CN106675494A - Water-based polyurethane adhesive for bullet-proof vest composite material and preparation method of water-based polyurethane adhesive - Google Patents
Water-based polyurethane adhesive for bullet-proof vest composite material and preparation method of water-based polyurethane adhesive Download PDFInfo
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
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- 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
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- C09J11/04—Non-macromolecular additives inorganic
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Abstract
The invention discloses water-based polyurethane adhesive for a bullet-proof vest composite material. The water-based polyurethane adhesive is prepared from the following raw materials: 80 to 140 parts of polymer polyols, 40 to 80 parts of modified polyisocyanates, 2 to 12 parts of hydrophilic chain-extending agent, 0.05 to 0.1 part of catalyst, 1 to 6 parts of cross-linking agent, 1 to 6 parts of neutralizing agent, 1 to 2 parts of thickener, and 0.5 to 1 part of flatting agent. The tensile performance of the adhesive is improved, the adhesive force when the adhesive is bonded with the bullet-proof composite material is increased, the heat conducting performance of the adhesive is improved, rapidness in heat dissipation can be realized, and the application requirement of the bullet-proof composite material can be met. The invention also discloses a preparation method of the water-based polyurethane adhesive for the bullet-proof composite material. The water-based polyurethane adhesive and the preparation method thereof are simple in process, low in production cost and environment-friendly.
Description
Technical field
The present invention relates to water-based polyurethane adhesive technical field, more particularly to a kind of flak jackets composite is poly- with aqueouss
Urethane adhesive and preparation method thereof.
Background technology
The adhesive of ballistic composite is applied to now mainly based on solvent-borne type, such as SIS glue, environmental pollution compared with
Greatly, environmental requirement is not met.With the development and the enhancing of people's environmental consciousness of research, the research of water-based polyurethane adhesive is fast
Speed development, it has the advantages that, and soft durometer scalable, low temperature resistant, pliability be good, adhesive strength is big, can bonded metal, nonmetallic
It is of many uses Deng multiple material.But water-based polyurethane adhesive is still deposited when bonding with the ballistic composite of low-surface-energy
Not strong in adhesive force, tensile strength is little, the shortcoming of poor thermal conductivity.
Graphene oxide is the important as precursors of the allotrope-Graphene of carbon, is a kind of Two-dimensional Carbon of monoatomic thickness
Lamellar structure, with various oxy radicals, the epoxy radicals and hydroxyl being such as located on the carboxyl and lamella at layer edge, it has intensity
Greatly, the characteristics of heat conduction is good, surface area is big.There is presently no is used for anti-spring-go with graphene oxide modified aqueous adhesion agent of polyurethane
The report of condensation material.
The content of the invention
The present invention proposes a kind of ballistic composite water-based polyurethane adhesive and preparation method thereof, using oxidation stone
Black alkene is modified to water-based polyurethane adhesive, solves when water-based polyurethane adhesive is bonded with ballistic composite and adheres to
Power is not strong, and tensile strength is little, the technical problem of poor thermal conductivity.
A kind of ballistic composite water-based polyurethane adhesive proposed by the present invention, its raw material includes by weight：80-
140 parts of polymer polyatomic alcohols, 40-80 part modified polyisocyanates, 2-12 part hydrophilic chain extenders, 0.05-0.1 part catalyst, 1-6
Part cross-linking agent, 1-6 part nertralizers, 1-2 part thickening agents, 0.5-1 part levelling agents.
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in solvent, is in ultrasonic frequency
Ultrasonic disperse obtains graphene oxide dispersion under the conditions of 4000-6000Hz, adds polyisocyanates, shielding gas is passed through, in temperature
Stirring reaction obtains modified polyisocyanate under the conditions of 70-90 DEG C of degree.
Preferably, graphene oxide and the weight proportion of polyisocyanates are 0.5-1：4-20.
Preferably, graphene oxide and the weight proportion of polyisocyanates are 1：10.
Preferably, solvent is DMF, acetone, toluene one or more mixture.
Preferably, solvent is DMF.
Preferably, during ultrasonic disperse, ultrasonic time is 1-2h.
Preferably, mixing time is 20-28h.
Preferably, mixing time is 24h.
Preferably, shielding gas is N2。
Preferably, its raw material includes by weight：100-130 part polymer polyatomic alcohols, 50-70 parts graphene oxide are modified
Polyisocyanates, 5-9 part hydrophilic chain extenders, 0.06-0.09 part catalyst, 2-5 part cross-linking agent, 2-5 part nertralizers, 1.2-1.8
Part thickening agent, 0.7-0.9 part levelling agents.
