CN108841305A - A kind of preparation method of high fire-retardance impact resistance polyurethane Composite Coating - Google Patents
A kind of preparation method of high fire-retardance impact resistance polyurethane Composite Coating Download PDFInfo
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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
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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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
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3225—Polyamines
- C08G18/3228—Polyamines acyclic
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- 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
- C08G18/62—Polymers of compounds having carbon-to-carbon double bonds
- C08G18/6216—Polymers of alpha-beta ethylenically unsaturated carboxylic acids or of derivatives thereof
- C08G18/622—Polymers of esters of alpha-beta ethylenically unsaturated carboxylic acids
- C08G18/6225—Polymers of esters of acrylic or methacrylic acid
- C08G18/6229—Polymers of hydroxy groups containing esters of acrylic or methacrylic acid with aliphatic polyalcohols
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- 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
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a kind of preparation methods of high fire-retardance impact resistance polyurethane Composite Coating, include the following steps：Oligomeric polyols, 2,6-di-tert-butyl p-cresol, light stabilizer, defoaming agent and chitosan are mixed, aqueous polyisocyanates and catalyst is then added, is stirred to react, obtains material A；Material A is mixed with diamine chain stretching agent, trimethylolpropane, soybean lecithin and hydroxyethyl cellulose, is stirred, carbon fiber, nano rare earth, nanometer calcium carbonate, polyvinyl alcohol, paraffin and silane coupling agent is then added, stirring obtains material B；Material B is mixed with styrene-acrylic emulsion, hydroxyl polyacrylate dispersion, sodium lignin sulfonate, triethylamine, deionized water, is stirred, defoaming is stood, obtains high fire-retardance impact resistance polyurethane Composite Coating.The high fire-retardance impact resistance polyurethane Composite Coating has excellent anti-flammability, splitting resistance and impact resistance, while also having good levelability, richness and the performances such as ageing-resistant.
Description
Technical field
The present invention relates to technical field of coatings more particularly to a kind of preparations of high fire-retardance impact resistance polyurethane Composite Coating
Method.
Background technique
Coating occupies an important position in chemical industry, develops in certain journey as a kind of multi-functional engineering material
A National Industrial development level can be measured on degree.Since aqueous polyurethane coating takes water as a solvent, compared to traditional coating
Generally using organic solvent as reactive diluent, the volatile organic compounds such as a large amount of benzene, formaldehyde will not be released after construction
(VOC), environmental pollution is small, and environment protecting is good, to be widely used.But there are still anti-flammabilitys, anti-for current polyurethane coating
The defect of cracking behavior and poor impact resistance limits the use of polyurethane coating.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of compound paintings of high fire-retardance impact resistance polyurethane
The preparation method of material with excellent anti-flammability, splitting resistance and impact resistance, while also having good levelability, rich
Full scale and the performances such as ageing-resistant.
A kind of preparation method of high fire-retardance impact resistance polyurethane Composite Coating proposed by the present invention, includes the following steps：
S1, by oligomeric polyols, 2,6-di-tert-butyl p-cresol, light stabilizer, defoaming agent and chitosan mix, then plus
Enter aqueous polyisocyanates and catalyst, be stirred to react, obtains material A；
S2, material A is mixed with diamine chain stretching agent, trimethylolpropane, soybean lecithin and hydroxyethyl cellulose, is stirred,
Then carbon fiber, nano rare earth, nanometer calcium carbonate, polyvinyl alcohol, paraffin and silane coupling agent is added, stirring obtains material B；
S3, by material B and styrene-acrylic emulsion, hydroxyl polyacrylate dispersion, sodium lignin sulfonate, triethylamine, deionization
Water mixing, stirring stand defoaming, obtain high fire-retardance impact resistance polyurethane Composite Coating.
Preferably, in S1, under the speed conditions of 200-400r/min, by weight by 100-150 parts of oligomeric polyols,
0.5-1 parts of 2,6-di-tert-butyl p-cresol, 0.2-0.8 parts of light stabilizers, 0.5-1 parts of defoaming agents and 2-4 parts of chitosan mixing, so
50-100 parts of aqueous polyisocyanates and 0.2-0.7 parts of catalyst are added afterwards, regulation system temperature is 75-85 DEG C, in 400-
3-4h is reacted under the mixing speed of 500r/min, obtains material A.
