CN115322647A - Antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint and preparation method thereof - Google Patents

Antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint and preparation method thereof Download PDF

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Publication number
CN115322647A
CN115322647A CN202210794573.0A CN202210794573A CN115322647A CN 115322647 A CN115322647 A CN 115322647A CN 202210794573 A CN202210794573 A CN 202210794573A CN 115322647 A CN115322647 A CN 115322647A
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graphitization
carbon fiber
fiber micro
preparation
rate
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CN202210794573.0A
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Chinese (zh)
Inventor
郑晓平
沈业鹏
李佼佼
于海阔
韦海翔
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Nanjing Tiansland Biotechnology Co ltd
NANJING TIANSHI NEW MATERIAL TECHNOLOGY CO LTD
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Nanjing Tiansland Biotechnology Co ltd
NANJING TIANSHI NEW MATERIAL TECHNOLOGY CO LTD
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Priority to CN202210794573.0A priority Critical patent/CN115322647A/en
Publication of CN115322647A publication Critical patent/CN115322647A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/14Paints containing biocides, e.g. fungicides, insecticides or pesticides
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/24Electrically-conducting paints
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/001Conductive additives

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Plant Pathology (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention relates to the technical field of coatings, in particular to an antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint and a preparation method thereof, wherein the preparation method comprises the following steps: 1) Preparing carbon fiber micro powder with high graphitization rate; 2) Adding a conductive agent into the epoxy resin, and stirring and dispersing at a high speed; 3) And after the mixture is uniformly dispersed, sequentially adding a flatting agent, a polyolefin wax rheological agent, a polysiloxane solvent antifoaming agent, an antibacterial agent and a halogen-free phosphorus-nitrogen flame retardant, uniformly stirring, adding a color filler, and stirring and dispersing at a high speed to obtain the antistatic epoxy floor coating. The antistatic epoxy floor coating has the advantages of good permanent conductivity, antistatic property, wear resistance, solvent resistance, antibacterial property, flame retardance and the like, has no solvent, is easy to color, does not contain heavy metal, meets the environmental protection requirement, and meanwhile, has the advantages of simple preparation method, low cost and strong applicability, and can be used for large-scale production.

