CN116656304A - Hot-melt polyurethane adhesive for transparent PET (polyethylene terephthalate) lamination and preparation method thereof - Google Patents

Hot-melt polyurethane adhesive for transparent PET (polyethylene terephthalate) lamination and preparation method thereof Download PDF

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Publication number
CN116656304A
CN116656304A CN202310810627.2A CN202310810627A CN116656304A CN 116656304 A CN116656304 A CN 116656304A CN 202310810627 A CN202310810627 A CN 202310810627A CN 116656304 A CN116656304 A CN 116656304A
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transparent pet
hot melt
polyurethane adhesive
acrylic resin
polyurethane prepolymer
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熊峰
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Guangdong Daoji New Material Co ltd
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Guangdong Daoji New Material Co ltd
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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
    • 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
    • C08G18/2805—Compounds having only one group containing active hydrogen
    • C08G18/288—Compounds containing at least one heteroatom other than oxygen or nitrogen
    • C08G18/289—Compounds containing at least one heteroatom other than oxygen or nitrogen containing silicon
    • 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
    • C08G18/4063—Mixtures of compounds of group C08G18/62 with other macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4202—Two or more polyesters of different physical or chemical nature
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/62—Polymers of compounds having carbon-to-carbon double bonds
    • C08G18/6216—Polymers of alpha-beta ethylenically unsaturated carboxylic acids or of derivatives thereof
    • 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
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • 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
    • C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
    • C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
    • C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
    • C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
    • C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
    • 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
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22—Plastics; Metallised plastics
    • C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/255—Polyesters
    • 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
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • 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
    • C09J2467/00—Presence of polyester
    • C09J2467/006—Presence of polyester in the substrate
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a hot melt polyurethane adhesive for transparent PET lamination and a preparation method thereof, wherein the adhesive comprises the following components in percentage by mass: 96-100% of polyurethane prepolymer and 0-4% of wetting leveling agent; the raw materials for preparing the polyurethane prepolymer comprise solid acrylic resin, polyether polyol and isocyanate; the mass ratio of the solid acrylic resin to the polyether polyol is 0.8-1.5:0.8-1.5; the Tg of the solid acrylic resin is 45-60 ℃, and the molecular weight is 50000-70000; the molecular weight of the polyether polyol is 1000-2000. Mixing a solid acrylic resin and a polyether polyol; dehydrating, adding isonitrile acid ester under inert atmosphere, and heating for reaction to obtain polyurethane prepolymer; and compounding the polyurethane prepolymer with a wetting and leveling agent to obtain the adhesive. The invention provides an environment-friendly transparent PET (polyethylene terephthalate) high-gloss laminating hot-melt polyurethane adhesive with a mirror effect.