Preferably, its raw material includes by weight：120 parts of polymer polyatomic alcohols, 60 parts of graphene oxides are modified many isocyanides
Acid esters, 7 parts of hydrophilic chain extenders, 0.07 part of catalyst, 4 parts of cross-linking agent, 4 parts of nertralizers, 1.5 parts of thickening agents, 0.8 part of levelling agent.
Preferably, polymer polyatomic alcohol includes PEPA and/or polyether polyol.
Preferably, polymer polyatomic alcohol includes polycaprolactone diols, polyadipate BDO esterdiol, Propylene Glycol
One or more mixture in polyethers, polyether triol, polytetrahydrofuran diol.
Preferably, polymer polyatomic alcohol is included in Propylene Glycol polyethers, polyadipate BDO esterdiol, polyether triol
One or more mixture.
Preferably, polymer polyatomic alcohol is Propylene Glycol polyethers.
Preferably, polyisocyanates includes hexamethylene diisocyanate, isophorone diisocyanate, toluene diisocyanate
Acid esters, 3- chlorophenyl isocyanates, 3,4- dichlorophenyl isocyanates, n-butyl isocyanate, t-butylisocyanate, 18
One kind in alkyl isocyanate, hexamethylene diisocyanate, triphenylmethane triisocyanate.
Preferably, hydrophilic chain extender is 2,2- dihydromethyl propionic acids or dihydroxy half ester.
Preferably, hydrophilic chain extender is 2,2- dihydromethyl propionic acids.
Preferably, catalyst is dibutyl tin laurate, stannous octoate, two (dodecyl sulfur) dibutyl tins, two vinegar
One or more mixture in sour dibutyl tin.
Preferably, catalyst is dibutyl tin laurate.
Preferably, cross-linking agent is trimethylolpropane or polypropylene oxide triol.
Preferably, cross-linking agent is trimethylolpropane.
Preferably, nertralizer is the one kind in ammonia, sodium hydroxide, triethylamine.
Preferably, nertralizer is triethylamine.
Preferably, thickening agent is polyurethane thickener or one or more mixture in acrylic thickener.
Preferably, levelling agent is acrylic type levelling agent and/or organic silicon type levelling agent.
A kind of method of ballistic composite water-based polyurethane adhesive, comprises the steps：By proportioning by polymer
Polyhydric alcohol is added in four-hole boiling flask, and shielding gas, Deca modified polyisocyanate, in temperature 70-90 DEG C are passed through in four-hole boiling flask
Prepolymerization reaction is carried out, base polyurethane prepolymer for use as is obtained, hydrophilic chain extender is added in base polyurethane prepolymer for use as, that catalyst carries out chain extension is anti-
Should, add cross-linking agent to carry out cross-linking reaction, viscosity reduction, cooling adds nertralizer, the emulsifying of deionized water dispersed with stirring that modified water is obtained
Property polyaminoester emulsion, add thickening agent, levelling agent to obtain ballistic composite aqueouss in modified aqueous polyurethane emulsion and gather
Urethane adhesive.
Preferably, the rate of addition of modified polyisocyanate is 1-2ml/min.
Preferably, shielding gas is N2。
Preferably, the heating-up temperature of prepolymerization reaction is 70-90 DEG C.
Preferably, the heating-up temperature of prepolymerization reaction is 80 DEG C.
Preferably, the prepolymerization reaction time is 1-3h.
Preferably, the prepolymerization reaction time is 2h.
Preferably, solid content is 20-35wt% in modified aqueous polyurethane emulsion.
Preferably, solid content is 30wt% in modified aqueous polyurethane emulsion.
Preferably, the viscosity of ballistic composite water-based polyurethane adhesive is 95-105mPa.s.
The viscosity of preferably ballistic composite water-based polyurethane adhesive is 100mPa.s.
Preferably, solvent is one or more mixture in acetone, butanone, N-Methyl pyrrolidone.
Preferably, solvent is acetone.
Preferably, the envelope-bulk to weight ratio ml of deionized water and polymer polyatomic alcohol:G is 3-5：1.
Preferably, the envelope-bulk to weight ratio ml of deionized water and polymer polyatomic alcohol:G is 4：1.
Preferably, in dispersed with stirring emulsion process, high speed agitator is used.
