CN116218301A - High-toughness thermal expansion microsphere composite graphene fireproof water-based paint - Google Patents

High-toughness thermal expansion microsphere composite graphene fireproof water-based paint Download PDF

Info

Publication number
CN116218301A
CN116218301A CN202211658120.1A CN202211658120A CN116218301A CN 116218301 A CN116218301 A CN 116218301A CN 202211658120 A CN202211658120 A CN 202211658120A CN 116218301 A CN116218301 A CN 116218301A
Authority
CN
China
Prior art keywords
parts
thermal expansion
graphene
water
based paint
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202211658120.1A
Other languages
Chinese (zh)
Inventor
张洲会
林逸伦
林德
高城
朱松青
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Deqing Yangtai Building Material Co ltd
Original Assignee
Deqing Yangtai Building Material Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Deqing Yangtai Building Material Co ltd filed Critical Deqing Yangtai Building Material Co ltd
Priority to CN202211658120.1A priority Critical patent/CN116218301A/en
Publication of CN116218301A publication Critical patent/CN116218301A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C09D133/00Coating 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • 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
    • C09D5/185Intumescent 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/63Additives non-macromolecular organic
    • 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
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2217Oxides; Hydroxides of metals of magnesium
    • C08K2003/222Magnesia, i.e. magnesium oxide
    • 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
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/322Ammonium phosphate
    • C08K2003/323Ammonium polyphosphate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Landscapes

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

Abstract

The invention discloses a high-toughness thermal expansion microsphere composite graphene fireproof water-based paint, which particularly relates to the field of water-based fireproof paint, and comprises the following components in parts by weight: 40-50 parts of water, 6-9 parts of graphene oxide, 13-15 parts of melamine, 15-20 parts of flame-retardant thermal expansion microspheres, 0.5-2 parts of a dispersing agent, 10-20 parts of a flame retardant, 10-20 parts of ammonium polyphosphate, 18-36 parts of acrylic resin, 10-20 parts of pentaerythritol, 20-25 parts of acrylic emulsion, 2-4 parts of magnesia powder and 1-3 parts of a defoaming agent. According to the high-toughness thermal expansion microsphere composite graphene fireproof water-based paint, graphene oxide is adopted as a raw material, so that compared with graphene, the graphene oxide is better in flexibility and better in hydrophilicity, the paint can have higher toughness, the strength of the paint adapting to external environment changes is effectively improved, and the hardness, wear resistance and flame retardance of the paint can be effectively enhanced by adding the flame-retardant thermal expansion microsphere into the paint.