Description

Antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint and preparation method thereof
Technical Field
The invention relates to the field of coatings, in particular to an epoxy floor coating and a preparation method thereof.
Background
The ground level is easy to accumulate a large amount of static charges due to frequent friction, thereby hindering the production process and influencing the product quality, and in severe cases, accidents such as fire, explosion and the like are caused. The antistatic terrace coating can endow the terrace with conductivity to eliminate the harm of static electricity, so that the antistatic terrace coating is widely applied to the high and new technical fields of electronics, microelectronics, communication, precision instruments, computers, aerospace, military and the like in recent years.
Along with the stricter trend of environmental protection regulations, the solvent-free antistatic self-leveling epoxy floor coating becomes a main product antistatic floor coating of the antistatic floor coating due to the advantages of attractive appearance, good comprehensive performance and the like, belongs to a functional coating, conductive fillers are added into the coating, and a conductive network is generated by the contact of the conductive fillers to form a continuous conductive network or approach to each other, and electrons cross a potential barrier due to a tunnel effect to form an electron circulation network. The conductive filler is usually conductive carbon fiber, metal filler, graphite powder, conductive mica, etc. and needs a sufficient filling amount to form a conductive chain. However, the dispersion is difficult due to the excessive filling amount, the self-leveling thick coating is settled, even the conductive filler is not uniformly distributed, and the appearance of the coating surface layer is damaged. And the surface of the epoxy floor paint produced at present is easy to generate mould, is inflammable and has other defects.
Therefore, developing a brand new antibacterial, flame retardant and antistatic epoxy floor paint is one of the technical problems to be solved urgently in the field.
Disclosure of Invention
The invention aims to provide the antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro powder type epoxy floor paint which is simple in preparation process, controllable, low in cost and suitable for large-scale production and the preparation method.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of an antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint comprises the following steps:
(1) Preparing the carbon fiber micro powder with high graphitization rate: taking back the collected carbon fibers or the chopped carbon fibers, adding a ferrous sulfate solution, slowly adding hydrogen peroxide, reacting for a period of time, and carrying out suction filtration and drying to obtain the carbon fibers with high graphitization rate; finally, crushing the high-graphitization-rate carbon fibers into carbon fiber micro-powder with different particle sizes by a jet milling method, thereby preparing the high-graphitization-rate carbon fiber micro-powder;
(2) Adding a conductive agent into the epoxy resin, and stirring and dispersing at a high speed;
(3) And after the mixture is uniformly dispersed, sequentially adding a flatting agent, a polyolefin wax rheological agent, a polysiloxane solvent antifoaming agent, an antibacterial agent and a halogen-free phosphorus-nitrogen flame retardant, uniformly stirring, adding a color filler, and stirring and dispersing at a high speed to obtain the antistatic epoxy floor coating.
Wherein the mass fraction of the ferrous sulfate solution in the step (1) is 8-30%.
Wherein the mass fraction of the hydrogen peroxide solution in the step (1) is 3-15%.
Wherein the reaction time in the step (1) is 1-5h.
Wherein, the conductive agent in the step (2) is one or a composition of the high-graphitization-rate carbon fiber micro powder, the common carbon fiber micro powder, the carbon nano tube and the graphene prepared in the step (1), and the addition part of the conductive agent in each 100 parts of the epoxy resin is 0.3-2 parts.
Wherein, the leveling agent in the step (3) is one or a composition of acrylates, fluorocarbon modified polyacrylates and modified organic siloxane, and the addition part is 0.3-1 part.
Wherein the addition part of the polysiloxane solvent antifoaming agent in the step (3) is 0.4-1 part.
Wherein, the antibacterial agent in the step (3) is one or a composition of quaternary ammonium salts, silver ions and acylaniline, and the adding part is 0.1-0.5 part.
Wherein the addition part of the halogen-free phosphorus-nitrogen flame retardant in the step (3) is 4-10 parts.
Compared with the prior art, the invention has the beneficial effects that:
the antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint has the advantages of better permanent conductivity and antistatic property, better coloring performance, wear resistance, solvent resistance, antibacterial property, flame retardance and the like, has the advantages of no solvent or heavy metal, meets the environmental protection requirement, and meanwhile, is simple in preparation method, low in cost and strong in applicability, and can be used for large-scale production.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, 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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1
