CN110093139A - A kind of resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane and its cleaning method - Google Patents
A kind of resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane and its cleaning method Download PDFInfo
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- CN110093139A CN110093139A CN201910377986.7A CN201910377986A CN110093139A CN 110093139 A CN110093139 A CN 110093139A CN 201910377986 A CN201910377986 A CN 201910377986A CN 110093139 A CN110093139 A CN 110093139A
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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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
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/6795—Unsaturated polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
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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
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
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- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a kind of resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane, which is made of following raw materials according: polyurethane prepolymer, vinyl chloride-vinyl acetate resin, liquid nitrile rubber, fire retardant, alumina silicate, surfactant, plasticizer, catalyst, polyethylene glycol, regulator, stabilizer, Polycarbosilane, ferrocene, vinyl ester resin, SODIUM PERCARBONATE, ferric acetyl acetonade, zinc oxide, konjaku glucomannan, acetone.The resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane disclosed by the invention, using the components blending and modifying such as vinyl chloride-vinyl acetate resin, nitrile rubber, one-step method assigns adhesive magnetism, and cost is greatly lowered and improves corrosion resistance and anti-flammability, resistance to ag(e)ing;The disadvantages such as substrate removing, glue film blistering, imperfect bonding, the fault in material that general adhesive for polyurethane easily occurs are also improved, preparation method is simple, at low cost, it has excellent performance, there is magnetism well, further increase its adhesive property to iron-based material, color inhibition, long service life.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of resistance to old gluing of fire-retardant magnetism of low-cost polyurethane
Agent and its cleaning method.
Background technique
Polyurethane adhesive is an important component in the polyurethane resin currently grown rapidly, is had excellent
Different performance, is all widely used in many aspects, is one of the important species in eight big synthetic adhesives.Poly- ammonia
Ester gum stick has excellent shear strength and impact property, is suitable for various structural bonding fields, and have excellent
Flexible nature.Polyurethane gluing stick has excellent rubber property, adapts to the bonding of different heat expansion coefficient substrate,
It is formed between substrate has soft-hard transition zone, and not only bonding force is strong, while also having excellent buffering, shock-absorbing function.
The low temperature and ultralow temperature performance of polyurethane gluing stick are more than the adhesive of every other type.But polyurethane currently on the market
Adhesive heat resistance is poor, the facile hydrolysis under high temperature, high humidity.Strong acid and strong alkali resistant performance is poor, and the intensity of bonded metal is low,
It can not meet the bonding in practical application to metal.
Magnetic adhesive is added magnetic powder and curing agent etc. and is formulated generally using epoxy resin as major ingredient.Usually answer
For radio and instrument and meter industry, it is bonded magnetism component, and bonding transformer core etc., it is also possible to this adhesive
Improve the magnetic behavior of component.Magnetic element is made of magnetic material.Adhesive is in magnetic material mainly as magnetic
Dielectric material in medium, effect have two o'clock, bonding and insulation.Bonding is by powdered ferrite bonding forming;Insulation be by
Ferrous powder granules are mutually isolated, and under action of alternating magnetic field, especially under high frequency magnetic field effect, reduce the vortex damage of magnetic medium
Consumption improves quality factor.Powdered ferrite usually is added as adhesive, such as polystyrene, poly- second using certain high molecular materials
Alkene, polypropylene and alcohol-soluble phenolic resin etc., are mainly used for the adhering and sealing of magnetic original part.Such as transformer, the iron core, small of coil
Type magnetic antenna and digital-magnetic tape machine magnetic head, in addition to requiring Precision Machining, precision assembly, it is necessary to using magnetic adhesive
Bonding, sealing technology, it is desirable that it is secured, wear-resisting, stress is small, impact resistance, resistivity are high, but at present because the dispersion of magnetic magnetic powder is uneven
It is even, cause adhesive adhesive property poor, and at present on magnetic adhesive in the market wear no resistance mostly, do not have mechanics and buffer
Performance, do not have elasticity, often fall off because of weak impact failure, and generally have cushion performance adhesive binding metal
Performance again it is poor.Those skilled in the art, it would be highly desirable to a kind of fire-retardant ageing-resistant adhesive of magnetism of low-cost polyurethane is developed, with full
Higher use demand in full border production and living.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of resistance to old adhesive of fire-retardant magnetism of low-cost polyurethane is provided
And its cleaning method.
