Integral hot melt adhesive packaging films and use thereof

Abstract

Propylene polymer based packaging films for encapsulating hot melt adhesives are disclosed. The packaging films are readily miscible with the various hot melt adhesive chemistries during the melting stage without deleteriously affecting the adhesive properties, making the packaging film particularly well suited for packaging hot melt adhesives in a pillow, cylinder, pouch, block, cartridge and like forms.

Claims

1. A method of forming a cylindrical integral hot melt adhesive package comprising the steps of: 1. preparing packaging film as an encapsulating vessel; 2. pumping or pouring the hot melt adhesive in a molten state into the packaging film, wherein the packaging film is in direct contact with a heat sink; 3. sealing the packaging film; and 4. cooling the sealed package; and wherein the packaging film comprises a polymer blend comprising at least 70 wt % of propylene and up to 15 wt % of ethylene content; and the packaging film has (a) a viscosity range of about 200,000 to 3,000,000 cps at 200 C. with a rheometer with near-zero shear; (b) a peak melting temperature range of about 90 to 140 C.; (c) a Tm offset temperature below 149 C.; and (d) a storage modulus (G) range of about 110.sup.6 to about 110.sup.8 Pascal at 100 C. with frequency at 10 rad/s; wherein the hot melt adhesive selected is from the group consisting of poly-alpha-olefins, rubbers, styrenic block-copolymers, ethylene-vinyl acetates, ethylene-butyl acetates, and mixtures thereof; and wherein the cooled sealed package is non-tacky.

2. The method of forming an integral hot melt adhesive package of claim 1 wherein pumping or pouring the hot melt adhesive in a molten state is conducted at temperatures of about 150 C. or below.

3. The method of forming an integral hot melt adhesive package of claim 1 wherein the heat sink is water.

Description

BRIEF DESCRIPTION OF THE DRAWING

(1) FIG. 1 is a DSC scan of Sample 4, showing peak melting point, Tm onset and Tm offset values.

DETAILED DESCRIPTION OF THE INVENTION

(2) The term olefin hot melt adhesive is used herein generically to refer to all polyolefin based hot melt adhesives, including but not limiting to hot melt adhesives made from amorphous olefin, polyethylene, polypropylene, polybutene and their copolymers.

(3) The terms wrapped, encapsulated and packaged are used interchangeable herein and mean that blocks of hot melt adhesives are encased within a layer of film. The film is a tackless or non-blocking layer and further serves to protect the adhesive from contamination, serves to allow easy shipping and handling.

(4) The term integral package film is used herein as package film that surrounds blocks of hot melt adhesive and can be processed (melted and applied onto substrates) without the removal of the film during the heating and application of the adhesive. Similar to packaged films, the integral package film is also non-blocking and protects the adhesives from contaminations.

(5) The integral packaging film comprises a polymer blend. The polymer blend comprises at least two thermoplastic polymers, and the blend has a propylene content of at least about 70 wt %, and up to about 99 wt %, based on the total weight of the polymer blend. Examples of propylene rich copolymers are LMPP 400 and LMPP 600 from Idemitsu Kosan Co., Ltd; Linxar 127, Vistamaxx 6202, Vistamaxx 6102, Vistamaxx 3980, Vistamaxx 3020, Vistamaxx 3000 from ExxonMobile Corp; and the like.

(6) In one embodiment, the other thermoplastic polymer(s) is a butene and/or ethylene comonomers. The other thermoplastic polymers may account from about 1 wt % to about 30 wt %, based on the total weight of the polymer blend. Ethylenes may be accountable up to 15 wt %, preferably below 10 wt %, based on the total weight of the polymer blend. Suitable commercial butene rich polymers include Vestoplast 308, Vestoplast 408, Vestoplast 508, Vestoplast 520, Vestoplast 608, Vestoplast 703 from Evonik Industries, and the like. Suitable commercial ethylene rich polymers include Affinity GA1950 from Dow Chemicals, and the like.

(7) At least one thermoplastic polymer is a metallocene catalyzed polymer. Suitable polymers include metallocene catalyzed polyethylenes, ethylene-butene and ethylene-octane elastomers, plastomers, propylene-butene, propylene-ethylene copolymers.

(8) The films may, if desired, contain antioxidants for enhanced stability as well as other optional components including slip agents such as erucamide, anti-blocking agents such as diatomaceous earth, fatty amides or other processing aids, anti-stats, stabilizers, plasticizers, dyes, perfumes, fillers such as talc or calcium carbonate and the like.