Preferably, a kind of method of ballistic composite water-based polyurethane adhesive, comprises the steps：Will by proportioning
Polymer polyatomic alcohol is added in four-hole boiling flask, and shielding gas, Deca modified polyisocyanate, in temperature are passed through in four-hole boiling flask
70-90 DEG C of reaction 1-3h, adds hydrophilic chain extender and catalyst, and in temperature 80-90 DEG C 1-3h is reacted, and adds cross-linking agent, adds
Solvent drop is glutinous, reacts 0.5-1.5h, and reaction resulting material temperature is down to into room temperature, adds nertralizer, neutralization reaction 0.5-1.5h,
Deionized water is added, with high speed agitator stirring and emulsifying 20-40min, modified aqueous polyurethane emulsion is obtained, it is poly- in modified water-soluble
Thickening agent, levelling agent is added to obtain ballistic composite water-based polyurethane adhesive in urethane emulsion.
Preferably, the temperature of chain extending reaction is 85 DEG C, and the response time is 2h.
Preferably, cross-linking reaction time is 1h.
Preferably, the time of neutralization reaction is 1h.
Preferably, emulsification times are 30min.
The present invention is modified using graphene oxide to polyisocyanates, is dispersed with the two-dimentional basal plane of graphene oxide
Polar group, such as hydroxyl and epoxy radicals and the carbonyl and carboxyl of edge, interact with polyisocyanates, improve adhesive
Tensile property, enhance adhesive force when bonding with ballistic composite, graphene oxide is evenly distributed in polyurethane adhesive
In stick, the heat conductivility of adhesive is improved, quick heat radiating can be realized, meet the use requirement of ballistic composite,
The lamellar structure and good automatic recovery ability that simultaneous oxidation Graphene has also imparts the good barrier property of adhesive
And self-healing capability, with the incomparable advantage of traditional adhesive；It is gluing polyurethane is enhanced using hydrophilic chain extender
While the viscosity of agent, also with environmental protection, free of contamination advantage adds the solid content symbol in cross-linking agent control polyaminoester emulsion
The use standard of bullet resistant material is closed, while carrying out basis for emulsion reaction, makes emulsion process to add emulsifying agent, under agitation
Emulsifying is can be achieved with, processing technology is simplified, production cost is reduced.
Specific embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of ballistic composite water-based polyurethane adhesive, its raw material includes by weight：80 parts of polymer polyols
Alcohol, 40 parts of modified polyisocyanates, 2 parts of hydrophilic chain extenders, 0.05 part of catalyst, 1 part of cross-linking agent, 1 part of nertralizer, 1 part of thickening
Agent, 0.5 part of levelling agent；
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in solvent, is in ultrasonic frequency
Ultrasonic disperse obtains graphene oxide dispersion under the conditions of 4000Hz, adds polyisocyanates, shielding gas is passed through, in temperature 70 C
Under the conditions of stirring obtain modified polyisocyanate.
Embodiment 2
A kind of ballistic composite water-based polyurethane adhesive, its raw material includes by weight：140 parts of polymer polyols
Alcohol, 80 parts of modified polyisocyanates, 12 parts of hydrophilic chain extenders, 0.1 part of catalyst, 6 parts of cross-linking agent, 6 parts of nertralizers, 2 parts of thickenings
Agent, 1 part of levelling agent；
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in solvent, is in ultrasonic frequency
Ultrasonic disperse obtains graphene oxide dispersion under the conditions of 6000Hz, adds polyisocyanates, control graphene oxide and polyisocyanate
The weight proportion of cyanate is 1:8, shielding gas is passed through, 20h is stirred under the conditions of 90 DEG C of temperature and obtains modified polyisocyanate.
Implement 3
A kind of ballistic composite water-based polyurethane adhesive, its raw material includes by weight：130 parts of polyether polyols
Alcohol, 70 parts of modified polyisocyanates, 9 parts of 2,2- dihydromethyl propionic acids, 0.09 part of dibutyl tin laurate, 5 parts of trihydroxy methyls
Propane, 5 parts of ammonia, 1.8 parts of polyurethane thickeners, 0.9 part of acrylic type levelling agent；
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in DMF, is in ultrasonic frequency
Ultrasonic disperse 1h obtains graphene oxide dispersion under the conditions of 5000Hz, adds hexamethylene diisocyanate, control oxidation stone
Black alkene is 1 with the weight proportion of hexamethylene diisocyanate:40, shielding gas is passed through, 28h is stirred under the conditions of 80 DEG C of temperature and is obtained
To modified hexamethylene diisocyanate.
