Process for preparing a surface treated filler material product with mono-substituted succinic anhydride(s) and a mixture of aliphatic linear or branched carboxylic acids comprising stearic acid

Abstract

The present invention relates to a process for preparing a surface treated filler material product with mono-substituted succinic anhydride(s) and a mixture of aliphatic linear or branched carboxylic acids comprising stearic acid, a surface treated filler material product, a polymer composition, a fiber and/or filament and/or film and/or thread and/or sheet and/or pipe and/or profile and/or mold and/or, injection molds and/or blow mold comprising the surface treated filler material product and/or the polymer composition, an article comprising the surface treated filler material product and/or the polymer composition and/or the fiber and/or filament and/or film and/or thread and/or sheet and/or pipe and/or profile and/or mold and/or injection mold and/or blow mold as well as the use of at least one mono-substituted succinic anhydride and/or salty reaction product(s) thereof in combination with a mixture of aliphatic linear or branched carboxylic acids comprising stearic acid and/or salty reaction product(s) thereof, for improving the flowability of a surface treated filler material product and for improving the dispersion of the calcium carbonate in the polymer matrix of a polymer composition.

Claims

1. A surface treated filler material product comprising a) at least one calcium carbonate-containing filler material, b) a treatment layer on the surface of the at least one calcium carbonate-containing filler material comprising at least one mono-substituted succinic anhydride and/or salty reaction product(s) thereof and a mixture of aliphatic linear or branched carboxylic acids comprising stearic acid in an amount of at least 10.0 wt. %, based on the total weight of the mixture, and one or more further saturated aliphatic linear or branched carboxylic acid(s) having a total amount of carbon atoms from C8 to C24, and/or salty reaction product(s) thereof, wherein the surface treated filler material product comprises the treatment layer in an amount of from 0.2 to 6 wt. %, based on the total dry weight of the at least one calcium carbonate-containing filler material, wherein the surface treated filler material product is in form of a powder.

2. The surface treated filler material product according to claim 1, wherein the calcium carbonate-containing filler material is selected from the group consisting of ground calcium carbonate, marble, limestone, dolomite, chalk, precipitated calcium carbonate (PCC), vaterite, calcite, aragonite, surface-reacted calcium carbonate (MCC) and mixtures thereof.

3. A polymer composition comprising at least one polymeric resin and from 1 to 95 wt.-%, based on the total weight of the polymer composition, of the surface treated filler material product according to claim 1.

4. The polymer composition according to claim 3, wherein the at least one polymeric resin is at least one thermoplastic polymer.

5. The polymer composition according to claim 3, wherein the polymer composition is a masterbatch.

6. A fiber and/or filament and/or film and/or thread and/or sheet and/or pipe and/or profile and/or mold and/or injection molds and/or blow mold comprising the surface treated filler product according to claim 1 or a polymer composition comprising at least one polymeric resin and from 1 to 95 wt. %, based on the total weight of the polymer composition, of the surface treated filler material product according to claim 1.

7. An article comprising the surface treated filler material product according to claim 1 or a polymer composition comprising at least one polymeric resin and from 1 to 95 wt. %, based on the total weight of the polymer composition, of the surface treated filler material product according to claim 1, wherein the article is selected from the group consisting of hygiene products, medical and healthcare products, filter products, geotextile products, agriculture and horticulture products, clothing, footwear and baggage products, household and industrial products, packaging products, and construction products.

8. The article according to claim 7 being a packaging product selected from the group consisting of carrier bags, waste bags, transparent foils, hygiene films, agriculture foils, paper like foils, bottles, thermoform foils, extrusion coated papers and boards, boxboards, paperboard cartons, paper bags, sacks, corrugated boxes, flexible tubes, bags, oriented and bi-oriented films, and trays.

