CN108531044A - A kind of preparation method of antibacterial hydrophobic epoxy coating - Google Patents

A kind of preparation method of antibacterial hydrophobic epoxy coating Download PDF

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Publication number
CN108531044A
CN108531044A CN201810500827.7A CN201810500827A CN108531044A CN 108531044 A CN108531044 A CN 108531044A CN 201810500827 A CN201810500827 A CN 201810500827A CN 108531044 A CN108531044 A CN 108531044A
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weight
parts
epoxy resin
modified
preparation
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高恒东
胡佳佳
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Wuhu Chuangyuan New Materials Co Ltd
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Wuhu Chuangyuan New Materials Co Ltd
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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
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/14—Polycondensates modified by chemical after-treatment
    • C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
    • C08G59/1438—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • 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
    • 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
    • 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
    • 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
    • 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
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2363/00—Characterised by the use of epoxy resins; 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
    • C08K3/16—Halogen-containing compounds
    • C08K2003/164—Aluminum halide, e.g. aluminium chloride
    • 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
    • C08K2003/2206—Oxides; Hydroxides of metals of calcium, strontium or barium
    • 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
    • C08K2003/2296—Oxides; Hydroxides of metals of zinc
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Emergency Medicine (AREA)
  • General Chemical & Material Sciences (AREA)
  • Plant Pathology (AREA)
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Abstract

The invention discloses a kind of preparation methods of antibacterial hydrophobic epoxy coating, crystal aluminum chloride and acetylacetone,2,4-pentanedione hybrid reaction are subjected to hydrophobically modified, atoleine is admixed after drying, and drying to constant weight, citric acid-modified is added dropwise into liquid epoxies, it adds hydrophobically modified crystal aluminum chloride and is mixed to get modified liquid epoxy resin, by barium monoxide, zinc oxide calcining and starch ground, graphene, anti-settling agent, neopelex mixing diatomite and modified liquid epoxy resin are prepared into coating later.The present invention later in modified epoxy, makes it have good mechanical performance and stability, the coating of preparation has hydrophobicity and antibiotic property by hydrophobically modified crystal aluminum chloride.

