CN110358492A - A kind of aqueous polyurethane flame-retardant adhesive and preparation method thereof - Google Patents
A kind of aqueous polyurethane flame-retardant adhesive and preparation method thereof Download PDFInfo
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- CN110358492A CN110358492A CN201910708591.0A CN201910708591A CN110358492A CN 110358492 A CN110358492 A CN 110358492A CN 201910708591 A CN201910708591 A CN 201910708591A CN 110358492 A CN110358492 A CN 110358492A
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- diisocyanate
- aqueous polyurethane
- ammonium polyphosphate
- polyurethane flame
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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
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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- 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
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
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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
- C08G18/48—Polyethers
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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
- C08G18/65—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
- C08G18/6603—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6607—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- 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
- C08G18/6603—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6607—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
- C08G18/6611—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 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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- 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
- C08G18/6625—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/34
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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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/73—Polyisocyanates or polyisothiocyanates 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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/06—Polyurethanes from polyesters
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/08—Polyurethanes from polyethers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- Chemical & Material Sciences (AREA)
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The present invention provides a kind of aqueous polyurethane flame-retardant adhesives and preparation method thereof, it is related to adhesive field, it is prepared by the raw material of following weight fraction: 30-40 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 10-18 parts of 4- diisocyanate, 5-10 parts of poly adipate succinic acid ester, 2, 20-30 parts of 2- bis- (methylol) propionic acid, 12-16 parts of polytetrahydrofuran ether glycol, 1-1.5 parts of trimethylolpropane, 0.1-0.5 parts of dibutyl tin dilaurate, 0.1-0.5 parts of stannous octoate, 4-8 parts of diglycol, 2-5 parts of bismaleimide, 10-20 parts of acetone, 1-2 parts of triethanolamine, 6-10 parts of sodium-based montmorillonite, 15-23 parts of melamine coated ammonium polyphosphate, 2-3 parts of plasticizer, 1-3 parts of thixotropic agent, 10-15 parts of deionized water, aqueous polyurethane flame-retardant adhesive of the present invention has extremely excellent mechanical property, and flame retardant rating is high, has broad application prospects and economic benefit.
Description
Technical field
The present invention relates to adhesive fields, and in particular to a kind of aqueous polyurethane flame-retardant adhesive and preparation method thereof.
Background technique
It is glued (bonding, bonding, cementing, gluing) and refers to the skill that homogeneous or heterogeneous surface is linked together with adhesive
The features such as art has stress distribution continuous, light-weight, or sealing, most technological temperatures are low.It is glued especially suitable for different materials
The connection of matter, different-thickness, ultra-thin specification and complex component.Splicing RECENT DEVELOPMENTS is most fast, and application industry is extremely wide.Point of adhesive
There are many class method, can be divided into thermoset, hot melt, room temperature curing type, pressure sensitive etc. by application method；It is divided into knot by application
Configuration, non-configuration or special gelatin；Water-soluble, emulsion type, solvent type and various solid-state versions etc. can be divided by connecing form.Synthesis chemistry
Worker often likes classifying adhesive by the chemical component of sizing.
Volatile organic compounds (VOC) in adhesive there are more, such as the organic solvent in solvent type adhesive, three
Free formaldehyde in aldehyde glue (phenolic aldehyde, ureaformaldehyde, melamino-formaldehyde), the styrene in unsaturated polyester (UP) adhesive, acrylate
Unreacted monomer in lotion adhesive, the methyl methacrylate in the fast fixing structure adhesive of modification acrylate, alpha-cyano
SO in acrylate adhesive2, methanol, the thickener ammonium hydroxide in acrylic acid ester emulsion etc. in 4115 building adhesives.These are easily
Volatile substance is discharged into atmosphere, endanger it is very big, and some occur photochemical action, generate ozone, low layer space it is smelly
Oxygen contamination atmosphere, influences the growth of biology and the health of the mankind, some halogenated hydrocarbon solvents are then the substances for destroying atmospheric ozone layer.