9. An article comprising the fiber and/or filament and/or film and/or thread and/or sheet and/or pipe and/or profile and/or mold and/or injection molds and/or blow mold according to claim 6, wherein the article is selected from the group consisting of hygiene products, medical and healthcare products, filter products, geotextile products, agriculture and horticulture products, clothing, footwear and baggage products, household and industrial products, packaging products, and construction products.

10. The surface treated filler material product according to claim 1, wherein the at least one calcium carbonate-containing filler material has a) a weight median particle size d.sub.50 value in the range from 0.1 μm to 7 μm and/or b) a top cut (d.sub.98) of ≤50 μm and/or c) a specific surface area (BET) of from 0.5 to 150 m.sup.2/g and/or d) a residual total moisture content of from 0.01 wt.-% to 1 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material.

11. The polymer composition according to claim 3, wherein the polymer composition is a masterbatch and the masterbatch comprises the surface treated filler material product in an amount of from 50 to 95 wt.-%.

12. The surface treated filler material product according to claim 1, wherein the at least one calcium carbonate-containing filler material has a) a weight median particle size d.sub.50 value in the range from 0.5 μm to 4 μm and/or b) a top cut (d.sub.98) of ≤15 μm and/or c) a specific surface area (BET) of from 0.5 to 10 m.sup.2/g and/or d) a residual total moisture content of from 0.04 wt.-% to 0.2 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material.

13. The surface treated filler material product according to claim 1, wherein the at least one mono-substituted succinic anhydride consists of succinic anhydride mono-substituted with a group selected from a linear, branched, aliphatic and cyclic group having a total amount of carbon atoms from C2 to C30 in the substituent.

14. The surface treated filler material product according to claim 1, wherein the at least one mono-substituted succinic anhydride is a) at least one alkyl mono-substituted succinic anhydride, ethylsuccinic anhydride, propylsuccinic anhydride, butylsuccinic anhydride, triisobutyl succinic anhydride, pentylsuccinic anhydride, hexylsuccinic anhydride, heptylsuccinic anhydride, octylsuccinic anhydride, nonylsuccinic anhydride, decyl succinic anhydride, dodecyl succinic anhydride, hexadecanyl succinic anhydride, octadecanyl succinic anhydride, and mixtures thereof, and/or b) at least one alkenyl mono-substituted succinic anhydride, ethenylsuccinic anhydride, propenylsuccinic anhydride, butenylsuccinic anhydride, triisobutenyl succinic anhydride, pentenylsuccinic anhydride, hexenylsuccinic anhydride, heptenylsuccinic anhydride, octenylsuccinic anhydride, nonenylsuccinic anhydride, decenyl succinic anhydride, dodecenyl succinic anhydride, hexadecenyl succinic anhydride, octadecenyl succinic anhydride, and mixtures thereof.

15. The surface treated filler material product according to claim 1, wherein the mixture of saturated aliphatic linear or branched carboxylic acids comprises stearic acid and one or more further saturated aliphatic linear or branched carboxylic acid(s) having a total amount of carbon atoms from C8 to C22.

16. A process for preparing a surface treated filler material product of claim 1, the process comprising the steps of: a) providing at least one calcium carbonate-containing filler material, b) providing at least one mono-substituted succinic anhydride, c) providing a mixture of aliphatic linear or branched carboxylic acids comprising stearic acid in an amount of at least 10.0 wt. %, based on the total weight of the mixture, and one or more further saturated aliphatic linear or branched carboxylic acid(s) having a total amount of carbon atoms from C8 to C24, d) contacting the surface of the at least one calcium carbonate-containing filler material of step a), under mixing, in one or more steps, in any order, with the at least one mono-substituted succinic anhydride of step b) and the mixture of aliphatic linear or branched carboxylic acids of step c) such that a treatment layer comprising the at least one mono-substituted succinic anhydride and/or salty reaction product(s) thereof and the mixture of aliphatic linear or branched carboxylic acids and/or salty reaction product(s) thereof is formed on the surface of said at least one calcium carbonate-containing filler material of step a), wherein the temperature before and/or during contacting step d) is adjusted such that the at least one mono-substituted succinic anhydride and the mixture of aliphatic linear or branched carboxylic acids is in a molten or liquid state, wherein the surface treated filler material product is in form of a powder.

