CN110607101A - Water-based fireproof heat-insulating coating, fireproof material and preparation method thereof - Google Patents

Water-based fireproof heat-insulating coating, fireproof material and preparation method thereof Download PDF

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Publication number
CN110607101A
CN110607101A CN201810616351.3A CN201810616351A CN110607101A CN 110607101 A CN110607101 A CN 110607101A CN 201810616351 A CN201810616351 A CN 201810616351A CN 110607101 A CN110607101 A CN 110607101A
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rectorite
water
parts
insulating coating
coating
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CN110607101B (en
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杨华明
解维闵
陈洪运
欧阳静
张毅
傅梁杰
刘赛男
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Central South University
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Central South University
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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
    • C09D131/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid, or of a haloformic acid; Coating compositions based on derivatives of such polymers
    • C09D131/02—Homopolymers or copolymers of esters of monocarboxylic acids
    • C09D131/04—Homopolymers or copolymers of vinyl acetate
    • 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
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • 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
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • 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
    • C08K3/32—Phosphorus-containing compounds
    • C08K2003/321—Phosphates
    • C08K2003/322—Ammonium phosphate
    • C08K2003/323—Ammonium polyphosphate

Abstract

The invention belongs to the field of fireproof heat-insulating materials, and particularly discloses a water-based fireproof heat-insulating coating, which is characterized in that: comprises an acid source, a carbon source, a gas source, intercalation modified rectorite, a film forming substance and water. The intercalation modified rectorite is inorganic cation and/or organic cation intercalation modified rectorite. According to the invention, the intercalated modified rectorite is innovatively used as the fireproof flame-retardant filler, and the organic modification treatment is carried out on the rectorite, so that the problem of large oil absorption of the rectorite is solved, the fireproof heat-insulating coating with excellent performance is obtained, the application field of the rectorite can be widened, and the recycling of the rectorite is realized.

Description

Water-based fireproof heat-insulating coating, fireproof material and preparation method thereof
Technical Field
The invention relates to the technical field of fireproof coatings, in particular to a water-based ultrathin intumescent fireproof heat-insulating coating and a preparation method thereof.
Background
For a long time, the fire disaster is a universal catastrophic problem in the world, seriously threatens the safety of human life and property, and the fire disaster caused by various reasons causes great loss to the life and property of people. Fire protection is an important field of fire-fighting science and technology, and the fire-proof coating is also an important component of a fire-proof material. The coating is coated on the surface of an object, usually plays a certain decorative role, is difficult to burn or non-combustible when meeting fire, has good protective effect on a matrix material, and wins time for fire extinguishment and personnel evacuation. And thus its research and application has attracted a wide attention of countries all over the world.
Compared with thick-coating and thin-coating fireproof coatings, the ultrathin fireproof coating has the advantages of fine granularity, thin coating, convenient construction, good decoration and the like, and can meet the requirements of flame retardance and high decoration of people. Because the coating of the fireproof coating is ultrathin, the use amount in engineering is greatly reduced, the total amount of engineering used in special occasions such as ships, airplanes and the like is also reduced, and meanwhile, the base material is effectively protected, so that the fireproof coating is vigorously popularized by fire departments at present, and is a research hotspot in the field of fireproof coatings. The water-based paint takes water as a solvent, disperses a film forming substance, a fireproof flame retardant, a pigment filler, an auxiliary agent and the like, and avoids organic solvents in the processes of production, transportation, construction and use, thereby avoiding the generation of volatile organic compounds, reducing environmental pollution and protecting the health of human beings. Therefore, the water-based ultrathin intumescent fire retardant coating has a great development prospect.
Rectorite is a rare layered silicate clay mineral with a special structure formed by a dioctahedral mica layer and a dioctahedral montmorillonite layer according to the ratio of 1: 1; it has unique laminated structure, high suspension property and high heat stability. At present, the research researchers mainly focus on the fields of high-quality deep drilling mud, catalyst carriers, lubricating esters, ceramics, rubber, environment-friendly materials, filtering materials, coating suspending agents and the like for developing and utilizing rectorite. No report is found about the preparation of fire-retardant coating by rectorite.
