A SURFACE-TREATED FILLER MATERIAL PRODUCT PROVIDING IMPROVED UV STABILITY FOR POLYMERIC ARTICLES
20220081530 · 2022-03-17
Inventors
- Matthias WELKER (Hésingue, FR)
- Tazio Fornera (Zofingen, CH)
- Karsten Udo SCHULZ (Kriens, CH)
- Samuel Rentsch (Spiegel bei Bern, CH)
Cpc classification
B29K2509/00
PERFORMING OPERATIONS; TRANSPORTING
C08K2201/003
CHEMISTRY; METALLURGY
C08K9/08
CHEMISTRY; METALLURGY
C08K9/08
CHEMISTRY; METALLURGY
C08L2201/08
CHEMISTRY; METALLURGY
C08K2201/005
CHEMISTRY; METALLURGY
B29C48/022
PERFORMING OPERATIONS; TRANSPORTING
C09C3/08
CHEMISTRY; METALLURGY
C08K3/014
CHEMISTRY; METALLURGY
C08L63/00
CHEMISTRY; METALLURGY
C09C3/10
CHEMISTRY; METALLURGY
C08K5/005
CHEMISTRY; METALLURGY
C01P2004/51
CHEMISTRY; METALLURGY
International classification
B29C48/00
PERFORMING OPERATIONS; TRANSPORTING
C08K9/08
CHEMISTRY; METALLURGY
Abstract
The present invention relates to a surface-treated filler material product comprising filler material comprising at least one epoxy-functional compound having one or more epoxy group(s) and/or reaction products thereof, a process for preparing said surface-treated filler material product, a polymer composition comprising at least one polymeric resin and from 1 to 70 wt.-%, based on the total weight of the polymer composition, of said surface-treated filler material product, a polymeric article comprising said surface-treated filler material product and/or the polymer composition as well as the use of the surface-treated filler material product to reduce degradation of the mechanical properties in a polymeric article comprising the surface-treated filler material product when exposed to UV light.
Claims
1. A surface-treated filler material product, wherein the surface-treated filler material product comprises A) at least one calcium carbonate-comprising filler material having a weight median particle size d.sub.50 in the range from 0.1 μm to 7 μm, a top cut particle size d.sub.98 of ≤50 μm, and B) a treatment layer on the surface of the at least one calcium carbonate-comprising filler material comprising at least one epoxy-functional compound having one or more epoxy group(s) and/or reaction products thereof, wherein the surface-treated filler material product comprises the treatment layer in an amount of from 0.1 to 3 wt.-%, based on the total dry weight of the at least one calcium carbonate-comprising filler material, wherein the treatment layer on the surface of the at least one calcium carbonate-comprising filler material further comprises at least one saturated aliphatic linear or branched carboxylic acid and/or reaction products thereof or at least one mono-substituted succinic anhydride and/or reaction products thereof.
2. The surface-treated filler material product of claim 1, wherein the at least one calcium carbonate-comprising filler material is selected from the group consisting of ground calcium carbonate, preferably marble, limestone, and/or chalk, precipitated calcium carbonate (PCC), preferably vaterite, calcite and/or aragonite, surface-reacted calcium carbonate (MCC) and mixtures thereof, more preferably the calcium carbonate-comprising filler material is ground calcium carbonate.
3. The surface-treated filler material product of claim 1, wherein the at least one calcium carbonate-comprising filler material has a) a weight median particle size d.sub.50 value in the range from 0.25 μm to 5 μm and most preferably from 0.5 μm to 4 μm, and/or b) a top cut (d.sub.98) of ≤40 μm, more preferably ≤25 μm and most preferably ≤15 μm, and/or c) a specific surface area (BET) of from 0.5 to 150 m.sup.2/g, preferably from 0.5 to 50 m.sup.2/g, more preferably from 0.5 to 35 m.sup.2/g and most preferably from 0.5 to 10 m.sup.2/g, measured using nitrogen and the BET method according to ISO 9277.