Description

Hot-melt polyurethane adhesive for transparent PET (polyethylene terephthalate) lamination and preparation method thereof
Technical Field
The invention relates to the field of hot melt polyurethane adhesives, in particular to a hot melt polyurethane adhesive for transparent PET lamination and a preparation method thereof.
Background
Compared with the traditional wood veneer large plate decoration, the high-gloss PET large plate decoration has the outstanding advantage of attractive appearance and high end, and further the added value of the plate can be improved. The traditional reactive polyurethane hot melt adhesive has low transparency and cannot achieve the effect of a mirror surface.
Disclosure of Invention
Aiming at the problem of low transparency of the polyurethane hot melt adhesive for transparent PET lamination in the prior art, the invention aims to provide the hot melt polyurethane adhesive for transparent PET lamination and a preparation method thereof.
The invention provides a hot melt polyurethane adhesive for transparent PET lamination, which comprises the following components in percentage by mass: 96% -100% of polyurethane prepolymer and 0-4% of wetting leveling agent;
raw materials for preparing the polyurethane prepolymer comprise solid acrylic resin, polyether polyol and isocyanate; the solid acrylic resin comprises the following components in percentage by mass: the polyether polyol=0.8-1.5:0.8-1.5; the glass transition temperature of the solid acrylic resin is 45-60 ℃, and the molecular weight is 50000-70000; the molecular weight of the polyether polyol is 1000-2000.
Preferably, the isocyanate comprises at least one of aromatic isocyanate and aliphatic isocyanate.
Preferably, the isocyanate comprises an aliphatic isocyanate. The aliphatic isocyanate has excellent yellowing resistance.
Preferably, the raw materials for preparing the polyurethane prepolymer further comprise aminosilicone. By introducing the aminosilicone, the aminosilicone can react with the-NCO in the raw materials in the preparation process of the hot melt polyurethane adhesive, so that the-NCO in an adhesive system can be blocked, and when the hot melt polyurethane adhesive is used for moisture curing, the generation of carbon dioxide bubbles after the reaction of active groups-NCO and water is inhibited, and the foaming residue in the adhesive is reduced.
Preferably, the aromatic isocyanate is more than one of diphenyl methylene diisocyanate (MDI, 4-diphenylmethanediisocyanate), 2,4'/4,4' -diphenylmethane diisocyanate (a mixture of 2,4 '-diphenylmethane diisocyanate and 4,4' -diphenylmethane diisocyanate, such as MDI-50, or 1, 6-Hexamethylene Diisocyanate (HDI)); the aliphatic isocyanate is one or more of isophorone diisocyanate, dicyclohexylmethane-4, 4' -diisocyanate (hydrogenated MDI) and 1, 6-Hexamethylene Diisocyanate (HDI).
Further preferably, the 2,4'/4,4' -diphenylmethane diisocyanate is Van der Waals MDI-50.
Preferably, the raw materials for preparing the polyurethane prepolymer comprise 20% -25% of the polyether polyol, 20% -25% of the solid acrylic resin, 8% -15% of the isocyanate and 1% -2% of the aminosilicone in terms of mass fraction.
Preferably, the raw materials for preparing the polyurethane prepolymer include 8 to 10% of the isocyanate in terms of mass fraction.
Preferably, the raw materials for preparing the polyurethane prepolymer further comprise 35-45% of polyester alcohol, wherein the polyester alcohol is at least one of polyester polyol and polyester diol.
Preferably, the viscosity number of the hot melt polyurethane adhesive for transparent PET lamination is 12000-17000cps at 120 ℃.
The invention also provides a preparation method of the hot melt polyurethane adhesive for transparent PET lamination, which is characterized by comprising the following steps:
(1) Uniformly mixing solid acrylic resin and polyether polyol to obtain a mixture;
(2) Dehydrating, and adding isonitrile acid ester under the protection of inert gas to perform heating reaction;
(3) Discharging under the protection of inert gas to obtain polyurethane prepolymer;
(4) And compounding the polyurethane prepolymer with a wetting and leveling agent to obtain the hot-melt polyurethane adhesive for transparent PET lamination.
Preferably, step (1) further comprises adding polyesterol after obtaining the mixture, heating to 120-140 ℃ and dissolving to be homogeneous.
Preferably, step (2) further comprises adding an isonitrile acid ester to heat the reaction followed by the aminosilicone.
Preferably, the water content after dehydration in the step (2) is below 200 PPM; and (3) the NCO of the polyurethane prepolymer in the step (3) reaches 0.
Preferably, in the step (2), the time of vacuumizing and dehydrating is 60-90 minutes.
Preferably, in the step (2), the temperature of the heating reaction is 100-130 ℃, the time of the heating reaction is 2.0-4.0 hours, and the rotating speed of the heating reaction is 60-150 rpm.
Preferably, in the step (3), the time for vacuumizing and removing bubbles is 45-60 minutes before the inert gas is used for discharging.
Preferably, the inert gas is one or more of nitrogen and argon.
Compared with the prior art, the invention has the following beneficial effects:
1. the solid acrylic resin used in the invention is crystalline polyester resin, has higher transparency, can achieve very good transparency after being melted in polyether polyol as tackifying resin, and can obtain polyurethane adhesive with very good transparency by matching with corresponding polyester polyol.
2. The invention controls the residual NCO content at a lower position, and uses aminosilicone to seal NCO, carbon dioxide is not generated in moisture curing, and bubbles generated in the reaction are eliminated.
3. Compared with the common hot melt polyurethane adhesive, the hot melt polyurethane adhesive has the advantages of high transparency, no carbon dioxide bubbles, small viscosity, low use temperature, good leveling property, low cost and the like, provides an environment-friendly transparent PET (polyethylene terephthalate) high-gloss adhesive with mirror effect, and particularly provides an environment-friendly hot melt polyurethane adhesive with outstanding laminating performance for high-gloss large plates.
