CN111073373A - Phosphatized epoxy coating and preparation method thereof - Google Patents
Phosphatized epoxy coating and preparation method thereof Download PDFInfo
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- CN111073373A CN111073373A CN201911386769.0A CN201911386769A CN111073373A CN 111073373 A CN111073373 A CN 111073373A CN 201911386769 A CN201911386769 A CN 201911386769A CN 111073373 A CN111073373 A CN 111073373A
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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
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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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
- C08G59/1488—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing phosphorus
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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
-
- 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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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Plant Pathology (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a phosphatized epoxy coating, which is composed of the following raw materials in parts by weight: 1-2 parts of oleic acid diethanolamide, 0.7-1 part of sodium myristate soap, 70-90 parts of phosphorus modified epoxy resin, 1-3 parts of tristearin, 1-2 parts of magnesium stearate, 0.5-1 part of zinc pyrithione and 3-5 parts of trimethylolpropane.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a phosphatized epoxy coating and a preparation method thereof.
Background
In the photocatalytic coating, active ingredients capable of absorbing and converting photon energy play a key role. Titanium oxide, which was originally found to be useful for photocatalytic decontamination and bacterial inhibition, is also the only commercially available photocatalytic active ingredient, and many photocatalytic coatings, tiles, plates, etc. on the market contain the active ingredient. However, titanium oxide only absorbs ultraviolet light which occupies a very small proportion of sunlight remarkably, and indoor long-time ultraviolet irradiation is not beneficial to health, so that other visible light catalysts must be screened to directly utilize indoor abundant visible light as a light source of the photocatalytic coating;
the epoxy resin is used in the anticorrosive paint with the largest share of liquid resin, but most of the paints used in industry at present are solvent-based paints, and the conventional solvent-based paints mostly use aromatic hydrocarbon, esters, alcohols, ketones and the like as solvents, and the solvents have toxicity of different degrees, and volatile matters are directly discharged into air, so that the environment pollution is serious. With the increasing awareness of environmental protection, novel anticorrosive coatings free of organic solvents or low VOC, such as powder coatings, solventless coatings, and water-based coatings, have been developed in succession. The powder coating has more severe curing conditions, so the development of the powder coating is limited; the solvent-free epoxy coating is relatively successful in the field of solvent-free coating, but is challenged and improved in aspects of low toxicity of reactive diluent, safe reliability of curing agent and the like in recent years; the water-based epoxy coating has the advantages of a solvent-based coating, is developing in the aspects of improving performance, reducing pollution, expanding application and the like, and the fields of the water-based epoxy coating include locomotives, aviation, food, buildings and the like, so the water-based epoxy coating is a very rapid field in recent years;
the inorganic component and the organic polymer are required to be fully and tightly bonded to prepare the high-quality inorganic-organic composite coating, and although the product has the bacteriostatic ability by utilizing visible light, the compatibility of inorganic carbon nitride powder and the organic polymer is not considered during production, so that the risk of uneven distribution and easy peeling loss of effective components during later construction and cleaning is caused.
Disclosure of Invention
The invention aims to provide a phosphatized epoxy coating and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a phosphatized epoxy coating is composed of the following raw materials in parts by weight:
1-2 parts of oleic acid diethanolamide, 0.7-1 part of sodium myristate soap, 70-90 parts of phosphorus modified epoxy resin, 1-3 parts of tristearin, 1-2 parts of magnesium stearate, 0.5-1 part of zinc pyrithione and 3-5 parts of trimethylolpropane.
The phosphorus modified epoxy resin is prepared from the following raw materials in parts by weight:
epoxy resin E5150-60, 2-thiol benzimidazole 1-2, tetrakis (hydroxymethyl) phosphonium sulfate 3-4, light calcium carbonate 7-9, and calcium ricinoleate 1-2.