Preferably, in S1, the raw material of oligomeric polyols includes by weight：60-100 parts of polyether polyol, polyester polyols
25-50 parts of alcohol.
Preferably, in S1, the molecular weight of oligomeric polyols is 500-3650.
Preferably, in S1, the raw material of catalyst includes by weight：2-5 parts of N, N- dimethyl cyclohexyl amine, dimethyleyelohexane
1-2 parts of amine.
Preferably, in S2, by weight by 100-200 parts of material As and 3-8 parts of diamine chain stretching agents, 1-2.5 parts of trihydroxy methyls
Propane, 2-4 part soybean lecithin and 2-5 parts of hydroxyethyl cellulose mixing, in 65-75 DEG C of stirring 1.5-2.5h, then 1-3 parts of addition
Carbon fiber, 2-4 part nano rare earth, 0.5-1.5 parts of nanometer calcium carbonates, 2-5 parts of polyvinyl alcohol, 2-4 parts of paraffin and 0.5-1 parts of silane
Coupling agent stirs 1-1.5h under the revolving speed of 400-500r/min, obtains material B.
Preferably, in S2, diamine chain stretching agent is prepared by following technique：By the chloro- 3- nitro-trifluoromethyl toluene of 4-, dibromo fourth
Enediol, natrium carbonicum calcinatum and n,N-Dimethylformamide mixing, heating stirring are tied again after removing n,N-Dimethylformamide
Crystalline substance, it is dry, obtain material A；Material A is mixed with active carbon, sodium disulfide, Iron trichloride hexahydrate and propylene glycol monomethyl ether, is stirred, warp
Purification is dried in vacuo, and sieving obtains diamine chain stretching agent.
Preferably, in S2, diamine chain stretching agent is prepared by following technique：By weight by the chloro- 3- nitro of 20-30 parts of 4-
Benzotrifluoride, 10-15 parts of dibromo butene glycol, 4-8 parts of natrium carbonicum calcinatums and 120-180 parts of n,N-Dimethylformamide mixing,
It is warming up to 90-100 DEG C of stirring 6-8h, is recrystallized after removing n,N-Dimethylformamide, vacuum is dry under the conditions of 70-80 DEG C of temperature
It is dry, obtain material A；By weight by 25-30 parts of material As and 2-3 parts of active carbons, 0.1-0.4 parts of sodium disulfides, 0.2-1 part six
Water iron chloride and 60-80 parts of propylene glycol monomethyl ether mixing, stir 6-8h under the conditions of 80-95 DEG C of temperature, purified, at 85-90 DEG C
It is dried in vacuo under the conditions of temperature, crosses 150-200 mesh and handle to obtain diamine chain stretching agent.
In above-mentioned diamine chain stretching agent, by the way that response parameter is rationally arranged, make active hydrogen in dibromo butene glycol hydroxyl with
Chlorine element in the chloro- 3- nitro-trifluoromethyl toluene of 4- occurs replacement reaction and is grafted both to make, and fluorine is had in the material A made
Element and bromo element, and both ends have nitro, then by optimization S2 step, nitro are made to be reduced into amino, and diamines obtained expands
Chain agent has many advantages, such as good compatibility, dispersibility, anti-flammability and reactivity.
Preferably, in S3, material B, styrene-acrylic emulsion, hydroxyl polyacrylate dispersion, sodium lignin sulfonate, triethylamine it
Between weight ratio be 100-200:15-25:20-35:2-6:2-4.