Disclosure of Invention
The invention aims to solve the defects in the prior fireproof coating technology, and provides a water-based fireproof heat-insulating coating (also called water-based ultrathin intumescent fireproof coating or simply called fireproof coating or coating) added with organic intercalation modified rectorite (also called intercalation modified rectorite in the invention) for improving the fire resistance and heat insulation performance of the water-based fireproof heat-insulating coating.
The second purpose of the invention is to provide a preparation method of the water-based fireproof heat-insulating coating.
The third object of the present invention is to provide a fire-proof material, which is improved in performance by using the novel water-based fire-proof heat-insulating coating.
Clay minerals such as kaolin, mica, talc, expanded vermiculite, sepiolite, attapulgite and the like have been disclosed as inorganic fillers to improve the expansion ratio and the fire endurance of the fire retardant coating material. Because rectorite has different structural properties from these clay minerals, there are few reports of using rectorite as an inorganic filler in the disclosed fire-retardant coating formulations and making full use of the layered structure of rectorite to improve the fire-retardant and heat-insulating properties of the coating. The invention tries to prepare the fireproof heat-insulating coating by taking rectorite as an inorganic filler, and is hindered in that the prepared fireproof heat-insulating coating is easy to crack and has short burning resistance time. Through extensive research, the inventor finds that the main reason that the fireproof heat-insulating coating prepared by adding the rectorite has short burning resistance time is that the oil absorption of the rectorite is large, a large amount of water needs to be added in the process of preparing the coating, so that small cracks are easy to appear in the drying process of the coating, and finally the coating is easy to crack in the burning process. Through further research, the invention discovers that the oil absorption of the rectorite can be obviously reduced after the rectorite is subjected to intercalation modification, particularly organic modification (organic intercalation modification), and the coating with excellent fireproof performance and heat-insulating performance is prepared, and specifically comprises the following steps:
a water-based fireproof heat-insulating coating comprises an acid source, a carbon source, a gas source, intercalation modified rectorite, a film-forming substance and water.
According to the invention, the intercalated modified rectorite is innovatively used as the fireproof flame-retardant filler, and the organic modification treatment is carried out on the rectorite, so that the problem of large oil absorption of the rectorite is solved, the fireproof heat-insulating coating with excellent performance is obtained, the application field of the rectorite can be widened, and the recycling of the rectorite is realized.
The intercalation modified rectorite is inorganic cation and/or organic cation intercalation modified rectorite. For example, the intercalated modified rectorite may be an inorganic intercalated modified rectorite (inorganic modified rectorite) obtained by intercalating and modifying an inorganic cation. Or organic intercalation modified rectorite (organic modified rectorite) obtained by organic cation intercalation modification. The rectorite can also be obtained by modifying an inorganic cation intercalation first and then modifying the inorganic cation intercalation by an organic cation intercalation.
Preferably, the inorganic cation is at least one of sodium ion, potassium ion and calcium ion;
preferably, the organic cation is an organic ammonium ion having C10-C30.
Preferably, the organic cation is provided by a cationic surfactant having C10-C30.
Further preferably, the intercalation-modified rectorite of the present invention may be at least one of sodium-modified rectorite (sodium-based rectorite), potassium-modified rectorite (potassium-based rectorite), calcified rectorite (calcium-based rectorite), and cationic surfactant intercalation-modified rectorite.
The cationic surfactant intercalation modified rectorite is, for example, rectorite obtained by performing intercalation modification treatment on rectorite by a cationic surfactant, or rectorite obtained by performing intercalation modification on at least one of sodium rectorite, potassium rectorite and calcified rectorite by a cationic surfactant.
Preferably, the intercalation modified rectorite is rectorite obtained by intercalation modification treatment of sodium rectorite with cationic surfactant. Researches find that the use of the preferred intercalated modified rectorite can obviously improve the fire resistance of the obtained fireproof coating and obviously improve the flame-retardant time.
Still more preferably: the intercalation modified rectorite is prepared by the following steps:
step (1): dispersing rectorite in water to prepare rectorite slurry;
step (2): adding sodium salt into the rectorite slurry, and performing sodium treatment to obtain sodium-treated rectorite slurry;
and (3): adding a cationic surfactant into the sodium-modified rectorite slurry, and stirring to obtain a suspension;
and (4): and carrying out solid-liquid separation, washing and drying on the suspension to obtain the catalyst.
