CALCIUM CARBONATE TREATED WITH FUNCTIONALIZED POLY- AND/OR PERFLUORINATED COMPOUNDS

Abstract

The present invention relates to a functionalized poly- and/or perfluorinated compound treated calcium carbonate, wherein the calcium carbonate is surface treated with at least one functionalized poly- and/or perfluorinated compound, a process for preparing the poly- and/or perfluorinated compound treated calcium carbonate, the use of the poly- and/or perfluorinated compound treated calcium carbonate as a filler and/or a surface coating agent, fillers and surface coating agents comprising the poly- and/or perfluorinated compound treated calcium carbonate, and polymers comprising the poly- and/or perfluorinated compound treated calcium carbonate.

Claims

1.-28. (canceled)

29. A fluorinated compound treated calcium carbonate, characterized in that the calcium carbonate is surface treated with at least one functionalized poly- and/or perfluorinated compound.

30. The fluorinated compound treated calcium carbonate according to claim 29, wherein the calcium carbonate is selected from the group consisting of natural ground calcium carbonate (GCC), marble, chalk, limestone, dolomite, precipitated calcium carbonate (PCC), PCC having aragonitic crystal forms, PCC having vateritic crystal forms, PCC having calcitic crystal forms, and mixtures thereof.

31. The fluorinated compound treated calcium carbonate according to claim 29, wherein the calcium carbonate has a) a weight median particle size d.sub.50 value in the range from 0.1 μm to 20 μm, and/or b) a top cut particle size (d.sub.98) of not more than 100 μm, and/or c) a specific surface area (BET) of from 0.5 to 150 m.sup.2/g as measured by the BET nitrogen method.

32. The fluorinated compound treated calcium carbonate according to claim 29, wherein the calcium carbonate is selected from the group consisting of a dry ground calcium carbonate having a weight median particle diameter d.sub.50 of 1.5 to 2.0 μm and a BET specific surface area of 3.3 to 4.8 m.sup.2/g; and a wet ground and spray dried calcium carbonate having a weight median particle diameter d.sub.50 of 0.5 to 0.9 μm and a BET specific surface area of 7.0 to 9.0 m.sup.2/g.

33. The fluorinated compound treated calcium carbonate according to claim 29, wherein the at least one functionalized poly- and/or perfluorinated compound has at least two functional terminal groups, which may be the same or different.

34. The fluorinated compound treated calcium carbonate according claim 29, characterized in that the at least one functionalized poly- and/or perfluorinated compound is selected from the group consisting of poly- and/or perfluorinated alkyl compounds having at least one functional group and fluoropolymers having at least one functional group.

35. The fluorinated compound treated calcium carbonate according to claim 29, wherein the at least one functionalized poly- and/or perfluorinated compound is selected from the group consisting of poly- and/or perfluorinated alkyl compounds having at least one functional group selected from the group consisting of hydroxyl, carboxyl, alkoxy, methoxy, ethoxy, alkoxycarbonyl, methoxycarbonyl, ethoxycarbonyl, methylene alcohol, allyl ether, amino, ammonio, carboxamido, sulfanyl, sulfonyl, sulfo, alkoxysulfonyl, their salts, derivatives and mixtures thereof.

36. The fluorinated compound treated calcium carbonate according to claim 29, wherein the at least one functionalized poly- and/or perfluorinated compound is selected from the group consisting of functionalized poly- and/or perfluoropolyethers, poly- and/or perfluorocarboxylic acids, poly- and/or perfluorosulfonic acids, their salts, derivatives and mixtures thereof.

37. The fluorinated compound treated calcium carbonate according to claim 29, wherein the at least one functionalized poly- and/or perfluorinated compound is selected from the group consisting of functionalized poly- and/or perfluoropolyethers having at least one functional group.

38. The fluorinated compound treated calcium carbonate according to claim 37, wherein the at least one functionalized poly- and/or perfluorinated compound is selected from the group consisting of functionalized poly- and/or perfluoropolyethers having at least one terminal functional group selected from the group consisting of a carboxyl group, a phosphate ester group, a hydroxy group, their salts, derivatives and mixtures thereof.

39. The fluorinated compound treated calcium carbonate according to claim 37, wherein the at least one functionalized poly- and/or perfluorinated compound is selected from the group consisting of poly(hexafluoropropylene oxide)s having a terminal carboxyl group located on the terminal fluoromethylene group thereof.