By optimization preparation process in the present invention, parameter is rationally set, first by oligomeric polyols, 2,6- under stirring
Di-tert-butyl p-cresol, light stabilizer, defoaming agent and chitosan mix, each component good dispersion in system, in the work of catalyst
Under, oligomeric polyols react in the material A sufficiently obtained that ester group and ether content are reasonable with aqueous polyisocyanates, make this
Invention product has both water-fast, cold-resistant, heat-resisting and resistance to ag(e)ing, then with diamine chain stretching agent, trimethylolpropane, soybean lecithin, hydroxyl
As polyurethane in modifying agent, with material A grafting and cross-linking reaction occur for ethyl cellulose cooperation, are effectively improved the sky of polyurethane
Between structure, crosslink density is moderate, has unique stable tridimensional network, soft segment and hard section point in polyurethane molecular structure
Cloth is reasonable, and dispersibility is good with compatibility in system, then passes through addition carbon fiber, nano rare earth, nanometer calcium carbonate, polyethylene
Alcohol, paraffin and silane coupling agent, each component cooperate, and compatibility and good dispersion in system are effectively improved system of the present invention
The performances such as product film forming, anti-flammability, hardness, splitting resistance, impact resistance；Again by material B and styrene-acrylic emulsion, hydroxyl polypropylene
Acid esters lotion is compound, and compatibility is good, not only remains the excellent properties that respective component has, while to each other there is collaboration to make
With material B and the further graft crosslinking of hydroxyl polyacrylate dispersion further improve inventive article crosslink density and sky
Between structure, while overcoming the film forming of styrene-acrylic emulsion and the defect that poor water resistance and surface drying time are long, keep inventive article attached
Property, richness and glossiness it is good, curing time is reasonable, and environmental pollution is small, while having excellent anti-flammability, corrosion-resistant
Property, impact resistance and weatherability, also there is good levelability, thermal stability and mechanical property etc., be easy to form a film.The present invention mentions
The preparation method for having gone out a kind of high fire-retardance impact resistance polyurethane Composite Coating, with excellent anti-flammability, splitting resistance and
Impact resistance, while also there are good levelability, richness and the performances such as ageing-resistant.
The preparation method of the high fire-retardance impact resistance polyurethane Composite Coating proposed in the present invention is tested for the property,
Surface drying time is more than 28% in 1.2-1.8h, film flawless, and oxygen index (OI) in 25-40min, dry-hard time, will be of the invention high
Flame retardant high impact polyurethane Composite Coating, which is coated on sheet tin, forms 40-50 μm, carries out impact resistance according to ASTM2794 method
Property test, impact strength is more than 35kg.cm, and tensile strength is more than 6.5MPa, shows excellent anti-flammability and impact resistance, suitable
In production and application.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of high fire-retardance impact resistance polyurethane Composite Coating proposed by the present invention, includes the following steps：
S1, by oligomeric polyols, 2,6-di-tert-butyl p-cresol, light stabilizer, defoaming agent and chitosan mix, then plus
Enter aqueous polyisocyanates and catalyst, be stirred to react, obtains material A；
S2, material A is mixed with diamine chain stretching agent, trimethylolpropane, soybean lecithin and hydroxyethyl cellulose, is stirred,
Then carbon fiber, nano rare earth, nanometer calcium carbonate, polyvinyl alcohol, paraffin and silane coupling agent is added, stirring obtains material B；
S3, by material B and styrene-acrylic emulsion, hydroxyl polyacrylate dispersion, sodium lignin sulfonate, triethylamine, deionization
Water mixing, stirring stand defoaming, obtain high fire-retardance impact resistance polyurethane Composite Coating.
