CN107987778B - A kind of household electrical appliances reaction type polyurethane hot-melt adhesive and preparation method thereof - Google Patents
A kind of household electrical appliances reaction type polyurethane hot-melt adhesive and preparation method thereof Download PDFInfo
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- CN107987778B CN107987778B CN201711291103.8A CN201711291103A CN107987778B CN 107987778 B CN107987778 B CN 107987778B CN 201711291103 A CN201711291103 A CN 201711291103A CN 107987778 B CN107987778 B CN 107987778B
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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
-
- 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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
-
- 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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4202—Two or more polyesters of different physical or chemical nature
-
- 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
-
- 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
- C08G18/62—Polymers of compounds having carbon-to-carbon double bonds
- C08G18/6216—Polymers of alpha-beta ethylenically unsaturated carboxylic acids or of derivatives thereof
- C08G18/625—Polymers of alpha-beta ethylenically unsaturated carboxylic acids; hydrolyzed polymers of esters of these acids
-
- 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
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
Abstract
The present invention provides a kind of household electrical appliances reaction type polyurethane hot-melt adhesive and preparation method thereof, the household electrical appliances are with reaction type polyurethane hot-melt adhesive by including that the raw material of following components is prepared: 100 parts by weight of polyester polyol~250 parts by weight；1 parts by weight of polyether polyol~150 parts by weight；50 parts by weight of isocyanates~100 parts by weight；70 parts by weight of tackifying resin~150 parts by weight；1 parts by weight of latent curing agent~10 parts by weight；1 parts by weight of antioxidant~5 parts by weight；5 parts by weight of coupling agent~10 parts by weight；0.01 parts by weight of catalyst~0.1 parts by weight；The polyester polyol by mass ratio be 1:(0.25~1.5) crystalline polyester polyols and amorphous polyester polyalcohol；The latent curing agent is aldimine latent curing agent or polybenzobisoxazole alkane latent curing agent.Compared with prior art, household electrical appliances provided by the invention use certain content component with reaction type polyurethane hot-melt adhesive, realize preferable interaction, obtained product solidification process bubble-free, and have excellent adhesion energy and water-fast, chemical resistance.
Description
Technical field
The present invention relates to polyurethane sealant technical fields, are to be related to a kind of poly- ammonia of household electrical appliances response type more specifically
Ester hot melt adhesive and preparation method thereof.
Background technique
Reaction type polyurethane hot-melt adhesive (abbreviation PUR): pre- containing end NCO polyurethane in moisture-curable polyurethane hot melt adhesive ingredient
Aggressiveness generates under the condition of high temperature, moisture or active hydrogen object in active functional group and air or on adherend after heating
Qualitative response and form part cross-linked structure, make the performances such as adhesive strength, chemicals-resistant, heat-resisting, hydrolysis better than general heat
Melten gel.Reaction type polyurethane hot-melt adhesive is widely used in the industries such as carpenter, weaving, automobile, electronics, household electrical appliances.Reaction type polyurethane heat
The synthesis of melten gel is one and chemically reacts the process combined with physical mixed.Reaction type polyurethane hot-melt adhesive in the prior art
The chemical reaction of synthesis generally refers to reacting for isocyanates and multicomponent alcoholics compound, and wherein isocyanates uses hexichol
Dicyclohexylmethane diisocyanate (abbreviation MDI), and multicomponent alcoholics compound be number average molecular 1000~5000 polyester and
Polyethers.
Currently, many household electrical appliances, for example be selection pressure sensitive adhesive tape mostly when the fixation of cover plate for washing machine, panel of refrigerator, and
Pressure sensitive adhesive tape generally requires manually to turn to match, and efficiency is relatively slow and overall cost is higher；In addition industrial pressure sensitive adhesive tape is due to just gluing
Power is final bonding force, and pressure (the pressure destruction reality of 96kg or so can only be born in terms of terms of mechanics especially pressure-bearing
Test), while the result in alcohol, detergent immersion experiment is also not highly desirable.From 2015, Haier, U.S. water chestnut, Hisense etc.
Domestic household electrical appliances industry mark post enterprise has begun using reaction type polyurethane hot-melt adhesive and replaces traditional industrial pressure sensitive adhesive tape, and
And there is actual use on the colorful glittering glass panel of certain refrigerators.
