CN114716959B - Polyurethane hot melt adhesive for automobile spare tire cover plate and preparation method thereof - Google Patents
Polyurethane hot melt adhesive for automobile spare tire cover plate and preparation method thereof Download PDFInfo
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- CN114716959B CN114716959B CN202111599242.3A CN202111599242A CN114716959B CN 114716959 B CN114716959 B CN 114716959B CN 202111599242 A CN202111599242 A CN 202111599242A CN 114716959 B CN114716959 B CN 114716959B
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- hot melt
- melt adhesive
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- polyurethane hot
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- 239000004831 Hot glue Substances 0.000 title claims abstract description 65
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 49
- 239000004814 polyurethane Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 63
- 229920000642 polymer Polymers 0.000 claims abstract description 63
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 30
- -1 aromatic isocyanate compound Chemical class 0.000 claims abstract description 27
- 229920001634 Copolyester Polymers 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229920000098 polyolefin Polymers 0.000 claims abstract description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 17
- 150000001412 amines Chemical class 0.000 claims abstract description 17
- 239000012948 isocyanate Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000000080 wetting agent Substances 0.000 claims abstract description 14
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 9
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 57
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 22
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 150000003606 tin compounds Chemical class 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000013530 defoamer Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000004743 Polypropylene Substances 0.000 abstract description 7
- 229920001155 polypropylene Polymers 0.000 abstract description 7
- 230000004913 activation Effects 0.000 abstract description 6
- 239000000853 adhesive Substances 0.000 abstract description 6
- 230000001070 adhesive effect Effects 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 6
- 239000003365 glass fiber Substances 0.000 abstract description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 18
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 description 17
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 14
- 239000000126 substance Substances 0.000 description 9
- 229920005604 random copolymer Polymers 0.000 description 8
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 description 7
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 239000000155 melt Substances 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 239000001164 aluminium sulphate Substances 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 150000002513 isocyanates Chemical class 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 150000002009 diols Chemical class 0.000 description 2
- GHLKSLMMWAKNBM-UHFFFAOYSA-N dodecane-1,12-diol Chemical compound OCCCCCCCCCCCCO GHLKSLMMWAKNBM-UHFFFAOYSA-N 0.000 description 2
- TVIDDXQYHWJXFK-UHFFFAOYSA-N dodecanedioic acid Chemical compound OC(=O)CCCCCCCCCCC(O)=O TVIDDXQYHWJXFK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007719 peel strength test Methods 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- HQHCYKULIHKCEB-UHFFFAOYSA-N tetradecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCC(O)=O HQHCYKULIHKCEB-UHFFFAOYSA-N 0.000 description 2
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- FOTKYAAJKYLFFN-UHFFFAOYSA-N decane-1,10-diol Chemical compound OCCCCCCCCCCO FOTKYAAJKYLFFN-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- QVTWBMUAJHVAIJ-UHFFFAOYSA-N hexane-1,4-diol Chemical compound CCC(O)CCCO QVTWBMUAJHVAIJ-UHFFFAOYSA-N 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- OEIJHBUUFURJLI-UHFFFAOYSA-N octane-1,8-diol Chemical compound OCCCCCCCCO OEIJHBUUFURJLI-UHFFFAOYSA-N 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001228 polyisocyanate Polymers 0.000 description 1
- 239000005056 polyisocyanate Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- C08G18/4833—Polyethers containing oxyethylene units
-
- 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
-
- 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
-
- 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
-
- 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
- C08G2170/00—Compositions for adhesives
- C08G2170/20—Compositions for hot melt adhesives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to the technical field of C09J hot melt adhesives, and in particular provides a polyurethane hot melt adhesive for an automobile spare tire cover plate and a preparation method thereof. The preparation raw materials of the polyurethane hot melt adhesive provided by the invention comprise a polymer with a hydroxyl end group, a crystalline alcohol modified copolyester, a polymer containing hydroxyl and alkoxy, an aromatic isocyanate compound, amine and derivatives thereof, an organotin compound, a random copolymerized polyolefin, an acrylic tackifier, a defoaming agent and an organosilicon wetting agent, and the prepared polyurethane hot melt adhesive has excellent peel strength, can realize secondary activation within 2 hours, has excellent adhesive force on the surface of a glass fiber polypropylene composite board, and effectively solves the problem that a felt surface in an automobile spare tire cover plate is easy to rebound a bridge edge.