The preparation method of the phosphorus modified epoxy resin comprises the following steps:
(1) adding 2-thiol benzimidazole into 10-14 times of anhydrous ethanol, stirring, heating to 50-55 deg.C, stirring for 20-30 min to obtain alcohol dispersion;
(2) mixing epoxy resin E51 and tetrakis (hydroxymethyl) phosphonium sulfate, adding into deionized water 30-40 times of the weight of the mixture, stirring, feeding into a reaction kettle, introducing nitrogen, stirring for 1-2 hours at 50-60 deg.C, discharging, and cooling to obtain epoxy dispersion;
(3) and (3) mixing the alcohol dispersion liquid and the epoxy dispersion liquid, uniformly stirring, adding light calcium carbonate and calcium ricinoleate, and carrying out ultrasonic treatment for 3-9 minutes to obtain the phosphorus modified epoxy resin.
A preparation method of phosphatized epoxy coating comprises the following steps:
(1) mixing sodium myristate soap with zinc pyrithione, adding into anhydrous ethanol 10-15 times of the weight of the mixture, and stirring to obtain alcohol dispersion;
(2) mixing the phosphorus modified epoxy resin with the last alcohol dispersion liquid, stirring uniformly, adding trimethylolpropane, raising the temperature to 60-70 ℃, keeping the temperature and stirring for 1-2 hours to obtain an epoxy premixed liquid;
(3) and mixing the epoxy premixed solution with oleic acid diethanolamide, tristearin and magnesium stearate, and performing ultrasonic treatment for 1-2 hours to obtain the phosphatized epoxy coating.
The invention has the advantages that:
firstly, taking tetrakis (hydroxymethyl) phosphonium sulfate as a raw material, modifying epoxy resin E51, and then blending with an alcoholic solution of 2-thiol benzimidazole to obtain an antioxidant phosphorus-doped epoxy resin solution; the resin coating disclosed by the invention is good in water dispersibility, good in antibacterial and antioxidant properties, uniform in film coating and high in use safety.
Detailed Description
Example 1
A phosphatized epoxy coating is composed of the following raw materials in parts by weight:
oleic acid diethanolamide 1, sodium myristate soap 0.7, phosphorus modified epoxy resin 70, glyceryl tristearate 1, magnesium stearate 1, zinc pyrithione 0.5 and trimethylolpropane 3.
The phosphorus modified epoxy resin is prepared from the following raw materials in parts by weight:
epoxy resin E5150, 2-thiol benzimidazole 1, tetrakis (hydroxymethyl) phosphonium sulfate 3, light calcium carbonate 7 and calcium ricinoleate 1.
The preparation method of the phosphorus modified epoxy resin comprises the following steps:
(1) adding 2-thiol benzimidazole into 10 times of anhydrous ethanol, stirring, heating to 50 deg.C, and stirring for 20 min to obtain alcohol dispersion;
(2) mixing epoxy resin E51 and tetrakis (hydroxymethyl) phosphonium sulfate, adding into deionized water 30 times of the weight of the mixture, stirring uniformly, feeding into a reaction kettle, introducing nitrogen, stirring for 1 hour at 50 ℃, discharging and cooling to obtain epoxy dispersion;
(3) and (3) mixing the alcohol dispersion liquid and the epoxy dispersion liquid, uniformly stirring, adding light calcium carbonate and calcium ricinoleate, and carrying out ultrasonic treatment for 3 minutes to obtain the phosphorus modified epoxy resin.
A preparation method of phosphatized epoxy coating comprises the following steps:
(1) mixing sodium myristate soap with zinc pyrithione, adding into anhydrous ethanol 10-15 times of the weight of the mixture, and stirring to obtain alcohol dispersion;
(2) mixing the phosphorus modified epoxy resin with the last alcohol dispersion liquid, stirring uniformly, adding trimethylolpropane, raising the temperature to 60 ℃, and stirring for 1 hour under heat preservation to obtain an epoxy premix;
(3) and mixing the epoxy premixed solution with oleic acid diethanolamide, tristearin and magnesium stearate, and performing ultrasonic treatment for 1 hour to obtain the phosphatized epoxy coating.
Example 2
A phosphatized epoxy coating is composed of the following raw materials in parts by weight:
oleic acid diethanolamide 2, myristic acid sodium soap 1, phosphorus-modified epoxy resin 90, tristearin 3, magnesium stearate 1, zinc pyrithione 1 and trimethylolpropane 5.