4. The surface-treated filler material product of claim 1, wherein the at least one epoxy-functional compound having one or more epoxy group(s) is a compound selected from i) an epoxy-functional aliphatic linear or branched carboxylic acid having a total amount of carbon atoms from C8 to C24, preferably an epoxy-functional aliphatic linear or branched carboxylic acid having one to three epoxy group(s), and/or ii) an epoxy-functional triglyceride comprising derivatized linolenic acid such as α-linolenic acid or γ-linolenic acid, linoleic acid and/or oleic acid, preferably epoxy-functional triglyceride comprising derivatized linoleic acid.
5. The surface-treated filler material product of claim 1, wherein the at least one epoxy-functional compound having one or more epoxy group(s) is selected from epoxy-functional vegetable oils, such as epoxy-functional soybean oil or epoxy-functional linseed oil, epoxy-functional octyl tallate, epoxy-functional octadeca-7,9-dienoic acid and esters thereof, and mixtures thereof.
6. The surface-treated filler material product of claim 1, wherein the at least one epoxy-functional compound having one or more epoxy group(s) is selected from an epoxy-functional styrene-(meth)acrylic oligomer or polymer, an epoxy-functional ethylene-(meth)acrylic oligomer or polymer and 1,5-epoxy resins.
7. The surface-treated filler material product of claim 6, wherein the epoxy-functional styrene-(meth)acrylic oligomer or polymer i) is the polymerization product of (i) at least one epoxy-functional (meth)acrylic monomer; and (ii) at least one styrene monomer and optionally (meth)acrylic monomer, and/or ii) has an average number of three to five, preferably an average number of four, epoxy groups per oligomer or polymer chain, and/or iii) has an epoxy equivalent weight of from about 180 to about 2800 g/mol, and/or iv) a glass transition temperature Tg in the range from −50 to +60° C., and/or v) a molecular weight (Mw) in the range from 1 000 to 9 000 g/mol.
8. The surface-treated filler material product of claim 6, wherein the epoxy-functional ethylene-(meth)acrylic oligomer or polymer i) is the polymerization product of (i) at least one epoxy-functional (meth)acrylic monomer; and (ii) at least one ethylene monomer and optionally (meth)acrylic monomer, and/or ii) has a melting temperature Tm in the range from 25 to 50° C., and/or iii) comprises epoxy-functional (meth)acrylic monomers in an amount ranging from 4 to 18 wt.-%, preferably from 5 to 12 wt.-% and most preferably from 6 to 10 wt.-%, based on the total weight of the epoxy-functional ethylene-(meth)acrylic oligomer or polymer, and/or iv) comprises (meth)acrylic monomers in an amount ranging from 12 to 40 wt.-%, preferably from 15 to 38 wt.-% and most preferably from 18 to 25 wt.-%, based on the total weight of the epoxy-functional ethylene-(meth)acrylic oligomer or polymer.
9. (canceled)
10. A process for preparing a surface-treated filler material product according to claim 1, the process comprising at least the steps of: a) providing at least one calcium carbonate-comprising filler material, b) providing at least one epoxy-functional compound having one or more epoxy group(s), c) contacting the surface of the at least one calcium carbonate-comprising filler material of step a), under mixing, in one or more steps, with the at least one epoxy-functional compound having one or more epoxy group(s) such that a treatment layer comprising the at least one epoxy-functional compound having one or more epoxy group(s) and/or reaction product(s) thereof is formed on the surface of said at least one calcium carbonate-comprising filler material of step a), wherein the temperature before and/or during contacting step c) is adjusted such that the at least one compound having one or more epoxy group(s) is in a molten or liquid state.