Preferably, in the step (1), the rectorite in the rectorite slurry accounts for 5-8% by mass.
Preferably, in step (2), the sodium salt is sodium pyrophosphate.
Preferably, the cationic surfactant is cetyltrimethylammonium bromide (CTAB).
Preferably, the concentration of the cationic surfactant in the suspension is controlled to be 80-100 g/L.
Most preferably, the intercalated modified rectorite is prepared by the steps of:
step (1): calculating the sodium salt amount required by sodium modification according to the Cation Exchange Capacity (CEC) of rectorite;
adding rectorite into distilled water, and stirring to obtain rectorite slurry;
step (2): adding the sodium salt with the design amount in the step (1) into the rectorite slurry, stirring uniformly, putting the rectorite slurry into a ball mill for ball milling for 1-3 h, taking out, sealing and aging for 20-24 h to obtain sodium rectorite slurry;
and (3): dissolving a certain amount of Cetyl Trimethyl Ammonium Bromide (CTAB) in the sodium rectorite slurry obtained in the step (2), and violently stirring at room temperature to obtain a suspension;
and (4): the suspension was filtered and washed with copious amounts of distilled water to remove excess CTAB until 0.1mol/L of AgNO was present in the filtrate3Br could not be detected in the solution-Obtaining organic modified rectorite slurry;
the resulting slurry of organically modified rectorite was filtered and dried in an oven to constant weight for 6h and passed through a 320 mesh screen (diameter about 46 microns).
Preferably, in step (1), the concentration of the rectorite slurry is 6%.
Preferably, in step (1), the stirring speed should be controlled at 700-1000 r/min.
Preferably, in step (1), the stirring time is controlled to be 8-15 min.
Preferably, in the step (2), the sodium salt is sodium pyrophosphate.
Preferably, in step (2), the stirring speed should be controlled at 700-1000 r/min.
Preferably, in the step (2), the stirring time is controlled to be 15-25 min.
Preferably, in the step (3), the concentration of the hexadecyl trimethyl ammonium bromide is 80-100 g/L.
Preferably, in step (3), the stirring speed should be controlled at 1500-.
Preferably, in step (3), the stirring time is controlled to be 3-5 h.
Preferably, in the step (4), the oven temperature is 70 ℃.
Preferably, the method comprises the following steps: the acid source is a material which can be decomposed into inorganic acid in the combustion process; preferably at least one of ammonium polyphosphate, ammonium dihydrogen phosphate and boric acid; further preferred is ammonium polyphosphate.
Preferably, the method comprises the following steps: the carbon source is a carbon forming agent commonly used in an expansion flame-retardant system, preferably a long-chain hydrocarbon containing three or more hydroxyl groups, and further preferably at least one of pentaerythritol, sorbitol, diglycol, starch, glucose and the like; most preferred is microemulsified pentaerythritol.
Preferably, the method comprises the following steps: the gas source is when the coating encounters high temperature and fireWhen in flame, inert or non-combustible gases (such as NH) can be released by self-decomposition3、HCl、H2O, etc.) to make the expanded carbon layer spongy, said gas source being also the blowing agent.
Preferably, the method comprises the following steps: the gas source is at least one of melamine, urea and the like; further preferred is melamine.
Preferably, the method comprises the following steps: the film forming material is a basic material for forming the coating and has the function of bonding other components in the coating to form a coating film; preferably at least one of acrylic resin, high chlorinated polyethylene, VAE emulsion, amino resin, methylated melamine formaldehyde resin, acrylic emulsion, chlorine partial emulsion and tertiary vinegar emulsion; further preferred is a VAE emulsion. The film forming material and other components have synergistic effect, and particularly, the film forming material is synergistic with the innovative intercalation modified rectorite, so that the flame retardant effect and the heat insulation effect of the coating can be obviously improved.