Some aromatic hydrocarbon solvent toxicity are very big, or even have carcinogenicity.The steam of benzene has fragranced, but to people's strong toxicity again, inhales
Enter and can all be poisoned through skin absorption, make one dizziness, headache, it is out of strength, serious when it is dead due to respiratory center spasm.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of aqueous polyurethane flame-retardant adhesives and preparation method thereof.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of aqueous polyurethane flame-retardant adhesive, is prepared by the raw material of following weight fraction:
30-40 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 10-18 parts of 4- diisocyanate, poly adipate succinic acid ester
5-10 parts, 20-30 parts of 2,2- bis- (methylol) propionic acid, 12-16 parts of polytetrahydrofuran ether glycol, 1-1.5 parts of trimethylolpropane,
0.1-0.5 parts of dibutyl tin dilaurate, 0.1-0.5 parts of stannous octoate, 4-8 parts of diglycol, bismaleimide 2-5
Part, 10-20 parts of acetone, 1-2 parts of triethanolamine, 6-10 parts of sodium-based montmorillonite, 15-23 parts of melamine coated ammonium polyphosphate, plasticizer
2-3 parts, 1-3 parts of thixotropic agent, 10-15 parts of deionized water.
Further, it is prepared by the raw material of following weight fraction:
32 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 13 parts of 4- diisocyanate, 8 parts of poly adipate succinic acid ester, 2,
Bis- 25 parts of (methylol) propionic acid of 2-, 14 parts of polytetrahydrofuran ether glycol, 1 part of trimethylolpropane, dibutyl tin dilaurate 0.3
Part, 0.1 part of stannous octoate, 6 parts of diglycol, 4 parts of bismaleimide, 10 parts of acetone, 2 parts of triethanolamine, sodium base cover
De- soil 7 parts, 18 parts of melamine coated ammonium polyphosphate, 3 parts of plasticizer, 2 parts of thixotropic agent, 12 parts of deionized water.
Further, it is prepared by the raw material of following weight fraction:
40 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 16 parts of 4- diisocyanate, 5 parts of poly adipate succinic acid ester, 2,
Bis- 22 parts of (methylol) propionic acid of 2-, 16 parts of polytetrahydrofuran ether glycol, 1.5 parts of trimethylolpropane, dibutyl tin dilaurate
0.4 part, 0.1 part of stannous octoate, 5 parts of diglycol, 3 parts of bismaleimide, 13 parts of acetone, 1 part of triethanolamine, sodium base
8 parts of montmorillonite, 18 parts of melamine coated ammonium polyphosphate, 3 parts of plasticizer, 3 parts of thixotropic agent, 12 parts of deionized water.
Further, the melamine coated ammonium polyphosphate the preparation method is as follows:
Melamine resin is add to deionized water, drips certain density phosphoric acid after being warming up to 40-50 DEG C of stirring and dissolving
It adds into drop is warming up to 80-90 DEG C of reaction 1-3h after finishing, ammonium polyphosphate is added again after filtering for heat, naturally cold after stirring 1-5h
But it is filtered to room temperature, vacuum drying is the melamine coated ammonium polyphosphate after filter cake washing.
Further, the mass concentration of the phosphoric acid is 80-85%.
Further, the plasticizer is di-n-octyl phthalate, BBP(Butyl Benzyl Phthalate, phthalic acid two
Secondary monooctyl ester, dicyclohexyl phthalate, dibutyl phthalate, diisobutyl phthalate, phthalic acid diformazan
Ester, diethyl phthalate, diisononyl phthalate, any one or more group in diisooctyl phthalate
It closes.
Further, the thixotropic agent is that organobentonite and polyamide wax 1:1 in mass ratio are mixed.