Description

High-toughness thermal expansion microsphere composite graphene fireproof water-based paint
Technical Field
The invention relates to the field of water-based fireproof coatings, in particular to a high-toughness thermal expansion microsphere composite graphene fireproof water-based coating.
Background
The fireproof paint belongs to a special functional paint. The fireproof paint is coated on the surface of the base material, and can prevent the spread of flame when fire occurs, control the development of fire and effectively protect the internal structure. Fireproof paint has been widely used in public buildings, vehicles, airplanes, ships, ancient buildings, cultural relics, etc.
Chinese patent document CN111471365a discloses a graphene-based water-based intumescent fire-retardant coating and Fang Bingxi acid emulsion prepared by the same, and the preparation method of the graphene-based acrylic acid emulsion comprises: grafting an alcohol hydroxyl group on the surface of graphene to obtain alcohol hydroxylated graphene; grafting an initiator ACVA on alcohol hydroxylation graphene to prepare a graphene-based initiator; initiating acrylic monomer polymerization by using a graphene-based initiator to obtain graphene-based acrylic emulsion; the graphene-based initiator mostly inherits the inherent structure and performance of original graphene and has excellent water-solubility characteristics, so that the graphene-based initiator is completely suitable for initiating acrylic acid monomers, the graphene has a plurality of excellent characteristics, and a compact isolation layer can be formed in the fireproof coating due to the two-dimensional lamellar structure of the graphene, so that the flame retardant effect is achieved; meanwhile, graphene and a matrix are crosslinked and compounded to form a protective layer, so that overflow of solid particles formed in the combustion process is effectively inhibited, and the smoke suppression effect is remarkable. However, the coating may have limited flexibility and may not be able to accommodate external changes.
Disclosure of Invention
The invention mainly aims to provide a high-toughness thermal expansion microsphere composite graphene fireproof water-based paint, which can effectively solve the problem of low flexibility of the paint.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the high-toughness thermal expansion microsphere composite graphene fireproof water-based paint comprises the following components in parts by weight: 40-50 parts of water, 6-9 parts of graphene oxide, 13-15 parts of melamine, 15-20 parts of flame-retardant thermal expansion microspheres, 0.5-2 parts of a dispersing agent, 10-20 parts of a flame retardant, 10-20 parts of ammonium polyphosphate, 18-36 parts of acrylic resin, 10-20 parts of pentaerythritol, 20-25 parts of acrylic emulsion, 2-4 parts of magnesia powder and 1-3 parts of a defoaming agent;
the preparation method of the composite graphene fireproof water-based paint comprises the following steps: (1) preparing graphene oxide; (2) And mixing other raw material components for preparing the graphene oxide to prepare the composite fireproof water-based paint.
Preferably, the graphene oxide is a large graphene oxide sheet, the diameter of the graphene oxide sheet is 35-50 mu m, and oxygen-containing active groups are distributed on the surface of the graphene.
Preferably, the flame-retardant thermal expansion microsphere is a particle with a core-shell structure, the shell is an acrylic resin copolymer, and the inner core is formed by mixing an oil-soluble flame retardant and an inert hydrocarbon.
Preferably, the flame retardant is at least one of halogen-based, phosphorus-based or nitrogen-based flame retardants.
Preferably, the dispersing agent is one of sodium salt of polycarboxylic acid, polyacrylate or a mixture thereof.
Preferably, the defoaming agent is an organosilicon defoaming agent.
Preferably, the graphene oxide preparation steps are as follows:
(1) And (3) a reaction bottle is assembled in an ice water bath, a proper amount of concentrated sulfuric acid is added, a solid mixture of 4 parts of graphite powder and 2 parts of sodium nitrate is added under stirring, 12 parts of potassium permanganate is added in multiple times, the reaction temperature is controlled to be not more than 22 ℃, and the reaction is carried out under stirring for a period of time.
(2) Heating to 38 ℃ and continuously stirring for 30min, slowly adding a certain amount of deionized water, continuously stirring for 20min, and adding a proper amount of hydrogen peroxide to reduce the residual oxidant.
(3) Filtered while hot and washed with 5% hc l solution and deionized water until no sulfate in the filtrate is detected.