Preferably, the method comprises the following steps: in the water-based fireproof heat-insulating coating, the weight parts of the components are as follows:
water: 15-20 parts of a solvent;
7.00-10.00 parts of an air source;
7.00-10.00 parts of carbon source;
25.00-28.00 parts of an acid source;
intercalation modified rectorite: 6.00-10.00 parts;
film-forming material: 18.00 to 21.00 portions. Under the preferable range, the coating has better heat insulation effect and longer flame-retardant time while achieving better physical and chemical properties.
The water-based fireproof heat insulation coating also comprises pigment and/or auxiliary agent.
The auxiliary agent is wetting dispersant, film forming auxiliary agent, thickening agent and the like.
The wetting dispersant is at least one of sodium hexametaphosphate, aliphatic polyester and segmented copolymerized polyurethane.
The film-forming assistant is at least one of alcohol ester dodeca, glycerol and ethylene glycol monoethyl ether.
The thickening agent is at least one of fibers, polyvinyl alcohols and polyacrylates.
The weight part of the auxiliary agent is not higher than 3 parts.
The pigment is titanium dioxide, and the preferable particle size is 400-500 meshes.
The weight part of the pigment is not more than 10 parts.
The invention discloses a preferable water-based fireproof heat-insulating coating which specifically comprises the following components in parts by weight:
water: 15-20 parts of a solvent;
melamine: 7.00-10.00 parts;
titanium dioxide: 5.00-6.00 parts;
micro-emulsified pentaerythritol: 7.00-10.00 parts;
ammonium polyphosphate: 25.00-28.00 parts;
intercalation modified rectorite: 8.00-10.00 parts;
VAE emulsion: 18.00-21.00 parts;
auxiliary agent: 1.70-3.0 parts;
preferably, the auxiliary agent comprises a wetting dispersant; film forming aids and thickeners; the proportion of each component is preferably 0.5-1.0; 0.5-0.8: 0.5-0.7. With this preferred combination of components and ratio ranges, the flame retardant time of the coating is significantly increased.
The preparation method of the water-based fireproof heat-insulating coating comprises the following steps:
step S1: stirring part of water and part of auxiliary agent at medium speed to obtain solution A;
step S2: adding an acid source, a carbon source, a gas source and a pigment into the solution A, and stirring at a high speed at a temperature of not higher than 45 ℃; then adding the intercalated modified rectorite and the rest water, and continuously stirring at a high speed at a temperature of not higher than 45 ℃ to obtain a solution B;
step S3: and adding the film forming substance and the rest of the auxiliary agent into the solution B, and stirring at a low speed to obtain the aqueous emulsion.
Preferably, in step S1, the rotation speed of the medium-speed stirring is 1200-1500 r/min.
Preferably, in step S1, the medium-speed stirring time is 20-25 min.
Preferably, the temperature during the high-speed stirring process in step S2 is 40-45 ℃.
Preferably, in step S2, the rotation speed of the high-speed stirring is 2000-.
Preferably, in step S3, the rotation speed of the low-speed stirring is 700-1000 r/min.
Preferably, in step S3, the low-speed stirring time is 30-40 min.
By the treatment at the different rotation speeds, the flame retardant and heat insulating properties of the resulting coating can be further synergistically improved.
The preparation method of the water-based fireproof heat-insulating coating comprises the following specific steps:
step S1: and (3) stirring at medium speed: water: 16.00 parts; wetting and dispersing agent: 0.50 part; step S2: high-speed stirring: adding the product of the step (1): melamine: 9.20 parts; titanium dioxide: 5.00 parts; micro-emulsified pentaerythritol: 9.20 parts; ammonium polyphosphate: 27.00 parts; dispersing at high speed for 10-20 min. Continuously adding modified rectorite: 9.30 parts; water: 1.50 parts; dispersing at high speed for 10-20 min.
Step S2: stirring at a low speed: adding the product of the step (2): VAE emulsion: 20.00 parts; wetting and dispersing agent: 0.30 part; film-forming auxiliary agent: 0.50 part; thickening agent: 0.50 part; water: 1.00 part.
The invention also provides a fireproof material, which comprises a base material and a fireproof coating compounded on the base material; the fireproof coating is obtained by drying and/or curing the water-based fireproof heat-insulating coating.
The base material can be wood, steel, building, veneer and the like.
The thickness of the fireproof coating is 2.3-3.0 mm.