But reaction type polyurethane hot-melt adhesive in the prior art can generate bubble in the curing process, cause glue-line table
Face is uneven, and adhesive property is poor, does not have water-fast, chemical resistance.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of household electrical appliances reaction type polyurethane hot-melt adhesive and its preparation sides
Method, reaction type polyurethane hot-melt adhesive solidification process bubble-free provided by the invention, and have excellent adhesion can and it is resistance to
Water, chemical resistance.
The present invention provides a kind of household electrical appliances reaction type polyurethane hot-melt adhesives, by the raw material preparation including following components
At:
100 parts by weight of polyester polyol~250 parts by weight；
1 parts by weight of polyether polyol~150 parts by weight；
50 parts by weight of isocyanates~100 parts by weight；
70 parts by weight of tackifying resin~150 parts by weight；
1 parts by weight of latent curing agent~10 parts by weight；
1 parts by weight of antioxidant~5 parts by weight；
5 parts by weight of coupling agent~10 parts by weight；
0.01 parts by weight of catalyst~0.1 parts by weight；
The polyester polyol by mass ratio be 1:(0.25~1.5) crystalline polyester polyols and amorphous polyester it is more
First alcohol；
The latent curing agent is aldimine latent curing agent or polybenzobisoxazole alkane latent curing agent.
Preferably, the crystalline polyester polyols be selected from succinic acid-butanediol ester glycol, tetramethylene adipate glycol,
One of pure and mild adipic acid hexylene glycol esterdiol of ethanedioic acid glycol ester two is a variety of.
Preferably, the amorphous polyester polyalcohol is selected from ethylene glycol/butanediol/diethylene glycol (DEG)/adipat copolymers, two sweet
Alcohol/phthalic anhydride copolymer, neopentyl glycol/phthalic anhydride copolymer, ethylene glycol/neopentyl glycol/succinic acid/isophthalic acid copolymers and two
One of glycol/trimethylolpropane/adipat copolymers are a variety of.
Preferably, the tackifying resin is selected from acrylic resin, hydroxyl terminated polyurethane, Petropols, polyolefins and increases
One of viscosity resin and terpene resin are a variety of.
Preferably, the antioxidant is selected from 2,6-di-tert-butyl p-methylphenol, four [β-(3,5- di-t-butyl -4- hydroxyls
Phenyl) propionic acid] pentaerythritol ester, β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecyl alcohol ester, three (bis- uncles of 2.4-
Butyl phenyl) one of phosphite ester and bis- (3,5- di-tert-butyl-hydroxy phenyl) thioethers or a variety of.
Preferably, the coupling agent is selected from γ-mercaptopropyl trimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-
Glycidyl ether oxygen propyl trimethoxy silicane, vinyltrimethoxysilane, γ-isocyanate group propyl-triethoxysilicane
With one of N- β-(aminoethyl)-γ-aminopropyltrimethoxysilane or a variety of.
Preferably, the catalyst is selected from dibutyl tin dilaurate, organo-bismuth, triethylenediamine and dimorpholine base two
One of ethylether is a variety of.
The present invention also provides a kind of preparation sides of household electrical appliances reaction type polyurethane hot-melt adhesive described in above-mentioned technical proposal
Method, comprising the following steps:
After crystalline polyester polyols, polyether polyol, amorphous polyester polyalcohol, antioxidant and tackifying resin are mixed
Dehydration, adds isocyanates and is reacted, and is eventually adding latent curing agent, coupling agent and catalyst and carries out vacuum defoamation, dispersion
Reaction type polyurethane hot-melt adhesive is obtained after uniformly.
Preferably, the temperature of the dehydration be 105 DEG C~130 DEG C, vacuum degree≤- 0.095MPa, the time be 1.5h~
2.5h。
Preferably, the temperature of the reaction is 93 DEG C~98 DEG C, and the time is 1h~3h.
The present invention provides a kind of household electrical appliances reaction type polyurethane hot-melt adhesive and preparation method thereof, the household electrical appliances response type
Polyurethane hot melt is by including that the raw material of following components is prepared: 100 parts by weight of polyester polyol~250 parts by weight；Polyethers
1 parts by weight of polyalcohol~150 parts by weight；50 parts by weight of isocyanates~100 parts by weight；70 parts by weight of tackifying resin~150 weights
Measure part；1 parts by weight of latent curing agent~10 parts by weight；1 parts by weight of antioxidant~5 parts by weight；5 parts by weight of coupling agent~10 weight
Part；0.01 parts by weight of catalyst~0.1 parts by weight；The polyester polyol by mass ratio be 1:(0.25~1.5) crystallinity
The pure and mild amorphous polyester polyalcohol of polyester polyols；The latent curing agent is aldimine latent curing agent or polybenzobisoxazole alkane latent curing agent.With
The prior art is compared, and household electrical appliances provided by the invention use certain content component with reaction type polyurethane hot-melt adhesive, is realized preferable
Interaction, obtained product solidification process bubble-free, and have excellent adhesion energy and water-fast, chemical resistance.