The invention is realized by the following technical scheme:
A kind of resistance to old adhesive of fire-retardant magnetism of low-cost polyurethane, is made: polyurethane prepolymer of the raw material of following parts by weight
46 ~ 59 parts, 34 ~ 39 parts of vinyl chloride-vinyl acetate resin, 3 ~ 7 parts of liquid nitrile rubber, 1 ~ 2 part of fire retardant, 7 ~ 11 parts of alumina silicate, vinyl esters tree
3 ~ 5 parts of rouge, 15 ~ 21 parts of plasticizer, 0.01 ~ 0.05 part of catalyst, 1 ~ 3 part of polyethylene glycol, 0.15 ~ 0.4 part of regulator, stabilizer
0.5 ~ 1 part, 1.5 ~ 3.5 parts of Polycarbosilane, 4.5 ~ 6.5 parts of ferrocene, 0.5 ~ 0.7 part of SODIUM PERCARBONATE, ferric acetyl acetonade 3.3 ~ 4.7
Part, 1.3 ~ 2.1 parts of zinc oxide, 1.5 ~ 2.1 parts of konjaku glucomannan, 3.5 ~ 4.1 parts of acetone.
Further, the vinyl chloride-vinyl acetate resin is the terpolymer of vinyl chloride and vinyl acetate, methyl methacrylate,
23 DEG C of its viscosity (ISO-3219) is 100 ~ 150mPas, and vinyl acetate content is 14 ~ 17%, and content of vinylchloride is 79 ~ 81%, K
Value is 50 ~ 55.
Further, the plasticizer is the mixing of dimethylbenzene, poly- decanedioic acid propylene glycol ester, tricresyl phosphate (2- chloroethyl) ester
Object, proportion are 1 ~ 2: 2 ~ 4: 3 ~ 5.
Further, the catalyst is stannous octoate, stannous oxalate, dibutyl tin dilaurate, maleic acid dibutyl
Tin, dibutyltin diacetate it is one or more.
Further, the stabilizer is at least one of zinc ricinate, triphenyl phosphite, calcium stearate;Institute
Stating fire retardant is that melamine cyanurate and decabromodiphenylethane, antimony oxide are mixed by 1: 1: 3 weight proportion
It is made after uniformly.
Further, the regulator be β-allylin, methyl diethanolamine, in 3,5-dimethylphenyl glycol extremely
Few one kind.
Further, the polyurethane prepolymer is with polypropylene glycol (molecular weight 4000 ~ 5000) and the poly- second two of allyl
Alcohol (molecular weight 1400 ~ 1700) according to parts by weight 2: 3 polyols blend 1.5mol, exist with 3 mol toluene di-isocyanate(TDI)s
Reaction 3h is made at 80 ~ 90 DEG C and under drying nitrogen protection.
Further, it is 800 ~ 1000 that the Polycarbosilane, which is molecular weight, and softening point is 160 ~ 170 DEG C;The vinyl
Ester resin is the mixed of one or more of bisphenol type epoxy vinylite and phenolic epoxy vinylite
Close object;The liquid nitrile rubber is that molecular weight is 3000 ~ 3500,23 DEG C (ISO-3219) for 1100 ~ 1500mPas, is replaced
Base is carboxyl.