(4) And (5) placing the filter cake in a vacuum drying oven at 60 ℃ for full drying and preserving for standby.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, graphene oxide is used as a raw material, compared with graphene, the graphene oxide has better flexibility and better hydrophilicity, and oxygen-containing active groups are distributed on the surface of the graphene oxide, so that the flexibility of the coating can be effectively improved, the coating can have higher toughness, and the strength of the coating adapting to external environment changes can be effectively improved.
2. According to the invention, the flame-retardant thermal expansion microsphere is added into the paint, so that the hardness, wear resistance and flame retardance of the paint can be effectively enhanced, and meanwhile, the shell of the thermal expansion microsphere is a thermoplastic polymer, so that the filled paint has an excellent heat insulation effect, and meanwhile, the thermal expansion microsphere is nontoxic and pollution-free, so that the paint is more environment-friendly and safe, the flame retardance of the paint can be effectively improved by adding the flame-retardant thermal expansion microsphere and the flame retardant into the paint, and the spread of fire can be effectively prevented or slowed down.
Detailed Description
The invention is further described in connection with the following detailed description, in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
Example 1
In the embodiment, the high-toughness thermal expansion microsphere composite graphene fireproof water-based paint is prepared from the following raw materials in percentage by weight: 40 parts of water, 6 parts of graphene oxide, 13 parts of melamine, 15 parts of flame-retardant thermal expansion microspheres, 0.5 part of a dispersing agent, 10 parts of a flame retardant, 10 parts of ammonium polyphosphate, 18 parts of acrylic resin, 10 parts of pentaerythritol, 20 parts of an acrylic emulsion, 2 parts of magnesia powder and 1 part of a defoaming agent.
The graphene oxide is a large graphene oxide sheet, the diameter of the graphene oxide sheet is 35 mu m, the number of layers is 8-10, and oxygen-containing active groups are distributed on the surface of the graphene; the flame-retardant thermal expansion microsphere is a particle with a core-shell structure, the shell is an acrylic resin copolymer, and the inner core is formed by mixing an oil-soluble flame retardant and an inert hydrocarbon; the flame retardant is halogen flame retardant; the dispersing agent is polycarboxylic acid sodium salt; the defoaming agent is an organosilicon defoaming agent.
The preparation method of the composite fireproof water-based paint prepared by the embodiment is as follows:
1. preparing graphene oxide:
(1) And (3) a reaction bottle is assembled in an ice water bath, a proper amount of concentrated sulfuric acid is added, a solid mixture of 4 parts of graphite powder and 2 parts of sodium nitrate is added under stirring, 12 parts of potassium permanganate is added in multiple times, the reaction temperature is controlled to be not more than 22 ℃, and the reaction is carried out under stirring for a period of time.
(2) Heating to 38 ℃ and continuously stirring for 30min, slowly adding a certain amount of deionized water, continuously stirring for 20min, and adding a proper amount of hydrogen peroxide to reduce the residual oxidant.
(3) Filtered while hot and washed with 5% hc l solution and deionized water until no sulfate in the filtrate is detected.
(4) And (5) placing the filter cake in a vacuum drying oven at 60 ℃ for full drying and preserving for standby.
2. Preparing a composite graphene fireproof water-based paint:
the water, melamine, flame-retardant thermal expansion microspheres, a dispersing agent, a flame retardant, ammonium polyphosphate, acrylic resin, pentaerythritol, acrylic emulsion, magnesia powder, a defoaming agent and graphene oxide are fully mixed according to the components to prepare the composite graphene fireproof water-based paint.
Example 2
In the embodiment, the high-toughness thermal expansion microsphere composite graphene fireproof water-based paint is prepared from the following raw materials in percentage by weight: 45 parts of water, 7 parts of graphene oxide, 14 parts of melamine, 19 parts of flame-retardant thermal expansion microspheres, 1 part of a dispersing agent, 15 parts of a flame retardant, 15 parts of ammonium polyphosphate, 24 parts of acrylic resin, 15 parts of pentaerythritol, 25 parts of acrylic emulsion, 2 parts of magnesia powder and 2 parts of a defoaming agent.
The graphene oxide is a large graphene oxide sheet, the diameter of the graphene oxide sheet is 40 mu m, the number of layers is 3-6, and oxygen-containing active groups are distributed on the surface of the graphene; the flame-retardant thermal expansion microsphere is a particle with a core-shell structure, the shell is an acrylic resin copolymer, and the inner core is formed by mixing an oil-soluble flame retardant and an inert hydrocarbon; the flame retardant is a phosphorus flame retardant; the dispersing agent is polyacrylate; the defoaming agent is an organosilicon defoaming agent.