(1) Preparing carbon fiber micro powder with high graphitization rate: adding 100g of recovered carbon fibers or chopped carbon fibers into 150ml of 10% ferrous sulfate solution, slowly adding 50ml of 10% hydrogen peroxide, reacting for 3 hours, carrying out suction filtration and drying to obtain high-graphitization-rate carbon fibers, and finally crushing the high-graphitization-rate carbon fibers into carbon fiber micro-powder with different particle sizes by using a jet milling method to obtain the high-graphitization-rate carbon fiber micro-powder.
(2) 0.5 part of carbon fiber micro powder with high graphitization rate is added into 100 parts of epoxy resin and stirred and dispersed for 30min at the speed of 1200 r/min.
(3) After the mixture is uniformly dispersed, 0.5 part of flatting agent (fluorocarbon modified polyacrylate), 0.2 part of polyolefin wax rheological agent, 0.6 part of polysiloxane solvent defoaming agent, 0.1 part of antibacterial agent (quaternary ammonium salt), 6 parts of halogen-free phosphorus-nitrogen flame retardant and other auxiliary agents are sequentially added, after uniform stirring, other auxiliary agents such as color filler and the like are added, and the mixture is stirred and dispersed for 30min at the speed of 1200r/min, so that the antistatic epoxy floor coating is prepared.
After being cured, the surface of the material is flat and smooth, has no phenomena of flooding, no bubbles and the like, and has the surface resistance of 5 multiplied by 10 4 Omega, flame retardant grade V0, and sterilization rate not less than 90%.
Example 2
The difference between this example and example 1 is that the part of the conductive agent high graphitization ratio carbon fiber fine powder in step (2) is 1 part, and the other treatment means are the same as those in example 1.
The prepared product has flat and smooth surface, no flooding, no bubble and other phenomena after being cured, and the surface resistance of the product is 3.4 multiplied by 10 4 Omega, flame retardant grade V0, and sterilization rate not less than 90%.
Example 3
The present example differs from example 1 in that: in the step (2), the part of the conductive agent high-graphitization-rate carbon fiber micro powder is 0.3, and other treatment means are the same as those in the embodiment 1.
The product has smooth surface, no color floating, no bubble, and surface resistance of 2.6 × 10 5 Omega, flame retardant grade V0, and sterilization rate not less than 90%.
Example 3
This example differs from example 1 in that: the conductive agent in the step (2) is common carbon fiber micro powder, and other processing means are the same as those in the embodiment 1.
After the product is cured, the surface is flat and smooth, no flooding color, no bubble and other phenomena exist, the surface resistance is 9.6 multiplied by 107 omega, the flame retardant grade is V0, and the sterilization rate is not lower than 90 percent.
Example 4
The present example differs from example 1 in that: the conductive agent in step (2) is carbon nanotubes, and other treatment methods are the same as those in example 1.
The product has smooth surface, no floating color, no bubble, and surface resistance of 1 × 10 5 Omega, flame retardant grade V0, sterilization rate not less than 90%。
Example 5
The present example differs from example 1 in that: the leveling agent in the step (3) is acrylate, and other treatment means are the same as those in the example 1.
The product has smooth surface, no floating color, no bubble, and surface resistance of 5.9 × 10 4 Omega, flame retardant grade V0, and sterilization rate not less than 90%.
Example 6
This example differs from example 1 in that: the antibacterial agent in the step (3) is silver ions, and other treatment means are the same as those in the example 1.
The product has smooth surface, no color floating, no bubble, and surface resistance of 5.9 × 10 4 Omega, flame retardant grade V0, and sterilization rate not less than 85%.
Example 7
The present example differs from example 1 in that: the addition part of the halogen-free phosphorus-nitrogen flame retardant in the step (3) is 4. The other treatment methods were the same as in example 1.
The product has smooth surface, no floating color, no bubble, and surface resistance of 5.9 × 10 4 Omega, flame retardant grade V1, and sterilization rate not less than 85%.
To highlight the advantageous effects of the present invention, the following comparative example experiments are exemplified.
Comparative example 1
The present example differs from example 1 in that: the step (2) was carried out without adding a conductive agent, and the other treatment methods were the same as those in example 1.
The prepared product has flat and smooth surface, no flooding, no bubbles and other phenomena after being cured, and the surface resistance of the product is 1 multiplied by 10 14 Omega, flame retardant grade V0, and the sterilization rate is not less than 90 percent.
Comparative example 2
This example differs from example 1 in that: no flame retardant was added in step (3), and the other treatment methods were the same as in example 1.
The obtained product has flat and smooth surface and no defects after being curedFloating color, no bubbles, etc., and surface resistance of 5.6 × 10 4 Omega, flame retardant grade V2, and the sterilization rate is not less than 90 percent.
Comparative example 3
This example differs from example 1 in that: in step (3), no antimicrobial agent was added, and the other treatment methods were the same as those in example 1.
