CN108239517A - A kind of environmental-protection quick consolidates no-solvent polyurethane structure sealant and its preparation method and application method - Google Patents
A kind of environmental-protection quick consolidates no-solvent polyurethane structure sealant and its preparation method and application method Download PDFInfo
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- CN108239517A CN108239517A CN201711384865.2A CN201711384865A CN108239517A CN 108239517 A CN108239517 A CN 108239517A CN 201711384865 A CN201711384865 A CN 201711384865A CN 108239517 A CN108239517 A CN 108239517A
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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
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/36—Hydroxylated esters of higher fatty acids
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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
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
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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
- C08G18/4804—Two or more polyethers of different physical or chemical nature
- C08G18/4812—Mixtures of polyetherdiols with polyetherpolyols having at least three hydroxy groups
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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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- 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
- C08G18/4829—Polyethers containing at least three hydroxy groups
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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
- C08G18/67—Unsaturated compounds having active hydrogen
- C08G18/671—Unsaturated compounds having only one group containing active hydrogen
- C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
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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
- C08G18/7657—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
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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
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/78—Nitrogen
- C08G18/79—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates
- C08G18/791—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups
- C08G18/794—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups formed by oligomerisation of aromatic isocyanates or isothiocyanates
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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
- 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
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08K3/34—Silicon-containing compounds
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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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- Polyurethanes Or Polyureas (AREA)
Abstract
The present invention provides quick-setting solvent-free polyurethane adhesives of a kind of environment-friendly type and preparation method thereof.It includes two components of first, second, its first component contains aromatic series and/or aliphatic and/or alicyclic diisocyanate, with two degrees of functionality and its more than polyester polyol and/or polyether polyol and/or the polyalcohol and Hydroxylated acrylic resin of plant oil modified polyalcohol and/or a length of below the C12 of carbochain and solid powder filler.Its component B contains the polyalcohol a of a length of below the C12 of at least one carbochain, at least two degrees of functionality and more than polyether polyol and/or polyester polyol and/or plant oil modified polyalcohol b, aromatic series and/or aliphatic and/or alicyclic diisocyanate c, solid powder filler d, silicone coupling agents e, curing rate conditioning agent f.It the advantage is that, rapid curing, operation is simple, safety is good, solvent-free, environmentally friendly；Excellent cementability and peel resistance；Preferable thermal-shock resistance.
Description
Technical field
The invention belongs to dual-component polyurethane adhesive field, more particularly to a kind of rapid curing, high heat conduction polyurethane
Structure sealant and its preparation method and application method.
Background technology
Dual-component polyurethane adhesive is widely used in the every field of people's production, life, and two-component polyurethane adhesive glues
Agent is with its excellent impact resistance, durability, lower temperature resistance, fatigue durability and good workability and first as many fields
The adhesive of choosing.But dual-component polyurethane adhesive is relative to other kinds of sqtructural adhesive that usually there are curing rates
Slowly, the relatively low disadvantage of adhesive strength is subject to certain restrictions its application.
Invention content
Present invention aims at provide a kind of environmental protection, rapid curing and the high no-solvent polyurethane gluing of adhesion strength
Agent.
The further object of the present invention, which is to provide, a kind of prepares above-mentioned environment-friendly type, quick-setting no-solvent polyurethane gluing
The preparation method of agent.
The further object of the present invention is to provide a kind of above-mentioned environment-friendly type, quick-setting solvent-free polyurethane adhesive
Application process.
To achieve the above object, the present invention uses following technical solution：
A kind of environment-friendly type, quick-setting solvent-free polyurethane adhesive, it is characterised in that：Including isocyanate-terminated poly-
The first component of urethane performed polymer and hydroxy-end capped base polyurethane prepolymer for use as component B.Wherein：
The first component contains aromatic series and/or aliphatic and/or alicyclic isocyanates 30wt%~60wt%, with
Two degrees of functionality and its more than polyester polyol and/or polyether polyol and/or plant oil modified polyalcohol and/or carbon chain length
For polyalcohol 20wt%~50wt% of below C12, Hydroxylated acrylic resin 0wt%~30wt%, solid powder filler 0wt%
~50wt%.
Component B contains polyalcohol a 0wt%~20wt% of a length of below the C12 of at least one carbochain, at least two degrees of functionality
And above polyether polyol and/or polyester polyol and/or plant oil modified polyalcohol b30wt%~80wt%, aromatic series
And/or aliphatic and/or alicyclic diisocyanate c 0wt%~30wt%, solid powder filler d 10wt%~
50wt%, coupling agent e 0wt%~10wt%, curing rate conditioning agent f 0.01wt%~1wt%.