Above-mentioned aqueous polyurethane flame-retardant adhesive the preparation method is as follows:
(1) melamine coated ammonium polyphosphate is added to deionized water, in acetone, ultrasonic vibration disperses 5-15min；
(2) by isophorone diisocyanate, Toluene-2,4-diisocyanate, 4- diisocyanate is added, and is warming up to 60-80 DEG C of reaction 2-
5h obtains prepolymer, by prepolymer vacuum outgas；
(3) again by bis- (methylol) propionic acid of poly adipate succinic acid ester, 2,2-, polytetrahydrofuran ether glycol, trihydroxy methyl
Propane, dibutyl tin dilaurate, stannous octoate, diglycol, bismaleimide, triethanolamine, sodium-based montmorillonite,
Plasticizer, thixotropic agent are added, and are injected into flat-die after reacting 40-60min, 90-100 DEG C of reaction 10-20min.
(3) beneficial effect
The present invention provides a kind of aqueous polyurethane flame-retardant adhesives and preparation method thereof, have the advantages that
Isophorone diisocyanate of the invention, Toluene-2,4-diisocyanate, the polyurethane that 4- diisocyanate generates can be free
Twining movement, and certain rigidity has also been introduced in the presence of phenyl so that the glue film of adhesive can obtain simultaneously it is biggish
Tensile strength and elongation at break, 2,2- bis- (methylol) propionic acid are introduced as chain extender, further improve the friendship of adhesive
Join density, improves intensity, and the conduct of methylol also gives the biggish toughness of glue film, is not easily susceptible to cracking after solidification, it is close
Amine coated ammonium polyphosphate has composite flame-retardant agent, more preferable compared to halogen flame flame retardant effect, and when burning is pollution-free to be produced
Raw toxic and harmful gas, by specifically testing it is found that aqueous polyurethane flame-retardant adhesive of the present invention has extremely excellent mechanical property
Can, and flame retardant rating is high, has broad application prospects and economic benefit.
Detailed description of the invention
Fig. 1 is preparation method flow chart of the present invention.
Specific embodiment
Embodiment 1:
A kind of aqueous polyurethane flame-retardant adhesive, is prepared by the raw material of following weight fraction:
32 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 13 parts of 4- diisocyanate, 8 parts of poly adipate succinic acid ester, 2,
Bis- 25 parts of (methylol) propionic acid of 2-, 14 parts of polytetrahydrofuran ether glycol, 1 part of trimethylolpropane, dibutyl tin dilaurate 0.3
Part, 0.1 part of stannous octoate, 6 parts of diglycol, 4 parts of bismaleimide, 10 parts of acetone, 2 parts of triethanolamine, sodium base cover
De- 7 parts of soil, 18 parts of melamine coated ammonium polyphosphate, 3 parts of plasticizer phthalic acid di-n-octyl, organobentonite and polyamide wax
2 parts of thixotropic agent that 1:1 in mass ratio is mixed, 12 parts of deionized water.
Melamine coated ammonium polyphosphate the preparation method is as follows:
Melamine resin is add to deionized water, the phosphoric acid for being 80% by mass concentration after 45 DEG C of stirring and dissolvings is warming up to
It is added dropwise and enters, drop is warming up to 90 DEG C of reaction 2h after finishing, ammonium polyphosphate is added again after filtering for heat, naturally cools to room after stirring 4h
Temperature filters, and vacuum drying is the melamine coated ammonium polyphosphate after filter cake washing.
Above-mentioned aqueous polyurethane flame-retardant adhesive the preparation method is as follows:
(1) melamine coated ammonium polyphosphate is added to deionized water, in acetone, ultrasonic vibration disperses 12min；
(2) by isophorone diisocyanate, Toluene-2,4-diisocyanate, 4- diisocyanate is added, is warming up to 70 DEG C of reaction 3h, obtains
Prepolymer, by prepolymer vacuum outgas；
(3) again by bis- (methylol) propionic acid of poly adipate succinic acid ester, 2,2-, polytetrahydrofuran ether glycol, trihydroxy methyl
Propane, dibutyl tin dilaurate, stannous octoate, diglycol, bismaleimide, triethanolamine, sodium-based montmorillonite,
Plasticizer, thixotropic agent are added, and are injected into flat-die after reacting 50min, 95 DEG C of reaction 15min.
