CN109135547A - A kind of insulation and fire-proof paint - Google Patents

A kind of insulation and fire-proof paint Download PDF

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Publication number
CN109135547A
CN109135547A CN201810762456.XA CN201810762456A CN109135547A CN 109135547 A CN109135547 A CN 109135547A CN 201810762456 A CN201810762456 A CN 201810762456A CN 109135547 A CN109135547 A CN 109135547A
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mixing
fire
mass ratio
insulation
proof paint
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田秋珍
陈建春
卢星
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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
    • C09D175/00Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04Polyurethanes
    • C09D175/08Polyurethanes from polyethers
    • 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
    • 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
    • C09D7/70Additives characterised by shape, e.g. fibres, flakes or microspheres
    • 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
    • C08K3/34Silicon-containing compounds
    • C08K3/36Silica
    • 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
    • C08K7/00Use of ingredients characterised by shape
    • C08K7/22Expanded, porous or hollow particles
    • C08K7/24Expanded, porous or hollow particles inorganic
    • C08K7/28Glass

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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)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Organic Insulating Materials (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention relates to a kind of insulation and fire-proof paints, belong to the field of building materials.The present invention makes composite modified polyurethane, polyurethane composite S iO using sodium metasilicate as raw material2, form tridimensional network, and SiO2The adsorbed hydroxyl content is high, it can polymerize with the group in isophorone diisocyanate and polyurethane, so that the internal performance of insulation and fire-proof paint system is promoted, the raw materials such as the metakaolin in auxiliary agent, it can be under heat effect, isolation film is formed in air and ground part, it can effective flame-resistant high-temperature-resistant, using phenol and formaldehyde as raw material, it makes prefabricated phenolic resin and mixes liquid, cooperate amphiphilic block copolymer poloxamer, large specific surface area processed, the suitable complex mesoporous material of Pore genesis, provides non-polar absorbent power CO absorption2, by irregular porous release CO can be stimulated when high temperature2Play the role of efficiently starvation, thus play fire extinguishing, improves fire protecting performance.The present invention solves the problems, such as to commonly use insulation and fire-proof paint heat insulating ability, heat resistance at present bad.

Description

A kind of insulation and fire-proof paint
Technical field
The present invention relates to the field of building materials, in particular to a kind of insulation and fire-proof paint.
Background technique
Due to the generation of a lot of building heat preservation event of fire in recent years, the thinking of each bound pair insulated fire is caused, has kept the temperature The unprecedented great attention for causing all circles in the industry of the fire protecting performance of material.However, many thermal insulation materials it is on fire be all It is generated in work progress, such as: electric welding, open fire, undesirable construction habit.What these materials constantly generated in combustion melts Object and toxic smoke are dripped, while the gases such as chlorofluorocarbons, hydrofluorocarbons, freon released can not also neglect the harm of environment Depending on.For this purpose, there are many fire proof and thermo-insulation coating materials in market.Common insulation and fire-proof paint heat insulating ability, heat resistance are bad at present, no It is able to satisfy the demand of people.
Summary of the invention
The technical problems to be solved by the invention: bad for current common insulation and fire-proof paint heat insulating ability, heat resistance Problem provides a kind of insulation and fire-proof paint.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of insulation and fire-proof paint, according to the mass fraction, including following component: 5 ~ 10 parts of auxiliary agents, 3 ~ 8 parts of glass beads, 6 ~ 10 Part surfactant, 2 ~ 5 rosin, 25 ~ 40 parts of water, which is characterized in that further include: 20 ~ 45 parts of composite modified polyurethane, 15 ~ 30 Part complex mesoporous material.
The preparation method of the composite modified polyurethane, includes the following steps:
(1) in 10 ~ 15 DEG C, 1:5 ~ 10 take sodium metasilicate, hydrochloric acid solution mixing in mass ratio, and the silicon of sodium metasilicate quality 20 ~ 35% is added The mixing of alkane coupling agent, reacts 3 ~ 5h, and the solvent mixing of NaCl and sodium metasilicate quality 30 ~ 45% that sodium metasilicate quality 8 ~ 15% is added are stirred It mixes, stands, filtering takes filtrate 4 ~ 9:1 in mass ratio that desiccant is added, it is mixed, closed standing, addition filtrate quality 20 ~ 30% polyoxypropyleneglycol, ultrasonic wave dispersion, decompression filter, and obtain dispersion liquid;
(2) in 80 ~ 90 DEG C, 1:1:10 ~ 15:2 in mass ratio takes polyoxypropyleneglycol, dihydromethyl propionic acid, dispersion liquid, N- first Base pyrrolidones mixing, ventilation protection, is warming up to 100 ~ 110 DEG C of heat preservations, is cooled to 75 ~ 85 DEG C, obtains mixed reactant, take mixing Reactant 8 ~ 12:1 in mass ratio ~ 3:1 adds dibutyl tin dilaurate, isophorone diisocyanate mixing, reacts 2 ~ 5h, drop Temperature obtains feed liquid, and triethylamine, acrylic acid, viscosity-controlling agent mixing is added in feeding liquid 4 ~ 8:1:2:1 in mass ratio, and shearing dispersion adds Enter the over cure potassium of feed liquid quality 16 ~ 25%, heat up, keep the temperature 3 ~ 5h, is evaporated under reduced pressure to get composite modified polyurethane.