Description
Technical Field
The invention relates to the technical field of C09J hot melt adhesives, and in particular provides a polyurethane hot melt adhesive for an automobile spare tire cover plate and a preparation method thereof.
Background
The automobile spare tire cover plate is an important product in a plurality of products processed by automobile parts, and plays roles in protecting the spare tire of an automobile and fixing articles of a trunk of the automobile. In general, an automobile spare tire cover plate is manufactured by hot-pressing a glass fiber polypropylene composite board coated with an adhesive and a felt. However, the time difference between the adhesive coating process and the hot pressing process is 0.5-1 hour, the adhesive is required to be activated for the second time in the actual preparation process, the hot melt adhesive in the prior art is solidified before hot pressing, so that the bonding effect between the felt and the polypropylene plate is poor, the rebound edge warping phenomenon easily occurs on the surface of the felt, the yield of the automobile spare tire cover plate is low, and the service life is short.
The Chinese patent publication No. CN111100592A discloses a latent type single-component polyurethane hot melt adhesive and a preparation method thereof, wherein a closed isocyanate curing agent is added into a polyurethane resin matrix in the patent publication, so that the problems of severe storage condition and long curing time of the polyurethane hot melt adhesive in the prior art are solved, but the polyurethane hot melt adhesive prepared by the scheme has strict requirements on the thickness of a coating in the actual use process, the bonding effect of the hot melt adhesive is unstable, and the actual use range of the latent type single-component polyurethane hot melt adhesive is limited;
the Chinese patent publication No. CN107987779A discloses a reactive polyurethane hot melt adhesive and a preparation method thereof, in the patent, through the interaction of polyether polyol of a specific type with tackifying resin and filler in a system, the water permeability of the hot melt adhesive before solidification is improved, and the prepared polyurethane hot melt adhesive has excellent high temperature resistance and thixotropic property, and has wide application in the field of hot melt adhesives for car lamps, but the initial strength and the final strength of the hot melt adhesive obtained by the scheme are not remarkably reflected.
Therefore, the polyurethane hot melt adhesive provided by the invention has strong controllability of curing time and rate, can realize secondary activation of the polyurethane hot melt adhesive in the preparation process of the automobile spare tire cover plate, and has excellent initial strength, final strength and weather resistance.
Disclosure of Invention
In order to solve the technical problems, the first aspect of the invention provides a polyurethane hot melt adhesive for a cover plate of an automobile spare tire, which comprises the following raw materials in percentage by weight: 5-10% of polymer with hydroxyl end group, 10-20% of crystalline alcohol modified copolyester, 40-60% of polymer containing hydroxyl and alkoxy, 10-20% of aromatic isocyanate compound, 0.1-1% of amine and derivative thereof, 0.002-0.006% of organic tin compound, 5-10% of random copolymerized polyolefin, 0.1-0.3% of defoaming agent, 0.4-0.6% of organosilicon wetting agent and the balance of acrylic tackifier.
As a preferred embodiment of the invention, the hydroxyl-terminated polymer has a hydroxyl number of from 20 to 40mg KOH/g.
As a more preferred embodiment of the present invention, the hydroxyl-terminated polymer has a hydroxyl number of 27 to 34mg KOH/g.
In a preferred embodiment of the present invention, the polymer having hydroxyl groups as the terminal groups is a polymer obtained by polycondensation of at least one of monoacids, diacids, monoalcohols, and diols.
In a more preferable embodiment of the present invention, the polymer having hydroxyl groups as the terminal groups is a polymer obtained by polycondensation of a dibasic acid or a diol.
As a preferable technical scheme of the invention, the dibasic acid comprises at least one of oxalic acid, sebacic acid, dodecanedioic acid and tetradecanedioic acid.
As a preferable technical scheme of the invention, the dihydric alcohol comprises at least one of 1, 2-glycol, 1, 4-hexanediol, 1, 8-octanediol, 1, 10-decanediol, 1, 12-dodecanediol, glycerol and neopentyl glycol.
As a preferred embodiment of the present invention, the number average molecular weight of the crystalline alcohol-modified copolyester is 2500 to 4500.
In a more preferred embodiment of the present invention, the crystalline alcohol-modified copolyester has a number average molecular weight of 3500.
As a preferred embodiment of the present invention, the viscosity of the hydroxyl-and alkoxy-containing polymer is 100 to 600cps at 25 ℃.