17. The process according to claim 16, wherein the at least one calcium carbonate-containing filler material of step a) is preheated before contacting step d) is carried out.

18. The process according to claim 16, wherein contacting step d) is carried out in that the at least one mono-substituted succinic anhydride of step b) and the mixture of saturated aliphatic linear or branched carboxylic acids of step c) are added in a weight ratio [succinic anhydride/mixture of carboxylic acids] of from 10:1 to 1:10.

19. The process according to claim 16, wherein the at least one mono-substituted succinic anhydride of step b) is added in contacting step d) in a total amount of from 0.1 to 3 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material of step a); and the mixture of saturated aliphatic linear or branched carboxylic acids of step c) is added in contacting step d) in a total amount of from 0.1 to 3 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material of step a).

20. The process according to claim 16, wherein contacting step d) is carried out at a temperature of from 20 to 200° C.

21. The process according to claim 16, wherein contacting step d) is carried out in that the at least one mono-substituted succinic anhydride of step b) and the mixture of saturated aliphatic linear or branched carboxylic acids of step c) are added simultaneously or in that the mixture of saturated aliphatic linear or branched carboxylic acids of step c) is added after the at least one mono-substituted succinic anhydride of step b).

22. The process according to claim 16, wherein the at least one calcium carbonate-containing filler material has a) a weight median particle size d.sub.50 value in the range from 0.1 μm to 7 μm and/or b) a top cut (d.sub.98) of ≤50 μm and/or c) a specific surface area (BET) of from 0.5 to 150 m.sup.2/g and/or d) a residual total moisture content of from 0.01 wt.-% to 1 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material.

23. The process according to claim 16, wherein the at least one mono-substituted succinic anhydride consists of succinic anhydride mono-substituted with a group selected from a linear, branched, aliphatic and cyclic group having a total amount of carbon atoms from C2 to C30 in the substituent.

Description

BRIEF DESCRIPTION OF THE FIGURES

(1) FIG. 1 refers to the powder flowability—Stability and variable flow rate of powders 1 to 4

(2) FIG. 2 refers to the powder flowability—Shear cell of powders 1, 2, and 4

(3) The following examples may additionally illustrate the invention but are not meant to restrict the invention to the exemplified embodiments. The examples below show the improved flowability of the surface treated filler material product and its improved dispersion in the polymer matrix of a polymer composition.

EXAMPLES

(4) A) Measurement Methods

(5) The following measurement methods are used to evaluate the parameters given in the examples and claims.

(6) Particle Size Distribution (Mass % Particles with a Diameter<X) and Weight Median Diameter (d.sub.50) of a Particulate Material

(7) As used herein and as generally defined in the art, the “d.sub.50” value is 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.

(8) 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 is carried out in an aqueous solution of 0.1 wt.-% Na.sub.4P.sub.2O.sub.7. The samples are dispersed using a high speed stirrer and supersonics.

(9) BET Specific Surface Area of a Material

(10) Throughout the present document, the specific surface area (in m.sup.2/g) of the mineral filler is determined using the BET method (using nitrogen as adsorbing gas), which is well known to the skilled man (ISO 9277:1995). The total surface area (in m.sup.2) of the mineral filler is then obtained by multiplication of the specific surface area and the mass (in g) of the mineral filler prior to treatment.

(11) Amount of Surface-Treatment Layer

(12) The amount of the treatment layer on the calcium carbonate-comprising filler material is calculated theoretically from the values of the BET of the untreated calcium carbonate-containing filler material and the amount of mono-substituted succinic anhydride and the mixture of aliphatic linear or branched carboxylic acids comprising stearic acid that is used for the surface-treatment. It is assumed that 100% of the mono-substituted succinic anhydride and the mixture of aliphatic linear or branched carboxylic acids comprising stearic acid added to the calcium carbonate-containing filler material are present as surface treatment layer on the surface of the calcium carbonate-containing filler material.