The preparation method of the composite fireproof water-based paint prepared by the embodiment is as follows:
1. preparing graphene oxide:
(1) And (3) a reaction bottle is assembled in an ice water bath, a proper amount of concentrated sulfuric acid is added, a solid mixture of 4 parts of graphite powder and 2 parts of sodium nitrate is added under stirring, 12 parts of potassium permanganate is added in multiple times, the reaction temperature is controlled to be not more than 22 ℃, and the reaction is carried out under stirring for a period of time.
(2) Heating to 38 ℃ and continuously stirring for 30min, slowly adding a certain amount of deionized water, continuously stirring for 20min, and adding a proper amount of hydrogen peroxide to reduce the residual oxidant.
(3) Filtered while hot and washed with 5% hc l solution and deionized water until no sulfate in the filtrate is detected.
(4) And (5) placing the filter cake in a vacuum drying oven at 60 ℃ for full drying and preserving for standby.
2. Preparing a composite graphene fireproof water-based paint:
the water, melamine, flame-retardant thermal expansion microspheres, a dispersing agent, a flame retardant, ammonium polyphosphate, acrylic resin, pentaerythritol, acrylic emulsion, magnesia powder, a defoaming agent and graphene oxide are fully mixed according to the components to prepare the composite graphene fireproof water-based paint.
Example 3
In the embodiment, the high-toughness thermal expansion microsphere composite graphene fireproof water-based paint is prepared from the following raw materials in percentage by weight: 50 parts of water, 8 parts of graphene oxide, 15 parts of melamine, 18 parts of flame-retardant thermal expansion microspheres, 1.5 parts of a dispersing agent, 10 parts of a flame retardant, 15 parts of ammonium polyphosphate, 28 parts of acrylic resin, 15 parts of pentaerythritol, 23 parts of acrylic emulsion, 3 parts of magnesium oxide powder and 1 part of a defoaming agent.
The graphene oxide is a large graphene oxide sheet, the diameter of the graphene oxide sheet is 35 mu m, the number of layers is 4-6, and oxygen-containing active groups are distributed on the surface of the graphene; the flame-retardant thermal expansion microsphere is a particle with a core-shell structure, the shell is an acrylic resin copolymer, and the inner core is formed by mixing an oil-soluble flame retardant and an inert hydrocarbon; the flame retardant is halogen flame retardant; the dispersing agent is a mixture of sodium salt of polycarboxylic acid and polyacrylate; the defoaming agent is an organosilicon defoaming agent.
The preparation method of the composite fireproof water-based paint prepared by the embodiment is as follows:
1. preparing graphene oxide:
(1) And (3) a reaction bottle is assembled in an ice water bath, a proper amount of concentrated sulfuric acid is added, a solid mixture of 4 parts of graphite powder and 2 parts of sodium nitrate is added under stirring, 12 parts of potassium permanganate is added in multiple times, the reaction temperature is controlled to be not more than 22 ℃, and the reaction is carried out under stirring for a period of time.
(2) Heating to 38 ℃ and continuously stirring for 30min, slowly adding a certain amount of deionized water, continuously stirring for 20min, and adding a proper amount of hydrogen peroxide to reduce the residual oxidant.
(3) Filtered while hot and washed with 5% hc l solution and deionized water until no sulfate in the filtrate is detected.
(4) And (5) placing the filter cake in a vacuum drying oven at 60 ℃ for full drying and preserving for standby.
2. Preparing a composite graphene fireproof water-based paint:
the water, melamine, flame-retardant thermal expansion microspheres, a dispersing agent, a flame retardant, ammonium polyphosphate, acrylic resin, pentaerythritol, acrylic emulsion, magnesia powder, a defoaming agent and graphene oxide are fully mixed according to the components to prepare the composite graphene fireproof water-based paint.
Example 4
In the embodiment, the high-toughness thermal expansion microsphere composite graphene fireproof water-based paint is prepared from the following raw materials in percentage by weight: 48 parts of water, 6 parts of graphene oxide, 14 parts of melamine, 15 parts of flame-retardant thermal expansion microspheres, 1 part of a dispersing agent, 10 parts of a flame retardant, 18 parts of ammonium polyphosphate, 30 parts of acrylic resin, 18 parts of pentaerythritol, 24 parts of acrylic emulsion, 4 parts of magnesia powder and 3 parts of a defoaming agent.
The graphene oxide is a large graphene oxide sheet, the diameter of the graphene oxide sheet is 45 mu m, the number of layers is 2-4, and oxygen-containing active groups are distributed on the surface of the graphene; the flame-retardant thermal expansion microsphere is a particle with a core-shell structure, the shell is an acrylic resin copolymer, and the inner core is formed by mixing an oil-soluble flame retardant and an inert hydrocarbon; the flame retardant is a nitrogen flame retardant; the dispersing agent is polycarboxylic acid sodium salt; the defoaming agent is an organosilicon defoaming agent.