As a more preferred embodiment of the present invention, the viscosity of the hydroxyl-and alkoxy-containing polymer is 200 to 400cps at 25 ℃.
As a preferred embodiment of the present invention, the weight average molecular weight of the polymer containing hydroxyl groups and alkoxy groups is 500 to 3000.
As a more preferred embodiment of the present invention, the weight average molecular weight of the polymer containing hydroxyl groups and alkoxy groups is 1000 to 2500.
As a most preferred embodiment of the present invention, the weight average molecular weight of the polymer containing hydroxyl groups and alkoxy groups is 2000.
As a preferable technical scheme of the invention, the weight ratio of the polymer with the end group of hydroxyl to the crystalline alcohol modified copolyester to the polymer containing hydroxyl and alkoxy is 1; (1-3): (4-8).
As a more preferable technical scheme of the invention, the weight ratio of the polymer with the end group of hydroxyl to the crystalline alcohol modified copolyester to the polymer containing hydroxyl and alkoxy is 1;2:7.
the applicant has found that when using a hydroxyl terminated polymer having a hydroxyl number of 27 to 34mg KOH/g, a crystalline alcohol modified copolyester having a number average molecular weight of 3500, a hydroxyl and alkoxy group containing polymer having a viscosity of 200 to 400cps at 25 ℃, especially when the weight ratio of the hydroxyl terminated polymer, the crystalline alcohol modified copolyester, the hydroxyl and alkoxy group containing polymer is 1;2: and 7, introducing polar groups with specific density into the system, and reacting with diphenylmethane diisocyanate in the system, so that the distribution of the polar groups in a soft segment and a hard segment in a polyurethane molecular chain is improved, the crosslinking density in a hot melt adhesive system is improved, the polarity of the interface area surface of the polyurethane hot melt adhesive system is improved, the bonding force between a polyurethane hot melt adhesive and a glass fiber polypropylene composite board and a felt is enhanced, the initial peeling strength, the final peeling strength and the weather resistance of the hot melt adhesive are improved, the requirement of secondary activation on the strength in the preparation process of the hot melt adhesive for the automobile spare tire cover plate is met, the service life of the automobile spare tire cover plate is prolonged, and the problem that the felt surface in the automobile spare tire cover plate is easy to rebound and warp is effectively solved.
As a preferable technical scheme of the invention, the aromatic isocyanate compound comprises at least one of toluene diisocyanate, diphenylmethane diisocyanate, polymethylene polyphenyl polyisocyanate and trimethylphenylmethane triisocyanate.
As a more preferable embodiment of the present invention, the aromatic isocyanate compound is diphenylmethane diisocyanate.
As a preferred technical scheme of the invention, the amine and the derivative thereof comprise at least one of dimorpholine diethyl ether, N-methyl diethanol amine and triethylene diamine.
As a preferred embodiment of the present invention, the amine and its derivative is dimorpholine diethyl ether.
As a preferable technical scheme of the invention, the organotin compound comprises at least one of dibutyl tin dilaurate and stannous octoate.
As a more preferable technical scheme of the invention, the organotin compound is dibutyl tin dilaurate.
The applicant has found that when the di-morpholine diethyl ether and the dibutyl tin dilaurate are added into the system, and the weight percentage of the di-morpholine diethyl ether is controlled to be 0.5%, and the weight percentage of the dibutyl tin dilaurate is controlled to be 0.004%, the di-morpholine diethyl ether and the dibutyl tin dilaurate can cooperate with random copolymerized polyolefin and propionic acid tackifier in the system, so that the polyurethane hot melt adhesive has excellent weather resistance, the controllability of the curing time of the polyurethane hot melt adhesive is obviously improved, the curing speed of the polyurethane hot melt adhesive is low or the polyurethane hot melt adhesive is not cured before 2 hours, the polyurethane hot melt adhesive is cured rapidly after 2 hours, the requirement of secondary activation within 2 hours of the hot melt adhesive is met, and the yield and the service life of the automobile spare tire cover plate are improved.
As a preferred embodiment of the present invention, the melt viscosity of the random copolymer polyolefin is 6000 to 10000 Pa.s at 190 ℃.
As a preferred embodiment of the present invention, the random copolymer polyolefin has a melt viscosity of 8000 Pa.s at 190 ℃.