Embodiment 4
A kind of ballistic composite water-based polyurethane adhesive, its raw material includes by weight：100 parts of polycaprolactones two
First alcohol, 50 parts of modified polyisocyanates, 5 parts of dihydroxy half esters, 0.06 part of stannous octoate, 2 parts of polypropylene oxide triols, 2 parts of hydrogen
Sodium oxide, 0.6 part of acrylic thickener, 0.6 part of polyurethane thickener, 0.4 part of organic silicon type levelling agent, 0.3 part of acrylic type
Levelling agent；
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in acetone and DMF mixed solvents,
Ultrasonic frequency is that ultrasonic disperse 2h obtains graphene oxide dispersion under the conditions of 4500Hz, adds isophorone diisocyanate
Ester, it is 1 to control graphene oxide with the weight proportion of isophorone diisocyanate:4, it is passed through N2, under the conditions of 85 DEG C of temperature
Stirring 24h obtains modified isophorone diisocyanate.
Embodiment 5
A kind of ballistic composite water-based polyurethane adhesive, its raw material includes by weight：60 parts of polyadipates 1,
4- butyl glycol ester diols, 60 parts of Propylene Glycol polyethers, 60 parts of modified polyisocyanates, 7 parts of dihydroxy half esters, 0.07 part two (12
Alkyl sulfide) dibutyl tin, 4 parts of trimethylolpropanes, 4 parts of triethylamines, 0.5 part of acrylic thickener, 1 part of polyurethane thickener,
0.8 part of organic silicon type levelling agent；
Modified polyisocyanate is adopted and is obtained with the following method：By graphene oxide be placed in DMF, acetone, toluene mixing it is molten
In agent, ultrasonic disperse 1.5h obtains graphene oxide dispersion under the conditions of ultrasonic frequency is 5500Hz, adds toluene two different
Cyanate, it is 1 to control graphene oxide with the weight proportion of toluene di-isocyanate(TDI):8, it is passed through N2, under the conditions of 83 DEG C of temperature
Stirring 22h obtains modified toluene diisocyanate.
Embodiment 6
A kind of ballistic composite water-based polyurethane adhesive, its raw material includes by weight：25 parts of polycaprolactones two
First alcohol, 25 parts of polyadipate BDO esterdiols, 50 parts of Propylene Glycol polyethers, 65 parts of modified polyisocyanates, 8 parts of 2,2- bis-
Hydroxymethyl propionic acid, 0.04 part of two (dodecyl sulfur) dibutyl tin, 0.03 part of dibutyltin diacetate, 4 parts of trimethylolpropanes,
4 parts of triethylamines, 0.8 part of polyurethane thickener, 0.8 part of acrylic thickener, 0.8 part of organic silicon type levelling agent；
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in acetone, is in ultrasonic frequency
Ultrasonic disperse 1.5h obtains graphene oxide dispersion under the conditions of 5500Hz, adds 3- chlorophenyl isocyanates, control oxidation stone
Black alkene is 1 with the weight proportion of 3- chlorophenyl isocyanates:10, it is passed through N2, stir 22h under the conditions of 83 DEG C of temperature and be modified
3- chlorophenyl isocyanates.
The method of ballistic composite water-based polyurethane adhesive, comprises the steps：By proportioning by polymer polyol
Alcohol is added in four-hole boiling flask, and shielding gas is passed through in four-hole boiling flask, and Deca modified polyisocyanate carries out pre-polymerization in temperature 70 C
Reaction, obtains base polyurethane prepolymer for use as, adds hydrophilic chain extender, catalyst to carry out chain extending reaction in base polyurethane prepolymer for use as, adds
Cross-linking agent carries out cross-linking reaction, and viscosity reduction, cooling adds nertralizer, the emulsifying of deionized water dispersed with stirring that the poly- ammonia of modified water-soluble is obtained
Ester emulsion, adds thickening agent, levelling agent to obtain ballistic composite water-borne polyurethane bond in modified aqueous polyurethane emulsion
Stick.