40. The fluorinated compound treated calcium carbonate according to claim 37, wherein the at least one functionalized poly- and/or perfluorinated compound is selected from the group consisting of fluorocarbon ether polymers of poly(hexafluoropropylene oxide).

41. The fluorinated compound treated calcium carbonate according to claim 37, wherein the at least one functionalized poly- and/or perfluorinated compound is selected from the group consisting of poly(hexafluoropropylene oxide)s with a chemical formula F—(CF(CF.sub.3)—CF.sub.2—O).sub.n—CF.sub.2CF.sub.3, wherein n is 10-60, which are functionalized with a carboxylic acid group situated on the terminal fluoromethylene group and have a molecular weight of about 2500 g/mole and poly(hexafluoropropylene oxide)s with a chemical formula F—(CF(CF.sub.3)—CF.sub.2—O).sub.n—CF.sub.2CF.sub.3, wherein n is 10-60, which are functionalized with a carboxylic acid group situated on the terminal fluoromethylene group and have a molecular weight of 7000-7500 g/mole.

42. The fluorinated compound treated calcium carbonate according to claim 37, wherein the at least one functionalized poly- and/or perfluorinated compound is selected from the group consisting of functionalized poly- and/or perfluoropolyethers having two terminal functional groups.

43. The fluorinated compound treated calcium carbonate according to claim 37, wherein the at least one functionalized poly- and/or perfluorinated compound is selected from the group consisting of functionalized poly- and/or perfluoropolyethers having two terminal functional groups selected from the group consisting of a carboxyl group, a phosphate ester group, a hydroxy group, their salts, derivatives and mixtures thereof.

44. The fluorinated compound treated calcium carbonate according to claim 29, characterized in that the at least one functionalized poly- and/or perfluorinated compound is selected from the group consisting of poly- and/or perfluorocarboxylic acids, perfluoroheptanoic acid (PFHpA), perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluorododecanoic acid, poly- and/or perfluorosulfonic acids, perfluorooctane sulfonic acid (PFOS), perfluorooctane sulfonamide (PFOSA), perfluorobutane sulfonic acid (PFBS), perfluorobutane sulfonamide (FBSA), perfluorohexane sulfonic acid (PFHxS), heptafluorobutyric acid (HFBA), their salts, derivatives and mixtures thereof.

45. The fluorinated compound treated calcium carbonate according to claim 29, wherein the fluorinated compound treated calcium carbonate comprises from 0.1 wt % to 10 wt % of the at least one functionalized poly- and/or perfluorinated compound relative to the weight of calcium carbonate.

46. A process for preparing the fluorinated compound treated calcium carbonate according to claim 29, wherein the process comprises the steps of providing at least one calcium carbonate, providing at least one functionalized poly- and/or perfluorinated compound, and combining the at least one calcium carbonate and the at least one functionalized poly- and/or perfluorinated compound.

47. The process according to claim 46, wherein the at least one calcium carbonate and the at least one functionalized poly- and/or perfluorinated compound, independently from each other, are provided in a dry form, or in the form of a slurry, dispersion, emulsion or solution.

48. The process according to claim 46, wherein the at least one functionalized poly- and/or perfluorinated compound is combined with the at least one calcium carbonate in an amount of from 0.1 wt % to 10 wt % relative to the weight of calcium carbonate.

49. The process according to claim 46, wherein the obtained poly- and/or perfluorinated compound treated calcium carbonate is dried and/or deagglomerated.

50. A fluorinated compound treated calcium carbonate obtained by the process according to claim 46.

51. A filler comprising the fluorinated compound treated calcium carbonate according to claim 29.

52. A surface coating composition comprising the fluorinated compound treated calcium carbonate according to claim 29.

53. A polymer comprising the fluorinated compound treated calcium carbonate according to claim 29.

54. The polymer according to claim 53, wherein the polymer is selected from the group consisting of acrylonitrile butadiene styrenes (ABS), polyamides (PA), PA6, polybutylene terephthalates (PBT), polycarbonates (PC), polyethylene terephthalates (PET), polyimides, polyoxymethylene plastics (POM/acetal), polyphenylene oxides (PPO), polysulphones (PSU), poly(ethylene succinate)s (PES), polyethylenimins (PEI), polystyrenes (PS), poly(methyl methacrylat)s (PMMA), thermoplastic elastomers (TPE), derivatives, and mixtures thereof.