The preparation method of the composite fireproof water-based paint prepared by the embodiment is as follows:
1. preparing graphene oxide:
(1) And (3) a reaction bottle is assembled in an ice water bath, a proper amount of concentrated sulfuric acid is added, a solid mixture of 4 parts of graphite powder and 2 parts of sodium nitrate is added under stirring, 12 parts of potassium permanganate is added in multiple times, the reaction temperature is controlled to be not more than 22 ℃, and the reaction is carried out under stirring for a period of time.
(2) Heating to 38 ℃ and continuously stirring for 30min, slowly adding a certain amount of deionized water, continuously stirring for 20min, and adding a proper amount of hydrogen peroxide to reduce the residual oxidant.
(3) Filtered while hot and washed with 5% hc l solution and deionized water until no sulfate in the filtrate is detected.
(4) And (5) placing the filter cake in a vacuum drying oven at 60 ℃ for full drying and preserving for standby.
2. Preparing a composite graphene fireproof water-based paint:
the water, melamine, flame-retardant thermal expansion microspheres, a dispersing agent, a flame retardant, ammonium polyphosphate, acrylic resin, pentaerythritol, acrylic emulsion, magnesia powder, a defoaming agent and graphene oxide are fully mixed according to the components to prepare the composite graphene fireproof water-based paint.
Example 5
In the embodiment, the high-toughness thermal expansion microsphere composite graphene fireproof water-based paint is prepared from the following raw materials in percentage by weight: 48 parts of water, 8 parts of graphene oxide, 13 parts of melamine, 20 parts of flame-retardant thermal expansion microspheres, 2 parts of a dispersing agent, 18 parts of a flame retardant, 18 parts of ammonium polyphosphate, 34 parts of acrylic resin, 18 parts of pentaerythritol, 22 parts of acrylic emulsion, 3 parts of magnesia powder and 3 parts of a defoaming agent.
The graphene oxide is a large graphene oxide sheet, the diameter of the graphene oxide sheet is 45 mu m, the number of layers is 2-3, and oxygen-containing active groups are distributed on the surface of the graphene; the flame-retardant thermal expansion microsphere is a particle with a core-shell structure, the shell is an acrylic resin copolymer, and the inner core is formed by mixing an oil-soluble flame retardant and an inert hydrocarbon; the flame retardant is halogen flame retardant; the dispersing agent is polycarboxylic acid sodium salt; the defoaming agent is an organosilicon defoaming agent.
The preparation method of the composite fireproof water-based paint prepared by the embodiment is as follows:
1. preparing graphene oxide:
(1) And (3) a reaction bottle is assembled in an ice water bath, a proper amount of concentrated sulfuric acid is added, a solid mixture of 4 parts of graphite powder and 2 parts of sodium nitrate is added under stirring, 12 parts of potassium permanganate is added in multiple times, the reaction temperature is controlled to be not more than 22 ℃, and the reaction is carried out under stirring for a period of time.
(2) Heating to 38 ℃ and continuously stirring for 30min, slowly adding a certain amount of deionized water, continuously stirring for 20min, and adding a proper amount of hydrogen peroxide to reduce the residual oxidant.
(3) Filtered while hot and washed with 5% hc l solution and deionized water until no sulfate in the filtrate is detected.
(4) And (5) placing the filter cake in a vacuum drying oven at 60 ℃ for full drying and preserving for standby.
2. Preparing a composite graphene fireproof water-based paint:
the water, melamine, flame-retardant thermal expansion microspheres, a dispersing agent, a flame retardant, ammonium polyphosphate, acrylic resin, pentaerythritol, acrylic emulsion, magnesia powder, a defoaming agent and graphene oxide are fully mixed according to the components to prepare the composite graphene fireproof water-based paint.
Example 6
In the embodiment, the high-toughness thermal expansion microsphere composite graphene fireproof water-based paint is prepared from the following raw materials in percentage by weight: 50 parts of water, 9 parts of graphene oxide, 15 parts of melamine, 20 parts of flame-retardant thermal expansion microspheres, 2 parts of a dispersing agent, 20 parts of a flame retardant, 20 parts of ammonium polyphosphate, 36 parts of acrylic resin, 20 parts of pentaerythritol, 25 parts of acrylic emulsion, 4 parts of magnesia powder and 3 parts of a defoaming agent.