The experimental results showed that household electrical appliances provided by the invention reaction type polyurethane hot-melt adhesive solidification process bubble-free, and product is viscous
Relay is 80kg~92kg, and the bonding force after detergent immersion is 60kg~78kg, alcohol impregnate after bonding force be 36kg~
50kg。
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts, belongs to this hair
The range of bright protection.
The present invention provides a kind of household electrical appliances reaction type polyurethane hot-melt adhesives, by the raw material preparation including following components
At:
100 parts by weight of polyester polyol~250 parts by weight；
1 parts by weight of polyether polyol~150 parts by weight；
50 parts by weight of isocyanates~100 parts by weight；
70 parts by weight of tackifying resin~150 parts by weight；
1 parts by weight of latent curing agent~10 parts by weight；
1 parts by weight of antioxidant~5 parts by weight；
5 parts by weight of coupling agent~10 parts by weight；
0.01 parts by weight of catalyst~0.1 parts by weight；
The polyester polyol by mass ratio be 1:(0.25~1.5) crystalline polyester polyols and amorphous polyester it is more
First alcohol；
The latent curing agent is aldimine latent curing agent or polybenzobisoxazole alkane latent curing agent.
In the present invention, the polyester polyol by mass ratio be 1:(0.25~1.5) crystalline polyester polyols and
Amorphous polyester polyalcohol.In the present invention, the mass ratio of the crystalline polyester polyols and amorphous polyester polyalcohol is
1:(0.25~1.5), preferably 1:(0.85~1.5).In the present invention, the crystalline polyester polyols primarily serve raising
The effect of initial bonding force, while helping to shorten the open hour of hot melt adhesive；Meanwhile cooperating amorphous polyester polyalcohol, at it
Under his component collective effect, reaction type polyurethane hot-melt adhesive can be improved to the adhesive property of polar substrates, and improve water-fast, resistance to
Chemicals energy.
In the present invention, the hydroxyl value of the crystalline polyester polyols is preferably 21KOH/mg~56KOH/mg, more preferably
For 31KOH/mg~36KOH/mg, water content is preferably smaller than equal to 0.1%.In the present invention, the crystalline polyester polyols
Be preferably selected from succinic acid-butanediol ester glycol, tetramethylene adipate glycol, the pure and mild adipic acid of ethanedioic acid glycol ester two oneself two
One of alcohol esterdiol is a variety of, more preferably adipic acid hexylene glycol esterdiol or succinic acid-butanediol ester glycol.The present invention
The source of the polyester polyol is not particularly limited, using above-mentioned succinic acid-butanediol ester well known to those skilled in the art
The commercial goods of glycol, tetramethylene adipate glycol, the pure and mild adipic acid hexylene glycol esterdiol of ethanedioic acid glycol ester two.
In the present invention, the hydroxyl value of the amorphous polyester polyalcohol is preferably 18KOH/mg~56KOH/mg, more preferably
For 21KOH/mg~36KOH/mg, water content is preferably smaller than equal to 0.1%.In the present invention, the amorphous polyester polyalcohol
It is preferably selected from ethylene glycol/butanediol/diethylene glycol (DEG)/adipat copolymers, diethylene glycol (DEG)/phthalic anhydride copolymer, neopentyl glycol/phthalic anhydride copolymerization
Object, ethylene glycol/neopentyl glycol/succinic acid/isophthalic acid copolymers and diethylene glycol (DEG)/trimethylolpropane/adipat copolymers
One of or a variety of, more preferably neopentyl glycol/phthalic anhydride copolymer or ethylene glycol/neopentyl glycol/succinic acid/M-phthalic acid
Copolymer；The present invention is not particularly limited the type of the amorphous polyester polyalcohol and source, using meeting above-mentioned parameter
It is required that amorphous polyester polyalcohol commercial goods.