Drawings
FIG. 1 is a graph showing the tensile test change of the hot melt polyurethane adhesive prepared in example 1.
Detailed Description
In order to make the objects, technical solutions and technical effects of the present invention more clear, the present invention will be described in further detail with reference to the following specific embodiments. It should be understood that the detailed description is presented herein for purposes of illustration only and is not intended to limit the invention.
Example 1
(1) Uniformly mixing 23g of solid acrylic resin (Mitsubishi BR106, tg 50 ℃ C., molecular weight 60000) and 23g of polyether polyol (Dow 2000LM, molecular weight 2000) to obtain a mixture;
(2) Adding the mixture obtained in the step (1), 40g of polyester polyol (25 g of Yingzhang Dynacoll7250 and 15g of Yingzhang Dynacoll 7380), 2.5g of wetting agent and 0.5g of antioxidant into a reactor, heating to 130 ℃ and dissolving to a uniform state;
(3) Vacuumizing and dehydrating for 80 minutes to remove water, wherein the water content is 85 PPM;
(4) Under the protection of nitrogen, 10g of isophorone diisocyanate (IPDI) is added under the condition of 90 ℃ and the reaction is kept at 120 ℃ for 3 hours under the condition of rotating speed of 100 revolutions per minute;
(5) 1g of monoaminosiloxane (silane coupling agent KH-550, gamma-aminopropyl triethoxysilane) is added for reaction until NCO reaction is complete, and sampling is carried out to measure NCO to be zero;
(6) Vacuumizing again to remove bubbles for 55 minutes;
(7) Discharging under the protection of nitrogen to obtain polyurethane prepolymer, namely the hot melt polyurethane adhesive for transparent PET lamination.
Example 2
This example is the same as example 1 except that in step (5) no monoaminosiloxane is added and the NCO is 0.19wt% (mass%) as measured by sampling.
Example 3
This example is the same as example 1 except that diphenyl Methylene Diisocyanate (MDI) is added instead of isophorone diisocyanate (IPDI) in step (4).
Example 4
97g of the polyurethane prepolymer obtained in example 1 was mixed with 3g of a wetting and leveling agent to obtain a hot melt polyurethane adhesive for transparent PET lamination, and the rest was the same as in example 1.
Comparative example 1
This comparative example is the same as example 1, except that a solid acrylic resin (Mitsubishi BR113, tg 75 ℃ C., molecular weight 30000) is used in step (1).
Comparative example 2
(1) Under nitrogen protection, 23g of solid acrylic resin (Mitsubishi BR106, tg 50 ℃ C., molecular weight 60000), 23g of polyether polyol (Dow 2000LM, molecular weight 2000), 40g of polyester polyol (25 g of Yingzhang Dynacoll7250 and 15g of Yingzhang Dynacoll 7380), 2.5g of wetting agent and 0.5g of antioxidant, 10g of isophorone diisocyanate (IPDI) were reacted at a rotation speed of 100 rpm for 3 hours at 120 ℃;
(2) 1g of monoaminosiloxane (silane coupling agent KH-550, gamma-aminopropyl triethoxysilane) is added for reaction until NCO reaction is complete, and sampling is carried out to measure NCO to be zero;
(3) Vacuumizing again to remove bubbles for 55 minutes;
(4) Discharging under the protection of nitrogen to obtain the polyurethane prepolymer.
Comparative example 3
The comparative examples were carried out in steps (4) to (6) each in air and the remainder were the same as in example 1.
Performance testing
The hot melt polyurethane adhesive prepared in the example 4 is sized by adopting a roller coating mode, the temperature of heat conduction oil is controlled between 140 and 150 ℃, the temperature of a rubber roller is controlled between 130 and 140 ℃, and the temperature of rubber is controlled between 120 and 130 ℃. Gluing by using ecological particle board, laminating transparent PET film (thickness of 0.14 mm), and controlling the glue amount at 30-40g/m 2 . Performance testing and performance analysis were performed at 25 ℃ and 55% rh (relative humidity) humidity conditions for 3 days of curing:
(1) And (3) tensile force test:
sample preparation: 2cm width 5 strips;
stretching speed: 50mm/min
And (3) recording results:
table 1 example 4 hot melt polyurethane adhesive tensile force value record
As is clear from Table 1, the final strength of example 4 was 56.57N/2cm, which reached a higher level.
Table 2 comparison of the Hot melt polyurethane adhesive properties of examples 1-4 and comparative examples 1-3
As can be seen from Table 2, the hot melt polyurethane adhesives prepared in examples 1-4 of the present invention all had high transparency, and example 2 was not blocked with a monoaminosiloxane, and was transparent first and then hazed due to air bubbles. Example 3 the same transparent effect was achieved using the aromatic isocyanate diphenyl Methylene Diisocyanate (MDI), but it was subject to yellowing. Example 4 in order to mix the polyurethane prepolymer prepared in example 1 with a wetting and leveling agent, the wetting and leveling agent can improve the workability of the polyurethane adhesive to achieve the fitting flatness, so that the obtained hot melt polyurethane adhesive is transparent and has the best overall effect (proper viscosity and good leveling). Comparative example 1 uses a solid acrylic resin with a Tg of 75 ℃ and a molecular weight of 30000, and the obtained hot melt polyurethane adhesive is semitransparent and has obvious chrysanthemum patterns, which indicates that the glass transition temperature of the used solid acrylic resin is 45-60 ℃ and the molecular weight of 50000-70000 can achieve the transparent beneficial effect of the invention. Comparative example 2 is a hot melt polyurethane adhesive which is prepared by directly mixing all the raw materials for reaction, and has no corresponding addition sequence, is semitransparent and has particles. Comparative example 3 is a reaction under air conditions, and the obtained hot melt polyurethane adhesive is translucent and has obvious chrysanthemum, and cannot obtain the transparent beneficial effect.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention.