The prepared product has flat and smooth surface, no flooding, no bubble and other phenomena after being cured, and the surface resistance of the product is 6.6 multiplied by 10 4 Omega, flame retardant grade V0, and the sterilization rate is less than 5%.
Comparative example 4
This example differs from example 1 in that: in the step (2), the part of the conductive agent high-graphitization-rate carbon fiber micro powder is 10 parts, and other treatment means are the same as those in the embodiment 1.
The prepared product has flat and smooth surface, no flooding, no bubble and other phenomena after being cured, and the surface resistance of the product is 2 multiplied by 10 3 Omega, flame retardant grade V0, and the sterilization rate is not less than 90 percent.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various 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. The preparation method of the antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint is characterized by comprising the following steps of:
(1) Preparing the carbon fiber micro powder with high graphitization rate: taking back the collected carbon fibers or the chopped carbon fibers, adding a ferrous sulfate solution, slowly adding hydrogen peroxide, reacting for a period of time, and performing suction filtration and drying to obtain the carbon fibers with high graphitization rate; finally, crushing the high-graphitization-rate carbon fibers into carbon fiber micro-powder with different particle sizes by using a jet milling method, thereby preparing the high-graphitization-rate carbon fiber micro-powder;
(2) Adding a conductive agent into the epoxy resin, and stirring and dispersing at a high speed;
(3) After the mixture is uniformly dispersed, sequentially adding a flatting agent, a polyolefin wax rheological agent, a polysiloxane solvent defoamer, an antibacterial agent and a halogen-free phosphorus-nitrogen flame retardant, stirring uniformly, adding a color filler, and stirring at a high speed for dispersion to obtain the antistatic epoxy floor coating.
2. The preparation method of the antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint according to claim 1 is characterized by comprising the following steps of: the mass fraction of the ferrous sulfate solution in the step (1) is 8-30%.
3. The preparation method of the antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint according to claim 1 is characterized by comprising the following steps of: the mass fraction of the hydrogen peroxide solution in the step (1) is 3-15%.
4. The preparation method of the antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint according to claim 1 is characterized by comprising the following steps of: the reaction time in the step (1) is 1-5h.
5. The preparation method of the antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint according to claim 1 is characterized by comprising the following steps of: the conductive agent in the step (2) is one or a composition of the high-graphitization-rate carbon fiber micro powder prepared in the step (1), common carbon fiber micro powder, carbon nano tubes and graphene, and the addition amount of the conductive agent in each 100 parts of epoxy resin is 0.3-2 parts.
6. The preparation method of the antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint according to claim 1 is characterized by comprising the following steps of: the leveling agent in the step (3) is one or a composition of acrylates, fluorocarbon modified polyacrylates and modified organic siloxane, and the addition part of the leveling agent is 0.3-1 part.
7. The preparation method of the antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint according to claim 1, which is characterized by comprising the following steps of: in the step (3), the addition part of the polysiloxane solvent defoaming agent is 0.4-1 part.
8. The preparation method of the antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint according to claim 1 is characterized by comprising the following steps of: the antibacterial agent in the step (3) is one or a composition of quaternary ammonium salts, silver ions and acylaniline, and the adding part is 0.1-0.5 part.
9. The preparation method of the antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint according to claim 1 is characterized by comprising the following steps of: 4-10 parts of halogen-free phosphorus-nitrogen flame retardant in the step (3).
10. The antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint prepared by the preparation method of any one of claims 1-9.
CN202210794573.0A 2022-07-05 2022-07-05 Antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint and preparation method thereof Pending CN115322647A (en)

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CN202210794573.0A CN115322647A (en) 2022-07-05 2022-07-05 Antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint and preparation method thereof

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CN202210794573.0A CN115322647A (en) 2022-07-05 2022-07-05 Antibacterial flame-retardant antistatic high-graphitization-rate carbon fiber micro-powder type epoxy floor paint and preparation method thereof

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1664034A (en) * 2005-02-22 2005-09-07 大庆石油管理局 Carbon fiber static-conducting coating and method for making same

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1664034A (en) * 2005-02-22 2005-09-07 大庆石油管理局 Carbon fiber static-conducting coating and method for making same

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