Embodiment 2:
A kind of aqueous polyurethane flame-retardant adhesive, is prepared by the raw material of following weight fraction:
40 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 16 parts of 4- diisocyanate, 5 parts of poly adipate succinic acid ester, 2,
Bis- 22 parts of (methylol) propionic acid of 2-, 16 parts of polytetrahydrofuran ether glycol, 1.5 parts of trimethylolpropane, dibutyl tin dilaurate
0.4 part, 0.1 part of stannous octoate, 5 parts of diglycol, 3 parts of bismaleimide, 13 parts of acetone, 1 part of triethanolamine, sodium base
8 parts of montmorillonite, 18 parts of melamine coated ammonium polyphosphate, 3 parts of plasticizer phthalic acid dicyclohexyl maleate, organobentonite and polyamide
3 parts of thixotropic agent that wax 1:1 in mass ratio is mixed, 12 parts of deionized water.
Melamine coated ammonium polyphosphate the preparation method is as follows:
Melamine resin is add to deionized water, the phosphoric acid for being 85% by mass concentration after 40 DEG C of stirring and dissolvings is warming up to
It is added dropwise and enters, drop is warming up to 85 DEG C of reaction 1.5h after finishing, ammonium polyphosphate is added again after filtering for heat, naturally cools to after stirring 5h
Room temperature filters, and vacuum drying is the melamine coated ammonium polyphosphate after filter cake washing.
Above-mentioned aqueous polyurethane flame-retardant adhesive the preparation method is as follows:
(1) melamine coated ammonium polyphosphate is added to deionized water, in acetone, ultrasonic vibration disperses 10min；
(2) by isophorone diisocyanate, Toluene-2,4-diisocyanate, 4- diisocyanate is added, is warming up to 70 DEG C of reaction 5h, obtains
Prepolymer, by prepolymer vacuum outgas；
(3) again by bis- (methylol) propionic acid of poly adipate succinic acid ester, 2,2-, polytetrahydrofuran ether glycol, trihydroxy methyl
Propane, dibutyl tin dilaurate, stannous octoate, diglycol, bismaleimide, triethanolamine, sodium-based montmorillonite,
Plasticizer, thixotropic agent are added, and are injected into flat-die after reacting 40min, 95 DEG C of reaction 15min.
Embodiment 3:
A kind of aqueous polyurethane flame-retardant adhesive, is prepared by the raw material of following weight fraction:
35 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 16 parts of 4- diisocyanate, 5 parts of poly adipate succinic acid ester, 2,
Bis- 25 parts of (methylol) propionic acid of 2-, 12 parts of polytetrahydrofuran ether glycol, 1 part of trimethylolpropane, dibutyl tin dilaurate 0.1
Part, 0.2 part of stannous octoate, 5 parts of diglycol, 2 parts of bismaleimide, 20 parts of acetone, 1 part of triethanolamine, sodium base cover
De- 8 parts of soil, 18 parts of melamine coated ammonium polyphosphate, 2 parts of plasticizer phthalic acid butyl benzyl, organobentonite and polyamide wax are pressed
2 parts of thixotropic agent that mass ratio 1:1 is mixed, 14 parts of deionized water.
Melamine coated ammonium polyphosphate the preparation method is as follows:
Melamine resin is add to deionized water, the phosphoric acid for being 85% by mass concentration after 40 DEG C of stirring and dissolvings is warming up to
It is added dropwise and enters, drop is warming up to 85 DEG C of reaction 2h after finishing, ammonium polyphosphate is added again after filtering for heat, naturally cools to room after stirring 5h
Temperature filters, and vacuum drying is the melamine coated ammonium polyphosphate after filter cake washing.