In the present invention, the household electrical appliances reaction type polyurethane hot-melt adhesive includes 100 parts by weight~250 parts by weight polyester
Polyalcohol, preferably 185 parts by weight~250 parts by weight.
In the present invention, the hydroxyl value of the polyether polyol is preferably 21KOH/mg~112KOH/mg, more preferably
56KOH/mg, water content are preferably smaller than equal to 0.1%.In the present invention, the polyether polyol is preferably selected from polypropylene oxide
One of glycol, the pure and mild polytetrahydrofuran ether glycol of polypropylene oxide three are a variety of；The present invention is to the polyether polyol
Type and source are not particularly limited, using the commercial goods for the polyether polyol for meeting above-mentioned parameter requirement.In this hair
In bright, the household electrical appliances reaction type polyurethane hot-melt adhesive includes 1 parts by weight~150 parts by weight polyether polyol, and preferably 100
Parts by weight~150 parts by weight.
In the present invention, the isocyanates is preferably selected from toluene di-isocyanate(TDI) (TDI), isophorone diisocyanate
(IPDI), two isocyanide of methyl diphenylene diisocyanate (MDI), dicyclohexyl methyl hydride diisocyanate (HMDI) and hexa-methylene
One of acid esters (HDI) is a variety of, more preferably methyl diphenylene diisocyanate (MDI).The present invention is to the isocyanic acid
The source of ester is not particularly limited, using above-mentioned toluene di-isocyanate(TDI) (TDI) well known to those skilled in the art, isophorone
Diisocyanate (IPDI), methyl diphenylene diisocyanate (MDI), dicyclohexyl methyl hydride diisocyanate (HMDI) He Liuya
The commercial goods of methyl diisocyanate (HDI).In the present invention, the household electrical appliances include with reaction type polyurethane hot-melt adhesive
50 parts by weight~100 parts by weight isocyanates, preferably 65 parts by weight~90 parts by weight.
In the present invention, the tackifying resin is preferably selected from acrylic resin, hydroxyl terminated polyurethane, Petropols, gathers
One of olefines tackifying resin and terpene resin are a variety of, more preferably acrylic resin.The present invention sets the thickening
The source of rouge is not particularly limited, using above-mentioned acrylic resin well known to those skilled in the art, hydroxyl terminated polyurethane, stone
The commercial goods of oleoresin, polyolefins tackifying resin and terpene resin.In the present invention, the tackifying resin mainly rises
To the effect for improving melt viscosity, reducing mobility.In the present invention, household electrical appliances reaction type polyurethane hot-melt adhesive includes 70
Parts by weight~150 parts by weight tackifying resin, preferably 75 parts by weight~100 parts by weight.
In the present invention, the latent curing agent is aldimine latent curing agent or polybenzobisoxazole alkane latent curing agent.The present invention is to described
The source of latent curing agent is not particularly limited, using above-mentioned aldimine latent curing agent well known to those skilled in the art and polybenzobisoxazole alkane
The commercial goods of latent curing agent.In the present invention, the latent curing agent can cooperate with other components, make to solidify
Latent curing agent is reacted prior to polyurethane with steam in journey, is formed double ammonia structures, then react to form cross-linked structure with PUR, is prevented
Only curable adhesive layer generates bubble and influences properties of product.In the present invention, household electrical appliances reaction type polyurethane hot-melt adhesive includes 1
Parts by weight~10 parts by weight latent curing agent, preferably 3 parts by weight~5 parts by weight.
In the present invention, the antioxidant is preferably selected from 2,6-di-tert-butyl p-methylphenol, four [β-(3,5- bis- tertiary fourths
Base -4- hydroxy phenyl) propionic acid] pentaerythritol ester, β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecyl alcohol ester, three
One of (2.4- di-tert-butyl-phenyl) phosphite ester and bis- (3,5- di-tert-butyl-hydroxy phenyl) thioethers are a variety of, more
Preferably 2,6- di-tert-butyl methyl phenol.The present invention is not particularly limited the source of the antioxidant, using this field
Above-mentioned 2,6- di-tert-butyl methyl phenol known to technical staff, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid]
Pentaerythritol ester, β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecyl alcohol ester, three (2.4- di-tert-butyl-phenyls) are sub-
The commercial goods of phosphate and bis- (3,5- di-tert-butyl-hydroxy phenyl) thioethers.In the present invention, the household electrical appliances are with instead
Answering type polyurethane hot melt adhesive includes 1 parts by weight~5 parts by weight antioxidant, preferably 1 parts by weight~2 parts by weight.