As a preferred embodiment of the present invention, the acrylic tackifier has a toluene solution viscosity of 100 to 500mPa.s at 25℃and 40% by mass.
As a more preferable technical scheme of the invention, the viscosity of the toluene solution with 40% mass concentration at 25 ℃ is 250-340mPa.s.
As a preferable technical scheme of the invention, the defoaming agent comprises at least one of polydimethylsiloxane, stearyl alcohol, polyoxypropylene glycerol, polyoxyethylene oxypropylene glycerol and carboxyl polydimethylsiloxane.
The invention provides a preparation method of polyurethane hot melt adhesive for a spare tire cover plate of an automobile, which comprises the following steps:
(1) Pretreatment of raw materials: adding a polymer with a hydroxyl end group, a crystalline alcohol modified copolyester, a polymer containing hydroxyl and alkoxy, a random copolymerized polyolefin, an acrylic tackifier and a defoaming agent into a reaction kettle, heating, introducing nitrogen, stirring, cooling and vacuumizing to obtain a dehydrated raw material;
(2) And (3) preparing a hot melt adhesive: cooling the dehydrated raw material in the step (1) to 60-90 ℃, adding an aromatic isocyanate compound to react for 20-60min under the condition of nitrogen at 80-85 ℃, heating to 100-120 ℃, vacuumizing, adding amine and derivatives thereof, adding an organic silicon wetting agent to react after the organic tin compound reacts, and discharging to obtain the polyurethane hot melt adhesive.
Wherein, in the step (1), the temperature is raised to 120-160 ℃, the replacement time of nitrogen is 20-40min, the stirring time is 1-2h, the temperature of cooling and vacuumizing is 100-140 ℃, and the vacuumizing vacuum degree is less than or equal to 0.05-0.5MPa;
the heating time in the step (2) is 20-60min, amine and derivatives thereof are added, the reaction time of the organic tin compound is 5-15min, and the reaction time of the organic silicon wetting agent is 1-10min.
Compared with the prior art, the invention has the following beneficial effects:
1. when the polymer with the end group of hydroxyl, the crystalline alcohol modified copolyester and the polymer containing hydroxyl and alkoxy are simultaneously used, the hydroxyl value of the polymer with the end group of hydroxyl is 27-34mg KOH/g, the number average molecular weight of the crystalline alcohol modified copolyester is 3500, the viscosity of the polymer with the hydroxyl and alkoxy at 25 ℃ is 200-400cps, and especially when the weight ratio of the polymer with the end group of hydroxyl, the crystalline alcohol modified copolyester and the polymer with the hydroxyl and alkoxy is 1;2:7, the polyurethane hot melt adhesive interacts with diphenylmethane diisocyanate in the system, so that the strength and weather resistance of the polyurethane hot melt adhesive can be obviously improved;
2. when the dimorpholine diethyl ether and the dibutyl tin dilaurate are added into the system, and the weight percentage of the dimorpholine diethyl ether is controlled to be 0.5 percent, and the weight percentage of the dibutyl tin dilaurate is controlled to be 0.004 percent, the dimorpholine diethyl ether and the dibutyl tin dilaurate interact with other components in the body, so that the weather resistance and the strength of the polyurethane hot melt adhesive are improved, the generation of byproducts in the system can be reduced, and due to the special space structures of the dimorpholine diethyl ether and the dibutyl tin dilaurate, the curing time and the curing rate of the polyurethane hot melt adhesive are improved when the adding amount of the dimorpholine diethyl ether and the dibutyl tin dilaurate are strictly controlled, the requirement of secondary activation of the hot melt adhesive within 2 hours is met, and the phenomenon that the felt surface in an automobile spare tire cover plate is easy to rebound and edge warping is effectively avoided;
3. when the random copolymerized olefin is added into the system, especially when the melt viscosity of the random copolymerized olefin at 190 ℃ is 800 Pa.s, the random copolymerized olefin can interact with other components in the system, so that the cohesiveness of the polyurethane hot melt adhesive on the surface of the glass fiber polypropylene composite board is improved, and the peel strength of the polyurethane hot melt adhesive is improved;
4. when the polyurethane hot melt adhesive is added into the system, the viscosity of the acrylic tackifier with the toluene solution viscosity of between 250 and 340mPa.s at 25 ℃ and the mass concentration of 40 percent improves the viscosity of the system, and on one hand, promotes the compatibility of the dimorpholine diethyl ether and the dibutyl tin dilaurate in the system; on the other hand, the leveling property and the diffusivity of the hot melt adhesive are improved, so that the viscosity of a system is in a certain range, the dual effects of enhancing the compatibility and the leveling property among components are achieved, and the wettability and the initial viscosity of the polyurethane hot melt adhesive on the surface of the glass fiber polypropylene composite board are improved;
5. the polyurethane hot melt adhesive prepared by the invention has the advantages that the hydroxyl value of the polymer with the end group of 27-34mg KOH/g and the hydroxyl and alkoxy containing polymer with the number average molecular weight of 3500, and diphenylmethane diisocyanate with the viscosity of 200-400cps at 25 ℃ are introduced into the polymer, and the auxiliary agents such as dimorpholine diethyl ether, dibutyl tin dilaurate and the like are introduced into the polymer, so that the polyurethane hot melt adhesive can realize secondary activation within 2 hours by strictly controlling the proportion of each component, has excellent adhesive force on the surface of the glass fiber polypropylene composite board, effectively solves the problem that the felt surface in the automobile spare tire cover plate is easy to rebound on the bridge edge, and simultaneously has excellent initial strength and final strength.