In a preferred embodiment of the invention, the polyether polyol in the first component is selected from polypropylene oxide two
Alcohol, polypropylene oxide triol, polypropylene oxide-ethylene oxide glycol, one kind in polytetrahydrofuran diol or it is arbitrary two kinds with
On mixture.
In a preferred embodiment of the invention, two degrees of functionality in the first component and its more than polyester polyol
Esterification condensation reaction is carried out for low molecular polyacid or multi-anhydride and low molecular polyalcohol to be made；Wherein, it is described more
The one kind or arbitrary two of first acid in M-phthalic acid, phthalic acid, terephthalic acid (TPA), adipic acid, decanedioic acid, azelaic acid
Kind or more mixture；The multi-anhydride be selected from isophthalic anhydride, phthalic anhydride, terephthalic anhydride, oneself two
One or more kinds of mixing in acid anhydrides, sebacic anhydride, azelaic acid acid anhydride, maleic anhydride；The polyalcohol is selected from second two
One in alcohol, a diethyl acetal, 1,4- butanediols, 1,6-HD, triethylene-glycol, neopentyl glycol, trimethylolpropane
Kind or arbitrary two or more mixture.
In a preferred embodiment of the invention, the plant oil modified polyalcohol in the first component is selected from using epoxy
Soybean oil modified polyalcohol, palm oil modified polyalcohol, coconut oil modified polyalcohol, one kind in castor oil modified polyalcohol or
Arbitrary two or more mixture.
In a preferred embodiment of the invention, the polyalcohol of a length of below the C12 of carbochain in the first component is selected from
Propylene glycol, ethylene glycol, a diethyl acetal, 1,4- butanediols, 1,6-HD, triethylene-glycol, neopentyl glycol, trihydroxy methyl
One kind or arbitrary two or more mixture in propane.
In a preferred embodiment of the invention, the aromatic series in the first component and/or aliphatic and/or alicyclic
Diisocyanate be selected from toluene di-isocyanate(TDI) TDI, diphenyl methane -4,4 '-diisocyanate or/and diphenyl methane -
2,4 '-diisocyanate MDI, liquefied mdi, 1,6 '-hexamethylene diisocyanate HDI, isophorone diisocyanate IPDI, benzene two are sub-
Methyl diisocyanate XDI, polyphenyl polymethylene polyisocyanates PAPI, one kind in HDI trimer or it is arbitrary two kinds with
On mixture.
In a preferred embodiment of the invention, the solid powder filler in the first component is selected from lightweight/heavy carbon
One kind or arbitrary two or more mixture in sour calcium, talcum powder, aerosil, carbon black, silicon powder.
In a preferred embodiment of the invention, the Hydroxylated acrylic resin of the first component is selected from methacrylic acid
Hydroxyl ethyl ester, hydroxy propyl methacrylate, methacrylate, hydroxy-ethyl acrylate, hydroxypropyl acrylate, acrylic acid hydroxyl fourth
One kind or arbitrary two or more mixture in ester.
In a preferred embodiment of the invention, the polyalcohol a of a length of below the C12 of carbochain in the component B is selected from
Propylene glycol, ethylene glycol, a diethyl acetal, 1,4- butanediols, 1,6-HD, triethylene-glycol, neopentyl glycol, trihydroxy methyl
One kind or arbitrary two or more mixture in propane.
In a preferred embodiment of the invention, at least two degrees of functionality in the component B and more than polyether polyols
Alcohol is included selected from polyoxypropyleneglycol, polypropylene oxide triol, polypropylene oxide-ethylene oxide glycol, PolyTHF two
One kind or arbitrary two or more mixture in alcohol.
In a preferred embodiment of the invention, at least two degrees of functionality in the component B and more than polyester polyols
Alcohol carries out esterification condensation reaction and is made for low molecular polyacid or multi-anhydride and low molecular polyalcohol；Wherein, it is described
The one kind or one kind of polyacid in M-phthalic acid, phthalic acid, terephthalic acid (TPA), adipic acid, decanedioic acid, azelaic acid
Above mixing；The multi-anhydride be selected from isophthalic anhydride, phthalic anhydride, terephthalic anhydride, adipic anhydride,
Sebacic anhydride, azelaic acid acid anhydride, one kind in maleic anhydride or arbitrary two or more mixture；The polyalcohol is selected from second two
One in alcohol, a diethyl acetal, 1,4- butanediols, 1,6-HD, triethylene-glycol, neopentyl glycol, trimethylolpropane
Kind or arbitrary two or more mixture.