11. The process of claim 10, wherein the at least one calcium carbonate-comprising filler material of step a) is preheated before contacting step c) is carried out, preferably the at least one calcium carbonate-comprising filler material of step a) is preheated at a temperature of from 20 to 200° C., more preferably of from 40 to 200° C., even more preferably of from 50 to 180° C. and most preferably of from 60 to 160° C.
12. The process of claim 10, wherein contacting step c) is carried out at a temperature of from 20 to 200° C., more preferably of from 40 to 200° C., even more preferably of from 50 to 180° C. and most preferably of from 60 to 160° C.
13. The process of claim 10, wherein the process further comprises a step d) of contacting the at least one calcium carbonate-comprising filler material of step a), under mixing, before, during and/or after step c), preferably before step c), in one or more steps, with at least one saturated aliphatic linear or branched carboxylic acid or at least one mono-substituted succinic anhydride.
14. Process for preparing a masterbatch or compound comprising a surface-treated filler material product according to claim 1, the process comprising at least the steps of mixing and/or kneading at least one polymeric resin, preferably selected from homopolymers and/or copolymers of polyolefins, more preferably polyethylene or polypropylene, and the surface-treated filler material product to form a mixture and continuously pelletizing the obtained mixture.
15. A polymer composition comprising at least one polymeric resin and from 1 to 70 wt.-%, preferably 1 to 40 wt.-%, and most preferably 1 to 20 wt.-%, based on the total weight of the polymer composition, of a surface-treated filler material product according to claim 1.
16. The polymer composition according to claim 15, wherein the at least one polymeric resin is selected from homopolymers and/or copolymers of polyolefins, preferably polyethylene or polypropylene.
17. Polymeric article, preferably processed by extrusion process, co-extrusion process, blown film extrusion process, cast film extrusion, tape extrusion process or sheet extrusion process, extrusion coating process, injection molding process, blow molding process, thermoforming process, or rotomolding, comprising a surface-treated filler material product according to claim 1.
18. Use of a surface-treated filler material product according to claim 1 to reduce degradation of the mechanical properties in a polymeric article comprising the surface-treated filler material product when exposed to UV light.
19. Polymeric article, preferably processed by extrusion process, co-extrusion process, blown film extrusion process, cast film extrusion, tape extrusion process or sheet extrusion process, extrusion coating process, injection molding process, blow molding process, thermoforming process, or rotomolding, comprising a polymer composition, wherein the polymer composition comprises at least one polymeric resin and from 1 to 70 wt.-%, preferably 1 to 40 wt.-%, and most preferably 1 to 20 wt.-%, based on the total weight of the polymer composition, of a surface-treated filler material product according to claim 1.
Description
EXAMPLES
[0215] A) Measurement Methods
[0216] The following measurement methods are used to evaluate the parameters given in the examples and claims.
[0217] Particle Size Distribution (Mass % Particles with a Diameter<X) and Weight Median Diameter (d.sub.50) of a Particulate Material
[0218] As used herein and as generally defined in the art, the “d.sub.50” value was determined based on measurements made by using a Sedigraph™ 5100 of Micromeritics Instrument Corporation and is defined as the size at which 50% (the median point) of the particle mass is accounted for by particles having a diameter equal to the specified value.
[0219] The method and the instrument are known to the skilled person and are commonly used to determine grain size of fillers and pigments. The measurement was carried out in an aqueous solution of 0.1 wt.-% Na.sub.4P.sub.2O.sub.7. The samples were dispersed using a high speed stirrer and supersonics.
[0220] BET Specific Surface Area of a Material
[0221] Throughout the present document, the specific surface area was measured via the BET method according to ISO 9277:2010 using nitrogen, following conditioning of the sample by heating at 250° C. for a period of 30 minutes. Prior to such measurements, the sample was filtered within a Büchner funnel, rinsed with deionised water and dried overnight at 90 to 100° C. in an oven. Subsequently, the dry cake was ground thoroughly in a mortar and the resulting powder was placed in a moisture balance at 130° C. until a constant weight was reached.