Above-mentioned aqueous polyurethane flame-retardant adhesive the preparation method is as follows:
(1) melamine coated ammonium polyphosphate is added to deionized water, in acetone, ultrasonic vibration disperses 15min；
(2) by isophorone diisocyanate, Toluene-2,4-diisocyanate, 4- diisocyanate is added, is warming up to 65 DEG C of reaction 5h, obtains
Prepolymer, by prepolymer vacuum outgas；
(3) again by bis- (methylol) propionic acid of poly adipate succinic acid ester, 2,2-, polytetrahydrofuran ether glycol, trihydroxy methyl
Propane, dibutyl tin dilaurate, stannous octoate, diglycol, bismaleimide, triethanolamine, sodium-based montmorillonite,
Plasticizer, thixotropic agent are added, and are injected into flat-die after reacting 50min, 90 DEG C of reaction 10min.
Embodiment 4:
A kind of aqueous polyurethane flame-retardant adhesive, is prepared by the raw material of following weight fraction:
30 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 10 parts of 4- diisocyanate, 5 parts of poly adipate succinic acid ester, 2,
Bis- 20 parts of (methylol) propionic acid of 2-, 12 parts of polytetrahydrofuran ether glycol, 1 part of trimethylolpropane, dibutyl tin dilaurate 0.1
Part, 0.1 part of stannous octoate, 4 parts of diglycol, 2 parts of bismaleimide, 10 parts of acetone, 1 part of triethanolamine, sodium base cover
De- 6 parts of soil, 15 parts of melamine coated ammonium polyphosphate, 2 parts of plasticizer phthalic acid dibutyl ester, organobentonite and polyamide wax are pressed
1 part of thixotropic agent that mass ratio 1:1 is mixed, 10 parts of deionized water.
Melamine coated ammonium polyphosphate the preparation method is as follows:
Melamine resin is add to deionized water, the phosphoric acid for being 80% by mass concentration after 40 DEG C of stirring and dissolvings is warming up to
It is added dropwise and enters, drop is warming up to 80 DEG C of reaction 1h after finishing, ammonium polyphosphate is added again after filtering for heat, naturally cools to room after stirring 1h
Temperature filters, and vacuum drying is the melamine coated ammonium polyphosphate after filter cake washing.
Above-mentioned aqueous polyurethane flame-retardant adhesive the preparation method is as follows:
(1) melamine coated ammonium polyphosphate is added to deionized water, in acetone, ultrasonic vibration disperses 5min；
(2) by isophorone diisocyanate, Toluene-2,4-diisocyanate, 4- diisocyanate is added, is warming up to 60 DEG C of reaction 2h, obtains
Prepolymer, by prepolymer vacuum outgas；
(3) again by bis- (methylol) propionic acid of poly adipate succinic acid ester, 2,2-, polytetrahydrofuran ether glycol, trihydroxy methyl
Propane, dibutyl tin dilaurate, stannous octoate, diglycol, bismaleimide, triethanolamine, sodium-based montmorillonite,
Plasticizer, thixotropic agent are added, and are injected into flat-die after reacting 40min, 90 DEG C of reaction 10min.
Embodiment 5:
A kind of aqueous polyurethane flame-retardant adhesive, is prepared by the raw material of following weight fraction:
40 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 18 parts of 4- diisocyanate, 10 parts of poly adipate succinic acid ester,
Bis- 30 parts of (methylol) propionic acid of 2,2-, 16 parts of polytetrahydrofuran ether glycol, 1.5 parts of trimethylolpropane, di lauric dibutyl
0.5 part of tin, 0.5 part of stannous octoate, 8 parts of diglycol, 5 parts of bismaleimide, 20 parts of acetone, 2 parts of triethanolamine, sodium
10 parts of base montmorillonite, 23 parts of melamine coated ammonium polyphosphate, 3 parts of plasticizer phthalic acid diethylester, organobentonite and polyamides
3 parts of thixotropic agent that amine wax 1:1 in mass ratio is mixed, 15 parts of deionized water.