Description

A kind of preparation method of antibacterial hydrophobic epoxy coating
Technical field
The invention belongs to coating manufacture fields, and in particular to a kind of preparation method of antibacterial hydrophobic epoxy coating.
Background technology
Epoxy resin is a kind of thermosetting resin, because having the characteristics such as excellent cementability, mechanical strength and electrical insulating property, And be widely used in adhesive, coating and matrices of composite material etc..Epoxy resin is applied in polymer matrix composite One of widest matrix resin carries out polycondensation reaction by the compound with epoxy group with multi-hydroxy or polyol compound Prepared by product, have excellent caking property, chemical resistance, electrical insulation properties, mechanical property, and be easy to plus Work, shrinking percentage are low, linear expansion coefficient is small and it is of low cost the advantages that.
Invention content
The present invention provides a kind of preparation method of antibacterial hydrophobic epoxy coating, and the present invention crystallizes three by hydrophobically modified Aluminium chloride makes it have good mechanical performance and stability later in modified epoxy, and the coating of preparation has hydrophobicity With antibiotic property.
The present invention is achieved by the following technical solutions：
A kind of preparation method of antibacterial hydrophobic epoxy coating, which is characterized in that include the following steps：
（1）Hydrophobically modified crystal aluminum chloride
10-15 parts by weight Crystalline alchlor is mixed with 18-23 times of absolute ethyl alcohol and is sufficiently stirred makes to be configured to solution, waits stirring 20-30 acetylacetone,2,4-pentanediones are slowly dropped in crystal aluminum chloride solution after mixing uniformly and are stirred for uniformly, by this solution in 50oC It stirs 1-2 hours, is spray-dried under water bath condition, 1-5 part by weight of liquid paraffin is added and stirs and evenly mixs, it is small that 5-8 is stirred under room temperature When, drying to constant weight；
（2）Modified liquid epoxy resin
1-5 parts by weight of lemon acid solutions are added dropwise into 70-80 parts of liquid epoxies, are heated to 110-150 DEG C, are added in (1) Gained hydrophobically modified crystal aluminum chloride is warming up to 80-100 DEG C and stirs 1-2 hours, is cooled to room temperature, obtains modified liquid ring Oxygen resin；
（3）Calcining
10-15 parts by weight barium monoxide, 10-15 part by weight of zinc oxide are dried into 3-4h, warp in 120-125 DEG C of hot-air oven 1500-1600 DEG C of high-temperature calcination 2-4 hours is added 5-12 parts of starch, is ground to 200-300 mesh, for use；
（4）Prepare the hydrophobic epoxy coating of toughening
Add 1-3 parts by weight of graphite alkene, 0.1-0.3 parts by weight anti-settling agent, 1-2 parts by weight dodecanes into 100-150 parts by weight water After base benzene sulfonic acid sodium salt stirs 3-5 minutes, step（3）Gains are stirred 3-5 minutes, and 40-60 parts by weight diatomite is added to stir 15-20 minutes, gained modified liquid epoxy resin stirred 20-25 minutes in step (2), add 0.4-0.5 parts per weight dispersing agents, 0.1-0.3 parts by weight antifoaming agent and 0.3-0.5 parts by weight levelling agents mix mixing, obtain antibacterial hydrophobic epoxy coating.
The epoxy resin is in bisphenol A type epoxy resin, bisphenol f type epoxy resin and resorcinol type epoxy resin Two or three composition.
The epoxy resin is heated to 110-150 DEG C, heating means use heating water bath.
The antifoaming agent is dimethyl silicone polymer.
It is an advantage of the invention that：
Crystal aluminum chloride and acetylacetone,2,4-pentanedione hybrid reaction are carried out hydrophobically modified by the present invention, and atoleine drying is admixed after dry To constant weight, citric acid-modified is added dropwise into liquid epoxies, adds hydrophobically modified crystal aluminum chloride and is mixed to get modification Liquid epoxies, by barium monoxide, zinc oxide calcining and starch ground, later by graphene, anti-settling agent, dodecyl benzene sulfonic acid Sodium mixing diatomite is prepared into coating with modified liquid epoxy resin.The present invention will mix crystal aluminum chloride with acetylacetone,2,4-pentanedione Reaction carries out hydrophobically modified, and aluminium oxide is high active substance, and powder is coated by atoleine, improves hydrophobic performance, Backward liquid epoxies in citric acid-modified is added dropwise, polymerisation occurs with the epoxy group of epoxy resin, crosslinking generates vertical The polymer of body reticular structure, citric acid increase the degree of cross linking of polymer, to change the mechanical performance of composition, while can make It obtains hydrophobically modified crystal aluminum chloride to be linked on strand, forms stable structure, used after barium monoxide, zinc oxide after calcining Starch so that the two is combined into composition, can be stabilized in coating, and zinc oxide can increase the antimicrobial form of coating, the present invention By hydrophobically modified crystal aluminum chloride, later in modified epoxy, good mechanical performance and stability are made it have, is made Standby coating has hydrophobicity and antibiotic property.
Specific implementation mode
A kind of preparation method of antibacterial hydrophobic epoxy coating, which is characterized in that include the following steps：
（1）Hydrophobically modified crystal aluminum chloride
12 parts by weight Crystalline alchlors are mixed with 20 times of absolute ethyl alcohols and are sufficiently stirred makes to be configured to solution, to be mixed uniform 24 acetylacetone,2,4-pentanediones are slowly dropped in crystal aluminum chloride solution afterwards and are stirred for uniformly, by this solution under 50oC water bath conditions Stirring 1.5 hours, spray drying are added 3 part by weight of liquid paraffin and stir and evenly mix, stirred 6 hours under room temperature, drying to constant weight；
（2）Modified liquid epoxy resin
3 parts by weight of lemon acid solutions are added dropwise into 75 parts of liquid epoxies, are heated to 130 DEG C, gained is hydrophobic in addition (1) changes Property crystal aluminum chloride, be warming up to 80 DEG C stir 1 hour, be cooled to room temperature, obtain modified liquid epoxy resin；
（3）Calcining
12 parts by weight barium monoxide, 12 part by weight of zinc oxide are dried into 3.5h in 120 DEG C of hot-air ovens, through 1500 DEG C of high-temperature calcinations 2-4 hours, 10 parts of starch are added, are ground to 200-300 mesh, for use；
（4）Prepare the hydrophobic epoxy coating of toughening
Add 2 parts by weight of graphite alkene, 0.2 parts by weight anti-settling agent, 1.5 parts by weight neopelexes into 100 parts by weight water After stirring 3-5 minutes, step（3）Gains are stirred 3-5 minutes, add 50 parts by weight diatomite to stir 15 minutes, step (2) Middle gained modified liquid epoxy resin stirs 20 minutes, adds 0.45 parts per weight dispersing agent, 0.2 parts by weight antifoaming agent and 0.4 weight Part levelling agent mixes mixing, obtains antibacterial hydrophobic epoxy coating.
The epoxy resin is in bisphenol A type epoxy resin, bisphenol f type epoxy resin and resorcinol type epoxy resin Two or three composition.
The epoxy resin is heated to 140 DEG C, heating means use heating water bath.
The antifoaming agent is dimethyl silicone polymer.