[0222] Amount of Surface-Treatment Layer
[0223] The amount of the treatment layer on the calcium carbonate-comprising filler material was calculated theoretically from the values of the BET of the untreated calcium carbonate-comprising filler material and the amount of surface treatment agent that was used for the surface-treatment. It is assumed that 100% of the surface treatment agents added to the calcium carbonate-comprising filler material are present as surface treatment layer on the surface of the calcium carbonate-comprising filler material.
[0224] Melt Flow Rate MFR.sub.2
[0225] The melt flow rate MFR.sub.2 (230° C., 2.16 kg) was measured at 230° C. under a load of 2.16 kg according to ISO 1133. Alternatively, the melt flow rate MFR.sub.2 (230° C., 2.16 kg) may be measured according to ASTM D1238. The melt flow Rate MFR.sub.2 (190° C., 2.16 kg) was measured at 190° C. under a load of 2.16 kg according to ISO 1133. Alternatively, the melt flow rate MFR.sub.2 (190° C., 2.16 kg) may be measured according to ASTM D1238.
[0226] Epoxy Equivalent Weight
[0227] The epoxy equivalent weight was determined according to EN ISO 3001.
[0228] Glass Transition Temperature Tg and Melting Temperature Tm
[0229] The glass transition temperature Tg was measured by dynamic mechanical analysis according to ISO 6721-7. The melting temperature (Tm), was determined by differential scanning calorimeter (DSC) according to ISO 11357.
[0230] Molecular Weight (M.sub.w)
[0231] The molecular weight averages (Mw) were determined by Gel Permeation Chromatography (GPC) according to ISO 16014-4:2003 and ASTM D 6474-99.
[0232] Density
[0233] The density of polymers was determined according to ISO1183.
[0234] Tensile Properties
[0235] a) Examples Test UV2 and Test UV3:
[0236] The tensile properties were measured on an Allround Z020 traction device from Zwick Roell. The instruments and the measuring method are known to the skilled person. Measurements were performed with a testing samples of 50 mm×15 mm, a preload force of 0.2 N and a speed of 500 mm/min. The tensile strain at break was obtained under standard conditions. The max. force is determined from the highest point of the stress-strain curve in the tensile test, i.e. from the ultimate strength point. All measurements were performed on samples that have been stored under similar conditions after preparation.
[0237] b) Examples Test UV1:
[0238] The test method corresponds to the test method for Examples Test UV2 and Test UV3 as set out above with the following amendment:
[0239] Testing samples: 50 mm×25 mm
[0240] Speed: 100 mm/min
[0241] Preload force: 5 N
[0242] B) Preparation of Surface-Treated Filler Materials
[0243] Materials Used:
[0244] ASA 1
[0245] Mono-substituted alkenyl succinic anhydride (2,5-furandione, dihydro-, mono-C.sub.15-20-alkenyl derivs., CAS No. 68784-12-3) is a blend of mainly branched octadecenyl succinic anhydrides (CAS #28777-98-2) and mainly branched hexadecenyl succinic anhydrides (CAS #32072-96-1). More than 80% of the blend is branched octadecenyl succinic anhydrides. The purity of the blend is >95 wt.-%. The residual olefin content is below 3 wt.-%.
[0246] Fatty Acids Mixture 2
[0247] Fatty acid mixture 2 is a 1:1 mixture of stearic acid and palmitic acid
[0248] Epoxide-Containing Compound 3:
[0249] Epoxide-containing compound 3 is an epoxidized soybean oil produced by Galata Chemicals (Drapex 392)
[0250] Epoxide-Containing Compound 4:
[0251] Epoxide-containing compound 4 is a styrene-glycidyl methacrylate copolymer from BASF (Joncryl ADR4368C)
[0252] Epoxide-Containing Compound 5:
[0253] Epoxide-containing compound 5 is a Poly(ethylene-co-methyl acrylate-co-glycidyl methacrylate) from Sigma-Aldrich
[0254] PPH Repol H305FG
[0255] PPH Repol H305FG is a polypropylene homopolymer, available from Repol, under the tradename “H350FG”. The polypropylene homopolymer has a melt flow rate (230° C./2.16 kg) as determined according to ISO 1133 of 35 g/10 min.