In the present invention, the coupling agent is preferably selected from γ-mercaptopropyl trimethoxysilane, gamma-aminopropyl-triethoxy
Silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, vinyltrimethoxysilane, γ-three second of isocyanate group propyl
One of oxysilane and N- β-(aminoethyl)-γ-aminopropyltrimethoxysilane are a variety of, more preferably γ-mercapto propyl
Trimethoxy silane or γ-isocyanate group propyl-triethoxysilicane.The present invention is not special to the source of the coupling agent
Limitation, using above-mentioned γ-mercaptopropyl trimethoxysilane well known to those skilled in the art, gamma-aminopropyl-triethoxy-silane,
γ-glycidyl ether oxygen propyl trimethoxy silicane, vinyltrimethoxysilane, γ-isocyanate group propyl triethoxy
Silane and N- β-(aminoethyl)-γ-aminopropyltrimethoxysilane commercial goods.In the present invention, the household electrical appliances are used
Reaction type polyurethane hot-melt adhesive includes 5 parts by weight~10 parts by weight coupling agent, preferably 4 parts by weight~5 parts by weight.
In the present invention, the catalyst is preferably selected from dibutyl tin dilaurate, organo-bismuth, triethylenediamine and two
One of morpholinyl Anaesthetie Ether (DMDEE) is a variety of, more preferably dibutyl tin dilaurate, organo-bismuth and dimorpholine base
One or both of Anaesthetie Ether (DMDEE).The present invention is not particularly limited the source of the catalyst, using this field
Above-mentioned dibutyl tin dilaurate, organo-bismuth known to technical staff, triethylenediamine and dimorpholine base Anaesthetie Ether
(DMDEE) commercial goods.In the present invention, the reaction type polyurethane hot-melt adhesive includes 0.01 parts by weight~0.1 weight
Measure the antioxidant of part, preferably 0.1 parts by weight.
Household electrical appliances provided by the invention use certain content component with reaction type polyurethane hot-melt adhesive, realize preferable phase interaction
With, obtained product solidification process bubble-free, and have excellent adhesion energy and water-fast, chemical resistance.
The present invention also provides a kind of preparation sides of household electrical appliances reaction type polyurethane hot-melt adhesive described in above-mentioned technical proposal
Method, comprising the following steps:
After crystalline polyester polyols, polyether polyol, amorphous polyester polyalcohol, antioxidant and tackifying resin are mixed
Dehydration, adds isocyanates and is reacted, and is eventually adding latent curing agent, coupling agent and catalyst and carries out vacuum defoamation, dispersion
Reaction type polyurethane hot-melt adhesive is obtained after uniformly.
The present invention is first by crystalline polyester polyols, polyether polyol, amorphous polyester polyalcohol, antioxidant and thickening
Resin mixing；The mixed process is preferred specifically:
Crystalline polyester polyols, polyether polyol, amorphous polyester polyalcohol and antioxidant are mixed, are warming up to 75 DEG C
~85 DEG C, tackifying resin is added, completes mixed process.
In the present invention, the temperature of the dehydration is preferably 105 DEG C~130 DEG C, more preferably 115 DEG C~120 DEG C；It is described
The vacuum degree of dehydration preferably≤- 0.095MPa；The time of the dehydration is preferably 1.5h~2.5h, more preferably 2h.
After completing the dehydration, isocyanates is added in the reaction system and reacts by the present invention；The reaction
Temperature is preferably 93 DEG C~98 DEG C, more preferably 95 DEG C；The time of the reaction is preferably 1h~3h, more preferably 2h.
After completing the reaction process, latent curing agent, coupling agent and catalyst are added in the reaction system and carries out by the present invention
Vacuum defoamation obtains reaction type polyurethane hot-melt adhesive after being uniformly dispersed.In the present invention, the time of the vacuum defoamation is preferably
0.5h~1h.