Claims (10)

1. The hot melt polyurethane adhesive for transparent PET lamination is characterized by comprising the following components in percentage by mass: 96% -100% of polyurethane prepolymer and 0-4% of wetting leveling agent;
raw materials for preparing the polyurethane prepolymer comprise solid acrylic resin, polyether polyol and isocyanate; the solid acrylic resin comprises the following components in percentage by mass: the polyether polyol=0.8-1.5:0.8-1.5; the glass transition temperature of the solid acrylic resin is 45-60 ℃, and the molecular weight is 50000-70000; the molecular weight of the polyether polyol is 1000-2000.
2. The hot melt polyurethane adhesive for transparent PET lamination of claim 1, wherein the isocyanate comprises at least one of an aromatic isocyanate and an aliphatic isocyanate.
3. The hot melt polyurethane adhesive for transparent PET lamination of claim 2, wherein the isocyanate comprises an aliphatic isocyanate.
4. The hot melt polyurethane adhesive for transparent PET lamination of claim 1, wherein the raw materials for preparing the polyurethane prepolymer further comprise aminosilicone.
5. The hot melt polyurethane adhesive for transparent PET lamination according to claim 4, wherein the raw materials for preparing the polyurethane prepolymer comprise 20% -25% of the polyether polyol, 20% -25% of the solid acrylic resin, 8% -15% of the isocyanate and 1% -2% of the aminosilicone in terms of mass fraction.
6. The hot melt polyurethane adhesive for transparent PET lamination according to claim 5, wherein the raw materials for preparing the polyurethane prepolymer further comprise 35-45% of polyesterol, wherein the polyesterol is at least one of polyesterpolyol and polyesterdiol according to mass fraction.
7. A method for preparing a hot melt polyurethane adhesive for transparent PET lamination as defined in any one of claims 1 to 6, comprising the steps of:
(1) Uniformly mixing solid acrylic resin and polyether polyol to obtain a mixture;
(2) Dehydrating, and adding isonitrile acid ester under the protection of inert gas to perform heating reaction;
(3) Discharging under the protection of inert gas to obtain polyurethane prepolymer;
(4) And compounding the polyurethane prepolymer with a wetting and leveling agent to obtain the hot-melt polyurethane adhesive for transparent PET lamination.
8. The method of preparing a hot melt polyurethane adhesive for transparent PET lamination as defined in claim 7, wherein step (1) further comprises adding polyesterol after obtaining the mixture, and heating and dissolving until homogeneous phase.
9. The method of claim 7, wherein step (2) further comprises adding an isonitrile acid ester, heating, and adding an aminosilicone.
10. The method for producing a hot melt polyurethane adhesive for transparent PET lamination according to claim 7, wherein the water content after dehydration in step (2) is 200PPM or less; and (3) the NCO of the polyurethane prepolymer in the step (3) reaches 0.
CN202310810627.2A 2023-07-03 2023-07-03 Hot-melt polyurethane adhesive for transparent PET (polyethylene terephthalate) lamination and preparation method thereof Pending CN116656304A (en)

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