(9) The polymer blends may be blended by any means known in the art. In one embodiment, the polymer blend is processed in a twin screw extruder for mixing and melting. The melted blend is then cast to a film by any means known in the art. The thickness of the film will generally vary from about 0.5 mil to about 5 mil, preferably from about 1 mil to about 3 mil. The thickness of the particular film also varies depending upon the composition and application temperature. The film may be a monolayer or multi-layered film.

(10) It has been discovered that the packaging film must have a specific combination of properties in order to form an integral hot melt adhesive package that is chemically compatible with various hot melt adhesive chemistries while maintaining integrity as a packaging film for the hot melt adhesives. Such packaging film requires (a) a viscosity range of about 200,000 to 3,000,000 cps at 200 C.; (b) a peak melting temperature (Tm) range of about 90 to 140 C. (c) a melting temperature (Tm) offset temperature below 149 C.; and (d) a storage modulus (G) range of about 110.sup.6 to about 110.sup.8 Pascal at 100 C.

(11) The peak melting points and offset can be determined by various methods known in the art. The reported peak melting points and Tm offset values reported herein were determined with a DSC (differential scanning calorimetry). Unless otherwise stated, about 5 mg of the film sample was sealed in a crimped alumina pan, cooled the sample to 40 C., and reheated it to 180 C. at a rate of 10 C./min with 2920 DSC TA Instruments. The endothermic melting peak on the second heat up cycle was used to evaluate the peak melting point and heat of fusion, and the end of melting peak was the Tm offset temperature.

(12) The packaging film must encompass all of the above properties in order to form a packaging film, maintain integrity of the film while encapsulating a molten adhesive, result in a non-tacky barrier seal for the molten adhesive and dissolve completely in with the hot melt adhesive upon melting without any agitation. The packaging film is non-blocking at elevated temperatures, temperatures that simulate box car conditions (35-45 C.). The packaging film melts at temperatures above about 149 C. without any agitation or additional energy within 5 hours. The packaging film is meltable together with various and multiple hot melt adhesives and is blendable into the molten hot melt adhesives without deleteriously affecting the properties of the adhesive.

(13) Another embodiment is directed to an article comprising a hot melt adhesive encased with a packing film. The article is an integral hot melt adhesive package formed as a pillow, cylinder, pouch, block, cartridge or chub.

(14) The hot melt adhesive of the integral hot melt adhesive package comprises various thermoplastic polymers. The hot melt adhesives are mainly composed of polymers that include poly-alpha-olefins, rubbers, styrenic block-copolymers, ethylene-vinyl acetates, ethylene-butyl acetates, and/or mixtures thereof. The hot melt adhesives may optionally comprise tackifiers, plasticizer, oils, waxes, and additives.

(15) In one embodiment, the packaging film comprise up to about 2% by weight of the integral hot melt adhesive package, and preferably from about 0.1 to about 1.5%, in order to prevent undue dilution of the adhesive properties. Typically, each packing film has a thickness range of from about 0.5 mil to about 5 mil, preferably from about 1 mil to about 3 mil.

(16) The packaging film of the integral hot melt adhesive package is miscible in various hot melt adhesives without any portions of the film separating from the molten hot melt adhesive by floating on the surface of the hot melt or adhering to the walls of the melt tank.

(17) Typically to form a miscible, chemically compatible and non-separating adhesive, the packaging film is chosen based on the predominant polymer used in the hot melt adhesive. Failure to pick a compatible hot melt adhesive and packaging film results in portions of the films floating on the surface of the hot melt or adhering to the walls of the melt tank. It has been discovered that the instant packaging film is miscible with multiple hot melt adhesive chemistries, e.g., polyolefins, rubbers, ethylene-vinyl acetate copolymers, polyamides, polyesters, polyurethanes, and the like, while forming a non-tacky outer protection.