Embodiment 2
A kind of preparation method of high fire-retardance impact resistance polyurethane Composite Coating proposed by the present invention, includes the following steps：
S1, under the speed conditions of 200r/min, by weight by 100 parts of oligomeric polyols, 0.5 part of 2,6- di-t-butyl
Paracresol, 0.2 part of light stabilizer, 0.5 part of defoaming agent and the mixing of 2 parts of chitosans, be then added 50 parts of aqueous polyisocyanates and
0.2 part of catalyst, regulation system temperature are 75 DEG C, react 4h under the mixing speed of 400r/min, obtain material A；Wherein, low
The raw material of polyvalent alcohol includes by weight：60 parts of polyether polyol, 40 parts of polyester polyol；The raw material of catalyst is by weight
Including：2 parts of N, N- dimethyl cyclohexyl amine, 1 part of dimethyl cyclohexyl amine；
S2, by weight by 100 parts of material As and 3 parts of diamine chain stretching agents, 1 part of trimethylolpropane, 4 parts of soybean lecithins and 2
Then 1 part of carbon fiber, 2 parts of nano rare earths, 1.5 parts of nano-calcium carbonates is added in 65 DEG C of stirring 1.5h in part hydroxyethyl cellulose mixing
Calcium, 2 parts of polyvinyl alcohol, 2 parts of paraffin and 0.5 part of silane coupling agent, stir 1.5h under the revolving speed of 400r/min, obtain material B；
Wherein, diamine chain stretching agent is prepared by following technique：By the chloro- 3- nitro-trifluoromethyl toluene of 4-, dibromo butene glycol, Carbon Dioxide
Sodium and n,N-Dimethylformamide mixing, heating stirring recrystallize after removing n,N-Dimethylformamide, dry, obtain material
A；Material A is mixed with active carbon, sodium disulfide, Iron trichloride hexahydrate and propylene glycol monomethyl ether, is stirred, purified, vacuum drying, mistake
Sieve, obtains diamine chain stretching agent；
S3, by material B and styrene-acrylic emulsion, hydroxyl polyacrylate dispersion, sodium lignin sulfonate, triethylamine, deionization
Water mixing, stirring stand defoaming, obtain high fire-retardance impact resistance polyurethane Composite Coating；Wherein, material B, styrene-acrylic emulsion, contain
Hydroxy polyacrylate lotion, sodium lignin sulfonate, the weight ratio between triethylamine are 100:15:20:2:2.
Embodiment 3
A kind of preparation method of high fire-retardance impact resistance polyurethane Composite Coating proposed by the present invention, includes the following steps：
S1, under the speed conditions of 300r/min, by weight by 115 parts of oligomeric polyols, 0.8 part of 2,6- di-t-butyl
Paracresol, 0.5 part of light stabilizer, 0.8 part of defoaming agent and the mixing of 3 parts of chitosans, be then added 80 parts of aqueous polyisocyanates and
0.5 part of catalyst, regulation system temperature are 80 DEG C, react 3.5h under the mixing speed of 450r/min, obtain material A；Wherein,
The raw material of oligomeric polyols includes by weight：90 parts of polyether polyol, 25 parts of polyester polyol；The raw material of catalyst is by weight
Part include：4.5 parts of N, N- dimethyl cyclohexyl amine, 1.5 parts of dimethyl cyclohexyl amine；
S2, by weight by 150 parts of material As and 5 parts of diamine chain stretching agents, 1.5 parts of trimethylolpropanes, 3 parts of soybean lecithins
It is mixed with 4 parts of hydroxyethyl celluloses, in 70 DEG C of stirring 2h, 2 parts of carbon fibers, 3 parts of nano rare earths, 1 part of nano-calcium carbonate is then added
Calcium, 4 parts of polyvinyl alcohol, 3 parts of paraffin and 0.8 part of silane coupling agent, stir 1.2h under the revolving speed of 450r/min, obtain material B；
Wherein, diamine chain stretching agent is prepared by following technique：By weight by the chloro- 3- nitro-trifluoromethyl toluene of 25 parts of 4-, 12 parts of dibromos
Butylene glycol, 5.5 parts of natrium carbonicum calcinatums and 150 parts of n,N-Dimethylformamide mixing, are warming up to 95 DEG C of stirring 7h, remove N, N-
It is recrystallized after dimethylformamide, is dried in vacuo under the conditions of 75 DEG C of temperature, obtains material A；By weight by 28 parts of material As with
2.5 parts of active carbons, 0.2 part of sodium disulfide, 0.5 part of Iron trichloride hexahydrate and 70 parts of propylene glycol monomethyl ether mixing, in 88 DEG C of temperature conditions
Lower stirring 7h, it is purified, it is dried in vacuo under the conditions of 88 DEG C of temperature, crosses 180 meshes, obtain diamine chain stretching agent；
S3, by material B and styrene-acrylic emulsion, hydroxyl polyacrylate dispersion, sodium lignin sulfonate, triethylamine, deionization
Water mixing, stirring stand defoaming, obtain high fire-retardance impact resistance polyurethane Composite Coating；Wherein, material B, styrene-acrylic emulsion, contain
Hydroxy polyacrylate lotion, sodium lignin sulfonate, the weight ratio between triethylamine are 150:20:25:5:3.