The present invention provides a kind of household electrical appliances reaction type polyurethane hot-melt adhesive and preparation method thereof, the household electrical appliances response type
Polyurethane hot melt is by including that the raw material of following components is prepared: 100 parts by weight of polyester polyol~250 parts by weight；Polyethers
1 parts by weight of polyalcohol~150 parts by weight；50 parts by weight of isocyanates~100 parts by weight；70 parts by weight of tackifying resin~150 weights
Measure part；1 parts by weight of latent curing agent~10 parts by weight；1 parts by weight of antioxidant~5 parts by weight；5 parts by weight of coupling agent~10 weight
Part；0.01 parts by weight of catalyst~0.1 parts by weight；The polyester polyol by mass ratio be 1:(0.25~1.5) crystallinity
The pure and mild amorphous polyester polyalcohol of polyester polyols；The latent curing agent is aldimine latent curing agent or polybenzobisoxazole alkane latent curing agent.With
The prior art is compared, and household electrical appliances provided by the invention use certain content component with reaction type polyurethane hot-melt adhesive, is realized preferable
Interaction, obtained product solidification process bubble-free, and have excellent adhesion energy and water-fast, chemical resistance.
The experimental results showed that household electrical appliances provided by the invention reaction type polyurethane hot-melt adhesive solidification process bubble-free, and product is viscous
Relay is 80kg~92kg, and the bonding force after detergent immersion is 60kg~78kg, alcohol impregnate after bonding force be 36kg~
50kg。
In order to further illustrate the present invention, it is described in detail below by following embodiment.Following embodiment of the present invention
Raw material used is commercial goods, wherein amorphous polyester polyalcohol used in Examples 1 to 2 and comparative example 1 is new penta 2
Alcohol/phthalic anhydride copolyester dihydric alcohol；Amorphous polyester polyalcohol used in embodiment 3 is ethylene glycol/neopentyl glycol/fourth two
Acid/M-phthalic acid copolyester dihydric alcohol.
Embodiment 1
The raw materials used formula ratio ginseng of embodiment 1 is shown in Table 1.
The raw materials used formula ratio of 1 embodiment 1 of table
| Raw material | Parts by weight |
| Adipic acid hexylene glycol esterdiol (hydroxyl value 31KOH/mg) | 100 |
| Polyether polyol (PPG2000, hydroxyl value 56KOH/mg) | 150 |
| Amorphous polyester polyalcohol (7250, hydroxyl value 21KOH/mg) | 100 |
| MDI | 75 |
| Acrylic resin (BR-113) | 100 |
| Latent curing agent (polybenzobisoxazole alkane latent curing agent ALT-402) | 5 |
| Antioxidant (2,6- di-tert-butyl methyl phenol) | 1 |
| Coupling agent (γ-mercaptopropyl trimethoxysilane) | 5 |
| Catalyst (DMDEE) | 0.1 |
Adipic acid hexylene glycol esterdiol, polyether polyol, amorphous polyester polyalcohol and antioxidant are added by formula ratio
Into reaction kettle, 80 DEG C are warming up to, the acrylic resin (BR-113) of formula ratio is added, is warming up to 115 DEG C~120 DEG C,
2h is dehydrated under the conditions of vacuum degree≤- 0.095MPa, until water content≤500ppm, is then cooled to 80 DEG C, formula ratio is added
MDI is warming up to 95 DEG C of reaction 2h, until fully reacting, is eventually adding the latent curing agent, coupling agent and catalyst of formula ratio, vacuum
Deaeration 0.5h~1h, until be dispersed with stirring uniformly after can plastic emitting it is filling, obtain household electrical appliances reaction type polyurethane hot-melt adhesive.
Embodiment 2
The raw materials used formula ratio ginseng of embodiment 2 is shown in Table 2.
The raw materials used formula ratio of 2 embodiment 2 of table
| Raw material | Parts by weight |
| Adipic acid hexylene glycol esterdiol (hydroxyl value 31KOH/mg) | 100 |
| Polyether polyol (PPG2000, hydroxyl value 56KOH/mg) | 100 |
| Amorphous polyester polyalcohol (7250, hydroxyl value 21KOH/mg) | 85 |
| MDI | 65 |
| Acrylic resin (BR-113) | 85 |
| Latent curing agent (polybenzobisoxazole alkane latent curing agent Mega-EH) | 3 |
| Antioxidant (2,6- di-tert-butyl methyl phenol) | 1 |
| Coupling agent (γ-isocyanate group propyl-triethoxysilicane) | 4 |
| Catalyst (dibutyl tin dilaurate and organo-bismuth, 1:1) | 0.1 |
Adipic acid hexylene glycol esterdiol, polyether polyol, amorphous polyester polyalcohol and antioxidant are added by formula ratio
Into reaction kettle, 80 DEG C are warming up to, the acrylic resin (BR-113) of formula ratio is added, is warming up to 115 DEG C~120 DEG C,
2h is dehydrated under the conditions of vacuum degree≤- 0.095MPa, until water content≤500ppm, is then cooled to 80 DEG C, formula ratio is added
MDI is warming up to 95 DEG C of reaction 2h, until fully reacting, is eventually adding the latent curing agent, coupling agent and catalyst of formula ratio, vacuum
Deaeration 0.5h~1h, until be dispersed with stirring uniformly after can plastic emitting it is filling, obtain household electrical appliances reaction type polyurethane hot-melt adhesive.