A kind of resistance to old adhesive of fire-retardant magnetism of low-cost polyurethane, preparation method includes the following steps:
(1) raw material is configured, configures raw material according to weight percent;(2) ferrocene, ferric acetyl acetonade, konjaku glucomannan sugar are taken
It being put into aluminium alloy reaction kettle, is separately added into plasticizer and acetone, ultrasonic vibration 5min, stirring to solution is uniformly mixed, then plus
Enter SODIUM PERCARBONATE, polyethylene glycol and Polycarbosilane, after mixing, is placed in closed aluminium alloy reaction kettle, in 170 ~ 180 DEG C
React 16 ~ 19h during apply magnetic induction intensity be 1.2 ~ 1.4T, the alternating magnetic field that frequency is 30 ~ 40Hz, be cooled to room temperature
Afterwards to get the thick black-and-blue plasticiser mixture containing magnetic particle;(3) aluminium-alloy high-speed mixes at normal temperatures and pressures after
In machine, thick black-and-blue plasticiser mixture sequentially adds polyurethane prepolymer, vinyl chloride-vinyl acetate resin, liquid nitrile rubber, fire-retardant
Agent, alumina silicate, plasticizer, catalyst, regulator, stabilizer, the uniform 10 ~ 20min of mixed on low speed;(4) vinyl esters is added
Resin, zinc oxide, at the uniform velocity stir 20 ~ 30 minutes at 80 ~ 100 DEG C ultrasonic mixing it is uniform, be then cooled to room temperature, put into mixing
150 ~ 160 DEG C are warming up in machine, through mixing, extrusion, filling to get the resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane.
A kind of adhesive method of the resistance to old adhesive of fire-retardant magnetism of low-cost polyurethane, which is characterized in that the adhesive method
It can refer to following steps progress: first using acetone, ethyl acetate solvent scouring adherend surface, degreasing, dust, standing 1 ~
The resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane is warming up to 150 ~ 160 DEG C by 2min, and it is glutinous to coat heat after solvent volatilization is clean
Mixture, for coating weight with 0.1 ~ 0.2mm, the substrate for having coated binder should heat 0.5 ~ 1min in 2400 ~ 2450MHZ of microwave,
After taking-up pressure bonded to get.
Beneficial effects of the present invention:
The present invention uses solvent-thermal method, and additional alternating magnetic field has synthesized the plasticiser mixture containing magnetic nano-particle, material shape
Looks reach preferably, even particle size, good dispersion.People is added due to vinyl acetate, resin is made to have internal plasticization group, because
And the mobility under resin melting state, the flexibility of adhesive are improved, and reduce adhesive melting temperature.Processing temperature
It decreases, impact strength improves, and improves adhesive in the plasticization effect of plasticizer, has synergistic effect, further
Plasticization effect is improved, reduces the usage amount of plasticizer, and close with the solubility parameters of polyurethane, compatibility is good, is greatly lowered
The production cost of adhesive, due to the presence of vinyl chloride group, resistance to ag(e)ing, color inhibition, the anti-flammability of adhesive are significantly mentioned
Height, the good fluidity under molten condition, makes adhesive have good service performance.One-step method hydro-thermal composite algorithm controlled syntheses are magnetic
Nanoparticle, magnetic good dispersion apply additional alternating magnetic field, are directly originally to generate nano-magnetic microsphere, avoid magnetism
The reunion of microballoon during the growth process, improves its dimensional homogeneity, by controlling the size of nano-magnetic microsphere, further mentions
High nano material dimensional effect, and then enhance the magnetism of its material, directly plasticizer mixing of the synthesis containing magnetic nano-particle
Object, production operation step is simple, and the magnetism of adhesive not only can be improved, and magnetic nano-particle can also improve the heat-resisting of adhesive
Property, scantling shrinkage get a promotion, and remaining polyethylene glycol in synthesis process can be used as the profit in material processing
Lubrication prescription not will cause waste material and waste, and kill two birds with one stone, and reduce production cost, and the introducing of nano ferriferrous oxide improves indirectly
The light aging resisting property of adhesive.The surface of material pair is relatively smooth, and wearability is good.