Embodiment 4
A kind of preparation method of high fire-retardance impact resistance polyurethane Composite Coating proposed by the present invention, includes the following steps：
S1, under the speed conditions of 400r/min, by weight by 150 parts of oligomeric polyols, 1 part of 2,6- di-t-butyl pair
Cresols, 0.8 part of light stabilizer, 1 part of defoaming agent and 4 parts of chitosan mixing, are then added 100 parts of aqueous polyisocyanates and 0.7
Part catalyst, regulation system temperature are 85 DEG C, react 3h under the mixing speed of 500r/min, obtain material A；Wherein, oligomeric
The raw material of polyalcohol includes by weight：100 parts of polyether polyol, 50 parts of polyester polyol；The raw material of catalyst is by weight
Including：5 parts of N, N- dimethyl cyclohexyl amine, 2 parts of dimethyl cyclohexyl amine；
S2, by weight by 200 parts of material As and 8 parts of diamine chain stretching agents, 2.5 parts of trimethylolpropanes, 2 parts of soybean lecithins
It is mixed with 5 parts of hydroxyethyl celluloses, in 75 DEG C of stirring 2.5h, 3 parts of carbon fibers, 4 parts of nano rare earths, 1.5 parts of nanometers is then added
Calcium carbonate, 5 parts of polyvinyl alcohol, 4 parts of paraffin and 1 part of silane coupling agent, stir 1-1.5h under the revolving speed of 400-500r/min, obtain
To material B；Wherein, diamine chain stretching agent is prepared by following technique：By weight by the chloro- 3- nitro-trifluoromethyl toluene of 20 parts of 4-,
10 parts of dibromo butene glycol, 4 parts of natrium carbonicum calcinatums and 120 parts of n,N-Dimethylformamide mixing, are warming up to 90 DEG C of stirring 8h, remove
It is recrystallized after going n,N-Dimethylformamide, is dried in vacuo under the conditions of 70 DEG C of temperature, obtains material A；By weight by 25 parts
Material A is mixed with 3 parts of active carbons, 0.1 part of sodium disulfide, 0.2 part of Iron trichloride hexahydrate and 60 parts of propylene glycol monomethyl ethers, in 95 DEG C of temperature
Under the conditions of stir 6h, it is purified, be dried in vacuo under the conditions of 85 DEG C of temperature, cross 150 meshes, obtain diamine chain stretching agent；
S3, by material B and styrene-acrylic emulsion, hydroxyl polyacrylate dispersion, sodium lignin sulfonate, triethylamine, deionization
Water mixing, stirring stand defoaming, obtain high fire-retardance impact resistance polyurethane Composite Coating；Wherein, material B, styrene-acrylic emulsion, contain
Hydroxy polyacrylate lotion, sodium lignin sulfonate, the weight ratio between triethylamine are 200:25:35:6:4.