The graphene oxide is a large graphene oxide sheet, the diameter of the graphene oxide sheet is 50 mu m, the number of layers is 1-2, and oxygen-containing active groups are distributed on the surface of the graphene; the flame-retardant thermal expansion microsphere is a particle with a core-shell structure, the shell is an acrylic resin copolymer, and the inner core is formed by mixing an oil-soluble flame retardant and an inert hydrocarbon; the flame retardant is halogen flame retardant; the dispersing agent is polycarboxylic acid sodium salt; the defoaming agent is an organosilicon defoaming agent.
The preparation method of the composite fireproof water-based paint prepared by the embodiment is as follows:
1. preparing graphene oxide:
(1) And (3) a reaction bottle is assembled in an ice water bath, a proper amount of concentrated sulfuric acid is added, a solid mixture of 4 parts of graphite powder and 2 parts of sodium nitrate is added under stirring, 12 parts of potassium permanganate is added in multiple times, the reaction temperature is controlled to be not more than 22 ℃, and the reaction is carried out under stirring for a period of time.
(2) Heating to 38 ℃ and continuously stirring for 30min, slowly adding a certain amount of deionized water, continuously stirring for 20min, and adding a proper amount of hydrogen peroxide to reduce the residual oxidant.
(3) Filtered while hot and washed with 5% hc l solution and deionized water until no sulfate in the filtrate is detected.
(4) And (5) placing the filter cake in a vacuum drying oven at 60 ℃ for full drying and preserving for standby.
2. Preparing a composite graphene fireproof water-based paint:
the water, melamine, flame-retardant thermal expansion microspheres, a dispersing agent, a flame retardant, ammonium polyphosphate, acrylic resin, pentaerythritol, acrylic emulsion, magnesia powder, a defoaming agent and graphene oxide are fully mixed according to the components to prepare the composite graphene fireproof water-based paint.
Comparative example 1
In the embodiment, the high-toughness thermal expansion microsphere composite graphene fireproof water-based paint is prepared from the following raw materials in percentage by weight: 50 parts of water, 9 parts of graphene, 15 parts of melamine, 20 parts of flame-retardant thermal expansion microspheres, 2 parts of a dispersing agent, 20 parts of a flame retardant, 20 parts of ammonium polyphosphate, 36 parts of acrylic resin, 20 parts of pentaerythritol, 25 parts of an acrylic emulsion, 4 parts of magnesium oxide powder and 3 parts of a defoaming agent.
The flame-retardant thermal expansion microsphere is a particle with a core-shell structure, the shell is an acrylic resin copolymer, and the inner core is formed by mixing an oil-soluble flame retardant and an inert hydrocarbon; the flame retardant is halogen flame retardant; the dispersing agent is polycarboxylic acid sodium salt; the defoaming agent is an organosilicon defoaming agent.
The preparation method of the composite fireproof water-based paint prepared by the embodiment is as follows:
the water, melamine, flame-retardant thermal expansion microspheres, a dispersing agent, a flame retardant, ammonium polyphosphate, acrylic resin, pentaerythritol, acrylic emulsion, magnesia powder, a defoaming agent and graphene are fully mixed according to components to prepare the composite graphene fireproof water-based paint.
The high-toughness thermal expansion microsphere composite graphene fireproof water-based paint prepared in the 7 embodiments is tested and specifically comprises the following components: the method of flame resistance time test is referred to as T15442.2-1995, the method of strength test is referred to as GB/T1732, the method of flexibility test is referred to as GB/T1731, and the method of adhesion test is referred to as GB/T9286.
The results of the performance test of the various embodiments of the present invention are shown in Table 1
Table 1:
performance index Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Comparative example 1
Flame resistance time 200min 233min 210min 195min 240min 247min 243min
Strength of 98.7% 105.6% 102.2% 108.5% 110.1% 112.8% 97.9%
Flexibility of the product By passing through By passing through By passing through By passing through By passing through By passing through Failed to pass
The adhesive force/grade is less than or equal to 1 1 0 0 1 1 0 0
From the flame resistance time of table 1, it can be seen that the more flame retardant microspheres and flame retardant are added in each example, the better the flame retardant effect, the longer the flame retardant time, and the more flame retardant expansion micro-addition, the better the flame retardant effect can be seen by comparing example 3 with example 5.
As can be seen from the flexibility test results of Table 1, in the case that graphene oxide is used in example 6, graphene is used in comparative example 1, and the proportions of other raw materials are the same, the flexibility of the coating using graphene oxide is better than that of the coating using graphene.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (7)