Magnetic field has stirring action to reaction solution body, this can accelerate to radiate, and improves the generation of ferroso-ferric oxide microballoon
Rate rate, traditional four anti-three-iron microballoon of oxidation of hydro-thermal method preparation do not stir, and particle is easy to reunite.Secondly, stirring action
Can promote the convection current inside solution, on magnetic particle plasticizer dispersion process generate direct influence.The aggravation of convection current makes
Heat transfer rate improves, thus can reduce the temperature gradient in solution so that the Temperature Distribution in reaction kettle is more uniform.Outside
Add rotating excitation field to will affect the growth of magnetic particle, enhances magnetic particle in the diffusion of solution, influence the big of particle
Small, shape, and then improve the magnetism of adhesive.Ferrocene and ferric acetyl acetonade are source of iron, and excessive ferric acetyl acetonade can also glue
The adhesion strength of glutinous agent;Vinyl ester resin and liquid nitrile rubber collaboration promote to improve the flexibility of adhesive and corrosion-resistant
Property.Alumina silicate has photoextinction, can be used as a kind of delustering agent of economy, has good scrub resistance, weatherability, in addition can contract
Short surface drying time improves the hydrolytic resistance of adhesive, additionally it is possible to hardness, whiteness, wearability, weatherability, storage stability are improved,
Further increase the anti-flammability of adhesive.
The present invention has the advantage that the resistance to old glue of the fire-retardant magnetism of low-cost polyurethane disclosed by the invention compared with prior art
Containing being generated between very highly polar and chemically active isocyanate group and urethano, with the material containing active hydrogen in glutinous agent
Hydrogen bond action enhances intramolecular force, can make to be bonded stronger, there is excellent bonding force to multiple material;Good manufacturability,
It is easy infiltration, working life is long, and technique for sticking is easy, and operating characteristics is good;There is no side reaction generation, being not easy, which generates adhesive layer, lacks
It falls into;With good impact resistance, vibration resistance, endurance, wear-resisting, oil resistant, solvent resistant, chemical-resistant resistance, resistance to ozone and resistance to thin
The performances such as bacterium.Low temperature and ultralow temperature performance are more than the adhesive of every other type, and adhesive strength when low temperature is high.Heat resistance
Good, hardly possible hydrolyzes and reduces adhesive strength under high temperature, high humidity.Strong acid and strong alkali resistant performance is good.To not water sensitive, glue-line is not easy to produce
The intensity of anger bubble bonded metal is high, and ageing-resistant performance is prominent, has magnetic well, anti-flammability energy consumption, and inexpensive performance is excellent
Gesture is prominent, far below adhesive for polyurethane in the market.
Specific embodiment
Illustrate the present invention with specific embodiment below, but is not limitation of the present invention.
Embodiment 1
A kind of resistance to old adhesive of fire-retardant magnetism of low-cost polyurethane, is made: polyurethane prepolymer of the raw material of following parts by weight
59 parts, 39 parts of vinyl chloride-vinyl acetate resin, 7 parts of liquid nitrile rubber, 2 parts of fire retardant, 11 parts of alumina silicate, 5 parts of vinyl ester resin, plasticizer
21 parts, 0.05 part of catalyst, 3 parts of polyethylene glycol, 0.4 part of regulator, 1 part of stabilizer, 3.5 parts of Polycarbosilane, ferrocene 6.5
Part, 0.7 part of SODIUM PERCARBONATE, 4.7 parts of ferric acetyl acetonade, 2.1 parts of zinc oxide, 2.1 parts of konjaku glucomannan, 4.1 parts of acetone.
Further, the vinyl chloride-vinyl acetate resin is the terpolymer of vinyl chloride and vinyl acetate, methyl methacrylate,
23 DEG C of its viscosity (ISO-3219) is 100 ~ 150mPas, and vinyl acetate content is 14 ~ 17%, and content of vinylchloride is 79 ~ 81%, K
Value is 50 ~ 55.
Further, the plasticizer is the mixing of dimethylbenzene, poly- decanedioic acid propylene glycol ester, tricresyl phosphate (2- chloroethyl) ester
Object, proportion 1: 2: 3.
Further, the catalyst is stannous octoate, stannous oxalate, dibutyl tin dilaurate, maleic acid dibutyl
Tin, the mixture of dibutyltin diacetate, weight part ratio 1: 3: 1: 2: 1.
Further, the stabilizer is zinc ricinate, triphenyl phosphite, the mixture in calcium stearate, weight
Number ratio is 1: 2: 1;The fire retardant is that melamine cyanurate and decabromodiphenylethane, antimony oxide press 1: 1: 3
Weight proportion be mixed evenly after be made.
Further, the regulator be β-allylin, it is methyl diethanolamine, mixed in 3,5-dimethylphenyl glycol
Close object, weight part ratio 1: 1: 1.