Compared with the prior art, the invention has the characteristics and beneficial effects that:
(1) the rectorite is added as an inorganic filler, and the technical problem of short flame-retardant time of the coating caused by large oil absorption of the rectorite is solved by carrying out organic modification treatment on the rectorite, so that the process is simple and short in operation and low in cost, and the application field of the rectorite is widened;
(2) the flame-retardant time of the fireproof heat-insulating coating prepared by the invention is more than 120min and is far higher than the flame-retardant time specified by the fireproof coating standard;
(3) the fireproof heat-insulating coating prepared by the invention has obvious heat-insulating effect, and can reduce the surface temperature of a steel plate by 40-50 ℃ compared with the common fireproof heat-insulating coating.
Drawings
FIG. 1 is an X-ray diffraction pattern of rectorite and modified rectorite;
FIG. 2 is a graph showing the temperature change of the back surface of a steel sheet during combustion in the coatings prepared in example 2 of the present invention and comparative example 1;
FIG. 3 is a scanning electron microscope photograph of the carbon residue layer (pulverized) after combustion of the coatings prepared in example 2 of the present invention and comparative example 2;
FIG. 4 is a scanning electron microscope image of the carbon residue layer (bulk) after combustion of the coatings prepared in example 2 of the present invention and comparative example 2.
Detailed Description
All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The flame-retardant time and the heat insulation temperature are tested by adopting a large-plate combustion method, referring to GB 12441 and 2018, and the finish type fireproof coating is adopted.
And min and h are time units, wherein min is minutes and h is hours.
Example 1
(1) Weighing 15g of natural rectorite, adding the natural rectorite into 250mL of distilled water, stirring the mixture on a dispersion stirrer at the rotating speed of 800r/min for 10min, adding 5g of sodium pyrophosphate decahydrate, stirring the mixture at the same speed for 20min, putting the mixture into a ball mill for ball milling for 3h, taking out the mixture, sealing and aging the mixture for 24h to obtain sodium rectorite slurry; 15g of cetyltrimethylammonium bromide (CTAB) was dissolved in a sodium rectorite slurry, stirred vigorously at 2000r/min for 5h at room temperature on a dispersion stirrer, the resulting suspension was filtered and washed with a large volume of distilled water to remove excess CTAB until 0.1mol/L of AgNO was present in the filtrate3Br could not be detected in the solution-Obtaining organic modified rectorite slurry, and processing the slurryAnd (4) carrying out suction filtration, drying at the temperature of 70 ℃, and grinding to obtain the organic modified rectorite powder.
(2) The water-based ultrathin intumescent fire-proof heat-insulating coating comprises the following raw materials in parts by weight:
water: 18.50 parts;
melamine: 9.20 parts;
titanium dioxide: 5.00 parts;
micro-emulsified pentaerythritol: 9.20 parts;
ammonium polyphosphate: 27.00 parts;
(1) the obtained organic modified rectorite: 6.00 parts;
VAE emulsion: 20.00 parts;
auxiliary agent: 1.8 parts.
Preferably, the particle size of the titanium dioxide is 480 meshes.
The VAE emulsion manufacturer is the company Seranies.
The auxiliary agent comprises a wetting dispersant; a film-forming aid; a thickening agent.
Wetting and dispersing agent: borchers, Inc., brand name: CF-18495
Film-forming auxiliary agent: shanghai Tantake Technique, Inc.
Thickening agent: shanghai deep bamboo chemical technology Co., Ltd, brand: u605 and U905 were mixed at a ratio of 2: 1.
(3) The water-based ultrathin intumescent fire retardant coating is prepared by the following steps according to the components in the step (2):
s1: and (3) stirring at medium speed: water: 16.00 parts; wetting and dispersing agent: 0.50 part; stirring the mixture evenly on a dispersion stirrer at the rotating speed of 1200 r/min.
S2: high-speed stirring: the product of S1 was added: melamine: 9.20 parts; titanium dioxide: 5.00 parts; micro-emulsified pentaerythritol: 9.20 parts; ammonium polyphosphate: 27.00 parts; dispersing on a dispersion mixer at a high speed of 2000r/min for 15 min. Continuously adding modified rectorite: 6.00 parts; water: 1.50 parts; dispersing at the same rotation speed for 20 min.