Embodiment 3
The raw materials used formula ratio ginseng of embodiment 3 is shown in Table 3.
The raw materials used formula ratio of 3 embodiment 3 of table
Succinic acid-butanediol ester glycol, polyether polyol, amorphous polyester polyalcohol and antioxidant are added by formula ratio
Into reaction kettle, 80 DEG C are warming up to, the acrylic resin (1630) of formula ratio is added, 115 DEG C~120 DEG C is warming up to, true
2h is dehydrated under the conditions of reciprocal of duty cycle≤- 0.095MPa, until water content
Then≤500ppm is cooled to 80 DEG C, the MDI of formula ratio is added, and is warming up to 95 DEG C of reaction 2h, until fully reacting,
It is eventually adding the latent curing agent, coupling agent and catalyst of formula ratio, vacuum defoamation 0.5h~1h, until after being dispersed with stirring uniformly
Plastic emitting is filling, obtains household electrical appliances reaction type polyurethane hot-melt adhesive.
Comparative example 1
The raw materials used formula ratio ginseng of comparative example 1 is shown in Table 4.
The raw materials used formula ratio of 4 comparative example of table
| Raw material | Parts by weight |
| Adipic acid hexylene glycol esterdiol (hydroxyl value 31KOH/mg) | 100 |
| Polyether polyol PPG2000 (hydroxyl value 56KOH/mg) | 150 |
| Amorphous polyester polyalcohol (7250, hydroxyl value 21KOH/mg) | 100 |
| MDI | 75 |
| Acrylic resin (BR-113) | 100 |
| Antioxidant (2,6- di-tert-butyl methyl phenol) | 1 |
| Coupling agent (γ-mercaptopropyl trimethoxysilane) | 5 |
| Catalyst (DMDEE) | 0.1 |
Adipic acid hexylene glycol esterdiol, polyether polyol, amorphous polyester polyalcohol and antioxidant are added by formula ratio
Into reaction kettle, 80 DEG C are warming up to, the acrylic resin (1630) of formula ratio is added, 115 DEG C~120 DEG C is warming up to, true
It is dehydrated 2h under the conditions of reciprocal of duty cycle≤- 0.095MPa, until water content≤500ppm, is then cooled to 80 DEG C, the MDI of formula ratio is added,
95 DEG C of reaction 2h are warming up to, until fully reacting, are eventually adding the coupling agent and catalyst of formula ratio, vacuum defoamation 0.5h~1h,
To be dispersed with stirring uniformly after can plastic emitting it is filling, obtain household electrical appliances reaction type polyurethane hot-melt adhesive.
Comparative example 2
Commercially available household electrical appliances pressure sensitive adhesive tape.
The household electrical appliances of reaction type polyurethane hot-melt adhesive, the offer of comparative example 2 that the embodiment of the present invention 1~3 and comparative example 1 are provided
It is detected with the properties of pressure sensitive adhesive tape, wherein bonding force test: glue will be played and be fully cured or be stained with pressure sensitive adhesive
The test sample (panel of refrigerator, cover plate for washing machine) of band is suspended vacantly in test box, places the weight of constant weight in bonding plane
Code, observes the weight that can bear；Detergent immersion experiment: will play glue and be fully cured or be stained with the test of pressure sensitive adhesive tape
Exemplar is fully immersed in 25 DEG C of water, is impregnated 336 hours, is taken out and is repeated bonding force test；Alcohol immersion test: glue will be played
The water and test sample for being fully cured or being stained with pressure sensitive adhesive tape is fully immersed in alcohol takes out after alcohol volatilizees completely and repeats
Bonding force test.As a result ginseng is shown in Table 5.