Further, the polyurethane prepolymer is with polypropylene glycol (molecular weight 4000 ~ 5000) and the poly- second two of allyl
Alcohol (molecular weight 1400 ~ 1700) according to parts by weight 2: 3 polyols blend 1.5mol, exist with 3 mol toluene di-isocyanate(TDI)s
Reaction 3h is made at 80 ~ 90 DEG C and under drying nitrogen protection.
Further, it is 800 ~ 1000 that the Polycarbosilane, which is molecular weight, and softening point is 160 ~ 170 DEG C;The vinyl
Ester resin is the mixed of one or more of bisphenol type epoxy vinylite and phenolic epoxy vinylite
Close object;The liquid nitrile rubber is that molecular weight is 3000 ~ 3500,23 DEG C (ISO-3219) for 1100 ~ 1500mPas, is replaced
Base is carboxyl.
A kind of resistance to old adhesive of fire-retardant magnetism of low-cost polyurethane, preparation method includes the following steps:
(1) raw material is configured, configures raw material according to weight percent;(2) ferrocene, ferric acetyl acetonade, konjaku glucomannan sugar are taken
It being put into aluminium alloy reaction kettle, is separately added into plasticizer and acetone, ultrasonic vibration 5min, stirring to solution is uniformly mixed, then plus
Enter SODIUM PERCARBONATE, polyethylene glycol and Polycarbosilane, after mixing, is placed in closed aluminium alloy reaction kettle, is reacted in 180 DEG C
Apply during 19h magnetic induction intensity be 1.4T, the alternating magnetic field that frequency is 40Hz, to get containing being magnetic after being cooled to room temperature
The thick black-and-blue plasticiser mixture of particle;(3) after at normal temperatures and pressures in aluminium-alloy high-speed mixing machine, thick blue-black
Color plasticiser mixture sequentially adds polyurethane prepolymer, vinyl chloride-vinyl acetate resin, liquid nitrile rubber, fire retardant, alumina silicate, plasticising
Agent, catalyst, regulator, stabilizer, the uniform 20min of mixed on low speed;(4) vinyl ester resin, zinc oxide are added, is at the uniform velocity stirred
Mix 30 minutes at 100 DEG C ultrasonic mixing it is uniform, be then cooled to room temperature, put into mixer and be warming up to 160 DEG C, through mixing,
It squeezes out, is filling to get the resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane.
A kind of adhesive method of the resistance to old adhesive of fire-retardant magnetism of low-cost polyurethane, which is characterized in that the adhesive method
It can refer to following steps progress: first using acetone, ethyl acetate solvent scouring adherend surface, degreasing, dust, stand
The resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane is warming up to 160 DEG C by 2min, coats heat bonding after solvent volatilization is clean
Agent, for coating weight with 0.2mm, the substrate for having coated binder should heat 1min in microwave 2450MHZ, and pressure is glued after taking-up
Knot to get.
Embodiment 2
A kind of resistance to old adhesive of fire-retardant magnetism of low-cost polyurethane, is made: polyurethane prepolymer of the raw material of following parts by weight
46 parts, 34 parts of vinyl chloride-vinyl acetate resin, 3 parts of liquid nitrile rubber, 1 part of fire retardant, 7 parts of alumina silicate, 3 parts of vinyl ester resin, plasticizer
15 parts, 0.03 part of catalyst, 1 part of polyethylene glycol, 0.15 part of regulator, 0.5 part of stabilizer, 1.5 parts of Polycarbosilane, ferrocene
4.5 parts, 0.5 part of SODIUM PERCARBONATE, 3.3 parts of ferric acetyl acetonade, 1.3 parts of zinc oxide, konjaku glucomannan 1.5,3.5 parts of acetone.
Further, the vinyl chloride-vinyl acetate resin is the terpolymer of vinyl chloride and vinyl acetate, methyl methacrylate,
23 DEG C of its viscosity (ISO-3219) is 100 ~ 150mPas, and vinyl acetate content is 14 ~ 17%, and content of vinylchloride is 79 ~ 81%, K
Value is 50 ~ 55.