Embodiment 7
A kind of ballistic composite water-based polyurethane adhesive, its raw material includes by weight：20 parts of polyadipates 1,
4- butyl glycol ester diols, 30 parts of Propylene Glycol polyethers, 20 parts of polyether triols, 40 parts of polytetrahydrofuran diols, 60 parts of many isocyanides that are modified
Acid esters, 7 parts of 2,2- dihydromethyl propionic acids, 0.03 part of dibutyl tin laurate, 0.03 part of stannous octoate, 0.03 part of two acetic acid two
Butyl tin, 4 parts of trimethylolpropanes, 4 parts of triethylamines, 0.7 part of polyurethane thickener, 0.8 part of acrylic thickener, 0.8 part have
Machine silicon type levelling agent；
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in acetone, is in ultrasonic frequency
Ultrasonic disperse 1.5h obtains graphene oxide dispersion under the conditions of 5500Hz, adds 3,4- dichlorophenyl isocyanates, controls oxygen
Graphite alkene is 1 with the weight proportion of 3,4- dichlorophenyl isocyanates:30, it is passed through N2, under the conditions of 83 DEG C of temperature 22h is stirred
Obtain modified 3,4- dichlorophenyl isocyanates.
The method of ballistic composite water-based polyurethane adhesive, comprises the steps：Polymer polyatomic alcohol is added
In four-hole boiling flask, shielding gas is passed through in four-hole boiling flask, Deca modified polyisocyanate reacts 1h, adds parent in temperature 70 C
Water chain extender and catalyst, in 80 DEG C of reaction 1h of temperature, add cross-linking agent, add acetone drop glutinous, 0.5h are reacted, by reaction gained
Temperature of charge is down to room temperature, adds nertralizer, neutralization reaction 0.5h to add deionized water, deionized water and polymer polyatomic alcohol
Envelope-bulk to weight ratio ml:G is 3：1, with high speed agitator stirring and emulsifying 20min, solid content is obtained poly- for 20wt% modified water-solubles
Urethane emulsion, adds thickening agent, levelling agent in modified aqueous polyurethane emulsion, and material viscosity is adjusted to into 95mPa.s, is prevented
Elastic composite material water-based polyurethane adhesive.
Embodiment 8
A kind of ballistic composite water-based polyurethane adhesive, its raw material includes by weight：30 parts of polycaprolactones two
First alcohol, 30 parts of polyadipate BDO esterdiols, 30 parts of Propylene Glycol polyethers, 30 parts of polyether triols, 20 parts of PolyTHFs
Glycol, 60 parts of modified polyisocyanates, 7 parts of 2,2- dihydromethyl propionic acids, 0.025 part of dibutyl tin laurate, 0.025 part it is pungent
Sour stannous, 0.02 part of two (dodecyl sulfur) dibutyl tin, 0.02 part of dibutyltin diacetate, 4 parts of trimethylolpropanes, 4 parts
Triethylamine, 1.5 parts of polyurethane thickeners, 0.8 part of organic silicon type levelling agent；
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in toluene, is in ultrasonic frequency
Ultrasonic disperse 1.5h obtains graphene oxide dispersion under the conditions of 5500Hz, adds n-butyl isocyanate, controls graphite oxide
Alkene is 1 with the weight proportion of n-butyl isocyanate:25, it is passed through N2, stir 22h under the conditions of 83 DEG C of temperature and obtain the positive fourth that is modified
Based isocyanate.
The method of ballistic composite water-based polyurethane adhesive, comprises the steps：Polymer polyatomic alcohol is added
In four-hole boiling flask, shielding gas is passed through in four-hole boiling flask, Deca modified polyisocyanate, in 90 DEG C of reaction 3h of temperature, adds parent
Water chain extender and catalyst, in 90 DEG C of reaction 3h of temperature, add cross-linking agent, add acetone drop glutinous, 1.5h are reacted, by reaction gained
Temperature of charge is down to room temperature, adds nertralizer, neutralization reaction 1.5h to add deionized water, deionized water and polymer polyatomic alcohol
Envelope-bulk to weight ratio ml:G is 5：1, with high speed agitator stirring and emulsifying 40min, solid content is obtained poly- for 35wt% modified water-solubles
Urethane emulsion, adds thickening agent, levelling agent in modified aqueous polyurethane emulsion, and material viscosity is adjusted to into 105mPa.s, obtains
Ballistic composite water-based polyurethane adhesive.
Embodiment 9
A kind of ballistic composite water-based polyurethane adhesive, its raw material includes by weight：120 parts of Propylene Glycol are gathered
Ether, 60 parts of modified polyisocyanates, 7 parts of 2,2- dihydromethyl propionic acids, 0.07 part of dibutyl tin laurate, 4 parts of trihydroxy methyls
Propane, 4 parts of triethylamines, 1.5 parts of acrylic thickeners, 0.8 part of organic silicon type levelling agent；
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in DMF, is in ultrasonic frequency
Ultrasonic disperse 1.5h obtains graphene oxide dispersion under the conditions of 5500Hz, adds t-butylisocyanate, controls graphite oxide
Alkene is 1 with the weight proportion of n-butyl isocyanate:30, it is passed through N2, stir 22h under the conditions of 83 DEG C of temperature and obtain the tertiary fourth that is modified
Based isocyanate.