The phosphorus modified epoxy resin is prepared from the following raw materials in parts by weight:
epoxy resin E5160, 2-thiol benzimidazole 2, tetrakis (hydroxymethyl) phosphonium sulfate 4, light calcium carbonate 9 and calcium ricinoleate 2.
The preparation method of the phosphorus modified epoxy resin comprises the following steps:
(1) adding 2-thiol benzimidazole into 14 times of anhydrous ethanol, stirring, heating to 55 deg.C, and stirring for 30 min to obtain alcohol dispersion;
(2) mixing epoxy resin E51 and tetrakis (hydroxymethyl) phosphonium sulfate, adding into deionized water 40 times of the weight of the mixture, stirring uniformly, feeding into a reaction kettle, introducing nitrogen, stirring for 2 hours at 60 ℃, discharging and cooling to obtain epoxy dispersion;
(3) and (3) mixing the alcohol dispersion liquid and the epoxy dispersion liquid, uniformly stirring, adding light calcium carbonate and calcium ricinoleate, and carrying out ultrasonic treatment for 9 minutes to obtain the phosphorus modified epoxy resin.
A preparation method of phosphatized epoxy coating comprises the following steps:
(1) mixing sodium myristate soap with zinc pyrithione, adding into anhydrous ethanol 10-15 times of the weight of the mixture, and stirring to obtain alcohol dispersion;
(2) mixing the phosphorus modified epoxy resin with the last alcohol dispersion liquid, stirring uniformly, adding trimethylolpropane, raising the temperature to 70 ℃, and stirring for 2 hours under heat preservation to obtain an epoxy premix;
(3) and mixing the epoxy premixed solution with oleic acid diethanolamide, tristearin and magnesium stearate, and performing ultrasonic treatment for 2 hours to obtain the phosphatized epoxy coating.
And (3) performance testing:
the phosphatized epoxy coatings of examples 1 and 2 and the commercially available water-based epoxy coatings are subjected to bacteriostasis experiment determination by referring to the national standards of the people's republic of China HG/T3950-2007 antibacterial coating and GB/T21866-2008 antibacterial coating (paint film) antibacterial property determination method and antibacterial effect. The concrete measures are as follows: 1) respectively coating the paint on a test plate, coating the paint with a thickness of 0.5mm, drying, cutting the test plate into test plates with a thickness of 50mm multiplied by 50mm, and sterilizing the test plates for 5min on an ultra-clean workbench for later use; 2) culturing and diluting fresh activated strains by nutrient broth NB/normal saline, selecting a solution with a bacterial liquid concentration of (5-10) multiplied by 105cfu/mL for test, and operating according to the method of GB4789.2 'determination of total number of bacterial colonies for food hygiene microbiological inspection'; 3) respectively dripping 0.5ml of test bacterium liquid on a test plate, clamping a sterilization cover film with sterilization forceps to cover the test plate so as to enable the test bacterium liquid to be flat and bubble-free, placing the test bacterium liquid in a sterilization culture dish, transferring the test bacterium liquid to a biochemical incubator, arranging an 80-100W LED lamp in the sterilization culture dish, and illuminating for 3-5 hours under the conditions of (37 +/-1) DEG C and relative humidity RH being more than 90%; 4) after the light irradiation is finished, the test plate and the cover film are washed by 20mL of physiological saline, the washing solution is inoculated into an agar medium NA, and after the culture is carried out for 24 hours at the temperature of (37 +/-1), the counting is carried out according to GB4789.2 'determination of total number of bacterial colonies for food hygiene microbiological examination'.
And (3) measuring:
phosphated epoxy coating of example 1 of the invention:
the bacteriostatic rate of staphylococcus aureus is as follows: 99.7%, and the bacteriostasis rate of Escherichia coli is as follows: 99.8 percent;
phosphatized epoxy coating of example 2 of the invention:
the bacteriostatic rate of staphylococcus aureus is as follows: 99.8 percent, and the bacteriostasis rate of the Escherichia coli is as follows: 99.8 percent;
the invention discloses a commercial waterborne epoxy coating:
the bacteriostatic rate of staphylococcus aureus is as follows: 40.1 percent, and the bacteriostasis rate of the Escherichia coli is as follows: 33.6 percent.