Melamine coated ammonium polyphosphate the preparation method is as follows:
Melamine resin is add to deionized water, the phosphoric acid for being 85% by mass concentration after 50 DEG C of stirring and dissolvings is warming up to
It is added dropwise and enters, drop is warming up to 90 DEG C of reaction 3h after finishing, ammonium polyphosphate is added again after filtering for heat, naturally cools to room after stirring 5h
Temperature filters, and vacuum drying is the melamine coated ammonium polyphosphate after filter cake washing.
Above-mentioned aqueous polyurethane flame-retardant adhesive the preparation method is as follows:
(1) melamine coated ammonium polyphosphate is added to deionized water, in acetone, ultrasonic vibration disperses 15min；
(2) by isophorone diisocyanate, Toluene-2,4-diisocyanate, 4- diisocyanate is added, is warming up to 80 DEG C of reaction 5h, obtains
Prepolymer, by prepolymer vacuum outgas；
(3) again by bis- (methylol) propionic acid of poly adipate succinic acid ester, 2,2-, polytetrahydrofuran ether glycol, trihydroxy methyl
Propane, dibutyl tin dilaurate, stannous octoate, diglycol, bismaleimide, triethanolamine, sodium-based montmorillonite,
Plasticizer, thixotropic agent are added, and are injected into flat-die after reacting 60min, 100 DEG C of reaction 20min.
Embodiment 6:
A kind of aqueous polyurethane flame-retardant adhesive, is prepared by the raw material of following weight fraction:
30 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 18 parts of 4- diisocyanate, 5 parts of poly adipate succinic acid ester, 2,
Bis- 30 parts of (methylol) propionic acid of 2-, 12 parts of polytetrahydrofuran ether glycol, 1.5 parts of trimethylolpropane, dibutyl tin dilaurate
0.1 part, 0.5 part of stannous octoate, 4 parts of diglycol, 5 parts of bismaleimide, 10 parts of acetone, 2 parts of triethanolamine, sodium base
6 parts of montmorillonite, 23 parts of melamine coated ammonium polyphosphate, 2 parts of plasticizer phthalic acid dinonyl, organobentonite and polyamide
3 parts of thixotropic agent that wax 1:1 in mass ratio is mixed, 10 parts of deionized water.
Melamine coated ammonium polyphosphate the preparation method is as follows:
Melamine resin is add to deionized water, the phosphoric acid for being 80% by mass concentration after 50 DEG C of stirring and dissolvings is warming up to
It is added dropwise and enters, drop is warming up to 90 DEG C of reaction 1h after finishing, ammonium polyphosphate is added again after filtering for heat, naturally cools to room after stirring 5h
Temperature filters, and vacuum drying is the melamine coated ammonium polyphosphate after filter cake washing.
Above-mentioned aqueous polyurethane flame-retardant adhesive the preparation method is as follows:
(1) melamine coated ammonium polyphosphate is added to deionized water, in acetone, ultrasonic vibration disperses 5min；
(2) by isophorone diisocyanate, Toluene-2,4-diisocyanate, 4- diisocyanate is added, is warming up to 80 DEG C of reaction 2h, obtains
Prepolymer, by prepolymer vacuum outgas；
(3) again by bis- (methylol) propionic acid of poly adipate succinic acid ester, 2,2-, polytetrahydrofuran ether glycol, trihydroxy methyl
Propane, dibutyl tin dilaurate, stannous octoate, diglycol, bismaleimide, triethanolamine, sodium-based montmorillonite,
Plasticizer, thixotropic agent are added, and are injected into flat-die after reacting 60min, 90 DEG C of reaction 20min.