[0256] Dow PPH H358-02
[0257] Dow PPH H358-02 is a polypropylene homopolymer resin, available from the Dow Chemical Company, under the tradename “Dow™ Polypropylene H358-02”. The polypropylene homopolymer has a melt flow rate (230° C./2.16 kg) as determined according to ISO 1133 of 2.1 g/10 min and a density determined according to ISO1183 of 0.900 g/cm.sup.3.
[0258] Ampacet 11977-N White PE MB
[0259] Ampacet 11977-N White PE MB is a masterbatch of a LDPE/LLDPE resin, available from Ampacet Europe S.A., under the tradename “11977-N White PE MB”. The resin has a melt flow rate (190° C./2.16 kg) as determined according to ISO 1133 of min. 2 g/10 min.
[0260] UV-MB Additive Masterbatch
[0261] UV-MB Additive Masterbatch is a polyethylene masterbatch, available from Deep Plast Industries, as “Additive Masterbatch (U.V MB)”. The masterbatch comprises Tinuvin-783 of BASF as UV stabilizer.
[0262] Moplen HP522H
[0263] Moplen HP522H is a polypropylene homopolymer, available from LyondellBasell, under the tradename “Moplen HP522H”. The polypropylene homopolymer has a melt flow rate (230° C./2.16 kg) as determined according to ISO 1133 of 2.0 g/10 min and a density determined according to ISO1183 of 0.900 g/cm.sup.3.
[0264] Calcium Carbonate Fillers:
[0265] Fillers for Test UV 1:
[0266] All surface-treated calcium carbonate samples were prepared with a dry ground calcium carbonate from Turkey (d.sub.50=3 μm, d.sub.98=12.5 μm).
[0267] Surface treatments were carried out in a high speed mixer (MTI Mixer, MTI Mischtechnik International GmbH, Germany), and conditioned by stirring for 10 minutes at the treatment temperature (3000 rpm). After that time, the additives were added to the mixture and stirring and heating is then continued for another 20 minutes (3000 rpm). After that time, the mixture is allowed to cool and the powder was collected. In table 1, the materials (additives), amounts and treatment conditions used for preparing the surface-treated calcium carbonate powders for test UV1 are shown.
TABLE-US-00001 TABLE 1 Preparation of the surface-treated calcium carbonate powders for test UV1 Additive 1 (parts Calcium by weight per Additive 2 carbonate hundred parts (parts by weight per Treatment Example (amount, kg) CaCO.sub.3) hundred parts CaCO.sub.3) temperature Powder CE1 1.3 / / Powder CE2 1.3 Fatty acid / 130° C. mixture 2 (0.6) Powder E1 1.3 Fatty acid Epoxide-containing 140° C. mixture 2 (0.6) compound 3 (0.4) Powder E2 1.3 Fatty acid Epoxide-containing 140° C. mixture 2 (0.6) compound 3 (1.0) Powder E3 1.3 Fatty acid Epoxide-containing 140° C. mixture 2 (0.6) compound 5 (1.0)
[0268] Fillers for Tests UV 2 & 3:
[0269] All surface-treated calcium carbonate samples were prepared with a dry ground calcium carbonate from Turkey (d.sub.50=3 μm, d.sub.98=12.5 μm).
[0270] Surface treatments were carried in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany), and conditioned by stirring for 10 minutes at the treatment temperature (1000 rpm). After that time, the additives were added to the mixture and stirring and heating is then continued for another 15 minutes (2000 rpm). After that time, the mixture was allowed to cool and the powder was collected. In table 2, the materials (additives), amounts and treatment conditions used for preparing the surface-treated calcium carbonate powders for tests UV2 and UV3 are shown.