S3: stirring at a low speed: the product of S2 was added: VAE emulsion: 20.00 parts; wetting and dispersing agent: 0.30 part; film-forming auxiliary agent: 0.50 part; 0.50 part of thickening agent; water: 1.00 part; stirring at 800r/min for 40 min. And obtaining the fireproof heat-insulating coating.
The coating is coated on a steel plate, the coating thickness is 2.5mm, the flame-retardant time is 70min, and compared with comparative example 1, the temperature of the back surface of the steel plate can be reduced by about 25 ℃.
Example 2
(1) The method for producing the organically modified rectorite powder was the same as (1) in example 1.
(2) The water-based ultrathin intumescent fire-proof heat-insulating coating disclosed by the embodiment is prepared from the following raw materials in parts by weight:
water: 18.50 parts;
melamine: 9.20 parts;
titanium dioxide: 5.00 parts;
micro-emulsified pentaerythritol: 9.20 parts;
ammonium polyphosphate: 27.00 parts;
(1) the obtained organic modified rectorite: 9.30 parts;
VAE emulsion: 20.00 parts;
auxiliary agent: 1.80 parts.
Preferably, the particle size of the titanium dioxide is 480 meshes.
The auxiliaries are as in example 1.
(3) The water-based ultrathin intumescent fire retardant coating is prepared by the following steps according to the components in the step (2):
s1: and (3) stirring at medium speed: water: 16.00 parts; wetting and dispersing agent: 0.50 part; stirring the mixture evenly on a dispersion stirrer at the rotating speed of 1200 r/min.
S2: high-speed stirring: the product of S1 was added: melamine: 9.20 parts; titanium dioxide: 5.00 parts; micro-emulsified pentaerythritol: 9.20 parts; ammonium polyphosphate: 27.00 parts; dispersing on a dispersion mixer at a high speed of 2000r/min for 15 min. Continuously adding modified rectorite: 9.30 parts; water: 1.50 parts; dispersing at the same rotation speed for 20 min.
S3: stirring at a low speed: the product of S2 was added: VAE emulsion: 20.00 parts; wetting and dispersing agent: 0.30 part; film-forming auxiliary agent: 0.50 part; thickening agent: 0.50 part; water: 1.00 part; stirring at 800r/min for 40 min. And obtaining the fireproof heat-insulating coating.
The coating is coated on a steel plate, the coating thickness is 2.5mm, the flame-retardant time exceeds 120min, and compared with comparative example 1, the temperature of the back surface of the steel plate can be reduced by about 40 ℃.
Comparative example 1
The difference compared to example 2 is that the modified rectorite was replaced with an equal amount of ultrafine kaolin. The water-based ultrathin intumescent fire-proof heat-insulating coating of the comparative example consists of the following raw materials in parts by weight:
water: 18.50 parts;
melamine: 9.20 parts;
titanium dioxide: 5.00 parts;
micro-emulsified pentaerythritol: 9.20 parts;
ammonium polyphosphate: 27.00 parts;
superfine kaolin: 9.30 parts;
VAE emulsion: 20.00 parts;
auxiliary agent: 1.80 parts.
Preferably, the particle size of the titanium dioxide is 480 meshes.
The auxiliaries are as in example 1.
The water-based ultrathin intumescent fire retardant coating of the comparative example is prepared by the following steps:
s1: and (3) stirring at medium speed: water: 16.00 parts; wetting and dispersing agent: 0.50 part; stirring the mixture evenly on a dispersion stirrer at the rotating speed of 1200 r/min.
S2: high-speed stirring: the product of S1 was added: melamine: 9.20 parts; titanium dioxide: 5.00 parts; micro-emulsified pentaerythritol: 9.20 parts; ammonium polyphosphate: 27.00 parts; dispersing on a dispersion mixer at a high speed of 2000r/min for 15 min. Continuously adding superfine kaolin: 9.30 parts; water: 1.50 parts; dispersing at the same rotation speed for 20 min.
S3: stirring at a low speed: the product of S2 was added: VAE emulsion: 20.00 parts; wetting and dispersing agent: 0.30 part; film-forming auxiliary agent: 0.50 part; thickening agent: 0.50 part; water: 1.00 part; stirring at 800r/min for 40 min. And obtaining the fireproof heat-insulating coating.