(13) Water Pick-Up

(14) The moisture pick up susceptibility of a material as referred to herein is determined in mg moisture/g after exposure to an atmosphere of 10 and 85% relative humidity, respectively, for 2.5 hours at a temperature of +23° C. (±2° C.). For this purpose, the sample is first kept at an atmosphere of 10% relative humidity for 2.5 hours, then the atmosphere is changed to 85% relative humidity at which the sample is kept for another 2.5 hours. The weight increase between 10 and 85% relative humidity is then used to calculate the moisture pick-up in mg moisture/g of sample.

(15) Powder Flowability—Stability and Variable Flow Rate Method

(16) The Basic flowability energy (BFE), stability index (SI), specific energy (SE), flow rate index (FRI) and conditioned bulk density (CBD) are measured on a FT4 Powder Rheometer (Freeman Technology, UK) equipped with the Powder Rheometer software (v 5.000.00012) and Freeman Technology Data Analysis Software version 4.0.17, using the stability and variable flow rate method, using the stability and variable flow rate method.

(17) This method consists of filling a cylindric vessel (25 mm×25 mL glass vessel). The first stage of the test process is to obtain a homogeneous, conditioned powder state to allow highly repeatable measurements to be made. A conditioning cycle comprises of the dynamic test blade slicing downward through the powder followed by an upward traverse that lifts the powder and drops it over the blade. This process helps to remove the effect of different sampling methodologies and powder storage times.

(18) After that initial conditioning step, the powder volume is adjusted to the vessel size to remove excess powder (“split”)—and the mass is recorded after the splitting step. Following that, 8 repeating cycles of conditioning and measurements with a 23.5 mm blade are performed. For each test cycle, the blade is inserted into the powder bed downward (anti-clockwise, tip speed −100 mm/s, helix angle=5°/target height 5 mm), and upward. For conditioning steps, the blade is inserted into the powder bed downwards (tip speed −40 mm/s/helix angle 5°, target height 5 mm), and upwards. After those 8 tests, 3 more cycles of (conditioning+tests) are performed at variable flow rates, i.e. with a blade tip speed of 70 mm/s (Test 9), 40 mm/s (Test 10) and finally 10 mm/s (Test 11). The energy and torque are recorded and allow to calculate various flow parameters, defined as follow: Basic flowability energy (BFE, mJ): Energy Cycle 7 (downwards) Stability index: (Energy Test 7)/(Energy Cycle 1) Specific energy (SE, mJ/g): (Up Energy cycle 6+Up Energy cycle 7)/(2×split mass) Flow Rate Index (FRI): (Energy Test 11)/(Energy Test 8) Conditioned bulk density (CBD, g/mL): (Split mass)/(Split volume)

(19) Powder Flowability—Shear Cell Method

(20) Shear cell characteristic are measured using a FT4 Powder rheometer (Freeman Technology, UK) according to ASTM D7891-15, using a cylindric vessel (50 mm×85 mL or 25 mm×10 mL glass vessel), a 48 mm or 24 mm shear cell and 15 kPa pre-shear normal stress.

(21) The measurement was carried out using the following stepwise methodology.

(22) Initial Powder Conditioning:

(23) The first stage of the test process is to obtain a homogeneous, conditioned powder state to allow highly repeatable measurements to be made. A conditioning cycle comprises of the dynamic test blade slicing downward through the powder followed by an upward traverse that lifts the powder and drops it over the blade. This process helps to remove the effect of different sampling methodologies and powder storage times.

(24) Initial Compaction

(25) The conditioned column of powder is compacted using a ventilated compaction piston (allowing entrained air to escape), with a force equal to that of the pre-shear normal stress.