Claims (4)

1. a kind of preparation method of antibacterial hydrophobic epoxy coating, which is characterized in that include the following steps：
Hydrophobically modified crystal aluminum chloride
10-15 parts by weight Crystalline alchlor is mixed with 18-23 times of absolute ethyl alcohol and is sufficiently stirred makes to be configured to solution, waits stirring 20-30 acetylacetone,2,4-pentanediones are slowly dropped in crystal aluminum chloride solution after mixing uniformly and are stirred for uniformly, by this solution in 50oC It stirs 1-2 hours, is spray-dried under water bath condition, 1-5 part by weight of liquid paraffin is added and stirs and evenly mixs, it is small that 5-8 is stirred under room temperature When, drying to constant weight；
（2）Modified liquid epoxy resin
1-5 parts by weight of lemon acid solutions are added dropwise into 70-80 parts of liquid epoxies, are heated to 110-150 DEG C, are added in (1) Gained hydrophobically modified crystal aluminum chloride is warming up to 80-100 DEG C and stirs 1-2 hours, is cooled to room temperature, obtains modified liquid ring Oxygen resin；
（3）Calcining
10-15 parts by weight barium monoxide, 10-15 part by weight of zinc oxide are dried into 3-4h, warp in 120-125 DEG C of hot-air oven 1500-1600 DEG C of high-temperature calcination 2-4 hours is added 5-12 parts of starch, is ground to 200-300 mesh, for use；
（4）Prepare the hydrophobic epoxy coating of toughening
Add 1-3 parts by weight of graphite alkene, 0.1-0.3 parts by weight anti-settling agent, 1-2 parts by weight dodecanes into 100-150 parts by weight water After base benzene sulfonic acid sodium salt stirs 3-5 minutes, step（3）Gains are stirred 3-5 minutes, and 40-60 parts by weight diatomite is added to stir 15-20 minutes, gained modified liquid epoxy resin stirred 20-25 minutes in step (2), add 0.4-0.5 parts per weight dispersing agents, 0.1-0.3 parts by weight antifoaming agent and 0.3-0.5 parts by weight levelling agents mix mixing, obtain antibacterial hydrophobic epoxy coating.
2. according to a kind of preparation method of antibacterial hydrophobic epoxy coating of claim 1, which is characterized in that the asphalt mixtures modified by epoxy resin Fat is two or three of composition in bisphenol A type epoxy resin, bisphenol f type epoxy resin and resorcinol type epoxy resin.
3. according to a kind of preparation method of antibacterial hydrophobic epoxy coating of claim 1, which is characterized in that the epoxy resin It is heated to 110-150 DEG C, heating means use heating water bath.
4. according to a kind of preparation method of antibacterial hydrophobic epoxy coating of claim 1, which is characterized in that the antifoaming agent is Dimethyl silicone polymer.
CN201810500827.7A 2018-05-23 2018-05-23 A kind of preparation method of antibacterial hydrophobic epoxy coating Pending CN108531044A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1401575A (en) * 2001-08-09 2003-03-12 中国科学院生态环境研究中心 Method for mfg. nano alumina
CN102180497A (en) * 2011-03-15 2011-09-14 宣城晶瑞新材料有限公司 Non-hydrolytic sol-gel method for preparing high- dispersity nano alumina
CN102229771A (en) * 2011-06-17 2011-11-02 李学东 Diatomaceous earth active paint and preparation method thereof
CN103059304A (en) * 2012-12-21 2013-04-24 海洋化工研究院有限公司 Preparation and application of long-acting anticorrosion temperature-resistant coating
CN103159437A (en) * 2011-12-15 2013-06-19 张国庆 Temperature adjusting humidity adjusting coating and preparation method thereof
CN106349874A (en) * 2016-08-29 2017-01-25 佛山市高明区尚润盈科技有限公司 Anticorrosion coating preparing method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1401575A (en) * 2001-08-09 2003-03-12 中国科学院生态环境研究中心 Method for mfg. nano alumina
CN102180497A (en) * 2011-03-15 2011-09-14 宣城晶瑞新材料有限公司 Non-hydrolytic sol-gel method for preparing high- dispersity nano alumina
CN102229771A (en) * 2011-06-17 2011-11-02 李学东 Diatomaceous earth active paint and preparation method thereof
CN103159437A (en) * 2011-12-15 2013-06-19 张国庆 Temperature adjusting humidity adjusting coating and preparation method thereof
CN103059304A (en) * 2012-12-21 2013-04-24 海洋化工研究院有限公司 Preparation and application of long-acting anticorrosion temperature-resistant coating
CN106349874A (en) * 2016-08-29 2017-01-25 佛山市高明区尚润盈科技有限公司 Anticorrosion coating preparing method

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