The family of reaction type polyurethane hot-melt adhesive, the offer of comparative example 2 that 5 embodiment of the present invention 1~3 of table and comparative example 1 provide
The properties data of electric pressure sensitive adhesive tape
As shown in Table 5, the household electrical appliances that the embodiment of the present invention 1~3 provides are with reaction type polyurethane hot-melt adhesive solidification process without gas
Bubble, and have excellent adhesion energy and water-fast, chemical resistance；Meanwhile in applied at elevated temperature, has and suitably open
Time and preferable workability are put, good adhesive property is all had to non-polar substrate, polar substrates.
The above description of the disclosed embodiments, enables those skilled in the art to implement or use the present invention.It is right
A variety of modifications of these embodiments will be readily apparent to those skilled in the art, and as defined herein one
As principle can realize in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention will
It will not be intended to be limited to the embodiments shown herein, and be to fit to consistent with the principles and novel features disclosed herein
Widest scope.
Claims (8)
1. a kind of household electrical appliances reaction type polyurethane hot-melt adhesive is prepared by the raw material for including following components:
185 parts by weight of polyester polyol~250 parts by weight；
100 parts by weight of polyether polyol~150 parts by weight；
65 parts by weight of isocyanates~90 parts by weight；
70 parts by weight of tackifying resin~150 parts by weight；
1 parts by weight of latent curing agent~10 parts by weight；
1 parts by weight of antioxidant~5 parts by weight；
5 parts by weight of coupling agent~10 parts by weight；
0.01 parts by weight of catalyst~0.1 parts by weight；
The polyester polyol by mass ratio be 1:(0.85~1.5) crystalline polyester polyols and amorphous polyester polyalcohol
Composition；
The crystalline polyester polyols are selected from adipic acid hexylene glycol esterdiol or succinic acid-butanediol ester glycol；
The amorphous polyester polyalcohol is neopentyl glycol/phthalic anhydride copolymer or ethylene glycol/neopentyl glycol/succinic acid/isophthalic two
Formic acid copolymer；
The latent curing agent is aldimine latent curing agent or polybenzobisoxazole alkane latent curing agent.
2. household electrical appliances reaction type polyurethane hot-melt adhesive according to claim 1, which is characterized in that the tackifying resin is selected from
One of acrylic resin, hydroxyl terminated polyurethane, Petropols, polyolefins tackifying resin and terpene resin are a variety of.
3. household electrical appliances reaction type polyurethane hot-melt adhesive according to claim 1, which is characterized in that the antioxidant is selected from 2,
6- di-tert-butyl methyl phenol, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, β-(3,5- bis-
Tert-butyl-hydroxy phenyl) propionic acid n-octadecyl alcohol ester, three (2.4- di-tert-butyl-phenyl) phosphite esters and bis- (bis- uncles of 3,5-
Butyl -4- hydroxy phenyl) one of thioether or a variety of.
4. household electrical appliances reaction type polyurethane hot-melt adhesive according to claim 1, which is characterized in that the coupling agent is selected from
γ-mercaptopropyl trimethoxysilane, gamma-aminopropyl-triethoxy-silane, γ-glycidyl ether oxygen propyl trimethoxy silicane,
Vinyltrimethoxysilane, γ-isocyanate group propyl-triethoxysilicane and N- β-(aminoethyl)-γ-aminopropyl front three
One of oxysilane is a variety of.
5. household electrical appliances reaction type polyurethane hot-melt adhesive according to claim 1, which is characterized in that the catalyst is selected from two
One of dibutyl tin laurate, organo-bismuth, triethylenediamine and dimorpholine base Anaesthetie Ether are a variety of.
6. a kind of preparation method of the described in any item household electrical appliances reaction type polyurethane hot-melt adhesives of Claims 1 to 5, including it is following
Step:
It is dehydrated after polyester polyol, polyether polyol, antioxidant and tackifying resin are mixed, adds isocyanates and carry out instead
It answers, is eventually adding latent curing agent, coupling agent and catalyst and carries out vacuum defoamation, reaction type polyurethane hot melt is obtained after being uniformly dispersed
Glue.
7. preparation method according to claim 6, which is characterized in that the temperature of the dehydration is 105 DEG C~130 DEG C, very
Reciprocal of duty cycle≤- 0.095MPa, time are 1.5h~2.5h.
8. preparation method according to claim 6, which is characterized in that the temperature of the reaction is 93 DEG C~98 DEG C, the time
For 1h~3h.
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