(26) Critical Consolidation

(27) Points on the yield loci represent the values of shear stress corresponding to incipient failure at each normal stress level. To achieve incipient failure the specimen must be over-consolidated with respect to the normal stress applied during shearing. This is realised by reaching a critical consolidation level at steady state flow and then reducing the normal stress for shearing. Thus, shear testing is a two stage process consisting of:

(28) 1. Pre-Shearing

(29) The purpose of pre-shearing is to reach critical consolidation at a given pre-shear normal stress level. During this process shearing is continued until a steady state flow is achieved at which point pre-shearing is complete.

(30) 2. Shear Test

(31) The normal stress is reduced so that the sample is now over consolidated with respect to the normal stress now applied. Shearing is then restarted and the point of incipient failure is measured. For each pre-shear normal stress, five measurements are taken at the five normal stresses defined by the standard (9; 8; 7; 6 and 5 kPa). A measurement of shear stress is also taken at the preshear normal stress level i.e. at 15 kPa. The five measurements taken make up the yield loci for each pre-shear normal stress level. The yield loci are plotted on a shear stress vs. normal stress graph, from which Mohr's circles can be added in order to extrapolate various flow data.

(32) Data extrapolated include: Cohesion, (C, kPa)—the Shear Stress where the Best Fit Line intercepts the y-axis, i.e. Nornal stress=0 Unconfined Yield Strength, (UYS, kPa)—the greater of the 2 values at which the smaller Mohr circle intercepts the x-axis, (also known as σc) Major Principal Stress, (MPS, kPa)—the greater of the two values at which the larger Mohr circle intercepts the x-axis, (also known as 61). Angle of internal friction (AIF, °)—the angle created by the best fit line with the horizontal axis Flow factor (FF): corresponds to MPS/UYS Bulk density (BD, g/mL): conditioned bulk density after initial compaction

(33) Extrusion Simulation

(34) The extrusion simulation was developed to evaluate the mineral dispersion in a polymer composition. The test was performed on a commercially available Collin Pressure Filter Test Teach-Line FT-E20T-IS.

(35) The test method with each of the corresponding polymer compositions, wherein no melt pump was used, the extruder screw speed was kept at 100 rpm, and wherein the melt temperature was 225 to 230° C. (temperature setting extruder: 190° C.-210° C.-230° C.; temperature setting die: 230° C.-230° C.).

(36) Each of the corresponding polymer compositions (900 g effective Powder A or B per 2500 g of final sample obtained by diluting the polymer composition in LLDPE ExxonMobil LL 1001 VX) was measured using a 40 μm filter (GKD Gebr. Kufferath AG, Duren, Germany, Artikelnummer 12102170055).

(37) The results are expressed in bar and can be calculated by subtracting the final melt pressure (determined after 5 min of purging with pure polymer material) from the initial pressure of the pure polymer material (LLDPE ExxonMobil LL 1001 VX).

(38) Ash Content

(39) The ash content test was performed by burning 5 to 30 g of the corresponding polymer composition at 570° C. for 120 minutes.

(40) B) Materials

(41) Calcium Carbonate-Containing Filler Materials

(42) Calcium Carbonate-Comprising Filler Material 1 (Powder 1; Comparative)

(43) 0.7 kg of a wet ground and spray dried marble from Carrara, Italy (d.sub.50=1.6 μm, BET specific surface area=4.1 m.sup.2/g) is placed in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany), and conditioned by stirring for 10 minutes (1000 rpm, 120° C.). After that time, 0.6 parts by weight relative to 100 parts by weight CaCO.sub.3 of mono-substituted succinic anhydride 1 is added to the mixture. Stirring and heating is then continued for another 15 minutes (120° C., 1000 rpm). After that time, the mixture is allowed to cool and the powder is collected (powder 1).