Drawings
FIG. 1 is a graph showing the cure time controllability of the polyurethane hot melt adhesives prepared in examples 1 to 3.
Wherein A is example 2; b is example 3; c is example 1.
Detailed Description
Examples
Examples1
The embodiment 1 provides a polyurethane hot melt adhesive for a spare tire cover plate of an automobile, which comprises the following raw materials in percentage by weight: 6% of polymer with hydroxyl as a terminal group, 12% of crystalline alcohol modified copolyester, 42% of polymer containing hydroxyl and alkoxy, 15% of aromatic isocyanate compound, 0.5% of amine and derivative thereof, 0.004% of organic tin compound, 8% of random copolymerized polyolefin, 0.2% of defoamer, 0.5% of organosilicon wetting agent and the balance of acrylic tackifier.
The polymer with the end group being hydroxyl is purchased from Shanghai Kaijin chemical engineering Co., ltd, the model is dynacoll 7380, and the hydroxyl value of the polymer with the end group being hydroxyl is 27-34mg KOH/g;
the crystallization type alcohol modified copolyester is purchased from Shanghai Kaijin chemical industry Co., ltd, the model is dynacoll 7360, and the number average molecular weight of the crystallization type alcohol modified copolyester is 3500;
the polymer containing hydroxyl and alkoxy is purchased from Jiangsu Bonsheng chemical Co., ltd, the model is N220, the viscosity of the polymer containing hydroxyl and alkoxy is 200-400cps at 25 ℃, and the weight average molecular weight is 2000;
the aromatic isocyanate compound is diphenylmethane diisocyanate, and the CAS number of the diphenylmethane diisocyanate is 101-68-8;
the amine and the derivative thereof are dimorpholine diethyl ether, and the CAS number of the dimorpholine diethyl ether is 6425-39-4;
the organotin compound is dibutyl tin dilaurate, and the CAS number of the dibutyl tin dilaurate is 77-58-7;
the random copolymer polyolefin is purchased from Shanghai Kaijin chemical industry Co., ltd, the model is winning VESTOPLAAST 508, and the melt viscosity of the random copolymer polyolefin at 190 ℃ is 800 Pa.s;
the acrylic tackifier is purchased from Hebao plastic limited company of Dongguan, the model is Mitsubishi BR113, and the toluene solution viscosity of the acrylic tackifier at 25 ℃ and 40% mass concentration is 250-340mPa.s;
the defoaming agent is stearyl alcohol, and the CAS number of the stearyl alcohol is 112-92-5;
the organosilicon wetting agent is purchased from Mianyang chemical new material technology Co., ltd, and the model is E-520;
the preparation method of the polyurethane hot melt adhesive comprises the following steps:
(1) Pretreatment of raw materials: adding a polymer with a hydroxyl end group, a crystalline alcohol modified copolyester, a polymer containing hydroxyl and alkoxy, a random copolymerized polyolefin, an acrylic tackifier and a defoaming agent into a reaction kettle, heating, introducing nitrogen, stirring, cooling and vacuumizing to obtain a dehydrated raw material;
(2) And (3) preparing a hot melt adhesive: and (3) cooling the dehydrated raw material in the step (1) to 80, adding an aromatic isocyanate compound under the condition of nitrogen to react for 40min at 85 ℃, heating to 110 ℃, vacuumizing, adding amine and derivatives thereof, adding an organic silicon wetting agent to react after adding an organic tin compound to react, and discharging to obtain the polyurethane hot melt adhesive.