Solvent in the step (1): 1:4 ~ 8 take acetone, ethyl alcohol mixing to get solvent in mass ratio.
Desiccant in the step (1): 5:1 ~ 2 take CaSO in mass ratio4、CaCl2Mixing is to get desiccant.
Viscosity-controlling agent in the step (2): urea, hydroxylamine hydrochloride, any one in hydroxyl sulfate.
The preparation method of the complex mesoporous material, includes the following steps:
S1. in 40 ~ 60 DEG C, 1:6 ~ 10 take phenol, NaOH solution to be mixed in mass ratio, and 3 ~ 7 times of formaldehyde of phenol quality are added Solution mixing, is warming up to 70 ~ 85 DEG C, stirs, cooling, adjusts pH, is concentrated under reduced pressure, and is evaporated in vacuo, obtains reactant, reactant is taken to add Enter 3 ~ 5 times of reactant quality of dehydrated alcohol, be uniformly mixed, obtains prefabricated phenolic resin and mix liquid;
S2. take poloxamer liquid 5 ~ 8:2:4 in mass ratio that ethyl orthosilicate is added, prefabricated phenolic resin mixes liquid, stirring, hot polymerization It closes, nitrogen protection, temperature programming to 350 ~ 500 DEG C of heat preservations is warming up to 800 ~ 900 DEG C of 1 ~ 2h of heat preservation, obtains heat treatment object, and it is cooling, 3 ~ 5 times of heat-treated substance amount of maceration extract is added to impregnate, filtering takes filter residue and drying to get complex mesoporous material.
Poloxamer liquid in the step S2: 1:3 ~ 5:6 in mass ratio takes poloxamer, ethyl alcohol, hydrochloric acid solution mixing, Up to poloxamer liquid.
Maceration extract in the step S2: 1:1 ~ 3:10 ~ 15 take chitosan, Dopamine hydrochloride, acetic acid solution in mass ratio Mixing is to get maceration extract.
The surfactant: 4:1 ~ 2 take empgen BB, sodium secondary alkyl sulfonate mixing to get table in mass ratio Face activating agent.
The auxiliary agent: 6:1:1 ~ 2 take metakaolin, amine carbonate, magnesium stearate mixing to get auxiliary agent in mass ratio.
The present invention is compared with other methods, and advantageous effects are:
(1) present invention makes composite modified polyurethane using sodium metasilicate as raw material, has excellent long-term effect, durability, chemical stabilization Property, the SiO of sodium metasilicate hydrolysis generation2Particle and its Si-OH on surface and polyurethane molecular form physics crosslinked action, so that poly- The movement of urethane molecule segment is fettered, and tensile strength is caused to increase, SiO2For rigid particles, reduce elongation at break, After effect reaches to a certain degree, due to SiO2The aggtegation of particle, so that physical crosslinking density reduces, tensile strength and fracture are stretched Long rate decline, polyurethane composite S iO2, form tridimensional network, and SiO2The adsorbed hydroxyl content is high, can be different with isophorone two Group in cyanate and polyurethane polymerize, so that the internal performance of insulation and fire-proof paint system is promoted;
(2) raw materials such as metakaolin in auxiliary agent of the present invention can form glassy net as inorganic anti-flaming material under heat effect, To form isolation film in air and ground part, can effective flame-resistant high-temperature-resistant, cooperate glass bead,
, the thermal insulation property of system can be greatly promoted, using phenol and formaldehyde as raw material, prefabricated phenolic resin is made and mixes liquid, cooperate both sexes Block copolymer poloxamer, large specific surface area processed, the suitable complex mesoporous material of Pore genesis provide the suction of non-polar absorbent power Attached CO2, by irregular porous release CO can be stimulated when high temperature2Play the role of efficiently starvation, thus play fire extinguishing, Improve fire protecting performance.
Specific embodiment
Solvent: 1:4 ~ 8 take acetone, ethyl alcohol mixing to get solvent in mass ratio.