Further, the plasticizer is the mixing of dimethylbenzene, poly- decanedioic acid propylene glycol ester, tricresyl phosphate (2- chloroethyl) ester
Object, proportion 2: 4: 5.
Further, the catalyst is stannous octoate, stannous oxalate, dibutyl tin dilaurate, maleic acid dibutyl
Tin, the mixture of dibutyltin diacetate, weight part ratio 1: 1: 1: 1: 1.
Further, the stabilizer is the mixture of zinc ricinate, triphenyl phosphite, calcium stearate, parts by weight
Number ratio is 1: 1: 3;The fire retardant is melamine cyanurate and decabromodiphenylethane, antimony oxide by 1: 1: 3
Weight proportion is made after being mixed evenly.
Further, the regulator is the mixing of β-allylin, methyl diethanolamine, 3,5-dimethylphenyl glycol
Object, weight part ratio 1: 1: 3.
Further, the polyurethane prepolymer is with polypropylene glycol (molecular weight 4000 ~ 5000) and the poly- second two of allyl
Alcohol (molecular weight 1400 ~ 1700) according to parts by weight 2: 3 polyols blend 1.5mol, exist with 3 mol toluene di-isocyanate(TDI)s
Reaction 3h is made at 80 ~ 90 DEG C and under drying nitrogen protection.
Further, it is 800 ~ 1000 that the Polycarbosilane, which is molecular weight, and softening point is 160 ~ 170 DEG C;The vinyl
Ester resin is bisphenol type epoxy vinylite;The liquid nitrile rubber is that molecular weight is 3000 ~ 3500,23 DEG C of (ISO-
It 3219) is 1100 ~ 1500mPas, substituent group is carboxyl.
A kind of resistance to old adhesive of fire-retardant magnetism of low-cost polyurethane, preparation method includes the following steps:
(1) raw material is configured, configures raw material according to weight percent;(2) ferrocene, ferric acetyl acetonade, konjaku glucomannan sugar are taken
It being put into aluminium alloy reaction kettle, is separately added into plasticizer and acetone, ultrasonic vibration 5min, stirring to solution is uniformly mixed, then plus
Enter SODIUM PERCARBONATE, polyethylene glycol and Polycarbosilane, after mixing, is placed in closed aluminium alloy reaction kettle, is reacted in 170 DEG C
Apply during 16h magnetic induction intensity be 1.2T, the alternating magnetic field that frequency is 30Hz, to get containing being magnetic after being cooled to room temperature
The thick black-and-blue plasticiser mixture of particle;(3) after at normal temperatures and pressures in aluminium-alloy high-speed mixing machine, thick blue-black
Color plasticiser mixture sequentially adds polyurethane prepolymer, vinyl chloride-vinyl acetate resin, liquid nitrile rubber, fire retardant, alumina silicate, plasticising
Agent, catalyst, regulator, stabilizer, the uniform 10min of mixed on low speed;(4) vinyl ester resin, zinc oxide are added, is at the uniform velocity stirred
Mix 230 minutes at 100 DEG C ultrasonic mixing it is uniform, be then cooled to room temperature, put into mixer and be warming up to 160 DEG C, through mixing,
It squeezes out, is filling to get the resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane.
A kind of adhesive method of the resistance to old adhesive of fire-retardant magnetism of low-cost polyurethane, which is characterized in that the adhesive method
It can refer to following steps progress: first using acetone, ethyl acetate solvent scouring adherend surface, degreasing, dust, standing 1 ~
The resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane is warming up to 160 DEG C by 2min, coats heat bonding after solvent volatilization is clean
Agent, for coating weight with 0.2mm, the substrate for having coated binder should heat 1min in microwave 2450MHZ, and pressure is glued after taking-up
Knot to get.
Comparative example 1
This comparative example compared with Example 2, weighs in step in raw material, saves liquid nitrile rubber ingredient, method in addition to this
Step is all the same.
Comparative example 2
This comparative example compared with Example 2, in step (2), saves additional alternating magnetic field, method and step in addition to this is homogeneous
Together.