Wherein, the temperature of the step (1) is raised to 150 ℃, the replacement time of nitrogen is 30min, the stirring time is 1.5h, the temperature of cooling and vacuumizing is 125 ℃, and the vacuumizing vacuum degree is less than or equal to 0.1MPa;
the heating time in the step (2) is 40min, the reaction time of adding amine and derivatives thereof and the reaction time of adding organic tin compounds is 10min, and the reaction time of adding organic silicon wetting agents is 5min.
Examples2
The embodiment 2 provides a polyurethane hot melt adhesive for a spare tire cover plate of an automobile, which comprises the following raw materials in percentage by weight: 8% of polymer with hydroxyl as a terminal group, 12% of crystalline alcohol modified copolyester, 40% of polymer containing hydroxyl and alkoxy, 15% of aromatic isocyanate compound, 0.3% of amine and derivative thereof, 0.006% of organic tin compound, 8% of random copolymerized polyolefin, 0.2% of defoamer, 0.5% of organosilicon wetting agent and the balance of acrylic tackifier.
The polymer with the end group being hydroxyl is purchased from Shanghai Kaijin chemical engineering Co., ltd, the model is dynacoll 7380, and the hydroxyl value of the polymer with the end group being hydroxyl is 27-34mg KOH/g;
the crystallization type alcohol modified copolyester is purchased from Shanghai Kaijin chemical industry Co., ltd, the model is dynacoll 7360, and the number average molecular weight of the crystallization type alcohol modified copolyester is 3500;
the polymer containing hydroxyl and alkoxy is purchased from Jiangsu Bonsheng chemical Co., ltd, the model is N220, the viscosity of the polymer containing hydroxyl and alkoxy is 200-400cps at 25 ℃, and the weight average molecular weight is 2000;
the aromatic isocyanate compound is diphenylmethane diisocyanate, and the CAS number of the diphenylmethane diisocyanate is 101-68-8;
the amine and the derivative thereof are dimorpholine diethyl ether, and the CAS number of the dimorpholine diethyl ether is 6425-39-4;
the organotin compound is dibutyl tin dilaurate, and the CAS number of the dibutyl tin dilaurate is 77-58-7;
the random copolymer polyolefin is purchased from Shanghai Kaijin chemical industry Co., ltd, the model is winning VESTOPLAAST 508, and the melt viscosity of the random copolymer polyolefin at 190 ℃ is 800 Pa.s;
the acrylic tackifier is purchased from Hebao plastic limited company of Dongguan, the model is Mitsubishi BR113, and the toluene solution viscosity of the acrylic tackifier at 25 ℃ and 40% mass concentration is 250-340mPa.s;
the defoaming agent is stearyl alcohol, and the CAS number of the stearyl alcohol is 112-92-5;
the organosilicon wetting agent is purchased from Mianyang chemical new material technology Co., ltd, and the model is E-520;
the preparation method of the polyurethane hot melt adhesive is the same as that of the example 1.
Examples3
The embodiment 3 provides a polyurethane hot melt adhesive for a spare tire cover plate of an automobile, which comprises the following raw materials in percentage by weight: 6% of polymer with hydroxyl as a terminal group, 10% of crystalline alcohol modified copolyester, 44% of polymer containing hydroxyl and alkoxy, 15% of aromatic isocyanate compound, 0.7% of amine and derivative thereof, 0.002% of organic tin compound, 8% of random copolymerized polyolefin, 0.2% of defoamer, 0.5% of organosilicon wetting agent and the balance of acrylic tackifier.