Embodiment 5
A kind of preparation method of high fire-retardance impact resistance polyurethane Composite Coating proposed by the present invention, includes the following steps：
S1, under the speed conditions of 350r/min, by weight by 140 parts of oligomeric polyols, 0.8 part of 2,6- di-t-butyl
Paracresol, 0.7 part of light stabilizer, 0.6 part of defoaming agent and 3.5 parts of chitosan mixing, are then added 90 parts of aqueous polyisocyanates
With 0.6 part of catalyst, regulation system temperature is 82 DEG C, reacts 3.2h under the mixing speed of 450r/min, obtains material A；Its
In, the raw material of oligomeric polyols includes by weight：95 parts of polyether polyol, 35 parts of polyester polyol；The raw material of catalyst is pressed
Parts by weight include：4 parts of N, N- dimethyl cyclohexyl amine, 1.5 parts of dimethyl cyclohexyl amine；
S2, by weight by 180 parts of material As and 6.5 parts of diamine chain stretching agents, 2 parts of trimethylolpropanes, 3.5 parts of soybean phosphorus
Rouge and 4 parts of hydroxyethyl celluloses mix, and in 72 DEG C of stirring 2.2h, 2.5 parts of carbon fibers, 3.5 parts of nano rare earths, 1.2 are then added
Part nanometer calcium carbonate, 4 parts of polyvinyl alcohol, 3.5 parts of paraffin and 0.8 part of silane coupling agent, are stirred under the revolving speed of 500r/min
1.2h obtains material B；Wherein, diamine chain stretching agent is prepared by following technique：By weight by the chloro- 3- nitrotrimethylolmethane of 30 parts of 4-
Toluene fluoride, 15 parts of dibromo butene glycol, 8 parts of natrium carbonicum calcinatums and 180 parts of n,N-Dimethylformamide mixing, are warming up to 100 DEG C
6h is stirred, is recrystallized after removing n,N-Dimethylformamide, is dried in vacuo under the conditions of 80 DEG C of temperature, obtains material A；By weight
Part mixes 30 parts of material As with 2 parts of active carbons, 0.4 part of sodium disulfide, 1 part of Iron trichloride hexahydrate and 80 parts of propylene glycol monomethyl ethers, 80
Stir 8h under the conditions of DEG C temperature, it is purified, be dried in vacuo under the conditions of 90 DEG C of temperature, cross 200 meshes, obtain diamine chain stretching agent；
S3, by material B and styrene-acrylic emulsion, hydroxyl polyacrylate dispersion, sodium lignin sulfonate, triethylamine, deionization
Water mixing, stirring stand defoaming, obtain high fire-retardance impact resistance polyurethane Composite Coating；Wherein, material B, styrene-acrylic emulsion, contain
Hydroxy polyacrylate lotion, sodium lignin sulfonate, the weight ratio between triethylamine are 180:22:25:3:3.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of high fire-retardance impact resistance polyurethane Composite Coating, which is characterized in that include the following steps：
S1, oligomeric polyols, 2,6-di-tert-butyl p-cresol, light stabilizer, defoaming agent and chitosan are mixed, water is then added
Property polyisocyanates and catalyst, are stirred to react, obtain material A；
S2, material A is mixed with diamine chain stretching agent, trimethylolpropane, soybean lecithin and hydroxyethyl cellulose, is stirred, then
Carbon fiber, nano rare earth, nanometer calcium carbonate, polyvinyl alcohol, paraffin and silane coupling agent is added, stirring obtains material B；
S3, material B and styrene-acrylic emulsion, hydroxyl polyacrylate dispersion, sodium lignin sulfonate, triethylamine, deionized water are mixed
It closes, stirring stands defoaming, obtains high fire-retardance impact resistance polyurethane Composite Coating.
2. the preparation method of high fire-retardance impact resistance polyurethane Composite Coating according to claim 1, which is characterized in that S1
In, under the speed conditions of 200-400r/min, by weight by 100-150 parts of oligomeric polyols, 0.5-1 part 2, the tertiary fourth of 6- bis-
Base paracresol, 0.2-0.8 part light stabilizer, 0.5-1 parts of defoaming agents and 2-4 parts of chitosan mixing, are then added 50-100 parts of water
Property polyisocyanates and 0.2-0.7 parts of catalyst, regulation system temperature is 75-85 DEG C, in the mixing speed of 400-500r/min
Lower reaction 3-4h, obtains material A.
3. the preparation method of high fire-retardance impact resistance polyurethane Composite Coating according to claim 1 or claim 2, which is characterized in that
In S1, the raw material of oligomeric polyols includes by weight：60-100 parts of polyether polyol, 25-50 parts of polyester polyol.
4. the preparation method of high fire-retardance impact resistance polyurethane Composite Coating described in any one of -3 according to claim 1, special
Sign is, in S1, the molecular weight of oligomeric polyols is 500-3650.
5. the preparation method of high fire-retardance impact resistance polyurethane Composite Coating described in any one of -4 according to claim 1, special
Sign is, in S1, the raw material of catalyst includes by weight：2-5 parts of N, N- dimethyl cyclohexyl amine, 1-2 parts of dimethyl cyclohexyl amine.