(18) To package a hot melt adhesive with the packaging film, the hot melt adhesive is melted and pumped or poured into a cylindrical thermoplastic film, where the cylindrical tube being in direct contact with a heat sink, e.g., cooled water or a cooled liquid or gaseous environment. Wrapping and sealing the film can occur either manually or, more preferably, by an automated procedure. The hot melt adhesive being poured or pumped is at a temperature at or above the melting point of the packaging film and the interior of the packaging film becomes melted together with the molten hot melt adhesive and blended into the molten adhesive without deleteriously affecting the properties of the adhesive. The molten hot melt adhesive filled cylinder is sealed and allowed to solidify. Optionally, air is removed with a vacuum during the sealing process, and as a result no gap exists between the film and the hot melt adhesive. The resultant individually integral hot melt adhesive packages can be stored, handled and used without the individual packages sticking together, adhering to other objects, or becoming contaminated even if exposed to increased pressure and/or temperature.

(19) To ultimately utilize the integral hot melt adhesive packages as an adhesive, the package is placed to the melt tank, without removing the film. The strong interface or interphase, between the hot melt adhesive and integral packaging film, requires very little additional energy to melt and blend the film into the adhesive itself.

EXAMPLES

Example 1

(20) Samples 1-7 were formed as packaging film. The propylene (PP) and butene/ethylene comonomer contents are listed in Table 1. Viscosity was measured at 200 C. with a rheometer with near-zero shear. The films were formed by melting the polymer components through a twin-screw extruder, and then casting it on a cold roll at a thickness of 1.5 mil. The miscibility of the film was evaluated by melting approximately 10,000 grams of an amorphous poly alpha-olefin adhesive (DISPOMELT LITE 300 from Henkel Corporation) in a melt tank with about 0.5 wt % (based on the adhesive) of the film sample at 160 C. The length of time that it took for the film sample to melt into the adhesive, without any agitation, was recorded. For Sample 8, EVA film with 3% VA content blow film was also employed for this study.

(21) TABLE-US-00001 TABLE 1 Polymer blend. Butene/ Ethylene Viscosity MFR (ref.) Film Propylen Comonomer (cps at g/10 min @ Film Film Sample (%) (%) 200 C.) 230 C. Feasibility Miscibility 1 36.4 63.4 45,000 N/A Difficult N/A 2 73.2 26.8 1,000,000 N/A good 3 h 3 91.5 8.5 3,000,000 8.3 good 3 h 4 97 3 1,800,000 12 good 3 h 5 97 3 680,000 30 good 3 h 6 97 3 810,000 N/A good 3 h 7 Non-metallocene-(PP) 2,200,000 12 good >5 h based polymer (~97% PP and 3% comonomer) 8 EVA with 3% VA 5,000,000 2.3 good >24 h N/Anot available

(22) Film sample 1, with a low melt viscosity, less than 200,000 at 200 C., could not be converted to a film. All other samples, Film Samples 2-8, were cast as films.

(23) Film samples 2-6 were melted into DISPOMELT LITE 300, and became a homogeneous mass in less than three hours. Film sample 7 also became homogenous mass, but the non-metallocene based polypropylene copolymer film took greater than five hours to become miscible with the amorphous poly-alpha-olefin type hot melt adhesive. EVA film, Film Sample 8, took more than 24 hours to melt into the adhesive. Moreover, the EVA film gelled and formed hard clusters, and some of the hard clusters floated on the hot melt tank surfaces. Such hard clusters are undesirable for they tend to block the spray or slot nozzles.

Example 2

(24) The melting temperature and melt modulus of the sample films were characterized to assess their melt strength, and the results are shown in Table 2. Melting points were determined with a 2920 DSC (differential scanning calorimetry) TA Instruments. About 5-10 mg of a sample was sealed in a crimped alumina pan, cooled to 40 C., and reheated it to 180 C. at a rate of 10 C./min with 2920 DSC TA Instruments. The second heat up cycle was used to evaluate the peak melting point and Tm offset values.

(25) The storage modulus (G) of the film at 100 C. was measured by a Rheometric Dynamic Analyzer (RDA III) and TA Orchestrator software version 7.2.0.2. The adhesive sample is loaded into parallel plates 7.9 mm in diameter and separated by a gap of about 2 mm. The sample was then cooled to about 30 C., and the time program was started. The program test increased the temperature at 5 C. intervals followed by a soak time at each temperature of 10 seconds. The convection oven containing the sample was flushed continuously with nitrogen. The frequency is maintained at 10 rad/s. The initial strain at the start of the test was 0.05% (at the outer edge of the plates). An autostrain option in the software was used to maintain an accurately measurable torque throughout the test. The option was configured such that the maximum applied strain allowed by the software was 30%. The autostrain program adjusted the strain at each temperature increment. The shear storage or elastic modulus (G) was calculated by the software from the torque and strain data.