The polymer with the end group being hydroxyl is purchased from Shanghai Kaijin chemical engineering Co., ltd, the model is dynacoll 7380, and the hydroxyl value of the polymer with the end group being hydroxyl is 27-34mg KOH/g;
the crystallization type alcohol modified copolyester is purchased from Shanghai Kaijin chemical industry Co., ltd, the model is dynacoll 7360, and the number average molecular weight of the crystallization type alcohol modified copolyester is 3500;
the polymer containing hydroxyl and alkoxy is purchased from Jiangsu Bonsheng chemical Co., ltd, the model is N220, the viscosity of the polymer containing hydroxyl and alkoxy is 200-400cps at 25 ℃, and the weight average molecular weight is 2000;
the aromatic isocyanate compound is diphenylmethane diisocyanate, and the CAS number of the diphenylmethane diisocyanate is 101-68-8;
the amine and the derivative thereof are dimorpholine diethyl ether, and the CAS number of the dimorpholine diethyl ether is 6425-39-4;
the organotin compound is dibutyl tin dilaurate, and the CAS number of the dibutyl tin dilaurate is 77-58-7;
the random copolymer polyolefin is purchased from Shanghai Kaijin chemical industry Co., ltd, the model is winning VESTOPLAAST 508, and the melt viscosity of the random copolymer polyolefin at 190 ℃ is 800 Pa.s;
the acrylic tackifier is purchased from Hebao plastic limited company of Dongguan, the model is Mitsubishi BR113, and the toluene solution viscosity of the acrylic tackifier at 25 ℃ and 40% mass concentration is 250-340mPa.s;
the defoaming agent is stearyl alcohol, and the CAS number of the stearyl alcohol is 112-92-5;
the organosilicon wetting agent is purchased from Mianyang chemical new material technology Co., ltd, and the model is E-520;
the preparation method of the polyurethane hot melt adhesive is the same as that of the example 1.
Evaluation of Performance
(1) Peel strength test
The polyurethane hot melt adhesive prepared in examples 1-3 was coated on a 200mm×25mm PVC sheet, and after 30s pressing at 200 ℃, the peel strength of the product was tested according to GB/T2791-1995 adhesive T peel strength test method, and the measured data are shown in Table 1;
(2) Cure time controllability test
The polyurethane hot melt adhesive prepared in the examples 1-3 is coated on a PVC plate with the length of 200mm multiplied by 25mm, the plate is placed in an environment with the temperature of 25 ℃ and the humidity of 50%, the content of isocyanate in the hot melt adhesive is detected, the lower the content of isocyanate is, the more complete the curing of the polyurethane hot melt adhesive is indicated, and the test data are shown in the figure 1;
TABLE 1
Claims (2)
1. The polyurethane hot melt adhesive for the automobile spare tire cover plate is characterized by comprising the following raw materials in parts by weight: 5-10% of polymer with hydroxyl end group, 10-20% of crystalline alcohol modified copolyester, 40-60% of polymer containing hydroxyl and alkoxy, 10-20% of aromatic isocyanate compound, 0.5% of amine and derivative thereof, 0.004% of organic tin compound, 5-10% of random copolymerized polyolefin, 0.1-0.3% of defoamer, 0.4-0.6% of organosilicon wetting agent and the balance of acrylic tackifier; the hydroxyl value of the polymer with the end group being hydroxyl is 27-34mgKOH/g;
the number average molecular weight of the crystalline alcohol modified copolyester is 3500;
the weight average molecular weight of the polymer containing hydroxyl and alkoxy groups is 2000;
the weight ratio of the polymer with the end group of hydroxyl to the crystalline alcohol modified copolyester to the polymer containing hydroxyl and alkoxy is 1:2:7, preparing a base material;
the amine and the derivative thereof are dimorpholine diethyl ether;
the organotin compound is dibutyl tin dilaurate.
2. A process for preparing a polyurethane hot melt adhesive according to claim 1, comprising the steps of:
(1) Pretreatment of raw materials: adding a polymer with a hydroxyl end group, a crystalline alcohol modified copolyester, a polymer containing hydroxyl and alkoxy, a random copolymerized polyolefin, an acrylic tackifier and a defoaming agent into a reaction kettle, heating, introducing nitrogen, stirring, cooling and vacuumizing to obtain a dehydrated raw material;
(2) And (3) preparing a hot melt adhesive: cooling the dehydrated raw material in the step (1) to 60-90 ℃, adding an aromatic isocyanate compound to react for 20-60min under the condition of nitrogen at 80-85 ℃, heating to 100-120 ℃, vacuumizing, adding amine and derivatives thereof, adding an organic silicon wetting agent to react after the organic tin compound reacts, and discharging to obtain the polyurethane hot melt adhesive.
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