Description

EXAMPLES

1. Analytical Methods:

[0120] Particle Size Distribution (Mass % Particles with a Diameter<X) and Weight Median Diameter (d.sub.50) of a Particulate Material

[0121] Particle sizes were determined by using a Sedigraph™ 5120 instrument of Micromeritics Instrument Corporation. The method and the instrument are known to the skilled person and are commonly used to determine the particle size of fillers and pigments. The measurements were 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.

BET Specific Surface Area of a Material

[0122] The “specific surface area” (expressed in m.sup.2/g) of a material as used throughout the present document is determined by the Brunauer Emmett Teller (BET) method with nitrogen as adsorbing gas and by use of a ASAP 2460 instrument from Micromeritics. The method is well known to the skilled person and defined in ISO 9277:2010. Samples are conditioned at 100° C. under vacuum for a period of 30 min prior to measurement. The total surface area (in m.sup.2) of said material can be obtained by multiplication of the specific surface area (in m.sup.2/g) and the mass (in g) of the material.

Powder Flowability—Stability and Variable Flow Rate Method

[0123] 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.

[0124] This method consists of filling a cylindrical vessel (25 mm×25 ml glass vessel).

[0125] 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 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.

[0126] 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.

[0127] 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: [0128] Basic flowability energy (BFE, mJ): Energy Cycle 7 (downwards) [0129] Stability index: (Energy Test 7)/(Energy Cycle 1) [0130] Specific energy (SE, mJ/g): (Up Energy cycle 6+Up Energy cycle 7)/(2×split mass) [0131] Flow Rate Index (FRI): (Energy Test 11)/(Energy Test 8) [0132] Conditioned bulk density (CBD, g/ml): (Split mass)/(Split volume)

Moisture Pick Up Susceptibility

[0133] 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.

Contact Angle Measurements

[0134] Contact angles were measured by image analysis using images taken with a Canon EOS 600D and EF 1:2.8 MP-E 65 mm 1-5× macro-lens on a Kaiser stand and daylight illumination. For each sample, 5 microdroplets (5 μl) of each test liquid (water and/or hexadecane and/or diiodomethane) were deposited on the samples in the form of tablets. Images were taken 20s after applying the droplets. Contact angle and height and width were measured manually with the measurement tool of the ImageAccess database. Height and width were used to calculate contact angle of a spherical drop.

Surface Energy

[0135] The OCA 50 (DataPhysics Instruments GmbH, Filderstadt, Germany) is a measuring device for the analysis of the wettability of solid surfaces and the determination of the surface free energy of planar solids using the sessile drop technique. A high-speed microscope camera captures the evolution of the droplet configuration overtime after it is deposited on the surface. Image analysis and chosen curvature fitting software can be applied in relation to a user-defined linear continuous liquid-solid interface to determine the droplet meniscus shape, droplet volume and contact angle with the surface. By using various relevant liquids having defined polar and dispersive surface energy components (water, diiodomethane and ethylene glycol), it is possible to derive a measure of the surface energy of the solid according to the method of Owens, Wendt, Rabel and Kalble (OWRK) (1-3).

Tensile Properties

[0136] The tensile properties are measured according to ISO527-1:2012 Type BA(1:2) on an Allround Z020 traction device from Zwick Roell. Measurements are performed with an initial load of 0.1 MPa. For the measurement of the E-modulus, a speed of 1 mm/min is used, then it is increased to 500 mm/min. The tensile strain at break is obtained under standard conditions. All measurements are performed on samples that have been stored under similar conditions after preparation.

Impact Properties

[0137] The impact properties are measured according to ISO 179-1eU:2010-11 on a HIT5.5P device from Zwick Roell. Measurements are performed on un-notched samples with a hammer of 5J. All measurements are performed on samples that have been stored under similar conditions after preparation.

Thermal Conductivity

[0138] Thermal conductivity was measured with the Hot Disk TPS system according to ISO 22007-2:2008-12 Plastics—Determination of thermal conductivity and thermal diffusivity—transient plane heat source (hot disc) method under the following conditions: [0139] Hot Disk TPS 3500+software module ANISOTROPIC [0140] Kapton sensor 5465 (3.189 mm rayon) [0141] measuring temperature: 22° C.±1° C.; 155° C.±1° C.