TABLE-US-00002 TABLE 2 Preparation of the surface-treated calcium carbonate powders for tests UV2 and UV3 Calcium Additive 1 (parts carbonate by weight per Additive 2 (amount, hundred parts (parts by weight per Treatment Example kg) CaCO.sub.3) hundred parts CaCO.sub.3) temperature Powder CE3 0.8 / / / Powder CE4 0.8 Fatty acid / 120° C. mixture 2 (0.6) Powder E4 0.8 Fatty acid Epoxide-containing 120° C. mixture 2 (0.6) compound 3 (0.5) Powder E5 0.8 ASA 1 Epoxide-containing 140° C. (0.5) compound 4 (0.8) Powder E6 0.8 Fatty acid Epoxide-containing 140° C. mixture 2 (0.6) compound 4 (0.8) Powder E7 0.8 ASA 1 Epoxide-containing 120° C. (0.5) compound 3 (0.8)
[0271] C) Preparation of Polypropylene Cast Films
[0272] Preparation of Cast Films for Test UV 1:
[0273] The preparation of the masterbatches for Test UV 1 was carried out as set out in table 3.
TABLE-US-00003 TABLE 3 Preparation of the masterbatches for Test UV 1 Sample Polymer (wt.-%) CaCO.sub.3 (wt.-%) MB-CE1 Dow PPH H358-02 CE2 (70%) (30%) MB-E1 Dow PPH H358-02 E1 (70%) (30%) MB-E2 Dow PPH H358-02 E2 (70%) (30%) MB-E3 Dow PPH H358-02 E3 (70%) (30%)
[0274] The films were produced on a Dr. Collin cast film line (Extruder Type 30x 30 D, die: 250 mm) with the following line settings: [0275] Extruder temperatures: 50° C. (feeding)—190° C./200° C./230C./240° C./240° C. [0276] Pipes temperatures: 240° C./240° C. [0277] Die temperatures: 240° C./240° C. [0278] Screw speed: 35rpm [0279] Chill roll speed: 3.5-4.0 m/min [0280] Die gap: 0.7-0.75 mm [0281] Chill roll temperature: 60° C. [0282] Temperature other rolls: 40° C. [0283] Sieve: 74 μm [0284] Film thickness: 50 μm±2 μm
[0285] The cast film formulations for the test UV1 are set out in Table 4.
TABLE-US-00004 TABLE 4 Cast film formulations Cast film ref. Filler (wt.-%) CE100 96% Dow PPH H358-02 + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch CE101 93.7% Dow PPH H358-02 + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch + 4.3% MB-CE2 CE102 83.7% Dow PPH H358-02 + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch + 14.3% MB-CE2 E101 93.7% Dow PPH H358-02 + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch + 4.3% MB-E1 E102 83.7% Dow PPH H358-02 + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch + 14.3% MB-E1 E103 83.7% Dow PPH H358-02 + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch + 14.3% MB-E2 E104 83.7% Dow PPH H358-02 + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch + 14.3% MB-E3
[0286] Preparation of Cast Films for Test UV 2:
[0287] The preparation of the masterbatches for Test UV2 was carried out as set out in table 5.