In a preferred embodiment of the invention, it is big to be selected from epoxy for the plant oil modified polyalcohol in the component B
Soya-bean oil polyalcohol, palm oil polyalcohol, coconut oil polyalcohol, one kind in castor oil polyhydric alcohol or arbitrary two or more mixing
Object.
In a preferred embodiment of the invention, the aromatic series in the component B and/or aliphatic and/or alicyclic
Diisocyanate c be selected from toluene di-isocyanate(TDI) TDI, diphenyl methane -4,4 '-diisocyanate or/and diphenyl methane -
2,4 '-diisocyanate MDI, liquefied mdi, 1,6 '-hexamethylene diisocyanate HDI, isophorone diisocyanate IPDI, benzene two are sub-
Methyl diisocyanate XDI, polyphenyl polymethylene polyisocyanates PAPI, one kind in HDI trimer or it is arbitrary two kinds with
On mixture.
In a preferred embodiment of the invention, the solid powder filler d in the component B is selected from lightweight/heavy carbon
One kind or arbitrary two or more mixture in sour calcium, talcum powder, aerosil, carbon black, silicon powder.
In a preferred embodiment of the invention, the coupling agent e in the component B is selected from vinyl silanes, epoxy group
Silane, styryl silane, isobutenyl silane, isobutenyl silane, acrylsilanes, acrylic silane, amino silane,
Ureido silane, chloropropyl silane, hydrosulphonyl silane, vulcanizer silane, one kind in isocyanates base silane or arbitrary two or more
Mixture.
In a preferred embodiment of the invention, the curing conditioning agent f in the component B is contains 2~8 carbon originals
The organic acid and/or organic salt of son.
In a preferred embodiment of the invention, the organic acid containing 2~8 carbon atoms is selected from maleic two
One kind in acid, citric acid, tartaric acid or in one kind or arbitrary two or more mixture.
In a preferred embodiment of the invention, the organic salt is included selected from tin and/or zinc and/or zirconium and/or cobalt
And/or one kind in the carboxylate of bismuth metal or in one kind or arbitrary two or more mixture.
A kind of preparation method of the above-mentioned quick-setting solvent-free polyurethane adhesive of environment-friendly type, includes the following steps：
1) by two degrees of functionality in first component and its more than polyester polyol and/or polyether polyol and/or vegetable oil
The polyalcohol of modified polyalcohol and/or a length of below the C12 of carbochain, hydroxy acrylic acid resin are added in reaction kettle, are heated to 60
DEG C~150 DEG C of dehydration 0.5h~4h under vacuum degree ＜ -0.08MPa, until material moisture ＜ 0.1%；Then 60 DEG C are cooled to
After below, aromatic series and/or aliphatic and/or alicyclic isocyanates is added portionwise, at 60 DEG C~120 DEG C react 1h~
6h generates base polyurethane prepolymer for use as；Be subsequently added into 0.1% solid powder fillers of water content ＜, after stirring evenly vacuum degree ＜-
Deaeration 1h~4h under 0.08MPa, cooling filtering plastic emitting obtain terminal isocyanate group base polyurethane prepolymer for use as；
2) by the polyalcohol a of a length of below the C12 of carbochain in component B, at least two degrees of functionality and more than polyether polyol
And/or polyester polyol and/or plant oil modified polyalcohol b are added in reaction kettle, are heated to 60 DEG C~150 DEG C in vacuum degree
0.5h~4h is dehydrated under ＜ -0.08MPa, until material moisture ＜ 0.1%；Then after cooling to less than 60 DEG C, aromatic series is added in
And/or aliphatic and/or alicyclic diisocyanate c, 1h~6h is reacted at 60 DEG C~120 DEG C；It is subsequently added into solid powder
Last filler d is heated to 60 DEG C~120 DEG C and 1h~4h is dehydrated under vacuum degree ＜ -0.08MPa, it is desirable that water content ＜ 0.1%；Drop
Temperature is eventually adding silicone coupling agents e and curing rate conditioning agent f to after less than 40 DEG C, is stirred at 45 DEG C~55 DEG C equal
Room temperature is cooled to after even 0.5h~2h, filtering and discharging obtains hydroxyl-terminated polyurethane performed polymer.
A kind of above-mentioned quick-setting solvent-free polyurethane adhesive of environment-friendly type, can be applied to include metal (including and not
Be only limitted to iron, steel, aluminium, galvanized iron, stainless steel etc.), timber (including and be not limited only to solid wood, wood shavings wood etc.), plastics (including and
Be not limited only to PE, PP, ABS, PET, PVC etc.) and the hard arbitrary two kinds of materials of expanded material (polyurethane foam material etc.) bonding.