The method of ballistic composite water-based polyurethane adhesive, comprises the steps：Polymer polyatomic alcohol is added
In four-hole boiling flask, shielding gas is passed through in four-hole boiling flask, Deca modified polyisocyanate, in 80 DEG C of reaction 2h of temperature, adds parent
Water chain extender and catalyst, in 85 DEG C of reaction 2h of temperature, add cross-linking agent, add acetone drop glutinous, react 1h, will react gains
Material temperature degree is down to room temperature, adds nertralizer, neutralization reaction 1h to add the body of deionized water, deionized water and polymer polyatomic alcohol
Product weight compares ml:G is 4：1, with high speed agitator stirring and emulsifying 30min, it is 30wt% modified aqueous polyurethanes that solid content is obtained
Emulsion, adds thickening agent, levelling agent in modified aqueous polyurethane emulsion, and material viscosity is adjusted to into 100mPa.s, obtains shellproof
Composite water-based polyurethane adhesive.
Embodiment 10
A kind of ballistic composite water-based polyurethane adhesive, its raw material includes by weight：120 parts of Propylene Glycol are gathered
Ether, 60 parts of modified polyisocyanates, 7 parts of 2,2- dihydromethyl propionic acids, 0.07 part of dibutyl tin laurate, 4 parts of trihydroxy methyls
Propane, 4 parts of triethylamines, 1.5 parts of polyurethane thickeners, 0.8 part of organic silicon type levelling agent；
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in DMF, is in ultrasonic frequency
Ultrasonic disperse 1.5h obtains graphene oxide dispersion under the conditions of 5500Hz, adds octadecylisocyanate, control oxidation stone
Black alkene is 1 with the weight proportion of n-butyl isocyanate:30, it is passed through N2, stir 22h under the conditions of 83 DEG C of temperature and obtain modified ten
Eight alkyl isocyanates.
The method of ballistic composite water-based polyurethane adhesive, comprises the steps：Polymer polyatomic alcohol is added
In four-hole boiling flask, shielding gas is passed through in four-hole boiling flask, Deca modified polyisocyanate reacts 2h at 80 DEG C of temperature, adds
Hydrophilic chain extender and catalyst, react 2h under the conditions of 85 DEG C of temperature, add cross-linking agent, add acetone drop glutinous, react 1h, will be anti-
Answer resulting material temperature to be down to room temperature, add nertralizer, neutralization reaction 1h to add deionized water, deionized water and polymer are more
The envelope-bulk to weight ratio ml of first alcohol:G is 4：1, with high speed agitator stirring and emulsifying 30min, it is 30wt% modified waters that solid content is obtained
Property polyaminoester emulsion, in modified aqueous polyurethane emulsion add thickening agent, levelling agent, material viscosity is adjusted to into 100mPa.s,
Obtain ballistic composite water-based polyurethane adhesive.
Embodiment 11
A kind of ballistic composite water-based polyurethane adhesive, its raw material includes by weight：120 parts of Propylene Glycol are gathered
Ether, 60 parts of modified polyisocyanates, 7 parts of 2,2- dihydromethyl propionic acids, 0.07 part of dibutyl tin laurate, 4 parts of trihydroxy methyls
Propane, 4 parts of triethylamines, 1.5 parts of acrylic thickeners, 0.8 part of organic silicon type levelling agent；
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in DMF, is in ultrasonic frequency
Ultrasonic disperse 1.5h obtains graphene oxide dispersion under the conditions of 5500Hz, adds hexamethylene diisocyanate, control oxidation
Graphene is 1 with the weight proportion of n-butyl isocyanate:30, it is passed through N2, stir 22h under the conditions of 83 DEG C of temperature and be modified
Hexamethylene diisocyanate.