(44) Calcium Carbonate-Containing Filler Material 2 (Powder 2; Inventive)

(45) 0.7 kg of a wet ground and spray dried marble from Carrara, Italy (d.sub.50=1.6 μm, BET specific surface area=4.1 m.sup.2/g) is placed in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany), and conditioned by stirring for 10 minutes (1000 rpm, 120° C.). After that time, 0.5 parts by weight relative to 100 parts by weight CaCO.sub.3 of mono-substituted succinic anhydride 1 and 0.2 parts by weight relative to 100 parts by weight CaCO.sub.3 of carboxylic acids mixture 2 is added simultaneously to the mixture. Stirring and heating is then continued for another 15 minutes (120° C., 1000 rpm). After that time, the mixture is allowed to cool and the powder is collected (powder 2).

(46) Calcium Carbonate-Containing Filler Material 3 (Powder 3; Inventive)

(47) 0.7 kg of a wet ground and spray dried marble from Carrara, Italy (d.sub.50=1.6 μm, BET specific surface area=4.1 m.sup.2/g) is placed in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany), and conditioned by stirring for 10 minutes (1000 rpm, 120° C.). After that time, 0.4 parts by weight relative to 100 parts by weight CaCO.sub.3 of mono-substituted succinic anhydride 1 and 0.4 parts by weight relative to 100 parts by weight CaCO.sub.3 of carboxylic acids mixture 2 is added simultaneously to the mixture. Stirring and heating is then continued for another 15 minutes (120° C., 1000 rpm). After that time, the mixture is allowed to cool and the powder is collected (powder 3).

(48) Calcium Carbonate-Containing Filler Material 4 (Powder 4; Inventive)

(49) 0.7 kg of a wet ground and spray dried marble from Carrara, Italy (d.sub.50=1.6 μm, BET specific surface area=4.1 m.sup.2/g) is placed in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany), and conditioned by stirring for 10 minutes (1000 rpm, 120° C.). After that time, 0.4 parts by weight relative to 100 parts by weight CaCO.sub.3 of mono-substituted succinic anhydride 1 is added to the mixture. Stirring and heating is then continued for another 15 minutes (120° C., 1000 rpm). Then, 0.2 parts by weight relative to 100 parts by weight CaCO.sub.3 of carboxylic acids mixture 2 is added to the mixture and stirring and heating is then continued for another 15 minutes (120° C., 1000 rpm). After that time, the mixture is allowed to cool and the powder is collected (powder 4).

(50) Mono-Substituted Succinic Anhydride

(51) Mono-Substituted Succinic Anhydride (ASA) 1

(52) Mono-substituted alkenyl succinic anhydride (2,5-Furandione, dihydro-, mono-C15-20-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.-%.

(53) Carboxylic Acids Mixture 2

(54) Carboxylic acids mixture 2 is a 1:1 mixture of stearic acid and palmitic acid.

(55) Powder A (inventive): Dry grinded limestone from Nocera Umbria (d.sub.50=3.2, top cut=12 μm; BET specific surface area=3.0 m.sup.2/g), treated with 0.35% by weight of mono-substituted succinic anhydride 1 and 0.15% by weight of carboxylic acid mixture 2.

(56) Powder B (prior art): Dry grinded limestone from Nocera Umbria (d.sub.50=3.2, top cut=12 μm; BET specific surface area=3.0 m.sup.2/g), treated with 0.45% by weight of mono-substituted succinic anhydride 1.

(57) Analysis and Test Results

Example 1: Water Pick-Up Results

(58) TABLE-US-00001 TABLE 1 Water pick-up values for powders 1 to 4. waterpickup Powder (mg/g) powder 1; comparative 0.5 powder 2; inventive 0.4 powder 3; inventive 0.45 powder 4; inventive 0.2

Example 2: Powder Flowability: Stability and Variable Flow Rate

(59) Powder flowability of powders 1 to 4 was measured on a FT4 Powder Rheometer from Freeman Technology using the stability and variable flow rate method in a 25 mm×25 mL measuring cell. Improved powder flowabilities were achieved with powders 2-4, compared to the reference powder 1, as can be seen from the lower basic flowability energy obtained with those powders (FIG. 1 & Table 2)