Claims (4)
1. The phosphatized epoxy coating is characterized by comprising the following raw materials in parts by weight:
1-2 parts of oleic acid diethanolamide, 0.7-1 part of sodium myristate soap, 70-90 parts of phosphorus modified epoxy resin, 1-3 parts of tristearin, 1-2 parts of magnesium stearate, 0.5-1 part of zinc pyrithione and 3-5 parts of trimethylolpropane.
2. The phosphatized epoxy coating as claimed in claim 1, wherein the phosphatized epoxy resin is composed of the following raw materials in parts by weight:
epoxy resin E5150-60, 2-thiol benzimidazole 1-2, tetrakis (hydroxymethyl) phosphonium sulfate 3-4, light calcium carbonate 7-9, and calcium ricinoleate 1-2.
3. A phosphatized epoxy coating as claimed in claim 2, wherein the preparation method of the phosphatized epoxy resin comprises the following steps:
(1) adding 2-thiol benzimidazole into 10-14 times of anhydrous ethanol, stirring, heating to 50-55 deg.C, stirring for 20-30 min to obtain alcohol dispersion;
(2) mixing epoxy resin E51 and tetrakis (hydroxymethyl) phosphonium sulfate, adding into deionized water 30-40 times of the weight of the mixture, stirring, feeding into a reaction kettle, introducing nitrogen, stirring for 1-2 hours at 50-60 deg.C, discharging, and cooling to obtain epoxy dispersion;
(3) and (3) mixing the alcohol dispersion liquid and the epoxy dispersion liquid, uniformly stirring, adding light calcium carbonate and calcium ricinoleate, and carrying out ultrasonic treatment for 3-9 minutes to obtain the phosphorus modified epoxy resin.
4. A process for preparing a phosphatized epoxy coating as claimed in claim 1, comprising the steps of:
(1) mixing sodium myristate soap with zinc pyrithione, adding into anhydrous ethanol 10-15 times of the weight of the mixture, and stirring to obtain alcohol dispersion;
(2) mixing the phosphorus modified epoxy resin with the last alcohol dispersion liquid, stirring uniformly, adding trimethylolpropane, raising the temperature to 60-70 ℃, keeping the temperature and stirring for 1-2 hours to obtain an epoxy premixed liquid;
(3) and mixing the epoxy premixed solution with oleic acid diethanolamide, tristearin and magnesium stearate, and performing ultrasonic treatment for 1-2 hours to obtain the phosphatized epoxy coating.
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CN201911386769.0A CN111073373A (en) | 2019-12-29 | 2019-12-29 | Phosphatized epoxy coating and preparation method thereof |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107118669A (en) * | 2017-06-27 | 2017-09-01 | 林鹏鑫 | A kind of preparation method of anticorrosion water-soluble heat radiation coating |
CN108624189A (en) * | 2018-04-04 | 2018-10-09 | 湖北娅安科技开发有限公司 | A kind of fire resistant coating and its preparation method and application for ship bulkhead |
CN108641494A (en) * | 2018-03-27 | 2018-10-12 | 繁昌县盛民机械制造有限公司 | A kind of whisker type powdery paints and preparation method thereof |
CN110527367A (en) * | 2019-10-12 | 2019-12-03 | 中北大学 | A kind of indoor visible light long-acting bacteriostatic water paint |
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2019
- 2019-12-29 CN CN201911386769.0A patent/CN111073373A/en not_active Withdrawn
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107118669A (en) * | 2017-06-27 | 2017-09-01 | 林鹏鑫 | A kind of preparation method of anticorrosion water-soluble heat radiation coating |
CN108641494A (en) * | 2018-03-27 | 2018-10-12 | 繁昌县盛民机械制造有限公司 | A kind of whisker type powdery paints and preparation method thereof |
CN108624189A (en) * | 2018-04-04 | 2018-10-09 | 湖北娅安科技开发有限公司 | A kind of fire resistant coating and its preparation method and application for ship bulkhead |
CN110527367A (en) * | 2019-10-12 | 2019-12-03 | 中北大学 | A kind of indoor visible light long-acting bacteriostatic water paint |
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