Desiccant: 5:1 ~ 2 take CaSO in mass ratio4、CaCl2Mixing is to get desiccant.
Viscosity-controlling agent: urea, hydroxylamine hydrochloride, any one in hydroxyl sulfate.
Surfactant: 4:1 ~ 2 take empgen BB, sodium secondary alkyl sulfonate mixing living to get surface in mass ratio Property agent.
Auxiliary agent: 6:1:1 ~ 2 take metakaolin, amine carbonate, magnesium stearate mixing to get auxiliary agent in mass ratio.
Poloxamer liquid: 1:3 ~ 5:6 in mass ratio takes the hydrochloric acid solution mixing of poloxamer, ethyl alcohol, concentration 0.1mol/L, Up to poloxamer liquid.
Maceration extract: 1:1 ~ 3:10 ~ 15 chitosan, Dopamine hydrochloride, mass fraction that take deacetylation 90% in mass ratio 10% acetic acid solution mixes to get maceration extract.
The preparation method of composite modified polyurethane, includes the following steps:
(1) in 10 ~ 15 DEG C, 1:5 ~ 10 take the hydrochloric acid solution of sodium metasilicate, concentration 0.1mol/L to mix in mass ratio, and sodium metasilicate is added The silane coupling agent of quality 20 ~ 35% mixes, and reacts 3 ~ 5h, be added sodium metasilicate quality 8 ~ 15% NaCl and sodium metasilicate quality 30 ~ 45% solvent mixing, stirs 2 ~ 4h with 250 ~ 400r/min, stands 25 ~ 40min, and filtering takes filtrate 4 ~ 9:1 in mass ratio to add Entering desiccant, is mixed 10 ~ 15min, room temperature is closed to stand 20 ~ for 24 hours, the polypropylene oxide two of filtrate quality 20 ~ 30% is added Alcohol disperses 15 ~ 25min with 300W ultrasonic wave, and decompression filters, and obtains dispersion liquid;
(2) 80 ~ 90 DEG C are bathed in grease, 1:1:10 ~ 15:2 in mass ratio takes polyoxypropyleneglycol, dihydromethyl propionic acid, dispersion Liquid, N-Methyl pyrrolidone mixing, lead to nitrogen protection, are warming up to 100 ~ 110 DEG C of 20 ~ 30min of heat preservation, are cooled to 75 ~ 85 DEG C, obtain Mixed reactant takes mixed reactant 8 ~ 12:1 in mass ratio ~ 3:1 to add dibutyl tin dilaurate, isophorone diisocyanate Ester mixing, reacts 2 ~ 5h, is cooled to 55 ~ 65 DEG C, obtains feed liquid, and triethylamine, propylene is added in feeding liquid 4 ~ 8:1:2:1 in mass ratio Acid, viscosity-controlling agent mixing and emulsifying shear 15 ~ 30min of dispersion with 300 ~ 500r/min, the over cure of feed liquid quality 16 ~ 25% are added Change potassium, be warming up to 65 ~ 75 DEG C, keep the temperature 3 ~ 5h, is evaporated under reduced pressure to get composite modified polyurethane.
The preparation method of complex mesoporous material, includes the following steps:
S1. in 40 ~ 60 DEG C of water-bath, the 1:6 ~ 10 NaOH solution mixing that takes phenol, mass fraction 15% in mass ratio, with 300 ~ 450r/min stirs 20 ~ 45min, and the formalin that the mass fraction for being added 3 ~ 7 times of phenol quality is 25% mixes, it is warming up to 70 ~ 85 DEG C, continue 10 ~ 20min of stirring, cooled to room temperature adjusts pH to 6.8 ~ 7.2 with the hydrochloric acid solution of concentration 1mol/L, subtracts Pressure concentration, is evaporated in vacuo to constant weight, obtains reactant, takes reactant that 3 ~ 5 times of reactant quality of dehydrated alcohol is added, and mixing is equal It is even, it obtains prefabricated phenolic resin and mixes liquid;
S2. take poloxamer liquid 5 ~ 8:2:4 in mass ratio that the mixed liquid of ethyl orthosilicate, prefabricated phenolic resin is added, with 300 ~ 350r/ Min stirring moves to tube furnace after 90 ~ 100 DEG C of thermal polymerizations 20 ~ for 24 hours, under nitrogen protection, with 5 ~ 10 DEG C/min temperature programming To 350 ~ 500 DEG C of 3 ~ 5h of heat preservation, 800 ~ 900 DEG C of 1 ~ 2h of heat preservation are warming up to, obtain heat treatment object, after cooled to room temperature, are added Enter 3 ~ 5 times of heat-treated substance amount of maceration extract and impregnate 2 ~ 5h, filtering takes filter residue in 60 ~ 80 DEG C of oven dryings to get composite mesopore Material.
A kind of insulation and fire-proof paint, according to the mass fraction, including following component: 5 ~ 10 parts of auxiliary agents, 3 ~ 8 parts of glass beads, 6 ~ 10 parts of surfactants, 2 ~ 5 rosin, 25 ~ 40 parts of water, which is characterized in that further include: 20 ~ 45 parts of composite modified polyurethane, 15 ~ 30 parts of complex mesoporous materials.
A kind of preparation method of insulation and fire-proof paint, includes the following steps:
(1) according to the mass fraction, 5 ~ 10 parts of auxiliary agents, 3 ~ 8 parts of glass beads, 6 ~ 10 parts of surfactants, 2 ~ 5 rosin, 25 ~ 40 are taken Part water, 20 ~ 45 parts of composite modified polyurethane, 15 ~ 30 parts of complex mesoporous materials;
(2) auxiliary agent, glass bead, rosin, water is taken to mix in reaction kettle, prior to 30 ~ 45 DEG C with 300 ~ 500r/min magnetic agitation After 25 ~ 50min, be added composite modified polyurethane, surfactant, complex mesoporous material mixing, with 300W supersonic oscillations 20 ~ 30min is passed through CO in 0.9MPa, 20 ~ 25 DEG C with 200 ~ 300mL/min2, 2 ~ 4h is stood to get insulation and fire-proof paint.
Embodiment 1
Solvent: 1:4 in mass ratio takes acetone, ethyl alcohol mixing to get solvent.
Desiccant: 5:1 takes CaSO in mass ratio4、CaCl2Mixing is to get desiccant.
Viscosity-controlling agent: urea.
Surfactant: 4:1 in mass ratio takes empgen BB, sodium secondary alkyl sulfonate mixing to get surface-active Agent.
Auxiliary agent: 6:1:1 in mass ratio takes metakaolin, amine carbonate, magnesium stearate mixing to get auxiliary agent.
Poloxamer liquid: 1:3:6 in mass ratio takes the hydrochloric acid solution mixing of poloxamer, ethyl alcohol, concentration 0.1mol/L, i.e., Obtain poloxamer liquid.
Maceration extract: 1:1:10 in mass ratio takes the second of the chitosan of deacetylation 90%, Dopamine hydrochloride, mass fraction 10% Acid solution mixes to get maceration extract.
The preparation method of composite modified polyurethane, includes the following steps:
(1) in 10 DEG C, 1:5 in mass ratio takes the hydrochloric acid solution mixing of sodium metasilicate, concentration 0.1mol/L, and sodium metasilicate quality is added 20% silane coupling agent mixing, reacts 3h, and the NaCl of sodium metasilicate quality 8% and the solvent mixing of sodium metasilicate quality 30% is added, with 25r/min stirs 2h, stands 25min, and filtering takes filtrate 4:1 in mass ratio that desiccant is added, and 10min is mixed, and room temperature is close It closes and stands 20h, the polyoxypropyleneglycol of filtrate quality 20% is added, min is dispersed with 300W ultrasonic wave, decompression filters, must disperse Liquid;
(2) 80 DEG C are bathed in grease, 1:1:10:2 in mass ratio takes polyoxypropyleneglycol, dihydromethyl propionic acid, dispersion liquid, N- first The mixing of base pyrrolidones, leads to nitrogen protection, is warming up to 100 DEG C of heat preservation 20min, is cooled to 75 DEG C, obtains mixed reactant, take mixing Reactant 8:1:1 in mass ratio adds dibutyl tin dilaurate, isophorone diisocyanate mixing, reacts 2h, is cooled to 55 DEG C, feed liquid is obtained, triethylamine, acrylic acid, viscosity-controlling agent mixing and emulsifying is added in feeding liquid 4:1:2:1 in mass ratio, with 300r/ Min shearing dispersion 15min, is added the over cure potassium of feed liquid quality 16%, is warming up to 65 DEG C, keep the temperature 3h, be evaporated under reduced pressure to get multiple Close modified polyurethane.
The preparation method of complex mesoporous material, includes the following steps:
S1. in 40 DEG C of water-bath, 1:6 in mass ratio takes the NaOH solution mixing of phenol, mass fraction 15%, is stirred with 300r/min 20min, the formalin that the mass fraction for being added 3 times of phenol quality is 25% mix, and are warming up to 70 DEG C, continue to stir 10min, Cooled to room temperature adjusts pH to 6.8 with the hydrochloric acid solution of concentration 1mol/L, is concentrated under reduced pressure, is evaporated in vacuo to constant weight, obtains instead Object is answered, takes reactant that 3 times of reactant quality of dehydrated alcohol is added, is uniformly mixed, prefabricated phenolic resin is obtained and mixes liquid;
S2. it takes poloxamer liquid 5:2:4 in mass ratio that the mixed liquid of ethyl orthosilicate, prefabricated phenolic resin is added, is stirred with 300r/min It mixes, after 90 DEG C of thermal polymerization 20h, moves to tube furnace, under nitrogen protection, with 5 DEG C/min temperature programming to 350 DEG C of heat preservation 3h Afterwards, 800 DEG C of heat preservation 1h are warming up to, obtain heat treatment object, after cooled to room temperature, 3 times of heat-treated substance amount of maceration extract is added 2h is impregnated, filtering takes filter residue in 60 DEG C of oven dryings to get complex mesoporous material.
A kind of insulation and fire-proof paint, according to the mass fraction, including following component: 5 parts of auxiliary agents, 3 parts of glass beads, 6 parts of tables Face activating agent, 2 rosin, 25 parts of water, which is characterized in that further include: 20 parts of composite modified polyurethane, 15 parts of complex mesoporous materials.
A kind of preparation method of insulation and fire-proof paint, includes the following steps:
(1) according to the mass fraction, take 5 parts of auxiliary agents, 3 parts of glass beads, 6 parts of surfactants, 2 rosin, 25 parts of water, 20 parts it is compound Modified polyurethane, 15 parts of complex mesoporous materials;
(2) auxiliary agent, glass bead, rosin, water is taken to mix in reaction kettle prior to 30 DEG C, after 300r/min magnetic agitation 25min, Composite modified polyurethane, surfactant, complex mesoporous material mixing is added, with 300W supersonic oscillations 20min, in 0.9MPa, 20 DEG C CO is passed through with 200mL/min2, 2h is stood to get insulation and fire-proof paint.
Embodiment 2
Solvent: 1:6 in mass ratio takes acetone, ethyl alcohol mixing to get solvent.
Desiccant: 5:1.5 takes CaSO in mass ratio4、CaCl2Mixing is to get desiccant.
Viscosity-controlling agent: hydroxylamine hydrochloride.
Surfactant: 4:1.5 in mass ratio takes empgen BB, sodium secondary alkyl sulfonate mixing living to get surface Property agent.
Auxiliary agent: 6:1:1.5 in mass ratio takes metakaolin, amine carbonate, magnesium stearate mixing to get auxiliary agent.
Poloxamer liquid: 1:4:6 in mass ratio takes the hydrochloric acid solution mixing of poloxamer, ethyl alcohol, concentration 0.1mol/L, i.e., Obtain poloxamer liquid.
Maceration extract: 1:2:13 in mass ratio takes the second of the chitosan of deacetylation 90%, Dopamine hydrochloride, mass fraction 10% Acid solution mixes to get maceration extract.
The preparation method of composite modified polyurethane, includes the following steps:
(1) in 12 DEG C, 1:7 in mass ratio takes the hydrochloric acid solution mixing of sodium metasilicate, concentration 0.1mol/L, and sodium metasilicate quality is added 30% silane coupling agent mixing, reacts 4h, and the NaCl of sodium metasilicate quality 12% and the solvent mixing of sodium metasilicate quality 40% is added, 3h is stirred with 320r/min, stands 30min, filtering takes filtrate 5:1 in mass ratio that desiccant is added, and 13min, room is mixed The closed standing 22h of temperature, is added the polyoxypropyleneglycol of filtrate quality 25%, disperses 20min with 300W ultrasonic wave, and decompression filters, Obtain dispersion liquid;
(2) 85 DEG C are bathed in grease, 1:1:12:2 in mass ratio takes polyoxypropyleneglycol, dihydromethyl propionic acid, dispersion liquid, N- first The mixing of base pyrrolidones, leads to nitrogen protection, is warming up to 105 DEG C of heat preservation 25min, is cooled to 80 DEG C, obtains mixed reactant, take mixing Reactant 9:2:1 in mass ratio adds dibutyl tin dilaurate, isophorone diisocyanate mixing, reacts 4h, is cooled to 60 DEG C, feed liquid is obtained, triethylamine, acrylic acid, viscosity-controlling agent mixing and emulsifying is added in feeding liquid 5:1:2:1 in mass ratio, with 350r/ Min shearing dispersion 20min, is added the over cure potassium of feed liquid quality 20%, is warming up to 70 DEG C, keep the temperature 4h, be evaporated under reduced pressure to get multiple Close modified polyurethane.
The preparation method of complex mesoporous material, includes the following steps:
S1. in 50 DEG C of water-bath, 1:8 in mass ratio takes the NaOH solution mixing of phenol, mass fraction 15%, is stirred with 400r/min 30min, the formalin that the mass fraction for being added 5 times of phenol quality is 25% mix, and are warming up to 80 DEG C, continue to stir 15min, Cooled to room temperature adjusts pH to 7 with the hydrochloric acid solution of concentration 1mol/L, is concentrated under reduced pressure, is evaporated in vacuo to constant weight, must react Object takes reactant that 4 times of reactant quality of dehydrated alcohol is added, and is uniformly mixed, and obtains prefabricated phenolic resin and mixes liquid;
S2. it takes poloxamer liquid 7:2:4 in mass ratio that the mixed liquid of ethyl orthosilicate, prefabricated phenolic resin is added, is stirred with 320r/min It mixes, after 95 DEG C of thermal polymerization 22h, moves to tube furnace, under nitrogen protection, with 7 DEG C/min temperature programming to 450 DEG C of heat preservation 4h Afterwards, 850 DEG C of heat preservation 1.5h are warming up to, obtain heat treatment object, after cooled to room temperature, 4 times of heat-treated substance amount of dipping is added Liquid impregnates 3h, and filtering takes filter residue in 70 DEG C of oven dryings to get complex mesoporous material.
A kind of insulation and fire-proof paint, according to the mass fraction, including following component: 7 parts of auxiliary agents, 6 parts of glass beads, 8 parts of tables Face activating agent, 3 rosin, 35 parts of water, which is characterized in that further include: 32 parts of composite modified polyurethane, 25 parts of complex mesoporous materials.
A kind of preparation method of insulation and fire-proof paint, includes the following steps:
(1) according to the mass fraction, take 7 parts of auxiliary agents, 5 parts of glass beads, 8 parts of surfactants, 4 rosin, 32 parts of water, 36 parts it is compound Modified polyurethane, 25 parts of complex mesoporous materials;
(2) auxiliary agent, glass bead, rosin, water is taken to mix in reaction kettle prior to 40 DEG C, after 400r/min magnetic agitation 35min, Composite modified polyurethane, surfactant, complex mesoporous material mixing is added, with 300W supersonic oscillations 25min, in 0.9MPa, 22 DEG C CO is passed through with 250mL/min2, 3h is stood to get insulation and fire-proof paint.
Embodiment 3
Solvent: 1:8 in mass ratio takes acetone, ethyl alcohol mixing to get solvent.
Desiccant: 5:2 takes CaSO in mass ratio4、CaCl2Mixing is to get desiccant.
Viscosity-controlling agent: hydroxyl sulfate.
Surfactant: 4:2 in mass ratio takes empgen BB, sodium secondary alkyl sulfonate mixing to get surface-active Agent.
Auxiliary agent: 6:1:2 in mass ratio takes metakaolin, amine carbonate, magnesium stearate mixing to get auxiliary agent.
Poloxamer liquid: 1:5:6 in mass ratio takes the hydrochloric acid solution mixing of poloxamer, ethyl alcohol, concentration 0.1mol/L, i.e., Obtain poloxamer liquid.
Maceration extract: 1:3:15 in mass ratio takes the second of the chitosan of deacetylation 90%, Dopamine hydrochloride, mass fraction 10% Acid solution mixes to get maceration extract.
The preparation method of composite modified polyurethane, includes the following steps:
(1) in 15 DEG C, 1:10 in mass ratio takes the hydrochloric acid solution mixing of sodium metasilicate, concentration 0.1mol/L, and sodium metasilicate quality is added 35% silane coupling agent mixing, reacts 5h, and the NaCl of sodium metasilicate quality 15% and the solvent mixing of sodium metasilicate quality 45% is added, 4h is stirred with 400r/min, stands 40min, filtering takes filtrate 9:1 in mass ratio that desiccant is added, and 15min, room is mixed For 24 hours, the polyoxypropyleneglycol of filtrate quality 30% is added in the closed standing of temperature, disperses 25min with 300W ultrasonic wave, and decompression filters, Obtain dispersion liquid;
(2) 90 DEG C are bathed in grease, 1:1:15:2 in mass ratio takes polyoxypropyleneglycol, dihydromethyl propionic acid, dispersion liquid, N- first The mixing of base pyrrolidones, leads to nitrogen protection, is warming up to 110 DEG C of heat preservation 30min, is cooled to 85 DEG C, obtains mixed reactant, take mixing Reactant 12:3:1 in mass ratio adds dibutyl tin dilaurate, isophorone diisocyanate mixing, reacts 5h, is cooled to 65 DEG C, feed liquid is obtained, triethylamine, acrylic acid, viscosity-controlling agent mixing and emulsifying is added in feeding liquid 8:1:2:1 in mass ratio, with 500r/ Min shearing dispersion 30min, is added the over cure potassium of feed liquid quality 25%, is warming up to 75 DEG C, keep the temperature 5h, be evaporated under reduced pressure to get multiple Close modified polyurethane.
The preparation method of complex mesoporous material, includes the following steps:
S1. in 60 DEG C of water-bath, 1:10 in mass ratio takes the NaOH solution mixing of phenol, mass fraction 15%, is stirred with 450r/min 45min, the formalin that the mass fraction for being added 7 times of phenol quality is 25% mix, and are warming up to 85 DEG C, continue to stir 20min, Cooled to room temperature adjusts pH to 7.2 with the hydrochloric acid solution of concentration 1mol/L, is concentrated under reduced pressure, is evaporated in vacuo to constant weight, obtains instead Object is answered, takes reactant that 5 times of reactant quality of dehydrated alcohol is added, is uniformly mixed, prefabricated phenolic resin is obtained and mixes liquid;
S2. it takes poloxamer liquid 8:2:4 in mass ratio that the mixed liquid of ethyl orthosilicate, prefabricated phenolic resin is added, is stirred with 350r/min It mixes, after 100 DEG C of thermal polymerizations for 24 hours, moves to tube furnace, under nitrogen protection, with 10 DEG C/min temperature programming to 500 DEG C of heat preservation 5h Afterwards, 900 DEG C of heat preservation 2h are warming up to, obtain heat treatment object, after cooled to room temperature, 5 times of heat-treated substance amount of maceration extract is added 5h is impregnated, filtering takes filter residue in 80 DEG C of oven dryings to get complex mesoporous material.
A kind of insulation and fire-proof paint, according to the mass fraction, including following component: 10 parts of auxiliary agents, 8 parts of glass beads, 10 parts Surfactant, 5 rosin, 40 parts of water, which is characterized in that further include: 45 parts of composite modified polyurethane, 30 parts of composite mesopore materials Material.
A kind of preparation method of insulation and fire-proof paint, includes the following steps:
(1) according to the mass fraction, take 10 parts of auxiliary agents, 8 parts of glass beads, 10 parts of surfactants, 5 rosin, 40 parts of water, 45 parts it is multiple Close modified polyurethane, 30 parts of complex mesoporous materials;
(2) auxiliary agent, glass bead, rosin, water is taken to mix in reaction kettle prior to 45 DEG C, after 500r/min magnetic agitation 50min, Composite modified polyurethane, surfactant, complex mesoporous material mixing is added, with 300W supersonic oscillations 30min, in 0.9MPa, 25 DEG C CO is passed through with 300mL/min2, 4h is stood to get insulation and fire-proof paint.
Comparative example 1: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking composite modified polyurethane.
Comparative example 2: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking complex mesoporous material.
Comparative example 3: the insulation and fire-proof paint of company of Hebei province production.
Embodiment 1,2,3 and comparative example are prepared into insulation and fire-proof paint and carry out Determination of conductive coefficients: by each sample while being set It moves back to drier and is cooled to room temperature in insulating box, drying to constant weight at a temperature of 378 scholar 5K;Open adding for thermal conductivity test instrument Each sample is individually placed in heating furnace position above and below testing element by hot stove lid, and the surface of sample each as far as possible keeps more close Contact, can test after shutting heating furnace cover;General supply is connected, control heating furnace automatic temperature control switch disk is allocated to scheduled control Furnace temperature (360K, 460K, 560K, 660K, 760K, 860K);Test macro switch is opened, is entered just to every test condition Normal state;Automatic calibration knob is opened, correction finishes, and calibrating knob slew test shelves automatically process data through microcomputer Afterwards, liquid crystal display watch starts to show the mean temperature and thermal coefficient at this temperature of tested sample, and each sample is at each temperature Thermal coefficient take three to the statistical average of (six pieces) random sampling.Test result such as table 1.
Table 1:
In conclusion as shown in Table 1, insulation and fire-proof paint good heat preservation performance prepared by the present invention, heat resistance are strong, are worth advocating energetically It uses.

Claims (10)

1. a kind of insulation and fire-proof paint, according to the mass fraction, including following component: 5 ~ 10 parts of auxiliary agents, 3 ~ 8 parts of glass beads, 6 ~ 10 parts of surfactants, 2 ~ 5 rosin, 25 ~ 40 parts of water, which is characterized in that further include: 20 ~ 45 parts of composite modified polyurethane, 15 ~ 30 parts of complex mesoporous materials.