The method of ballistic composite water-based polyurethane adhesive, comprises the steps：Polymer polyatomic alcohol is added
In four-hole boiling flask, shielding gas is passed through in four-hole boiling flask, Deca modified polyisocyanate, in 80 DEG C of reaction 2h of temperature, adds parent
Water chain extender and catalyst, in 85 DEG C of reaction 2h of temperature, add cross-linking agent, add acetone drop glutinous, react 1h, will react gains
Material temperature degree is down to room temperature, adds nertralizer, neutralization reaction 1h to add the body of deionized water, deionized water and polymer polyatomic alcohol
Product weight compares ml:G is 4：1, with high speed agitator stirring and emulsifying 30min, it is 30wt% modified aqueous polyurethanes that solid content is obtained
Emulsion, adds thickening agent, levelling agent in modified aqueous polyurethane emulsion, and material viscosity is adjusted to into 100mPa.s, obtains shellproof
Composite water-based polyurethane adhesive.
Embodiment 12
A kind of ballistic composite water-based polyurethane adhesive, its raw material includes by weight：120 parts of Propylene Glycol are gathered
Ether, 60 parts of modified polyisocyanates, 7 parts of 2,2- dihydromethyl propionic acids, 0.07 part of dibutyl tin laurate, 4 parts of trihydroxy methyls
Propane, 4 parts of triethylamines, 1.5 parts of acrylic thickeners, 0.8 part of organic silicon type levelling agent；
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in acetone, is in ultrasonic frequency
Ultrasonic disperse 1.5h obtains graphene oxide dispersion under the conditions of 5500Hz, adds triphenylmethane triisocyanate, controls oxygen
Graphite alkene is 1 with the weight proportion of n-butyl isocyanate:30, it is passed through N2, stir 22h under the conditions of 83 DEG C of temperature and changed
Property triphenylmethane triisocyanate.
The method of ballistic composite water-based polyurethane adhesive, comprises the steps：Polymer polyatomic alcohol is added
In four-hole boiling flask, shielding gas is passed through in four-hole boiling flask, Deca modified polyisocyanate, in 80 DEG C of reaction 2h of temperature, adds parent
Water chain extender and catalyst, in 85 DEG C of reaction 2h of temperature, add cross-linking agent, add acetone drop glutinous, react 1h, will react gains
Material temperature degree is down to room temperature, adds nertralizer, neutralization reaction 1h to add the body of deionized water, deionized water and polymer polyatomic alcohol
Product weight compares ml:G is 4：1, with high speed agitator stirring and emulsifying 30min, it is 30wt% modified aqueous polyurethanes that solid content is obtained
Emulsion, adds thickening agent, levelling agent in modified aqueous polyurethane emulsion, and material viscosity is adjusted to into 100mPa.s, obtains shellproof
Composite water-based polyurethane adhesive.
Reference examples
A kind of water-based polyurethane adhesive, its raw material includes by weight：120 parts of Propylene Glycol polyethers, 60 parts of polyisocyanic acid
Ester, 7 parts of 2,2- dihydromethyl propionic acids, 0.07 part of dibutyl tin laurate, 4 parts of trimethylolpropanes, 4 parts of triethylamines, 1.5 parts
Acrylic thickener, 0.8 part of organic silicon type levelling agent；
The method of water-based polyurethane adhesive, comprises the steps：Polymer polyatomic alcohol is added in four-hole boiling flask, Xiang Si
Shielding gas is passed through in mouth flask, Deca polyisocyanates, in 80 DEG C of reaction 2h of temperature, adds hydrophilic chain extender and catalyst,
85 DEG C of reaction 2h of temperature, add cross-linking agent, add acetone drop glutinous, react 1h, and reaction resulting material temperature is down to into room temperature, add
Nertralizer, neutralization reaction 1h adds the envelope-bulk to weight ratio ml of deionized water, deionized water and polymer polyatomic alcohol:G is 4：1, use
High speed agitator stirring and emulsifying 30min, it is 30wt% aqueous polyurethane emulsions that solid content is obtained, and is added in aqueous polyurethane emulsion
Enter thickening agent, levelling agent, material viscosity is adjusted to into 100mPa.s, water-based polyurethane adhesive.
By embodiment 10-12 adhesive and reference examples adhesive applications in flak jackets high density high-modulus polyethylene fibres UD
Cloth composite, the Kilograms Per Square Meter of surface density 6 carries out the anti-bullet test of GA141 standards V50, as a result as shown in table 1：
The V50 the performance test results of embodiment 10-12 of table 1
| Performance | Embodiment 10 | Embodiment 11 | Embodiment 12 | Reference examples |
| V50(m/s) | 650 | 640 | 660 | 550 |
As can be seen from Table 1 through the water-borne polyurethane bond that graphene oxide is modified, under similarity condition, bullet-proof
Can more preferably, the UD cloth composite reached required for same degree of protection is less, has saved cost；It is of the invention compound with shellproof
Material is bonded with strong adhesive force, and tensile resistance and heat conductivility are good, the ballistic performance of flak jackets are improve, while reducing
Production cost, with actual using value.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.