The coating is coated on a steel plate, the coating thickness is 2.5mm, and the flame-retardant time is 60 min.
Comparative example 2
Compared with the example 2, the difference is that the modified rectorite is replaced by the same amount of natural rectorite, namely, the organic intercalation modification treatment of (1) is not carried out on the rectorite:
the water-based ultrathin intumescent fire-proof heat-insulating coating of the comparative example consists of the following raw materials in parts by weight:
water: 18.50 parts;
melamine: 9.20 parts;
titanium dioxide: 5.00 parts;
micro-emulsified pentaerythritol: 9.20 parts;
ammonium polyphosphate: 27.00 parts;
natural rectorite: 9.30 parts;
VAE emulsion: 20.00 parts;
auxiliary agent: 1.80 parts.
Preferably, the particle size of the titanium dioxide is 480 meshes.
Preferably, the auxiliaries are as in example 1.
The aqueous ultrathin intumescent fire retardant coating of the comparative example is prepared by the following steps:
s1: and (3) stirring at medium speed: water: 16.00 parts; wetting and dispersing agent: 0.50 part; stirring the mixture evenly on a dispersion stirrer at the rotating speed of 1200 r/min.
S2: high-speed stirring: the product of S1 was added: melamine: 9.20 parts; titanium dioxide: 5.00 parts; micro-emulsified pentaerythritol: 9.20 parts; ammonium polyphosphate: 27.00 parts; dispersing on a dispersion mixer at a high speed of 2000r/min for 15 min. Continuing to add natural rectorite: 9.30 parts; water: 1.50 parts; dispersing at the same rotation speed for 20 min.
S3: stirring at a low speed: the product of S2 was added: VAE emulsion: 20.00 parts; wetting and dispersing agent: 0.30 part; film-forming auxiliary agent: 0.5 part; thickening agent: 0.50 part; water: 1.00 part; stirring at 800r/min for 40 min. And obtaining the fireproof heat-insulating coating.
The coating is coated on a steel plate, the coating thickness is 2.5mm, the flame-retardant time is 40min, and compared with comparative example 1, the temperature of the back surface of the steel plate can be reduced by about 30 ℃.
Example 3:
compared with the example 2, the difference is only that the rectorite used is sodium-modified rectorite, namely when the rectorite is subjected to modification treatment, only sodium is modified, and no further organic modification is carried out;
the coating prepared in the example is coated on a steel plate, the coating thickness is 2.5mm, the flame-retardant time is 110min, and compared with the comparative example 1, the temperature of the back surface of the steel plate can be reduced by about 30 ℃.
Comparative example 3:
compared with example 2, the only difference is that the film-forming material used is an epoxy resin;
the coating prepared by the comparative example is coated on a steel plate, the coating thickness is 2.5mm, the flame-retardant time is 20min, and compared with the comparative example 1, the temperature of the back surface of the steel plate can be reduced by about 15 ℃.
Comparative example 4
Compared with the example 2, the difference is that the organic modified rectorite obtained in the step (1) is not added in the coating, and the film-forming substance is epoxy resin;
the coating prepared in the comparative example was coated on a steel plate with a coating thickness of 2.5mm and a flame-retardant time of 5min, and the temperature of the back surface of the steel plate was higher than that in comparative example 1.
Comparative example 5:
the only difference compared to example 2 is that in S3, after the VAE emulsion was added, it was still stirred at high speed;
the coating prepared by the comparative example is coated on a steel plate, the coating thickness is 2.5mm, the flame-retardant time is 40min, and compared with the comparative example 1, the temperature of the back surface of the steel plate can be reduced by about 20 ℃.

Claims (10)

1. The water-based fireproof heat-insulating coating is characterized in that: comprises an acid source, a carbon source, a gas source, intercalation modified rectorite, a film forming substance and water.
2. The aqueous fireproof heat-insulating coating of claim 1, wherein:
the intercalation modified rectorite is inorganic cation and/or organic cation intercalation modified rectorite;
preferably, the inorganic cation is at least one of sodium ion, potassium ion and calcium ion;
the organic cation is organic ammonium ion of C10-C30.