1. A high-toughness thermal expansion microsphere composite graphene fireproof water-based paint is characterized in that: the composite graphene fireproof water-based paint comprises the following components in parts by weight: 40-50 parts of water, 6-9 parts of graphene oxide, 13-15 parts of melamine, 15-20 parts of flame-retardant thermal expansion microspheres, 0.5-2 parts of a dispersing agent, 10-20 parts of a flame retardant, 10-20 parts of ammonium polyphosphate, 18-36 parts of acrylic resin, 10-20 parts of pentaerythritol, 20-25 parts of acrylic emulsion, 2-4 parts of magnesia powder and 1-3 parts of a defoaming agent;
the preparation method of the composite graphene fireproof water-based paint comprises the following steps: (1) preparing graphene oxide; (2) And mixing other raw materials for preparing the graphene oxide according to the components to prepare the composite fireproof water-based paint.
2. The high-toughness thermal expansion microsphere composite graphene fireproof water-based paint according to claim 1, which is characterized in that: the graphene oxide is large graphene oxide with the diameter of 35-50 mu m, and oxygen-containing active groups are distributed on the surface of the graphene oxide.
3. The high-toughness thermal expansion microsphere composite graphene fireproof water-based paint according to claim 1, which is characterized in that: the flame-retardant thermal expansion microsphere is in a particle shape with a core-shell structure, the shell is an acrylic resin copolymer, and the inner core is formed by mixing an oil-soluble flame retardant and an inert hydrocarbon.
4. The high-toughness thermal expansion microsphere composite graphene fireproof water-based paint according to claim 1, which is characterized in that: the flame retardant is at least one of halogen-based, phosphorus-based or nitrogen-based flame retardants.
5. The high-toughness thermal expansion microsphere composite graphene fireproof water-based paint according to claim 1, which is characterized in that: the dispersing agent is one or a mixture of sodium polycarboxylate and polyacrylate.
6. The high-toughness thermal expansion microsphere composite graphene fireproof water-based paint according to claim 1, which is characterized in that: the defoaming agent is an organosilicon defoaming agent.
7. The high-toughness thermal expansion microsphere composite graphene fireproof water-based paint according to claim 2, which is characterized in that: the preparation method of the graphene oxide comprises the following steps:
(1) And (3) a reaction bottle is assembled in an ice water bath, a proper amount of concentrated sulfuric acid is added, a solid mixture of 4 parts of graphite powder and 2 parts of sodium nitrate is added under stirring, 12 parts of potassium permanganate is added in multiple times, the reaction temperature is controlled to be not more than 22 ℃, and the reaction is carried out under stirring for a period of time.
(2) Heating to 38 ℃ and continuously stirring for 30min, slowly adding a certain amount of deionized water, continuously stirring for 20min, and adding a proper amount of hydrogen peroxide to reduce the residual oxidant.
(3) Filtered while hot and washed with 5% hcl solution and deionized water until no sulfate is detected in the filtrate.
(4) And (5) placing the filter cake in a vacuum drying oven at 60 ℃ for full drying and preserving for standby.
CN202211658120.1A 2022-12-22 2022-12-22 High-toughness thermal expansion microsphere composite graphene fireproof water-based paint Pending CN116218301A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211658120.1A CN116218301A (en) 2022-12-22 2022-12-22 High-toughness thermal expansion microsphere composite graphene fireproof water-based paint