6. the preparation method of high fire-retardance impact resistance polyurethane Composite Coating described in any one of -5 according to claim 1, special
Sign is, in S2, by weight by 100-200 parts of material As and 3-8 parts of diamine chain stretching agents, 1-2.5 parts of trimethylolpropanes, 2-4
Part soybean lecithin and 2-5 part hydroxyethyl celluloses mixing, in 65-75 DEG C of stirring 1.5-2.5h, then 1-3 parts of carbon fibers of addition,
2-4 parts of nano rare earths, 0.5-1.5 parts of nanometer calcium carbonates, 2-5 parts of polyvinyl alcohol, 2-4 parts of paraffin and 0.5-1 parts of silane coupling agents,
1-1.5h is stirred under the revolving speed of 400-500r/min, obtains material B.
7. the preparation method of high fire-retardance impact resistance polyurethane Composite Coating described in any one of -6 according to claim 1, special
Sign is, in S2, diamine chain stretching agent is prepared by following technique：By the chloro- 3- nitro-trifluoromethyl toluene of 4-, dibromo butene glycol,
Natrium carbonicum calcinatum and n,N-Dimethylformamide mixing, heating stirring recrystallize after removing n,N-Dimethylformamide, dry,
Obtain material A；Material A is mixed with active carbon, sodium disulfide, Iron trichloride hexahydrate and propylene glycol monomethyl ether, is stirred, it is purified, very
Sky is dry, and sieving obtains diamine chain stretching agent.
8. the preparation method of high fire-retardance impact resistance polyurethane Composite Coating described in any one of -7 according to claim 1, special
Sign is, in S2, diamine chain stretching agent is prepared by following technique：By weight by the chloro- 3- nitro fluoroform of 20-30 parts of 4-
Benzene, 10-15 parts of dibromo butene glycol, 4-8 parts of natrium carbonicum calcinatums and 120-180 parts of n,N-Dimethylformamide mixing, are warming up to
90-100 DEG C of stirring 6-8h is recrystallized after removing n,N-Dimethylformamide, is dried in vacuo, obtains under the conditions of 70-80 DEG C of temperature
To material A；By weight by 25-30 parts of material As and 2-3 parts of active carbons, 0.1-0.4 parts of sodium disulfides, the six water chlorination of 0.2-1 part
Iron and 60-80 parts of propylene glycol monomethyl ether mixing, stir 6-8h under the conditions of 80-95 DEG C of temperature, purified, in 85-90 DEG C of temperature strip
It is dried in vacuo under part, crosses 150-200 mesh and handle to obtain diamine chain stretching agent.
9. the preparation method of high fire-retardance impact resistance polyurethane Composite Coating described in any one of -8 according to claim 1, special
Sign is, in S3, material B, styrene-acrylic emulsion, hydroxyl polyacrylate dispersion, sodium lignin sulfonate, the weight between triethylamine
Than for 100-200:15-25:20-35:2-6:2-4.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112746506A (en) * | 2021-01-20 | 2021-05-04 | 浙江麦斯特姆涂布有限公司 | Stain-resistant artificial leather with high skin-permeable feeling and preparation method thereof |
| CN115181232A (en) * | 2022-08-11 | 2022-10-14 | 中国科学院赣江创新研究院 | Polyurethane material and preparation method and application thereof |
| CN116253860A (en) * | 2023-03-21 | 2023-06-13 | 南通百川新材料有限公司 | Synthesis method of self-lubricating polyurethane insulating resin |
-
2018
- 2018-04-25 CN CN201810378315.8A patent/CN108841305A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112746506A (en) * | 2021-01-20 | 2021-05-04 | 浙江麦斯特姆涂布有限公司 | Stain-resistant artificial leather with high skin-permeable feeling and preparation method thereof |
| CN115181232A (en) * | 2022-08-11 | 2022-10-14 | 中国科学院赣江创新研究院 | Polyurethane material and preparation method and application thereof |
| CN115181232B (en) * | 2022-08-11 | 2023-11-07 | 中国科学院赣江创新研究院 | Polyurethane material and preparation method and application thereof |
| CN116253860A (en) * | 2023-03-21 | 2023-06-13 | 南通百川新材料有限公司 | Synthesis method of self-lubricating polyurethane insulating resin |
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