A kind of application process of the above-mentioned quick-setting solvent-free polyurethane adhesive of environment-friendly type is by first component and second
Component presses NCO:OH=0.85~1.8：1, it is bonded under 5 DEG C~45 DEG C room temperature with glue coating, operable time is 1 minute~10
Minute.At room temperature, basic curing in 0.5~2 hour, curing can reach use intensity for 24 hours.
Wherein preferably, NCO:OH=1.1~1.4：1.
Preferably, with glue coating bonding at 15 DEG C~30 DEG C.
The quick-setting solvent-free polyurethane adhesive of a kind of environment-friendly type in the present invention has the characteristics that：
1) rapid curing, operation are simple, easy to use；
2) safety is good, without fire, the danger of explosion；
3) it is solvent-free, it is environmentally friendly；
4) excellent cementability and peel resistance；
5) preferable thermal-shock resistance.
The present invention is suitable for the sealings such as automobile, container, machinery, freezer, building and high-strength structure bonding, available for replacing
For One component Sealant, and have the characteristics that curing rate is fast, adhesion strength is high.To steel, iron, copper, aluminium, concrete, fiberglass,
Plastics etc. have very high adhesion strength, have that bonding base material range is wide, salable gap is larger, low temperature resistant, anti-vibration, resistance to tired
The features such as labor, ageing-resistant, impact resistance, nontoxic, low taste；And automatic production line operation is applicable to, greatly improve production efficiency.
Specific implementation method
A kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type of the present invention, it is above-mentioned including two components of first, second
First component contain 20wt%~50wt% two degrees of functionality and its more than polyester polyol and/or polyether polyol and/or
The polyalcohol of plant oil modified a length of below the C12 of polyalcohol and/or carbochain, with 30wt%~60wt% aromatic series and/or fat
Fat race and/or alicyclic di-isocyanate reaction generation base polyurethane prepolymer for use as.And existing no-solvent polyurethane structure glue
Aromatic series and/or aliphatic and/or the usage amount of alicyclic diisocyanate are generally 99wt%~100wt%, the present invention
It is middle to use appropriate polyalcohol and diisocyanate prepolymer so that molecule chain growth in first component passes through the second group with the present invention
Part reaction, can obtain higher adhesive strength.
Component B contains the polyalcohol a of a length of below the C12 of 0wt%~20wt% carbochains, 3 at least two degrees of functionality and more than
Polyether polyol and/or polyester polyol and/or plant oil modified polyalcohol b 30wt%~80wt%, with 0wt%~
30wt% aromatic series and/or aliphatic and/or alicyclic diisocyanate c carry out reaction generation base polyurethane prepolymer for use as, make
With raising molecular chain length is, to obtain higher adhesive strength.The effect of solid powder filler d is enhancing structure glue
Cohesive force, the effect of silicone coupling agents e are bonding force of the increase structure glue to bonding interface, curing rate conditioning agent f's
Effect is curing rate of the adjustment structure glue under normal temperature state.
Characteristic in order to further illustrate the present invention is made to illustrate with reference to specific embodiment.
The synthesis of 1 A-1 of embodiment
By the plant oil modified polyalcohol (castor oil modified trihydroxylic alcohol) that 40 parts of molecular weight is 900,40 parts of point
Son amount is 2000 polyester polyol based on phthalic acid, is encased in reaction vessel, is heated to 120 DEG C of vacuum dehydration 2h,
Less than the 60 DEG C PAPI (polymethylene polyisocyanates) for adding in 100 parts are cooled to, the performed polymer being warming up to after 80 DEG C of reaction 2h
First component as double component solvent-free polyurethane structure glue.Hereinafter referred to as A-1.
The synthesis of 2 A-2 of embodiment
By the plant oil modified polyalcohol (castor oil modified trihydroxylic alcohol) that 30 parts of molecular weight is 900,10 parts of point
The polyether polyol that son amount is 350,20 parts of hydroxyethyl methacrylate are encased in reaction vessel, are heated to 120 DEG C of vacuum
2h is dehydrated, cools to less than the 60 DEG C PAPI (polymethylene polyisocyanates) for adding in 100 parts, after being warming up to 80 DEG C of reaction 2h,
40 parts of calcium carbonate vacuum defoamation 2h is added in, cooling discharge obtains the first component of double component solvent-free polyurethane structure glue.Following letter
Referred to as A-2.