3. The aqueous fireproof heat-insulating coating according to claim 2, wherein: the intercalation modified rectorite is cationic surfactant intercalation modified rectorite.
4. The aqueous fireproof heat-insulating coating of claim 3, wherein: the intercalation modified rectorite is prepared by the following steps:
step (1): dispersing rectorite in water to prepare rectorite slurry;
step (2): adding sodium salt into the rectorite slurry, and performing sodium treatment to obtain sodium-treated rectorite slurry;
and (3): adding a cationic surfactant into the sodium-modified rectorite slurry, and stirring to obtain a suspension;
and (4): and carrying out solid-liquid separation, washing and drying on the suspension to obtain the catalyst.
5. The water-based fireproof heat-insulating coating as claimed in any one of claims 1 to 4, wherein: the acid source is a material which can be decomposed into inorganic acid in the combustion process; preferably at least one of ammonium polyphosphate, ammonium dihydrogen phosphate and boric acid; further preferably ammonium polyphosphate;
preferably, the carbon source is a char-forming agent; preferably a long-chain hydrocarbon containing three or more hydroxyl groups, and further preferably at least one of pentaerythritol, sorbitol, diglycol, starch and glucose; most preferred is microemulsified pentaerythritol.
6. The water-based fireproof heat-insulating coating as claimed in any one of claims 1 to 5, wherein: the gas source is a material which can be decomposed to release inert or non-combustible gas when meeting high temperature and flame; preferably at least one of melamine and urea; still more preferably melamine;
preferably, the film-forming substance is at least one of acrylic resin, high chlorinated polyethylene, amino resin, methylated melamine formaldehyde resin, acrylic emulsion, chlorine partial emulsion and tertiary vinegar emulsion.
7. The water-based fireproof heat-insulating coating as claimed in any one of claims 1 to 6, wherein: the weight parts of each component are as follows:
water: 15-20 parts of a solvent;
7.00-10.00 parts of an air source;
7.00-10.00 parts of carbon source;
25.00-28.00 parts of an acid source;
intercalation modified rectorite: 6.00-10.00 parts;
film-forming material: 18.00 to 21.00 portions.
8. The water-based fireproof heat-insulating coating as claimed in any one of claims 1 to 7, wherein: also comprises pigment and/or auxiliary agent;
the auxiliary agent is at least one of a wetting dispersant, a film-forming auxiliary agent and a thickening agent;
the pigment is titanium dioxide, and the preferable particle size is 400-500 meshes;
the wetting dispersant is at least one of sodium hexametaphosphate, aliphatic polyester and block copolymerized polyurethane;
the film-forming additive is at least one of alcohol ester dodeca, glycerol and ethylene glycol monoethyl ether;
the thickening agent is at least one of fibers, polyvinyl alcohols and polyacrylates.
The weight part of the pigment is not more than 10 parts; the weight part of the auxiliary agent is not higher than 3 parts.
9. The preparation method of the water-based fireproof heat insulation coating as claimed in any one of claims 1 to 8, characterized in that: the method comprises the following steps:
step S1: stirring part of water and part of auxiliary agent at medium speed to obtain solution A;
step S2: adding an acid source, a carbon source, a gas source and a pigment into the solution A, and stirring at a high speed at a temperature of not higher than 45 ℃; then adding the intercalated modified rectorite and the rest water, and continuously stirring at a high speed at a temperature of not higher than 45 ℃ to obtain a solution B;
step S3: adding the film forming substance and the rest of the auxiliary agent into the solution B, and stirring at a low speed;
preferably, the rotation speed of the medium-speed stirring is 1200-1500 r/min;
preferably, the rotating speed of the high-speed stirring is 2000-;
preferably, the rotation speed of the low-speed stirring is 700-.
10. A fireproof material comprises a substrate and a fireproof coating compounded on the substrate; the fireproof coating is characterized by being obtained by drying and/or curing the water-based fireproof heat-insulating coating of any one of claims 1 to 8.
CN201810616351.3A 2018-06-14 2018-06-14 Water-based fireproof heat-insulating coating, fireproof material and preparation method thereof Active CN110607101B (en)

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