800 h.
2. Resistance to fluorine corrosion test
Examples 1-10 were each coated onto copper sheets to a dry film thickness of about 500 μm. Adhesion was determined according to GB/T5210-2006 in MPa. A saturated aqueous solution of sodium fluoride was prepared and the copper sheet was placed in it at room temperature for 20 days. After removal, the adhesion was measured again in MPa.
The test results are as follows.
The foregoing is by way of example only, and not limiting. It is intended that all equivalent modifications or variations not departing from the spirit and scope of the present invention be included in the claims.
Claims (4)
1. The corrosion-resistant glass flake resin is characterized by comprising a component A and a component B;
the preparation raw materials of the component A comprise the following components in parts by weight: 40-60 parts of allyl glycidyl ether, 20-30 parts of vinyl thiophene, 4-6 parts of mercaptosilane, 2-6 parts of aminosilane, 10-20 parts of vinyl benzimidazole, 20-30 parts of glass flake, 0.5-2 parts of titanium dioxide, 10-16 parts of methyl isobutyl ketone, 0.5-2 parts of calcium carbonate and 0.01-0.1 part of dimethyl silicone oil;
the component B is prepared from the following raw materials in parts by weight: 1-4 parts of pentaerythritol glycidyl ether, 56-10 parts of 2-aminomethyl-15-crown ether and 2-4 parts of tetrahydrofurfuryl alcohol;
the weight ratio of the component A to the component B is 1: (0.2-0.4);
the vinyl thiophene is selected from 2-vinyl thiophene or 3-vinyl thiophene;
the mercaptosilane is 2-mercaptoethyltriethoxysilane;
the aminosilane is 3-aminopropyltrimethoxysilane;
the vinyl benzimidazole is (5-vinyl-1H-benzimidazole-2-yl) methyl mercaptan.
2. The corrosion-resistant glass flake resin of claim 1, wherein the glass flake has a particle size of 350-400 mesh.
3. The corrosion-resistant glass flake resin of claim 1, wherein the calcium carbonate is precipitated calcium carbonate.
4. A method for preparing the corrosion-resistant glass flake resin of any one of claims 1-3, comprising the steps of:
(1) preparation of component A: stirring the glass flakes, calcium carbonate, titanium dioxide and methyl isobutyl ketone in a reaction kettle for 10min, adding mercaptosilane and aminosilane, and stirring for 1 h; then adding allyl glycidyl ether, vinyl thiophene and vinyl benzimidazole into a reaction kettle, adding cyclohexanone peroxide, heating to 158 ℃, reacting for 12 hours, cooling to room temperature, adding dimethyl silicone oil, stirring uniformly, and aging for 24 hours to obtain a component A;
(2) preparation of component B: uniformly stirring pentaerythritol glycidyl ether, 2-aminomethyl-15-crown ether-5 and tetrahydrofurfuryl alcohol at room temperature to obtain a component B;
(3) and mixing the component A and the component B, stirring uniformly, curing for 30min, and then performing brush coating construction.
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| CN1810866A (en) * | 2006-01-13 | 2006-08-02 | 上海昭和高分子有限公司 | Surface treatment method of scale resin with glass scale and prepn process of scale resin |
| CN103665331A (en) * | 2013-12-16 | 2014-03-26 | 北京彤程创展科技有限公司 | Resin for improving rubber tear resistance and preparation method thereof |
| CN105254854A (en) * | 2015-11-17 | 2016-01-20 | 北京彤程创展科技有限公司 | Resin for improving rubber tear resistance, preparation method and application of resin |
| CN106497259A (en) * | 2016-10-26 | 2017-03-15 | 沈阳理工大学 | Aqueous chromium-free Dacroment-fluorubber composite coating and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1810866A (en) * | 2006-01-13 | 2006-08-02 | 上海昭和高分子有限公司 | Surface treatment method of scale resin with glass scale and prepn process of scale resin |
| CN103665331A (en) * | 2013-12-16 | 2014-03-26 | 北京彤程创展科技有限公司 | Resin for improving rubber tear resistance and preparation method thereof |
| CN105254854A (en) * | 2015-11-17 | 2016-01-20 | 北京彤程创展科技有限公司 | Resin for improving rubber tear resistance, preparation method and application of resin |
| CN106497259A (en) * | 2016-10-26 | 2017-03-15 | 沈阳理工大学 | Aqueous chromium-free Dacroment-fluorubber composite coating and preparation method thereof |
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