TABLE-US-00005 TABLE 5 Preparation of the masterbatches for Test UV 2 Sample Polymer (wt.-%) CaCO.sub.3 (wt.-%) MB-CE4 PPH Repol H305FG CE4 (50%) (50%) MB-CE5 PPH Repol H305FG CE5 (50%) (50%) MB-E4 PPH Repol H305FG E4 (50%) (50%) MB-E5 PPH Repol H305FG E5 (50%) (50%) MB-E6 PPH Repol H305FG E6 (50%) (50%)
[0288] The films were produced on a Dr. Collin cast film line (Extruder Type 30x 30 D, die: 250 mm) with the following line settings: [0289] Extruder temperatures: 50° C. (feeding)—190° C./200° C./230C./240° C./240° C. [0290] Pipes temperatures: 240° C./240° C. [0291] Die temperatures: 240° C./240° C. [0292] Screw speed: 35 rpm [0293] Chill roll speed: 3.5-4.0 m/min [0294] Die gap: 0.7-0.75 mm [0295] Chill roll temperature: 60° C. [0296] Temperature other rolls: 40° C. [0297] Sieve: 74 μm [0298] Film thickness: 50 μm±2 μm
[0299] The cast film formulations for the test UV2 are set out in Table 5.
TABLE-US-00006 TABLE 6 Cast film formulations Cast film ref. Filler (wt.-%) CE103 96% PPH Repol H305FG + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch CE104 90% PPH Repol H305FG + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch + 6% MB-CE4 CE105 76% PPH Repol H305FG + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch + 20% MB-CE4 CE106 76% PPH Repol H305FG + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch + 20% MB-CE5 E105 76% PPH Repol H305FG + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch + 20% MB-E4 E106 76% PPH Repol H305FG + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch + 20% MB-E5 E107 76% PPH Repol H305FG + 2% Ampacet 11977-N White PE MB + 2% UV-MB Additive Masterbatch + 20% MB-E6
[0300] Preparation of Cast Films for Test UV 3:
[0301] The preparation of the masterbatches for Test UV3 was carried out as set out in table 7.
TABLE-US-00007 TABLE 7 Preparation of the masterbatches for Test UV 3 Sample Polymer (wt.-%) CaCO3 (wt.-%) MB-CE4 PPH Repol H305FG CE4 (50%) (50%) MB-CE5 PPH Repol H305FG CE5 (50%) (50%) MB-E7 PPH Repol H305FG E7 (50%) (50%)
[0302] The films were produced on a Dr. Collin cast film line (Extruder Type 30x 30 D, die: 250 mm) with the following line settings: [0303] Extruder temperatures: 50° C. (feeding)—190° C./200° C./230° C./240° C./240° C. [0304] Pipes temperatures: 240° C./240° C. [0305] Die temperatures: 240° C./240° C. [0306] Screw speed: 35 rpm [0307] Chill roll speed: 3.5-4.0 m/min [0308] Die gap: 0.7-0.75 mm [0309] Chill roll temperature: 60° C. [0310] Temperature other rolls: 40° C. [0311] Sieve: 74 μm [0312] Film thickness: 50 μm±2 μm
[0313] The cast film formulations for the test UV3 are set out in Table 8.
TABLE-US-00008 TABLE 8 Cast film formulations Cast film ref. Filler (wt %) CE107 92% Moplen HP522H + 2% UV-MB Additive Masterbatch + 6% MB-CE4 CE108 78% Moplen HP522H + 2% UV-MB Additive Masterbatch + 20% MB-CE4 CE109 78% Moplen HP522H + 2% UV-MB Additive Masterbatch + 20% MB-CE5 E108 78% Moplen HP522H + 2% UV-MB Additive Masterbatch + 20% MB-E7
[0314] D) UV Stability Tests
[0315] Example Test UV1:
[0316] In this test, the UV stability of the films is tested according to EN ISO21898. UV exposure is carried out using UVB-313 lamps (0.71 W/m.sup.2) for a total of 200 h in 25 cycles of 8 h UV light at 60° C. and 4 h condensation in the dark at 50° C.