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211658120.1A CN116218301A (en) 2022-12-22 2022-12-22 High-toughness thermal expansion microsphere composite graphene fireproof water-based paint

Publications (1)

Publication Number Publication Date
CN116218301A true CN116218301A (en) 2023-06-06

Family

ID=86579472

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202211658120.1A Pending CN116218301A (en) 2022-12-22 2022-12-22 High-toughness thermal expansion microsphere composite graphene fireproof water-based paint

Country Status (1)

Country Link
CN (1) CN116218301A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116769369A (en) * 2023-07-25 2023-09-19 上海纳米技术及应用国家工程研究中心有限公司 Intumescent fire-retardant coating and preparation method thereof
CN116925611A (en) * 2023-07-24 2023-10-24 上海纳米技术及应用国家工程研究中心有限公司 Fireproof coating and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103788789A (en) * 2013-10-21 2014-05-14 溧阳市浙大产学研服务中心有限公司 Fireproof coating used for steel structure buildings, preparation method thereof and coating process
CN106833191A (en) * 2017-01-13 2017-06-13 河北晨阳工贸集团有限公司 A kind of motor housing acrylic acid sealing wax and preparation method thereof
CN108084333A (en) * 2017-12-30 2018-05-29 扬州大学 A kind of low stain flame retardant type microspheres and preparation method thereof
CN110698944A (en) * 2019-11-06 2020-01-17 青岛爱尔家佳新材料股份有限公司 Graphene oxide modified water-based fireproof coating and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103788789A (en) * 2013-10-21 2014-05-14 溧阳市浙大产学研服务中心有限公司 Fireproof coating used for steel structure buildings, preparation method thereof and coating process
CN106833191A (en) * 2017-01-13 2017-06-13 河北晨阳工贸集团有限公司 A kind of motor housing acrylic acid sealing wax and preparation method thereof
CN108084333A (en) * 2017-12-30 2018-05-29 扬州大学 A kind of low stain flame retardant type microspheres and preparation method thereof
CN110698944A (en) * 2019-11-06 2020-01-17 青岛爱尔家佳新材料股份有限公司 Graphene oxide modified water-based fireproof coating and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
罗春华等: "材料制备与性能测试实验", vol. 1, 机械工业出版社, pages: 201 - 202 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116925611A (en) * 2023-07-24 2023-10-24 上海纳米技术及应用国家工程研究中心有限公司 Fireproof coating and preparation method thereof
CN116769369A (en) * 2023-07-25 2023-09-19 上海纳米技术及应用国家工程研究中心有限公司 Intumescent fire-retardant coating and preparation method thereof

Similar Documents

Publication Publication Date Title
CN116218301A (en) High-toughness thermal expansion microsphere composite graphene fireproof water-based paint
CN111234564B (en) Environment-friendly flame retardant and intumescent fire-retardant coating prepared from same
CN108676427B (en) Water-based microencapsulated ultra-thin steel structure fireproof coating and preparation method thereof
CN109627867B (en) Graphene modified fireproof coating and preparation method thereof
CN103694615A (en) Antistatic halogen-free environment-friendly flame-retardant sheet moulding compound and preparation method thereof
CN112029367A (en) Ultrathin expansion type fireproof coating
CN111995919A (en) Acrylic polymer emulsion for ultrathin intumescent fire-retardant coating and preparation method thereof
CN114059354B (en) Process for preparing Teflon high-temperature cloth based on impregnation method
CN116769369A (en) Intumescent fire-retardant coating and preparation method thereof
CN113402919A (en) Epoxy resin coating modified by core-shell flame retardant and preparation method thereof
CN103740337A (en) Novel shaped phase-change material and preparation method thereof
CN112574611A (en) Carbon fiber fireproof flame-retardant coating and preparation method thereof
CN114106647B (en) Environment-friendly structural water-based intumescent fire-retardant coating and preparation method thereof
CN114874481A (en) Polymethacrylimide foam with multi-layer wave-absorbing structure and preparation method thereof
CN113321959B (en) Epoxy expansion type steel structure fireproof paint for spraying fire scene
CN113354988A (en) Anticorrosive fireproof coating and preparation method thereof
CN112029157B (en) Anti-dripping composite intumescent flame retardant and preparation method and application thereof
CN111234463B (en) Bio-based flame-retardant EP composite material
CN108912261B (en) Flame-retardant acrylate miniemulsion and preparation method thereof
CN109111797B (en) Fireproof coating for power equipment and preparation method thereof
CN106833194A (en) A kind of flame-retardant coating material of cable and preparation method thereof
CN108485347B (en) Fireproof coating and preparation method thereof
CN116925611A (en) Fireproof coating and preparation method thereof
CN115785776B (en) Fluorine-containing alkyd environment-friendly paint and preparation method thereof
CN115873470A (en) Preparation method of graphene-like boron nitride-based self-extinguishing water-based fireproof coating

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination