CN105505180A - Flame-retardant water-based polyurethane paint - Google Patents
Flame-retardant water-based polyurethane paint Download PDFInfo
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- CN105505180A CN105505180A CN201511005107.6A CN201511005107A CN105505180A CN 105505180 A CN105505180 A CN 105505180A CN 201511005107 A CN201511005107 A CN 201511005107A CN 105505180 A CN105505180 A CN 105505180A
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/06—Polyurethanes from polyesters
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/46—Polycondensates having carboxylic or carbonic ester groups in the main chain having heteroatoms other than oxygen
- C08G18/4684—Polycondensates having carboxylic or carbonic ester groups in the main chain having heteroatoms other than oxygen containing phosphorus
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
- C08G18/6644—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203 having at least three hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/778—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur silicon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/78—Nitrogen
- C08G18/79—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates
- C08G18/791—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups
- C08G18/794—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups formed by oligomerisation of aromatic isocyanates or isothiocyanates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/692—Polyesters containing atoms other than carbon, hydrogen and oxygen containing phosphorus
- C08G63/6924—Polyesters containing atoms other than carbon, hydrogen and oxygen containing phosphorus derived from polycarboxylic acids and polyhydroxy compounds
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- 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
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- 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
- C09D7/45—Anti-settling agents
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- 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
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses flame-retardant water-based polyurethane paint which is prepared from 85-88 parts of modified polyurethane resin, 12-15 parts of resol resin, 7-10 parts of waterborne acrylic resin, 3-6 parts of bentonite, 15-18 parts of zeolite powder, 13-16 parts of diatomite, 12-15 parts of talcum powder, 2-4 parts of a thickening agent, 3-5 parts of a flatting agent, 1-2 parts of a defoaming agent, 1-2 parts of an anti-corrosion agent and 2-3 parts of pigment. The flame-retardant water-based polyurethane paint has excellent heat resistance, fireproof performance and flame retardancy, excellent in water resistance, high in adhesive force, high in hardness and high in drying speed.
Description
Technical field
The present invention relates to technical field of coatings, particularly relate to a kind of extinguishing waterborn polyurethane coating.
Background technology
Aqueous polyurethane, using water as dispersion medium, has the advantage such as environment-protecting asepsis, difficult to burn, and can be regulated the over-all properties of resin material by change soft or hard section kind and ratio.After the end of the sixties in last century, aqueous polyurethane was introduced into market, aqueous polyurethane with the viscosifying power of excellence, outstanding temp. variation resistant performance, excellent resistance to low temperature, good biocompatibility and the characteristic of environment-protecting asepsis and be widely used in multiple field.Although aqueous polyurethane molecular chain chemical structure is identical with solvent borne polyurethane, compared with solvent borne polyurethane, still there are some defects at aspect of performance, such as, molecular weight be little, poor water resistance and hardness little etc., because which limit its application.At present, aqueous polyurethane coating can not meet the requirement of society in water tolerance and flame retardant resistance, needs to carry out modification.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes a kind of extinguishing waterborn polyurethane coating, have excellent heat-resisting, fire retardant performance, water resistance is outstanding, and sticking power is high, and hardness is high, and rate of drying is fast.
A kind of extinguishing waterborn polyurethane coating that the present invention proposes, its raw material comprises by weight: modified polyurethane resin 85 ~ 88 parts, resol resins 12 ~ 15 parts, water-borne acrylic resin 7 ~ 10 parts, wilkinite 3 ~ 6 parts, zeolite powder 15 ~ 18 parts, 13 ~ 16 parts, diatomite, talcum powder 12 ~ 15 parts, thickening material 2 ~ 4 parts, flow agent 3 ~ 5 parts, defoamer 1 ~ 2 part, sanitas 1 ~ 2 part, pigment 2 ~ 3 parts.
Preferably, the weight ratio of modified polyurethane resin, resol resins, water-borne acrylic resin is 86 ~ 87:13 ~ 14:8 ~ 9.
Preferably, wilkinite, zeolite powder, diatomite, talcous weight ratio are 4 ~ 5:16 ~ 17:14 ~ 15:13 ~ 14.
Preferably, modified polyurethane resin is prepared as follows: after 65 ~ 68 parts of organophosphorus polyester polyols and 52 ~ 55 parts of trimeric benzene dimethylene diisocyanates being mixed by weight, heat up, insulation, add 4 ~ 5 parts of neopentyl glycol after cooling, 3 ~ 5 parts of quadrol base ethyl sulfonic acid sodium, 4 ~ 6 parts of tetramethylolmethanes and DMFs mix, then add 1.1 ~ 1.4 parts of sodium-o-phenyl phenolates, heat up, insulation obtains the first material; After the first material cooling, then drip the solution containing 3 ~ 4 parts of N-ethyldiethanolamine and 5.5 ~ 7 parts of two (2-hydroxypropyl) aniline, heat up, insulation obtains the second material; After second material is regulated pH to neutrality, vacuum removal DMF obtains modified polyurethane resin.
Preferably, in the preparation method of modified polyurethane resin, trimeric benzene dimethylene diisocyanate is prepared as follows: by xylylene diisocyanate and the mixing of N-tributyl tin imidazoles, pass into N
2protection, is warming up to 92 ~ 95 DEG C, does not stop to stir in temperature-rise period, and insulation 1.7 ~ 2h obtains material a; After tetraethoxysilane and the mixing of lauric acid bismuth, be added to the water and obtain material b; Mixed by material a and material b, be warming up to 53 ~ 56 DEG C, insulation 2.2 ~ 2.5h, vacuum distilling obtains trimeric benzene dimethylene diisocyanate.
Preferably, in the preparation method of modified polyurethane resin, trimeric benzene dimethylene diisocyanate is prepared as follows: by weight by 46 ~ 49 parts of xylylene diisocyanates and 3 ~ 6 parts of N-tributyl tin imidazoles mixing, pass into N
2protection, is warming up to 92 ~ 95 DEG C, does not stop to stir in temperature-rise period, and insulation 1.7 ~ 2h obtains material a; After 7 ~ 10 parts of tetraethoxysilanes and 1 ~ 1.5 part of lauric acid bismuth mixing, be added to the water and obtain material b; Mixed by material a and material b, be warming up to 53 ~ 56 DEG C, insulation 2.2 ~ 2.5h, vacuum distilling obtains trimeric benzene dimethylene diisocyanate.
Preferably, in the preparation method of modified polyurethane resin, the preparation method of organophosphorus polyester polyol is as follows: after 2-phosphate-1,2,4-tri carboxyl butane and the mixing of 1,6-hexylene glycol, pass into N
2as shielding gas, be then warming up to 107 ~ 110 DEG C, insulation 1.5 ~ 1.8h, then add tributyltin oxide, be warming up to 165 ~ 168 DEG C, insulation 4 ~ 5h, vacuum heat-preserving 2 ~ 3h obtains organophosphorus polyester polyol.
Preferably, in the preparation method of modified polyurethane resin, the preparation method of organophosphorus polyester polyol is as follows: by weight by after 32 ~ 35 parts of 2-phosphate-1,2,4-tri carboxyl butanes and 35 ~ 38 part of 1,6-hexylene glycol mixing, pass into N
2as shielding gas, be then warming up to 107 ~ 110 DEG C, insulation 1.5 ~ 1.8h, then add 3 ~ 4 parts of tributyltin oxides, be warming up to 165 ~ 168 DEG C, insulation 4 ~ 5h, vacuum heat-preserving 2 ~ 3h obtains organophosphorus polyester polyol.
Preferably, modified polyurethane resin is prepared as follows: after 65 ~ 68 parts of organophosphorus polyester polyols and 52 ~ 55 parts of trimeric benzene dimethylene diisocyanates being mixed by weight, be warming up to 77 ~ 80 DEG C, insulation 4 ~ 4.6h, 4 ~ 5 parts of neopentyl glycol, 3 ~ 5 parts of quadrol base ethyl sulfonic acid sodium, 4 ~ 6 parts of tetramethylolmethanes and N are added after being cooled to 39 ~ 42 DEG C, dinethylformamide mixes, add 1.1 ~ 1.4 parts of sodium-o-phenyl phenolates again, be warming up to 75 ~ 78 DEG C, insulation 5.5 ~ 6.5h obtains the first material; After first material is cooled to 30 ~ 40 DEG C, then drip the solution containing 3 ~ 4 parts of N-ethyldiethanolamine and 5.5 ~ 7 parts of two (2-hydroxypropyl) aniline, be warming up to 72 ~ 75 DEG C, insulation 3.5 ~ 4.5h obtains the second material; After second material is regulated pH to neutrality, vacuum removal DMF obtains modified polyurethane resin.
The present invention routinely technique prepares.
The present invention is by after xylylene diisocyanate and the mixing of N-tributyl tin imidazoles, heat up, to make in xylylene diisocyanate-NCO group reacts, three isocyanate groups polymerizations generate the isocyanurate group of six-membered ring structure, then tetraethoxysilane and lauric acid bismuth is added, under the effect of catalyzer lauric acid bismuth, tetraethoxysilane hydrolysis produce sulfydryl and xylylene diisocyanate tripolymer on isocyanate group react, make polysiloxane grafted on xylylene diisocyanate tripolymer, for the preparation of modified polyurethane resin is laid the groundwork.
The present invention adopts 2-phosphate-1,2,4-tri carboxyl butane and 1,6-hexylene glycol to carry out fat polymerization and obtains organophosphorus polyester polyol, then organophosphorus polyester polyol and trimeric benzene dimethylene diisocyanate is adopted to be prepared modified polyurethane resin, trimeric benzene dimethylene diisocyanate introduces huge side-chain radical on polyurethane structural, and organophosphorus polyester polyol introduces long carbon side chain and phosphorous group on polyurethane structural, side-chain radical is wound around mutually, make the viscosity of modified polyurethane resin and elongation at break little, further raising tensile strength, hardness, toughness, not only increase the lipophilicity of modified polyurethane resin, when the present invention is solidified, oleophilic group is outwards arranged to air, hydrophilic group is inwardly arranged, thus contact angle is increased, shipwreck is with the coatingsurface spreading wetting formed in the present invention, later stage can carry out oxygenation in atmosphere simultaneously, produce self-crosslinking phenomenon, system degree of crosslinking is increased, rigid structure increases, improve and cause coating deliquescing due to the introducing of phosphorus-containing groups, the shortcoming that sticking power is deteriorated, thus make of the present invention water-fast, heat-resisting and stretch-proof performance is further enhanced, trimeric benzene dimethylene diisocyanate have isocyanuric acid ester six-ring and organosilicon radical simultaneously, wherein isocyanuric acid ester six-ring has strong sucting electronic effect, the C=N bond polarity of-NCO in molecule is caused to increase, improve reactive behavior, accelerate the speed of response of trimeric benzene dimethylene diisocyanate and hydroxyl, improve degree of crosslinking, improve hardness and the sticking power of modified polyurethane resin, the introducing of phosphorus-containing groups simultaneously, make the present invention in combustion, the bond energy that bond energy due to C-C key is greater than C-P wants large, the P contained compound of ability of being heated takes the lead in decompositing phosphoric acid and multiple organic phospho acid plays covering effect, also cause polyhydroxylated polymer to dewater and form layer of charcoal that is heat insulation, oxygen barrier, thus improve flame retardant properties of the present invention, and containing four hydroxyls in tetramethylolmethane, can react with-NCO, generate the urethane with cross-linked structure, molecular chain movement is restricted, and large-scale being cross-linked makes intermolecular space diminish, water molecules is difficult to enter polyurethane molecular inside, the water-intake rate showing as resin constantly declines, and water tolerance improves, and the introducing of tetramethylolmethane makes urethane crosslinks degree increase, internal cohesive energy becomes large, improves thermostability of the present invention and hardness.
The present invention adopts modified polyurethane resin, resol resins and water-borne acrylic resin as filmogen, not only there is high gloss, high rigidity, anti-degraded and weather resisteant good, and water-fast, heat-resisting, fire retardant performance is outstanding, sticking power is high, and rate of drying is fast; And wilkinite is as anti-settling auxiliary agent of the present invention, greatly improve denseness of the present invention and anti-thixotropy, the filmogen in the present invention and packing strengthening agent are evenly distributed, substantially prolongs work-ing life of the present invention and shelf time; Wilkinite also with zeolite powder, diatomite, talcum powder as weighting material, make the present invention have excellent intensity, toughness, waterproof, anti-aging, wear-resisting and corrosion resistance after hardening; Wilkinite, zeolite powder, diatomite and talcum powder have huge specific surface area, surperficial many meso-hole structures and extremely strong adsorptive power, not only make the present invention after hardening, the harmful dust in adsorbable air, also make the present invention have good flame retardant properties.
Embodiment
Below, by specific embodiment, technical scheme of the present invention is described in detail.
Embodiment 1
A kind of extinguishing waterborn polyurethane coating that the present invention proposes, its raw material comprises by weight: modified polyurethane resin 85 parts, resol resins 15 parts, water-borne acrylic resin 7 parts, wilkinite 6 parts, zeolite powder 15 parts, 16 parts, diatomite, talcum powder 12 parts, thickening material 4 parts, flow agent 3 parts, defoamer 2 parts, sanitas 1 part, pigment 3 parts.
Modified polyurethane resin is prepared as follows: after 65 parts of organophosphorus polyester polyols and 55 parts of trimeric benzene dimethylene diisocyanates being mixed by weight, be warming up to 77 DEG C, insulation 4.6h, 5 parts of neopentyl glycol, 3 parts of quadrol base ethyl sulfonic acid sodium, 6 parts of tetramethylolmethanes and N are added after being cooled to 39 DEG C, dinethylformamide mixes, add 1.1 parts of sodium-o-phenyl phenolates again, be warming up to 78 DEG C, insulation 5.5h obtains the first material; After first material is cooled to 40 DEG C, then drip the solution containing 3 parts of N-ethyldiethanolamine and 7 parts of two (2-hydroxypropyl) aniline, be warming up to 72 DEG C, insulation 4.5h obtains the second material; After second material is regulated pH to neutrality, vacuum removal DMF obtains modified polyurethane resin.
Trimeric benzene dimethylene diisocyanate is prepared as follows: by weight by 46 parts of xylylene diisocyanates and 6 parts of N-tributyl tin imidazoles mixing, pass into N
2protection, is warming up to 92 DEG C, does not stop to stir in temperature-rise period, and insulation 2h obtains material a; After 7 parts of tetraethoxysilanes and 1.5 parts of lauric acid bismuth mixing, be added to the water and obtain material b; Mixed by material a and material b, be warming up to 53 DEG C, insulation 2.5h, vacuum distilling obtains trimeric benzene dimethylene diisocyanate.
The preparation method of organophosphorus polyester polyol is as follows: by weight by after 32 parts of 2-phosphate-1,2,4-tri carboxyl butanes and 38 part of 1,6-hexylene glycol mixing, pass into N
2as shielding gas, be then warming up to 107 DEG C, insulation 1.8h, then add 3 parts of tributyltin oxides, be warming up to 168 DEG C, insulation 4h, vacuum heat-preserving 3h obtains organophosphorus polyester polyol.
Embodiment 2
A kind of extinguishing waterborn polyurethane coating that the present invention proposes, its raw material comprises by weight: modified polyurethane resin 88 parts, resol resins 12 parts, water-borne acrylic resin 10 parts, wilkinite 3 parts, zeolite powder 18 parts, 13 parts, diatomite, talcum powder 15 parts, thickening material 2 parts, flow agent 5 parts, defoamer 1 part, sanitas 2 parts, pigment 2 parts.
Modified polyurethane resin is prepared as follows: after 68 parts of organophosphorus polyester polyols and 52 parts of trimeric benzene dimethylene diisocyanates being mixed by weight, be warming up to 80 DEG C, insulation 4h, 4 parts of neopentyl glycol, 5 parts of quadrol base ethyl sulfonic acid sodium, 4 parts of tetramethylolmethanes and N are added after being cooled to 42 DEG C, dinethylformamide mixes, add 1.4 parts of sodium-o-phenyl phenolates again, be warming up to 75 DEG C, insulation 6.5h obtains the first material; After first material is cooled to 30 DEG C, then drip the solution containing 4 parts of N-ethyldiethanolamine and 5.5 parts of two (2-hydroxypropyl) aniline, be warming up to 75 DEG C, insulation 3.5h obtains the second material; After second material is regulated pH to neutrality, vacuum removal DMF obtains modified polyurethane resin.
Trimeric benzene dimethylene diisocyanate is prepared as follows: by weight by 49 parts of xylylene diisocyanates and 3 parts of N-tributyl tin imidazoles mixing, pass into N
2protection, is warming up to 95 DEG C, does not stop to stir in temperature-rise period, and insulation 1.7h obtains material a; After 10 parts of tetraethoxysilanes and 1 part of lauric acid bismuth mixing, be added to the water and obtain material b; Mixed by material a and material b, be warming up to 56 DEG C, insulation 2.2h, vacuum distilling obtains trimeric benzene dimethylene diisocyanate.
The preparation method of organophosphorus polyester polyol is as follows: by weight by after 35 parts of 2-phosphate-1,2,4-tri carboxyl butanes and 35 part of 1,6-hexylene glycol mixing, pass into N
2as shielding gas, be then warming up to 110 DEG C, insulation 1.5h, then add 4 parts of tributyltin oxides, be warming up to 165 DEG C, insulation 5h, vacuum heat-preserving 2h obtains organophosphorus polyester polyol.
Embodiment 3
A kind of extinguishing waterborn polyurethane coating that the present invention proposes, its raw material comprises by weight: modified polyurethane resin 86 parts, resol resins 14 parts, water-borne acrylic resin 8 parts, wilkinite 5 parts, zeolite powder 16 parts, 15 parts, diatomite, talcum powder 13 parts, thickening material 3.5 parts, flow agent 3.5 parts, defoamer 1.8 parts, sanitas 1.5 parts, pigment 2.6 parts.
Modified polyurethane resin is prepared as follows: after 66 parts of organophosphorus polyester polyols and 54 parts of trimeric benzene dimethylene diisocyanates being mixed by weight, be warming up to 78 DEG C, insulation 4.4h, 4.5 parts of neopentyl glycol, 3.5 parts of quadrol base ethyl sulfonic acid sodium, 5.5 parts of tetramethylolmethanes and N are added after being cooled to 40 DEG C, dinethylformamide mixes, add 1.2 parts of sodium-o-phenyl phenolates again, be warming up to 77 DEG C, insulation 5.8h obtains the first material; After first material is cooled to 37 DEG C, then drip the solution containing 3.2 parts of N-ethyldiethanolamine and 6.5 parts of two (2-hydroxypropyl) aniline, be warming up to 73 DEG C, insulation 4.3h obtains the second material; After second material is regulated pH to neutrality, vacuum removal DMF obtains modified polyurethane resin.
Trimeric benzene dimethylene diisocyanate is prepared as follows: by weight by 47 parts of xylylene diisocyanates and 5 parts of N-tributyl tin imidazoles mixing, pass into N
2protection, is warming up to 93 DEG C, does not stop to stir in temperature-rise period, and insulation 1.9h obtains material a; After 8 parts of tetraethoxysilanes and 1.4 parts of lauric acid bismuth mixing, be added to the water and obtain material b; Mixed by material a and material b, be warming up to 54 DEG C, insulation 2.4h, vacuum distilling obtains trimeric benzene dimethylene diisocyanate.
The preparation method of organophosphorus polyester polyol is as follows: by weight by after 33 parts of 2-phosphate-1,2,4-tri carboxyl butanes and 37 part of 1,6-hexylene glycol mixing, pass into N
2as shielding gas, be then warming up to 108 DEG C, insulation 1.7h, then add 3.5 parts of tributyltin oxides, be warming up to 167 DEG C, insulation 4.2h, vacuum heat-preserving 2.7h obtains organophosphorus polyester polyol.
Embodiment 4
A kind of extinguishing waterborn polyurethane coating that the present invention proposes, its raw material comprises by weight: modified polyurethane resin 87 parts, resol resins 13 parts, water-borne acrylic resin 9 parts, wilkinite 4 parts, zeolite powder 17 parts, 14 parts, diatomite, talcum powder 14 parts, thickening material 2.5 parts, flow agent 4.5 parts, defoamer 1.2 parts, sanitas 1.8 parts, pigment 2.4 parts.
Modified polyurethane resin is prepared as follows: after 67 parts of organophosphorus polyester polyols and 53 parts of trimeric benzene dimethylene diisocyanates being mixed by weight, be warming up to 79 DEG C, insulation 4.2h, 4.3 parts of neopentyl glycol, 4.5 parts of quadrol base ethyl sulfonic acid sodium, 4.5 parts of tetramethylolmethanes and N are added after being cooled to 41 DEG C, dinethylformamide mixes, add 1.3 parts of sodium-o-phenyl phenolates again, be warming up to 76 DEG C, insulation 6.2h obtains the first material; After first material is cooled to 33 DEG C, then drip the solution containing 3.4 parts of N-ethyldiethanolamine and 6 parts of two (2-hydroxypropyl) aniline, be warming up to 74 DEG C, insulation 3.7h obtains the second material; After second material is regulated pH to neutrality, vacuum removal DMF obtains modified polyurethane resin.
Trimeric benzene dimethylene diisocyanate is prepared as follows: by weight by 48 parts of xylylene diisocyanates and 4 parts of N-tributyl tin imidazoles mixing, pass into N
2protection, is warming up to 94 DEG C, does not stop to stir in temperature-rise period, and insulation 1.8h obtains material a; After 9 parts of tetraethoxysilanes and 1.2 parts of lauric acid bismuth mixing, be added to the water and obtain material b; Mixed by material a and material b, be warming up to 55 DEG C, insulation 2.3h, vacuum distilling obtains trimeric benzene dimethylene diisocyanate.
The preparation method of organophosphorus polyester polyol is as follows: by weight by after 34 parts of 2-phosphate-1,2,4-tri carboxyl butanes and 36 part of 1,6-hexylene glycol mixing, pass into N
2as shielding gas, be then warming up to 109 DEG C, insulation 1.6h, then add 3.8 parts of tributyltin oxides, be warming up to 166 DEG C, insulation 4.5h, vacuum heat-preserving 2.4h obtains organophosphorus polyester polyol.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (9)
1. an extinguishing waterborn polyurethane coating, is characterized in that, its raw material comprises by weight: modified polyurethane resin 85 ~ 88 parts, resol resins 12 ~ 15 parts, water-borne acrylic resin 7 ~ 10 parts, wilkinite 3 ~ 6 parts, zeolite powder 15 ~ 18 parts, 13 ~ 16 parts, diatomite, talcum powder 12 ~ 15 parts, thickening material 2 ~ 4 parts, flow agent 3 ~ 5 parts, defoamer 1 ~ 2 part, sanitas 1 ~ 2 part, pigment 2 ~ 3 parts.
2. extinguishing waterborn polyurethane coating according to claim 1, it is characterized in that, the weight ratio of modified polyurethane resin, resol resins, water-borne acrylic resin is 86 ~ 87:13 ~ 14:8 ~ 9.
3. extinguishing waterborn polyurethane coating according to claim 1 or 2, is characterized in that, wilkinite, zeolite powder, diatomite, talcous weight ratio are 4 ~ 5:16 ~ 17:14 ~ 15:13 ~ 14.
4. extinguishing waterborn polyurethane coating according to any one of claim 1-3, it is characterized in that, modified polyurethane resin is prepared as follows: after 65 ~ 68 parts of organophosphorus polyester polyols and 52 ~ 55 parts of trimeric benzene dimethylene diisocyanates being mixed by weight, heat up, insulation, 4 ~ 5 parts of neopentyl glycol, 3 ~ 5 parts of quadrol base ethyl sulfonic acid sodium, 4 ~ 6 parts of tetramethylolmethanes and N are added after cooling, dinethylformamide mixes, add 1.1 ~ 1.4 parts of sodium-o-phenyl phenolates again, heat up, insulation obtains the first material; After the first material cooling, then drip the solution containing 3 ~ 4 parts of N-ethyldiethanolamine and 5.5 ~ 7 parts of two (2-hydroxypropyl) aniline, heat up, insulation obtains the second material; After second material is regulated pH to neutrality, vacuum removal DMF obtains modified polyurethane resin.
5. extinguishing waterborn polyurethane coating according to any one of claim 1-4, it is characterized in that, in the preparation method of modified polyurethane resin, trimeric benzene dimethylene diisocyanate is prepared as follows: by xylylene diisocyanate and the mixing of N-tributyl tin imidazoles, pass into N
2protection, is warming up to 92 ~ 95 DEG C, does not stop to stir in temperature-rise period, and insulation 1.7 ~ 2h obtains material a; After tetraethoxysilane and the mixing of lauric acid bismuth, be added to the water and obtain material b; Mixed by material a and material b, be warming up to 53 ~ 56 DEG C, insulation 2.2 ~ 2.5h, vacuum distilling obtains trimeric benzene dimethylene diisocyanate.
6. extinguishing waterborn polyurethane coating according to any one of claim 1-5, it is characterized in that, in the preparation method of modified polyurethane resin, trimeric benzene dimethylene diisocyanate is prepared as follows: by weight by 46 ~ 49 parts of xylylene diisocyanates and 3 ~ 6 parts of N-tributyl tin imidazoles mixing, pass into N
2protection, is warming up to 92 ~ 95 DEG C, does not stop to stir in temperature-rise period, and insulation 1.7 ~ 2h obtains material a; After 7 ~ 10 parts of tetraethoxysilanes and 1 ~ 1.5 part of lauric acid bismuth mixing, be added to the water and obtain material b; Mixed by material a and material b, be warming up to 53 ~ 56 DEG C, insulation 2.2 ~ 2.5h, vacuum distilling obtains trimeric benzene dimethylene diisocyanate.
7. extinguishing waterborn polyurethane coating according to any one of claim 1-6, is characterized in that, in the preparation method of modified polyurethane resin, the preparation method of organophosphorus polyester polyol is as follows: by 2-phosphate-1,2,4-tri carboxyl butane and 1, after the mixing of 6-hexylene glycol, pass into N
2as shielding gas, be then warming up to 107 ~ 110 DEG C, insulation 1.5 ~ 1.8h, then add tributyltin oxide, be warming up to 165 ~ 168 DEG C, insulation 4 ~ 5h, vacuum heat-preserving 2 ~ 3h obtains organophosphorus polyester polyol.
8. extinguishing waterborn polyurethane coating according to any one of claim 1-7, it is characterized in that, in the preparation method of modified polyurethane resin, the preparation method of organophosphorus polyester polyol is as follows: by weight by 32 ~ 35 parts of 2-phosphates-1,2, after 4-tri carboxyl butane and 35 ~ 38 part of 1,6-hexylene glycol mix, pass into N
2as shielding gas, be then warming up to 107 ~ 110 DEG C, insulation 1.5 ~ 1.8h, then add 3 ~ 4 parts of tributyltin oxides, be warming up to 165 ~ 168 DEG C, insulation 4 ~ 5h, vacuum heat-preserving 2 ~ 3h obtains organophosphorus polyester polyol.
9. extinguishing waterborn polyurethane coating according to any one of claim 1-8, it is characterized in that, modified polyurethane resin is prepared as follows: after 65 ~ 68 parts of organophosphorus polyester polyols and 52 ~ 55 parts of trimeric benzene dimethylene diisocyanates being mixed by weight, be warming up to 77 ~ 80 DEG C, insulation 4 ~ 4.6h, 4 ~ 5 parts of neopentyl glycol are added after being cooled to 39 ~ 42 DEG C, 3 ~ 5 parts of quadrol base ethyl sulfonic acid sodium, 4 ~ 6 parts of tetramethylolmethanes and N, dinethylformamide mixes, add 1.1 ~ 1.4 parts of sodium-o-phenyl phenolates again, be warming up to 75 ~ 78 DEG C, insulation 5.5 ~ 6.5h obtains the first material, after first material is cooled to 30 ~ 40 DEG C, then drip the solution containing 3 ~ 4 parts of N-ethyldiethanolamine and 5.5 ~ 7 parts of two (2-hydroxypropyl) aniline, be warming up to 72 ~ 75 DEG C, insulation 3.5 ~ 4.5h obtains the second material, after second material is regulated pH to neutrality, vacuum removal DMF obtains modified polyurethane resin.
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| CN109354992A (en) * | 2018-09-18 | 2019-02-19 | 安徽科赛富新材料科技有限公司 | A kind of intermediate coat and preparation method thereof that closed performance is excellent |
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| CN105860840A (en) * | 2016-04-25 | 2016-08-17 | 南京高崎电机有限公司 | Novel fireproof paint |
| CN105885660A (en) * | 2016-05-30 | 2016-08-24 | 福建盈浩工艺制品有限公司 | Flame-retardant environment-friendly paint and preparation method thereof |
| CN107163741A (en) * | 2017-07-12 | 2017-09-15 | 合肥轻风飏电气科技有限责任公司 | A kind of Electric Appliance Cabinet high fire-retardance anti-static coatings and preparation method |
| CN108707411A (en) * | 2018-07-03 | 2018-10-26 | 阜南县富昌恒业工艺品有限公司 | A kind of Wood craft anti-flaming dope |
| CN109354992A (en) * | 2018-09-18 | 2019-02-19 | 安徽科赛富新材料科技有限公司 | A kind of intermediate coat and preparation method thereof that closed performance is excellent |
| CN109354992B (en) * | 2018-09-18 | 2021-03-23 | 安徽科赛富新材料科技有限公司 | Intermediate paint with excellent sealing performance and preparation method thereof |
| CN110616033A (en) * | 2019-10-30 | 2019-12-27 | 马鞍山市谷庆门业有限公司 | Preparation method of flame-retardant low-odor wooden door coating |
| CN112062935A (en) * | 2020-09-04 | 2020-12-11 | 广东也乐新材料制造有限公司 | Preparation method and application of odorless water-dispersible polyisocyanate |
| CN112662353A (en) * | 2020-12-07 | 2021-04-16 | 浙江农林大学 | Surface wetting type phenolic resin adhesive for bamboo materials such as bamboo green, bamboo yellow and the like and synthetic method thereof |
| CN112662353B (en) * | 2020-12-07 | 2022-08-05 | 浙江农林大学 | Surface wetting type phenolic resin adhesive for bamboo materials such as bamboo green, bamboo yellow and the like and synthetic method thereof |
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