Comparative example 3
This comparative example compared with Example 2, weighs in step in raw material, saves Polycarbosilane ingredient, method and step in addition to this
It is all the same.
Comparative example 4
This comparative example compared with Example 2, weighs in step in raw material, saves vinyl chloride-vinyl acetate resin ingredient, method and step in addition to this
It is all the same.
Comparative example 5
This comparative example compared with Example 2, weighs in step in raw material, saves silicic acid aluminium component, and method and step in addition to this is equal
It is identical.
The performance test results of the resistance to old adhesive of the table fire-retardant magnetism of 1 each embodiment and comparative example low-cost polyurethane
Note: comparative test testing scheme are as follows: using magnetism adhesive made from embodiment and comparative example respectively together with four pieces of strips
Longitudinally bonding is connected into combination powder core to non-crystal block, turns to inductance, the dynamic magnetic of the powder core as made from the test of B-H analyzer
Conductance (μ) wherein the non-crystal block of strip select magnetic conductivity be 60 the non-crystal block of 60*20*20 strip.
The measurement of viscosity is measured by the measuring method of GB/T2794 adhesive viscosity;GB/T7124 is pressed in the measurement of shear strength
In pertinent regulations measurement;Oxygen index (OI) measures burning behavior according to GB/T2406.1-2008 plastics oxygen index method;GB/
The non-volatile assay of T2793-1995 adhesive;GB/T3186-2006 colored paint, varnish and colored paint and varnish are taken with raw material
Sample;The measurement of tensile strength according to G/T6329-1996 adhesive banjo fixing butt jointing tensile strength measurement;Density: GB/T6750-
The measurement of 2007 paint and varnish density, bottle method;The pH value of GB/T14518-1993 adhesive measures;Limits of harmful substances
IMO FTPC part 2 ship material flue gas and toxicity test.
Claims (10)
1. a kind of resistance to old adhesive of fire-retardant magnetism of low-cost polyurethane, which is characterized in that be made of the raw material of following parts by weight:
46 ~ 59 parts of polyurethane prepolymer, 34 ~ 39 parts of vinyl chloride-vinyl acetate resin, 3 ~ 7 parts of liquid nitrile rubber, 1 ~ 2 part of fire retardant, alumina silicate 7 ~ 11
Part, 3 ~ 5 parts of vinyl ester resin, 15 ~ 21 parts of plasticizer, 0.01 ~ 0.05 part of catalyst, 1 ~ 3 part of polyethylene glycol, regulator 0.15
~ 0.4 part, 0.5 ~ 1 part of stabilizer, 1.5 ~ 3.5 parts of Polycarbosilane, 4.5 ~ 6.5 parts of ferrocene, 0.5 ~ 0.7 part of SODIUM PERCARBONATE, acetyl
3.3 ~ 4.7 parts of acetone iron, 1.3 ~ 2.1 parts of zinc oxide, 1.5 ~ 2.1 parts of konjaku glucomannan, 3.5 ~ 4.1 parts of acetone.
2. the resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane according to claim 1, which is characterized in that the chlorine vinegar
Resin is the terpolymer of vinyl chloride and vinyl acetate, methyl methacrylate, 23 DEG C of viscosity (ISO-3219) for 100 ~
150mPas, vinyl acetate content are 14 ~ 17%, and content of vinylchloride is that 79 ~ 81%, K value is 50 ~ 55.
3. the resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane according to claim 1, which is characterized in that the plasticising
Agent is the mixture of dimethylbenzene, poly- decanedioic acid propylene glycol ester, tricresyl phosphate (2- chloroethyl) ester, and proportion is 1 ~ 2: 2 ~ 4: 3 ~ 5.
4. the resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane according to claim 1, which is characterized in that the catalysis
Agent be stannous octoate, stannous oxalate, dibutyl tin dilaurate, dibutyitin maleate, one kind of dibutyltin diacetate or
It is a variety of.
5. the resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane according to claim 1, which is characterized in that the stabilization
Agent is at least one of zinc ricinate, triphenyl phosphite, calcium stearate;The fire retardant is melamine cyanurate
It is made after being mixed evenly with decabromodiphenylethane, antimony oxide by 1: 1: 3 weight proportion.