[0317] Test samples: [0318] Width: 25 mm [0319] Height: 50 mm (between the clamps) [0320] Thickness: 50 μm [0321] Testing speed: 100 mm/min [0322] Preload force: 5N
[0323] Tensile properties in machine direction were measured before and after UV exposure. The remaining maximal force after UV exposure, expressed in % of the maximal force of non-exposed samples is summarized in Table 9 and
TABLE-US-00009 TABLE 9 Tensile properties after UV exposure for test UV1 Cast Film Filler Remaining max force after UV Sample (wt.-%) exposure (% of value before exposure) CE101 .sup. 3% CE2 63 CE102 .sup. 10% CE2 48 E101 3% E1 75 E102 10% E1 62 E103 10% E2 75 E104 10% E3 67
[0324] It can be gathered that the co-treatment of a filler material with a fatty acid and a surface-treatment agent having at least one epoxy-functional compound having one or more epoxy group(s) and/or reaction products thereof increases the remaining maximum force after UV exposure.
[0325] Example Test UV2:
[0326] In this test, the UV stability of the films is tested according to EN ISO21898:2004 Annex A. UV exposure is carried out in a Q-UV oven from Q-lab using UVB-313 lamps (0.71 W/m.sup.2) for a total of 100 and 200 h in cycles of 8 h UV light at 60° C. and 4 h condensation in the dark at 50° C.
[0327] Test Samples: [0328] Width: 15 mm [0329] Height: 50 mm [0330] Thickness: 50 μm [0331] Speed: 500 mm/min [0332] Preload: 0.2N
[0333] Tensile properties in machine direction were measured before and after UV exposure on an Allround Z020 traction device from Zwick Roell. The remaining maximal force after UV exposure, expressed in % of the maximal force of non-exposed samples, the tensile strain at beak as well as the remaining tensile strain at break are summarized in Table 10 and
TABLE-US-00010 TABLE 10 Tensile properties after UV exposure for test UV2 Remaining Remaining max force after Tensile tensile strain at Max force 100 h exposure strain at break after 100 h Cast after 100 h (% of value break (%) exposure (% of film Filler exposure before after 100 h value before sample (wt.-%) (N) exposure) exposure exposure) CE104 .sup. 3% CE4 42.8 81.2 418 83.5 (film 2) CE105 .sup. 10% CE4 30.6 72.5 257 51.9 (film 3) E105 10% E4 31.0 82.3 340 66.1 (film 8) E106 10% E5 33.5 86.7 455 86.4 (film 15) E107 10% E6 29.9 83.6 278 56.6 (film 7)
[0334] It can be gathered that the co-treatment of a filler material with a fatty acid or ASA and a surface-treatment agent having at least one epoxy-functional compound having one or more epoxy group(s) and/or reaction products thereof increases the remaining maximum force or tensile strain at break after UV exposure.
[0335] Example Test UV3:
[0336] In this test, the weathering test is carried out in a Q-UV oven from Q-lab using UVB-313 lamps (0.71 W/m.sup.2) for a total of 160 h in cycles of 8 h UV light at 60° C. and 4 h condensation in the dark at 50° C.
[0337] Test Samples: [0338] Width: 15 mm [0339] Height: 50 mm [0340] Thickness: 50 μm [0341] Speed: 500 mm/min [0342] Preload: 0.2N
[0343] Tensile properties in machine direction were measured before and after UV exposure on an Allround Z020 traction device from Zwick Roell. The remaining maximal force after UV exposure, expressed in % of the maximal force of non-exposed samples is summarized in Table 11 and
TABLE-US-00011 TABLE 11 Tensile properties after UV exposure for test UV3 Tensile strain at Remaining tensile strain at Cast Film Filler break (%) after break after 100 h exposure (% Sample (wt.-%) 100 h exposure of value before exposure) CE108 10% CE4 29.5 6.1 (film 3bis) E108 10% E7 .sup. 108 22.5 (film 8)
[0344] It can be gathered that the treatment of a filler material with a mono-substituted alkenyl succinic anhydride and a surface-treatment agent having at least one epoxy-functional compound having one or more epoxy group(s) and/or reaction products thereof increases the remaining tensile strain at break after UV exposure compared to a fatty acid treatment.