The synthesis of 3 B-1 of embodiment
By the polyoxypropyleneglycol that 100 parts of molecular weight is 2000,10 parts of molecular weight is 350 polypropylene oxide three
Alcohol, 10 parts of molecular weight are 1000 polyester polyol based on aromatic hydrocarbons, are encased in reaction vessel, are heated to 120 DEG C of vacuum
2h is dehydrated, cools to less than the 60 DEG C MDI for adding in 20 parts, is warming up to 80 DEG C of reaction 2h, adds 1 part of aerosil,
20 parts of talcum powder, 80 parts of powdered whiting are heated to 120 DEG C of vacuum dehydration 2h, cool to less than the 40 DEG C silicon for adding in 2 parts
Oxygen alkane coupling agent, 0.1 part of curing conditioning agent (dibutyl tin dilaurate) are heated to 50 DEG C of stirring 0.5h, then cool down
Expect the component B as double component solvent-free polyurethane structure glue.Hereinafter referred to as B-1.
The synthesis of 4 B-2 of embodiment
By the polyester polyol based on aromatic hydrocarbons-aliphatic hydrocarbon that 100 parts of molecular weight is 2000,10 parts of molecular weight is 350
Polypropylene oxide triol, 10 parts of molecular weight is 1000 polyester polyol based on aromatic hydrocarbons, is encased in reaction vessel, adds
Heat cools to less than the 60 DEG C MDI for adding in 20 parts, is warming up to 80 DEG C of reaction 2h, adds 1 part to 120 DEG C of vacuum dehydration 2h
Aerosil, 20 parts of talcum powder, 80 parts of powdered whiting are heated to 120 DEG C of vacuum dehydration 2h, cool to 40 DEG C with
The lower silicone coupling agents for adding in 2 parts, 0.1 part of curing conditioning agent (dibutyl tin dilaurate) are heated to 50 DEG C of stirrings
0.5h, then component B of the cooling discharge as double component solvent-free polyurethane structure glue.Hereinafter referred to as B-2.
The synthesis of 5 B-3 of embodiment
By the polyester polyol based on aromatic hydrocarbons-aliphatic hydrocarbon that 100 parts of molecular weight is 2000,10 parts of molecular weight is 350
Polypropylene oxide triol, 10 parts of molecular weight is 1000 polyester polyol based on aromatic hydrocarbons, be encased in reaction vessel,
120 DEG C of vacuum dehydration 2h are heated to, cool to less than the 60 DEG C MDI for adding in 20 parts, 80 DEG C of reaction 2h is warming up to, adds 1 part
Aerosil, 20 parts of talcum powder, 80 parts of powdered whiting is heated to 120 DEG C of vacuum dehydration 2h, cools to 40 DEG C
2 parts of silicone coupling agents are added in below, and 0.3 part of curing conditioning agent (dibutyl tin dilaurate) is heated to 50 DEG C of stirrings
0.5h, then component B of the cooling discharge as double component solvent-free polyurethane structure glue.Hereinafter referred to as B-3.
Embodiment 6
1 part of A-1 and 4 part of B-1 is sufficiently mixed at 25 DEG C of room temperature with glue, with reference to GB/T7124-2008 systems
Standby tensile shear strength tests test piece, and 90 ° of peel strength test test pieces are prepared, and placed under room temperature with reference to GJB 446-1988
It is tested after 2 days, obtains its tensile shear strength as 11.5MPa, 90 ° of peel strengths are 35.2N/cm.
25 DEG C of 20~30min of operating time, reach initial strength for 24 hours, and 48h reaches final strength.
Embodiment 7
1 part of A-2 and 1 part of B-1 is sufficiently mixed at 25 DEG C of room temperature with glue, with reference to GB/T7124-2008 systems
Standby tensile shear strength tests test piece, and 90 ° of peel strength test test pieces are prepared, and placed under room temperature with reference to GJB 446-1988
It is tested after 2 days, obtains its tensile shear strength as 18.2MPa, 90 ° of peel strengths are 40.5N/cm.
25 DEG C of 20~25min of operating time, reach initial strength for 24 hours, and 48h reaches final strength.
Embodiment 8
1 part of A-1 and 4 part of B-2 is sufficiently mixed at 25 DEG C of room temperature with glue, with reference to GB/T7124-2008 systems
Standby tensile shear strength tests test piece, and 90 ° of peel strength test test pieces are prepared, and placed under room temperature with reference to GJB 446-1988
It is tested after 2 days, obtains its tensile shear strength as 14.2MPa, 90 ° of peel strengths are 41.1N/cm.
25 DEG C of 10~15min of operating time, 1h~2h reach initial strength, and 36h reaches final strength.
Embodiment 9
1 part of A-2 and 1 part of B-2 is sufficiently mixed at 25 DEG C of room temperature with glue, with reference to GB/T7124-2008 systems
Standby tensile shear strength tests test piece, and 90 ° of peel strength test test pieces are prepared, and placed under room temperature with reference to GJB 446-1988
It is tested after 2 days, obtains its tensile shear strength as 21.3MPa, 90 ° of peel strengths are 44.4N/cm.