2. a kind of insulation and fire-proof paint according to claim 1, which is characterized in that the preparation side of the composite modified polyurethane Method includes the following steps:
(1) in 10 ~ 15 DEG C, 1:5 ~ 10 take sodium metasilicate, hydrochloric acid solution mixing in mass ratio, and the silicon of sodium metasilicate quality 20 ~ 35% is added The mixing of alkane coupling agent, reacts 3 ~ 5h, and the solvent mixing of NaCl and sodium metasilicate quality 30 ~ 45% that sodium metasilicate quality 8 ~ 15% is added are stirred It mixes, stands, filtering takes filtrate 4 ~ 9:1 in mass ratio that desiccant is added, it is mixed, closed standing, addition filtrate quality 20 ~ 30% polyoxypropyleneglycol, ultrasonic wave dispersion, decompression filter, and obtain dispersion liquid;
(2) in 80 ~ 90 DEG C, 1:1:10 ~ 15:2 in mass ratio takes polyoxypropyleneglycol, dihydromethyl propionic acid, dispersion liquid, N- first Base pyrrolidones mixing, ventilation protection, is warming up to 100 ~ 110 DEG C of heat preservations, is cooled to 75 ~ 85 DEG C, obtains mixed reactant, take mixing Reactant 8 ~ 12:1 in mass ratio ~ 3:1 adds dibutyl tin dilaurate, isophorone diisocyanate mixing, reacts 2 ~ 5h, drop Temperature obtains feed liquid, and triethylamine, acrylic acid, viscosity-controlling agent mixing is added in feeding liquid 4 ~ 8:1:2:1 in mass ratio, and shearing dispersion adds Enter the over cure potassium of feed liquid quality 16 ~ 25%, heat up, keep the temperature 3 ~ 5h, is evaporated under reduced pressure to get composite modified polyurethane.
3. a kind of insulation and fire-proof paint according to claim 2, which is characterized in that the solvent in the step (1): pressing quality Take acetone, ethyl alcohol mixing to get solvent than 1:4 ~ 8.
4. a kind of insulation and fire-proof paint according to claim 2, which is characterized in that the desiccant in the step (1): pressing matter Amount takes CaSO than 5:1 ~ 24、CaCl2Mixing is to get desiccant.
5. a kind of insulation and fire-proof paint according to claim 2, which is characterized in that the viscosity-controlling agent in the step (2): Urea, hydroxylamine hydrochloride, any one in hydroxyl sulfate.
6. a kind of insulation and fire-proof paint according to claim 1, which is characterized in that the preparation side of the complex mesoporous material Method includes the following steps:
S1. in 40 ~ 60 DEG C, 1:6 ~ 10 take phenol, NaOH solution to be mixed in mass ratio, and 3 ~ 7 times of formaldehyde of phenol quality are added Solution mixing, is warming up to 70 ~ 85 DEG C, stirs, cooling, adjusts pH, is concentrated under reduced pressure, and is evaporated in vacuo, obtains reactant, reactant is taken to add Enter 3 ~ 5 times of reactant quality of dehydrated alcohol, be uniformly mixed, obtains prefabricated phenolic resin and mix liquid;
S2. take poloxamer liquid 5 ~ 8:2:4 in mass ratio that ethyl orthosilicate is added, prefabricated phenolic resin mixes liquid, stirring, hot polymerization It closes, nitrogen protection, temperature programming to 350 ~ 500 DEG C of heat preservations is warming up to 800 ~ 900 DEG C of 1 ~ 2h of heat preservation, obtains heat treatment object, and it is cooling, 3 ~ 5 times of heat-treated substance amount of maceration extract is added to impregnate, filtering takes filter residue and drying to get complex mesoporous material.
7. a kind of insulation and fire-proof paint according to claim 6, which is characterized in that the poloxamer liquid in the step S2: 1:3 ~ 5:6 in mass ratio takes poloxamer, ethyl alcohol, hydrochloric acid solution mixing to get poloxamer liquid.
8. a kind of insulation and fire-proof paint according to claim 6, which is characterized in that the maceration extract in the step S2: pressing matter Amount takes chitosan, Dopamine hydrochloride, acetic acid solution mixing to get maceration extract than 1:1 ~ 3:10 ~ 15.
9. a kind of insulation and fire-proof paint according to claim 1, which is characterized in that the surfactant: 4:1 in mass ratio ~ 2 take empgen BB, sodium secondary alkyl sulfonate mixing to get surfactant.
10. a kind of insulation and fire-proof paint according to claim 1, which is characterized in that the auxiliary agent: 6:1:1 ~ 2 in mass ratio Take metakaolin, amine carbonate, magnesium stearate mixing to get auxiliary agent.
CN201810762456.XA 2018-07-12 2018-07-12 A kind of insulation and fire-proof paint Pending CN109135547A (en)

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Application publication date: 20190104