Embodiment 7:
A kind of aqueous polyurethane flame-retardant adhesive, is prepared by the raw material of following weight fraction:
40 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 10 parts of 4- diisocyanate, 10 parts of poly adipate succinic acid ester,
Bis- 20 parts of (methylol) propionic acid of 2,2-, 12 parts of polytetrahydrofuran ether glycol, 1.5 parts of trimethylolpropane, di lauric dibutyl
0.1 part of tin, 0.5 part of stannous octoate, 4 parts of diglycol, 5 parts of bismaleimide, 10 parts of acetone, 2 parts of triethanolamine, sodium
6 parts of base montmorillonite, 23 parts of melamine coated ammonium polyphosphate, 2 parts of plasticizer phthalic acid dimethyl ester, organobentonite and polyamide
3 parts of thixotropic agent that wax 1:1 in mass ratio is mixed, 10 parts of deionized water.
Melamine coated ammonium polyphosphate the preparation method is as follows:
Melamine resin is add to deionized water, the phosphoric acid for being 80% by mass concentration after 50 DEG C of stirring and dissolvings is warming up to
It is added dropwise and enters, drop is warming up to 90 DEG C of reaction 1h after finishing, ammonium polyphosphate is added again after filtering for heat, naturally cools to room after stirring 5h
Temperature filters, and vacuum drying is the melamine coated ammonium polyphosphate after filter cake washing.
Above-mentioned aqueous polyurethane flame-retardant adhesive the preparation method is as follows:
(1) melamine coated ammonium polyphosphate is added to deionized water, in acetone, ultrasonic vibration disperses 15min；
(2) by isophorone diisocyanate, Toluene-2,4-diisocyanate, 4- diisocyanate is added, is warming up to 80 DEG C of reaction 4h, obtains
Prepolymer, by prepolymer vacuum outgas；
(3) again by bis- (methylol) propionic acid of poly adipate succinic acid ester, 2,2-, polytetrahydrofuran ether glycol, trihydroxy methyl
Propane, dibutyl tin dilaurate, stannous octoate, diglycol, bismaleimide, triethanolamine, sodium-based montmorillonite,
Plasticizer, thixotropic agent are added, and are injected into flat-die after reacting 50min, 100 DEG C of reaction 15min.
Performance test:
The following table 1 is the performance test results of 1-3 of embodiment of the present invention aqueous polyurethane flame-retardant adhesive:
Table 1:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Tensile strength/MPa | 32.5 | 33.1 | 28.6 |
| Elongation at break/% | 688 | 682 | 653 |
| Swelling ratio/% | 106 | 103 | 117 |
| Flame retardant rating | V-0 | V-0 | V-0 |
By upper table 1 it is found that aqueous polyurethane flame-retardant adhesive of the present invention has extremely excellent mechanical property, and it is fire-retardant etc.
Grade is high.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (8)
1. a kind of aqueous polyurethane flame-retardant adhesive, which is characterized in that be prepared by the raw material of following weight fraction:
30-40 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 10-18 parts of 4- diisocyanate, poly adipate succinic acid ester 5-10
Part, 20-30 parts of 2,2- bis- (methylol) propionic acid, 12-16 parts of polytetrahydrofuran ether glycol, 1-1.5 parts of trimethylolpropane, February
0.1-0.5 parts of dilaurylate, 0.1-0.5 parts of stannous octoate, 4-8 parts of diglycol, 2-5 parts of bismaleimide,
10-20 parts of acetone, 1-2 parts of triethanolamine, 6-10 parts of sodium-based montmorillonite, 15-23 parts of melamine coated ammonium polyphosphate, plasticizer 2-3
Part, 1-3 parts of thixotropic agent, 10-15 parts of deionized water.