(60) TABLE-US-00002 TABLE 2 Powder flowability - Stability and variable flow rate (powders 1 to 4), Basic flowability energy (BFE), Stability index (SI), Flow rate index (FRI), specific energy (SE), conditioned bulk density (CBD) Powder BFE, mJ SI FRI SE, mJ/g CBD, g/ml Powder 1 158.13 1.07 1.81 7.89 0.69 Powder 2 122.42 1.10 1.96 6.95 0.70 Powder 3 99.49 1.10 2.10 6.17 0.71 Powder 4 142.47 1.06 1.78 7.19 0.70

(61) Improved powder flowabilities were achieved with powders 2-4, compared to the reference powder 1, as can be seen from the lower basic flowability energy obtained with those powders (FIG. 1 & Table 2)

Example 3. Production of a Polymer Composition (Masterbatch) and Test Result (Ash Content and Extrusion Simulation)

(62) Masterbatches (MB) were prepared following the protocol describe hereafter.

(63) The polymer compositions comprising 25 wt.-% of Dowlex 5056G (LLPDE, MFI=1 g/10 min) and 75 wt.-% Powder A or B respectively, (Masterbatch A or B), were prepared on a lab scale using a Buss kneader (PR46 from Buss AG, Switzerland, L/d of 10) at 10 kg/h and processed at the following machine setting: Temperature of the screw: 100° C. Temperature of extruder (2 zones): 190° C.-170° C. Temperature of the extraction (1 zone): 170° C. Screw speed: 200 rpm Dosing of polymer: 100% in main hopper Dosing of powder: 73% in main hopper, 27% in side feeder

(64) The obtained mixtures were pelletized on a spring load pelletizer, model SLC (Gala, USA) in a water bath having a starting temperature between 20 and 25° C. The compositions and filler contents of the prepared Masterbatches are compiled in Table 3 below. The precise filler contents were determined by the ash content. Furthermore, an extrusion simulation test was carried out in order to determine the dispersion quality of the filler material product in the polymer matrix of the compounded materials.

(65) The results shown in Table 3 confirm that Masterbatches A and B with good quality were produced. Furthermore, the extrusion simulation test revealed that the surface treated filler material product of the present invention, i.e. Masterbatch A, shows an improved dispersion quality in the compounded polymer matrix, compared to the prior art filler material product, i.e. Masterbatch B.

(66) TABLE-US-00003 TABLE 3 Compositions and properties of the prepared Masterbatches MB A MB B (based on (based on powder A) powder B) Amount of powder 74.3 74 (wt.-%) Amount of LLPDE (wt.-%) 25.7 26 Pressure increase during 12.4 13.4 extrusion simulation test at 40 pm pore size (bar)

(67) The pressure increase by extruding 900 g of powder A in a 40 μm sieve is lower than for powder B, thus demonstrating the advantageous properties, the improved dispersion of powder A in the compounded polymer matrix.

Example 4: Powder Flowability: Shear Cell

(68) Powder flowability of powders 1 to 4 was measured on a FT4 Powder Rheometer from Freeman Technology using the shear cell method (15 kPa) in a 25 mm×10 mL measuring cell. Improved powder flowabilities and lower cohesion were achieved with powders 2 and 4, compared to the reference powder 1, as can be seen from the lower cohesion values, lower unconfined yield strength (UYS) and higher flow factor (FF) obtained with those powders (FIG. 2 & Table 4)

(69) TABLE-US-00004 TABLE 4 Powder flowability - Shear cell (powders 1 to 4), Cohesion, Unconfined yield Strength (UYS), Major principal stress (MPS) and Flow factor (FF) Cohesion, UYS, MPS, Powder kPa kPa kPa FF Powder 1 3.25 10.85 24.56 2.26 Powder 2 2.64 8.68 23.37 2.69 Powder 4 2.71 8.66 22.97 2.65