6. the resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane according to claim 1, which is characterized in that the regulator
For at least one of β-allylin, methyl diethanolamine, 3,5-dimethylphenyl glycol.
7. the resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane according to claim 1, which is characterized in that the polyurethane
Prepolymer is with polypropylene glycol (molecular weight 4000 ~ 5000) and allyl polyglycol (molecular weight 1400 ~ 1700) according to weight
The polyols blend 1.5mol of number 2: 3 is anti-at 80 ~ 90 DEG C and under drying nitrogen protection with 3 mol toluene di-isocyanate(TDI)s
3h is answered to be made.
8. the resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane according to claim 1, which is characterized in that the poly- carbon silicon
Alkane is that molecular weight is 800 ~ 1000, and softening point is 160 ~ 170 DEG C;The vinyl ester resin is bisphenol type epoxy vinyl tree
The mixture of one or more of rouge and phenolic epoxy vinylite;The liquid nitrile rubber is molecule
It is 1100 ~ 1500mPas that amount, which is 3000 ~ 3500,23 DEG C (ISO-3219), and substituent group is carboxyl.
9. the resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane according to claim 1, which is characterized in that preparation method
The following steps are included:
(1) raw material is configured, configures raw material according to the weight percent described in claim 1;(2) ferrocene, acetylacetone,2,4-pentanedione are taken
Iron, konjaku glucomannan sugar are put into aluminium alloy reaction kettle, are separately added into plasticizer and acetone, ultrasonic vibration 5min, stirring is extremely
Solution is uniformly mixed, and adds SODIUM PERCARBONATE, polyethylene glycol and Polycarbosilane, after mixing, is placed in closed aluminium alloy reaction
In kettle, application magnetic induction intensity is 1.2 ~ 1.4T during 16 ~ 19h is reacted in 170 ~ 180 DEG C, and frequency is the friendship of 30 ~ 40Hz
Varying magnetic field, to get the thick black-and-blue plasticiser mixture containing magnetic particle after being cooled to room temperature;(3) normal in room temperature after
Depress aluminium-alloy high-speed mixing machine in, thick black-and-blue plasticiser mixture sequentially add polyurethane prepolymer, vinyl chloride-vinyl acetate resin,
Liquid nitrile rubber, fire retardant, alumina silicate, plasticizer, catalyst, regulator, stabilizer, the uniform 10 ~ 20min of mixed on low speed;
(4) vinyl ester resin, zinc oxide are added, at the uniform velocity stir 20 ~ 30 minutes at 80 ~ 100 DEG C ultrasonic mixing it is uniform, then drop
It warms to room temperature, puts into mixer and be warming up to 150 ~ 160 DEG C, through mixing, extrusion, filling to get the fire-retardant magnetic of low-cost polyurethane
The resistance to old adhesive of property.
10. using the adhesive method of the resistance to old adhesive of the fire-retardant magnetism of the described in any item low-cost polyurethanes of claim 1 ~ 9,
It is characterized in that, the adhesive method is carried out referring to following steps: first using acetone, ethyl acetate solvent scouring adherend surface,
It degreases, dust, stands 1 ~ 2min, the resistance to old adhesive of the fire-retardant magnetism of low-cost polyurethane is warming up to 150 ~ 160 DEG C, to molten
The hot binder of coating after agent volatilization is clean, coating weight with 0.1 ~ 0.2mm, coated binder substrate should microwave 2400 ~
In 2450MHZ heat 0.5 ~ 1min, after taking-up pressure bonded to get.
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CN114940005A (en) * | 2022-07-04 | 2022-08-26 | 张家港飞腾复合新材料股份有限公司 | High-heat-insulation heat-preservation composite board and production process thereof |
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Cited By (2)
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CN114940005A (en) * | 2022-07-04 | 2022-08-26 | 张家港飞腾复合新材料股份有限公司 | High-heat-insulation heat-preservation composite board and production process thereof |
CN114940005B (en) * | 2022-07-04 | 2024-06-04 | 张家港飞腾复合新材料股份有限公司 | High-heat-insulation heat-preservation composite board and production process thereof |
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