2. aqueous polyurethane flame-retardant adhesive as described in claim 1, which is characterized in that by the raw material system of following weight fraction
It is standby to form:
32 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 13 parts of 4- diisocyanate, 8 parts of poly adipate succinic acid ester, 2,2- are bis-
25 parts of (methylol) propionic acid, 14 parts of polytetrahydrofuran ether glycol, 1 part of trimethylolpropane, 0.3 part of dibutyl tin dilaurate,
0.1 part of stannous octoate, 6 parts of diglycol, 4 parts of bismaleimide, 10 parts of acetone, 2 parts of triethanolamine, sodium-based montmorillonite
7 parts, 18 parts of melamine coated ammonium polyphosphate, 3 parts of plasticizer, 2 parts of thixotropic agent, 12 parts of deionized water.
3. aqueous polyurethane flame-retardant adhesive as described in claim 1, which is characterized in that by the raw material system of following weight fraction
It is standby to form:
40 parts of isophorone diisocyanate, Toluene-2,4-diisocyanate, 16 parts of 4- diisocyanate, 5 parts of poly adipate succinic acid ester, 2,2- are bis-
22 parts of (methylol) propionic acid, 16 parts of polytetrahydrofuran ether glycol, 1.5 parts of trimethylolpropane, dibutyl tin dilaurate 0.4
Part, 0.1 part of stannous octoate, 5 parts of diglycol, 3 parts of bismaleimide, 13 parts of acetone, 1 part of triethanolamine, sodium base cover
De- soil 8 parts, 18 parts of melamine coated ammonium polyphosphate, 3 parts of plasticizer, 3 parts of thixotropic agent, 12 parts of deionized water.
4. aqueous polyurethane flame-retardant adhesive as described in claim 1, which is characterized in that the melamine coated ammonium polyphosphate
The preparation method is as follows:
Melamine resin is add to deionized water, be warming up to after 40-50 DEG C of stirring and dissolving by certain density phosphoric acid be added dropwise into
Enter, drop is warming up to 80-90 DEG C of reaction 1-3h after finishing, ammonium polyphosphate is added again after filtering for heat, naturally cools to after stirring 1-5h
Room temperature filters, and vacuum drying is the melamine coated ammonium polyphosphate after filter cake washing.
5. aqueous polyurethane flame-retardant adhesive as claimed in claim 4, which is characterized in that the mass concentration of the phosphoric acid is
80-85%.
6. aqueous polyurethane flame-retardant adhesive as described in claim 1, which is characterized in that the plasticizer is phthalic acid
Di-n-octyl, BBP(Butyl Benzyl Phthalate, di-sec-octyl phthalate, dicyclohexyl phthalate, phthalic acid two
Butyl ester, diisobutyl phthalate, repefral, diethyl phthalate, diisononyl phthalate,
Any one or more combination in diisooctyl phthalate.
7. aqueous polyurethane flame-retardant adhesive as described in claim 1, which is characterized in that the thixotropic agent is organobentonite
It is mixed with polyamide wax 1:1 in mass ratio.
8. a kind of preparation method of such as aqueous polyurethane flame-retardant adhesive of any of claims 1-7, feature exist
In specific as follows:
(1) melamine coated ammonium polyphosphate is added to deionized water, in acetone, ultrasonic vibration disperses 5-15min；
(2) by isophorone diisocyanate, Toluene-2,4-diisocyanate, 4- diisocyanate is added, is warming up to 60-80 DEG C of reaction 2-5h, obtains
To prepolymer, by prepolymer vacuum outgas；
(3) again by bis- (methylol) propionic acid of poly adipate succinic acid ester, 2,2-, polytetrahydrofuran ether glycol, trimethylolpropane,
Dibutyl tin dilaurate, stannous octoate, diglycol, bismaleimide, triethanolamine, sodium-based montmorillonite, plasticising
Agent, thixotropic agent are added, and are injected into flat-die after reacting 40-60min, 90-100 DEG C of reaction 10-20min.
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| CN117586472B (en) * | 2024-01-19 | 2024-03-15 | 广东荣昌纺织实业有限公司 | Terylene double-sided coating type flame-retardant waterproof tarpaulin, coating composition and preparation method thereof |
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