25 DEG C of 5~10min of operating time, 1h~2h reach initial strength, and 36h reaches final strength.
Embodiment 10
1 part of A-1 and 4 part of B-3 is sufficiently mixed at 25 DEG C of room temperature with glue, with reference to GB/T7124-2008 systems
Standby tensile shear strength tests test piece, and 90 ° of peel strength test test pieces are prepared, and placed under room temperature with reference to GJB 446-1988
It is tested after 2 days, obtains its tensile shear strength as 15.5MPa, 90 ° of peel strengths are 44.1N/cm.
25 DEG C of 5~10min of operating time, 1h~2h reach initial strength, reach final strength for 24 hours.
Embodiment 11
1 part of A-2 and 1 part of B-3 is sufficiently mixed at 25 DEG C of room temperature with glue, with reference to GB/T7124-2008 systems
Standby tensile shear strength tests test piece, and 90 ° of peel strength test test pieces are prepared, and placed under room temperature with reference to GJB 446-1988
It is tested after 2 days, obtains its tensile shear strength as 22.8MPa, 90 ° of peel strengths are 48.5N/cm.
25 DEG C of 1~5min of operating time, 0.5h~1h reach initial strength, reach final strength for 24 hours.
Comparative example 1
Embodiment 6 is distinguished as with embodiment 7, embodiment 8 with embodiment 9, the component A A- in embodiment 7 and embodiment 9
Hydroxyethyl methacrylate and solid powder filler are added in 2.By comparing it can be found that test result tensile shear strength
Embodiment 7 is more than embodiment 6, and embodiment 9 is more than embodiment 8, and tensile shear strength significantly increases, and 90 ° of peel strengths slightly have
Increase.Adhesive property preferably component A both more than comprehensive consideration is using A-2 to be excellent.
Comparative example 2
Embodiment 7 is distinguished as with embodiment 9, is added in the B-2 components in embodiment 9 based on aromatic hydrocarbons-aliphatic hydrocarbon
Polyester polyol, the B-1 in embodiment 7 add polyoxypropyleneglycol, and by comparing finding, test result tensile shear is strong
Degree and 90 ° of peel strength embodiments 9 are all higher than embodiment 7.
Comparative example 3
Embodiment 9 is distinguished as with embodiment 11, and 0.3 part of curing is added in the B component B-3 of embodiment 11 and is adjusted
Agent adds 0.1 part of curing conditioning agent in the B component B-2 of embodiment 9.By comparing it can be found that test result stretching is cut
Shearing stress and 90 ° of peel strength embodiments 11 are more than embodiment 9, and the operating time of embodiment 11, just solid and final strength
Time is respectively less than embodiment 9, the adhesive property and operating characteristics both more than comprehensive consideration with embodiment 11 for more preferably, preferably
B component is using B-3 to be excellent.
Example above institute target dosage is parts by weight.
The present invention relates to a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type, be mainly used for metal, timber,
The bonding of plastics and hard expanded material.
The present invention is not limited to the above embodiments, and the description in above embodiments and description only illustrates the present invention
Principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these variation and
Improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent
Object defines.
Claims (23)
1. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type, it is characterised in that：Isocyanate terminated urethane is pre-
The first component of aggressiveness and hydroxy-end capped base polyurethane prepolymer for use as component B, wherein：
The first component contains aromatic series and/or aliphatic and/or alicyclic isocyanates 30wt%~60wt%, with two officials
Energy degree and its more than polyester polyol and/or polyether polyol and/or plant oil modified polyalcohol and/or carbochain it is a length of
Polyalcohol 20wt%~50wt% of below C12, Hydroxylated acrylic resin 0wt%~30wt%, solid powder filler 0wt%~
50wt%；
Component B contains polyalcohol a 0wt%~20wt% of a length of below the C12 of at least one carbochain, at least two degrees of functionality and with
On polyether polyol and/or polyester polyol and/or plant oil modified polyalcohol b 30wt%~80wt%, aromatic series and/
Or aliphatic and/or alicyclic diisocyanate c 0wt%~30wt%, solid powder filler d 10wt%~50wt%,
Coupling agent e 0wt%~10wt%, curing rate conditioning agent f 0.01wt%~1wt%.
2. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：It is described
Polyether polyol in first component is selected from polyoxypropyleneglycol, polypropylene oxide triol, polypropylene oxide-ethylene oxide two
One kind or arbitrary two or more mixture in alcohol, polytetrahydrofuran diol.
3. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：It is described
Two degrees of functionality in first component and component B and its more than polyester polyol be low molecular polyacid or multi-anhydride and low
The polyalcohol of molecule carries out esterification condensation reaction and is made；Wherein, the polyacid be selected from M-phthalic acid, phthalic acid,
One kind or arbitrary two or more mixture in terephthalic acid (TPA), adipic acid, decanedioic acid, azelaic acid；The multi-anhydride
One kind in isophthalic anhydride, phthalic anhydride, terephthalic anhydride, adipic anhydride, sebacic anhydride, azelaic acid acid anhydride
Or more than one mixing；The polyalcohol is selected from ethylene glycol, a diethyl acetal, 1,4- butanediols, 1,6-HD, two contractings
One kind or arbitrary two or more mixture in triethylene glycol, neopentyl glycol, trimethylolpropane.
4. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：It is described
Plant oil modified polyalcohol in first component is selected from using epoxidized soybean oil modified polyalcohol, palm oil modified polyalcohol, coconut
Oily modified polyalcohol, one kind in castor oil modified polyalcohol or arbitrary two or more mixture.
5. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：It is described
The polyalcohol of a length of below the C12 of carbochain in first component is selected from propylene glycol, ethylene glycol, a diethyl acetal, 1,4- butanediols, 1,6-
One kind or arbitrary two or more mixture in hexylene glycol, triethylene-glycol, neopentyl glycol, trimethylolpropane.
6. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：It is described
Aromatic series and/or aliphatic and/or alicyclic diisocyanate in first component are selected from toluene di-isocyanate(TDI) TDI, hexichol
Methylmethane -4,4 '-diisocyanate or/and diphenyl methane -2,4 '-diisocyanate MDI, liquefied mdi, 1,6 '-oneself is two different
Cyanate HDI, isophorone diisocyanate IPDI, benzene dimethylene diisocyanate XDI, polyphenyl polymethylene polyisocyanate cyanogen
One kind or arbitrary two or more mixture in acid esters PAPI, HDI trimer.
7. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：It is described
Solid powder filler in first component is in lightweight/powdered whiting, talcum powder, aerosil, carbon black, silicon powder
A kind of or arbitrary two or more mixture.
8. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：It is described
First component Hydroxylated acrylic resin be selected from hydroxyethyl methacrylate, hydroxy propyl methacrylate, hydroxyethyl methacrylate fourth
One kind or arbitrary two or more mixture in ester, hydroxy-ethyl acrylate, hydroxypropyl acrylate, hy-droxybutyl.
9. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：It is described
The polyalcohol a of a length of below the C12 of carbochain in component B is selected from propylene glycol, ethylene glycol, a diethyl acetal, 1,4- butanediols, 1,
One kind or arbitrary two or more mixture in 6- hexylene glycols, triethylene-glycol, neopentyl glycol, trimethylolpropane.
10. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：, institute
State two degrees of functionality in component B and more than polyether polyol include selected from polyoxypropyleneglycol, polypropylene oxide triol,
Polypropylene oxide-ethylene oxide glycol, one kind in polytetrahydrofuran diol or arbitrary two or more mixture.
11. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：Institute
State two degrees of functionality in component B and more than polyester polyol be low molecular polyacid or multi-anhydride and low molecular more
First alcohol carries out esterification condensation reaction and is made；Wherein, the polyacid is selected from M-phthalic acid, phthalic acid, terephthaldehyde
One kind or arbitrary two or more mixture in acid, adipic acid, decanedioic acid, azelaic acid；The multi-anhydride is selected from isophthalic
Dicarboxylic acid anhydride, phthalic anhydride, terephthalic anhydride, adipic anhydride, sebacic anhydride, one kind in azelaic acid acid anhydride or it is a kind of with
On mixing；The polyalcohol is selected from ethylene glycol, a diethyl acetal, 1,4- butanediols, 1,6-HD, two three second two of contracting
One kind or arbitrary two or more mixture in alcohol, neopentyl glycol, trimethylolpropane.
12. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：Institute
State plant oil modified polyalcohol in component B be selected from epoxy soybean oil polyalcohol, palm oil polyalcohol, coconut oil polyalcohol,
One kind or arbitrary two or more mixture in castor oil polyhydric alcohol.
13. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：Institute
The aromatic series and/or aliphatic and/or alicyclic diisocyanate c stated in component B are selected from toluene di-isocyanate(TDI) TDI, two
Phenylmethane -4,4 '-diisocyanate or/and diphenyl methane -2,4 '-diisocyanate MDI, liquefied mdi, 1,6 '-oneself two
Isocyanates HDI, isophorone diisocyanate IPDI, benzene dimethylene diisocyanate XDI, polyphenyl polymethylene polyisocyanate
One kind or arbitrary two or more mixture in cyanate PAPI, HDI trimer.
14. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：Institute
The solid powder filler d stated in component B is selected from lightweight/powdered whiting, talcum powder, aerosil, carbon black, silicon powder
In one kind or arbitrary two or more mixture.
15. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：Institute
The silicone coupling agents e stated in component B is selected from vinylsiloxane, amino silicone, epoxy radical siloxane, methacryl
Oxygroup siloxanes, sulfydryl siloxanes, one kind in urea groups siloxanes or arbitrary two or more mixture.
16. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：Institute
The curing conditioning agent f stated in component B is organic acid and/or organic salt containing 2~8 carbon atoms.
17. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as claimed in claim 15, it is characterised in that：Institute
State the mixture that the organic acid containing 2~8 carbon atoms is selected from one or both of maleic acid, citric acid.
18. a kind of quick-setting solvent-free polyurethane adhesive of environment-friendly type as described in claim 1, it is characterised in that：Institute
It states organic salt and includes one kind or two kinds arbitrary in tin and/or zinc and/or zirconium and/or the carboxylate of cobalt and/or bismuth metal
Above mixture.
19. a kind of quick-setting no-solvent polyurethane gluing of environment-friendly type described in any one of claim 1 to 18 claim
The preparation method of agent, which is characterized in that include the following steps：
1) by the two one or more kinds of degrees of functionality in first component and its more than polyester polyol and/or polyether polyols
The polyalcohol of alcohol and/or plant oil modified polyalcohol and/or a length of below the C12 of carbochain, hydroxy acrylic acid resin are added to reaction
In kettle, it is heated to 60 DEG C~150 DEG C and 0.5h~4h is dehydrated under vacuum degree ＜ -0.08MPa, until material moisture ＜ 0.1%；So
After cool to less than 60 DEG C after, aromatic series and/or aliphatic and/or alicyclic isocyanates is added portionwise, 60 DEG C~120
1h~6h generation base polyurethane prepolymer for use as is reacted at DEG C；Be subsequently added into 0.1% solid powder fillers of water content ＜, after stirring evenly
Deaeration 1h~4h under vacuum degree ＜ -0.08MPa, cooling filtering plastic emitting obtain terminal isocyanate group base polyurethane prepolymer for use as；
2) by the polyalcohol a of a length of below the C12 of carbochain in component B, at least two degrees of functionality and more than polyether polyol and/
Or polyester polyol and/or plant oil modified polyalcohol b be added in reaction kettle be heated to 60 DEG C~150 DEG C vacuum degree ＜-
0.5h~4h is dehydrated under 0.08MPa, until material moisture ＜ 0.1%；Then after cooling to less than 60 DEG C, add in aromatic series and/
Or aliphatic and/or alicyclic diisocyanate c, 1h~6h is reacted at 60 DEG C~120 DEG C；Solid powder is subsequently added into fill out
Expect d, be heated to 60 DEG C~120 DEG C and 1h~4h is dehydrated under vacuum degree ＜ -0.08MPa, it is desirable that water content ＜ 0.1%；It cools to
After less than 40 DEG C, silicone coupling agents e and curing rate conditioning agent f is eventually adding, is stirred evenly at 45 DEG C~55 DEG C
Room temperature is cooled to after 0.5h~2h, filtering and discharging obtains hydroxyl-terminated polyurethane performed polymer.
20. a kind of quick-setting no-solvent polyurethane gluing of environment-friendly type described in any one of claim 1 to 19 claim
Agent, for the bonding of metal, timber, plastics and the arbitrary two kinds of materials of hard expanded material.
21. a kind of quick-setting no-solvent polyurethane gluing of environment-friendly type described in any one of claim 1 to 19 claim
The application process of agent, it is characterized in that first component and component B are pressed NCO:OH=0.85~1.8：1, under 5 DEG C~45 DEG C room temperature
It is coated with and is bonded with glue, glue-spread is 0.8~1.2Kg/m2, operable time is 1 minute~10 minutes, and at room temperature, 0.5~2 is small
Shi Jiben cures, and curing can reach use intensity for 24 hours.
22. application process as claimed in claim 21, which is characterized in that first component and component B press NCO:OH=1.1~
1.4：1 is matched.
23. application process as claimed in claim 21, which is characterized in that with glue coating bonding at 15 DEG C~30 DEG C.
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| CN201711384865.2A CN108239517A (en) | 2017-12-20 | 2017-12-20 | A kind of environmental-protection quick consolidates no-solvent polyurethane structure sealant and its preparation method and application method |
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