(26) The film strength of the film sample was evaluated by encapsulating a molten DISPOMELT LITE Lite 300 with the film samples to form a package. The quality and the strength of the package after cooling were visually evaluated. If the film sample maintained the integrity and formed an encasement of the hot melt adhesive, the film was given a rating of strong. If any holes or the hot melt adhesive destroyed the integrity of the film sample, then a rating of weak was given to the film.

(27) TABLE-US-00002 TABLE 2 Melt strength of films and their application in hot melt capsulation Melt Strength Film Tm Peak G at 100 C. Sample ( C.) (Pascal) Film strength 1 104 1.0 10.sup.4 Weak 2 82 4.5 10.sup.4 Weak 3 80 7.0 10.sup.4 Weak 8 106 2.0 10.sup.6 Strong 4 123 6.0 10.sup.6 Strong 5 138 1.55 10.sup.7 Strong 6 123 8.0 10.sup.6 Strong 7 147 2.5 10.sup.8 Strong 8 106 .sup.2 10.sup.6 Strong

(28) Samples 1-3 burst during the filling process, resulting in unacceptable packages. Sample 4-8 was strong enough to form acceptable packages without any bursts in the sample film. It was discovered that peak Tm ranges of about 90 to 140 C. and a storage modulus of about 110.sup.6 to about 110.sup.8 Pascal at 100 C. allowed the films to withstand the filling process and result in acceptable quality of packages.

Example 3

(29) Samples 4-8 were tested for their sprayability. About 10,000 g sample of DISPOMELT LITE Lite 300 adhesive was encapsulated with a sample film having a thickness of about 1.5 mil. The package was loaded into a hot melt tank set for 160 C. for three hours for samples 4-6 (ten hours for sample 7, and 24 hours for sample 8). The molten adhesive was then sprayed through a four-port ITW spray head (Nordson) and the number of stray globs/minute was recorded in Table 3. The Tm offset of each of the sample film are also recorded in Table 3.

(30) TABLE-US-00003 TABLE 3 Film/adhesive package's meltdown and sprayability Stray Sprayability Film Sample (with DISPOMELT LITE 300) Tm offset ( C.) 4 2 globs/min 134 5 2 globs/min 144 6 2 globs/min 144 7 >10 globs/min 158 8 >400 globs/min 115

(31) Sample 7 had greater than 10 stray globs/minute. In contrast, samples 4-6 had only two stray globs/minute. Unlike sample 7, samples 4-6 have Tm offset values lower than 149 C. It was discovered that packaging films having Tm offset value below 149 C. is an important factor to minimize strays in sprayability. While Sample 8 also has a Tm Offset value less than 149 C., immiscibility of the EVA film with the encapsulated adhesive is a limitation resulting in increased strays.

Example 4

(32) Hot melt adhesive packages with various hot melt adhesives (1,000 g) and packaging film (0.5 wt % based on the hot melt adhesive) were formed and are listed in Table 4. Each package was loaded into a hot melt tank and heated at the listed temperature without any agitation. The miscibility of the film in the hot melt adhesives was visually observed. Also, the length of time required to fully dissolve the film sample and become miscible in the adhesive was noted.

(33) TABLE-US-00004 TABLE 4 Film Miscibility with Various Hot Melt Adhesive Hot Melt Adhesive Testing Miscibility (polymer type) Film Temperature Observation DISPOMELT LITE 300 Film 160 C. Completely from Henkel Corporation sample 5 Miscible in less (Amorphous poly-alpha than 3 hours olefin adhesive) DISPOMELT 901B from Film 160 C. Completely Henkel Corporation sample 5 Miscible in less (Styrenic block copolymer than 3 hours based adhesive

(34) As observed above, the packaging film (1) made with a polypropylene copolymer that comprises at least 70 wt % propylene content; (2) has a viscosity range of about 200,000 to 3,000,000 cps at 200 C.; (3) has a melting peak temperature range of about 90 to 140 C., (4) has an Tm offset temperature below 149 C.; (5) has a storage modulus (G) at 100 C. of about 110.sup.6 to 110.sup.8 Pascal, is miscible with various and multiple hot melt adhesives formed from various polymers, and may be used as a universal packaging adhesive for integral hot melt adhesive packages.