Claims (10)
1. a kind of ballistic composite water-based polyurethane adhesive, it is characterised in that its raw material includes by weight：80-140
Part polymer polyatomic alcohol, 40-80 part modified polyisocyanates, 2-12 part hydrophilic chain extenders, 0.05-0.1 part catalyst, 1-6 parts
Cross-linking agent, 1-6 part nertralizers, 1-2 part thickening agents, 0.5-1 part levelling agents；
Modified polyisocyanate is adopted and is obtained with the following method：Graphene oxide is placed in solvent, is 4000- in ultrasonic frequency
Ultrasonic disperse obtains graphene oxide dispersion under the conditions of 6000Hz, adds polyisocyanates, shielding gas is passed through, in temperature 70-
Stirring under the conditions of 90 DEG C obtains modified polyisocyanate.
2. ballistic composite water-based polyurethane adhesive according to claim 1, it is characterised in that graphene oxide
It is 0.5-1 with the weight proportion of polyisocyanates：4-20；Preferably, graphene oxide is with the weight proportion of polyisocyanates
1：10；
3. ballistic composite water-based polyurethane adhesive according to claim 1, it is characterised in that mixing time is
20-28h；Preferably, mixing time is 24h.
4. ballistic composite water-based polyurethane adhesive according to claim 1, it is characterised in that its raw material is by weight
Amount part includes：100-130 part polymer polyatomic alcohols, 50-70 part graphene oxide modified polyisocyanates, the hydrophilic chain extension of 5-9 parts
Agent, 0.06-0.09 part catalyst, 2-5 part cross-linking agent, 2-5 part nertralizers, 1.2-1.8 part thickening agents, 0.7-0.9 part levelling agents；
Preferably, its raw material includes by weight：120 parts of polymer polyatomic alcohols, 60 parts of graphene oxide modified polyisocyanates,
7 parts of hydrophilic chain extenders, 0.07 part of catalyst, 4 parts of cross-linking agent, 4 parts of nertralizers, 1.5 parts of thickening agents, 0.8 part of levelling agent.
5. the ballistic composite water-based polyurethane adhesive according to any one of claim 1-4, it is characterised in that poly-
Compound polyhydric alcohol includes PEPA and/or polyether polyol.
6. the ballistic composite water-based polyurethane adhesive according to any one of claim 1-4, it is characterised in that parent
Water chain extender is 2,2- dihydromethyl propionic acids or dihydroxy half ester；Preferably, hydrophilic chain extender is 2,2- dihydromethyl propionic acids.
7. the ballistic composite water-based polyurethane adhesive according to any one of claim 1-4, it is characterised in that hand over
Connection agent is trimethylolpropane or polypropylene oxide triol；Preferably, cross-linking agent is trimethylolpropane.
8. a kind of preparation side of the ballistic composite water-based polyurethane adhesive according to any one of claim 1-7
Method, it is characterised in that comprise the steps：Polymer polyatomic alcohol is added in four-hole boiling flask by proportioning, is led to in four-hole boiling flask
Enter shielding gas, Deca modified polyisocyanate carries out prepolymerization reaction, obtains base polyurethane prepolymer for use as in temperature 70-90 DEG C, in poly- ammonia
Add hydrophilic chain extender, catalyst to carry out chain extending reaction in ester performed polymer, add cross-linking agent to carry out cross-linking reaction, viscosity reduction is lowered the temperature,
Add nertralizer, the emulsifying of deionized water dispersed with stirring that modified aqueous polyurethane emulsion is obtained, in modified aqueous polyurethane emulsion
Thickening agent, levelling agent is added to obtain ballistic composite water-based polyurethane adhesive.
9. the preparation method of described ballistic composite water-based polyurethane adhesive according to claim 8, it is special
Levy and be, the heating-up temperature of prepolymerization reaction is 80 DEG C.
10. the preparation method of described ballistic composite water-based polyurethane adhesive according to claim 8, it is special
Levy and be, solid content is 20-35wt% in modified aqueous polyurethane emulsion；Preferably, contain admittedly in modified aqueous polyurethane emulsion
Measure as 30wt%.
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| CN107779161A (en) * | 2017-11-13 | 2018-03-09 | 盐城市国泰高新防备有限公司 | Graphene is modified adhesive and preparation method thereof |
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