2. Material

Calcium Carbonate Powders

[0142] CC 1

[0143] CC 1 is dry ground calcium carbonate (marble) from Italy (d.sub.50=1.8 μm, d.sub.98=7.4 μm; BET=4.1 m.sup.2/g)

[0144] CC 2

[0145] CC 2 is a dry ground calcium carbonate (marble) from Italy (d.sub.50=3.4 μm, d.sub.98=13.8 μm; BET=2.6 m.sup.2/g)

[0146] CC 3

[0147] CC 3 is a wet ground and spray dried calcium carbonate (marble) from Italy (sedigraph: d.sub.50=1.9 μm, d.sub.98=5.8 μm; BET=2.9 m.sup.2/g)

[0148] CC 4

[0149] CC 4 is a wet ground and spray dried calcium carbonate (limestone) from France (sedigraph: d.sub.50=0.7 μm, d.sub.98=2.9 μm; BET=7.9 m.sup.2/g)

Treatment Agents

[0150] Treatment Agent A

[0151] Treatment agent A is a poly(hexafluoropropylene oxide) functionalized with a carboxylic acid group situated on the terminal fluoromethylene group. It can be obtained from Chemours under tradename Krytox® 157FS(L). Molecular weight: ca. 2500 Da, viscosity (cSt, 40° C.): 99.4-149, TAN (Total Acid Number according to ASTM D664) (mg KOH/g): 23-27, density (g/ml, −9° C.): 1.91.

[0152] Treatment Agent B

[0153] Treatment agent B is a poly(hexafluoropropylene oxide) functionalized with a carboxylic acid group situated on the terminal fluoromethylene group. It can be obtained from Chemours under tradename Krytox® 157FS(H). Molecular weight: 7000-7500 Da, viscosity (cSt, 40° C.): 703-1055, TAN (Total Acid Number according to ASTM D664) (mg KOH/g): 8-10, density (g/ml, −9° C.): 1.91.

[0154] Treatment Agent C

[0155] Treatment agent C is an aqueous emulsion of a fluoropolyether ammonium phosphate salt. It can be obtained from Solvay under tradename Fluorolink® P54. Dry content: 20 wt %, density: 1.1. Color: clear amber solution.

[0156] Treatment Agent D

[0157] Treatment agent D is perfluorododecanoic acid from Fluorochem Ltd (CAS: 307-55-1, Mw=614.1 g/mole, mp=107-109° C.)

[0158] Treatment Agent E

[0159] Treatment agent E is perfluorooctanoic acid from Fluorochem Ltd (CAS: 335-67-1, Mw=414.1 g/mole, mp=40-50° C.)

[0160] Treatment Agent F

[0161] Treatment agent F is a mono-substituted alkenyl succinic anhydride (2,5-furandione, dihydro-, mono-C.sub.15-20-alkenyl derivatives, CAS No. 68784-12-3), which 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 %.

[0162] Treatment Agent G

[0163] Treatment agent G is a fatty acid mixture, which consists of a 1:1 mixture of stearic acid and palmitic acid. Such surface treatment is known to the skilled person, e.g. from WO 2010/030579 referring to stearic acid treated calcium carbonate having low or no detectable free stearic acid. The method for treating calcium carbonate includes the combination of calcium carbonate, water and stearic acid, wherein the amount of water is at least 0.1% by weight relative to the total weight.

[0164] The following products were obtained by treatment with treatment agents A-G and summarized in table 1.

Compound Treated Calcium Carbonates (Comparative)

[0165] CCC 1

[0166] CCC 1 is CC 1 treated with treatment agent G. CCC 1 was prepared in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) by surface-treating CC 1. For that purpose, CC 1 (1 kg) was first conditioned in the high speed mixer by stirring for 5 minutes at 120° C. (1000 rpm). After that time, treatment agent G (1.1 wt % relative to the calcium carbonate amount) was added dropwise to the mixture and stirring and heating was then continued for another 10 minutes at 120° C. (1000 rpm). After that time, the mixture was allowed to cool and the treated CCC 1 was collected.

[0167] CCC 2

[0168] CCC 2 is CC 2 treated with treatment agent G. CCC 2 was prepared in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) by surface-treating CC 2. For that purpose, CC 2 (1 kg) was first conditioned in the high speed mixer by stirring for 5 minutes at 120° C. (1000 rpm). After that time, treatment agent G (0.6 wt % relative to the calcium carbonate amount) was added dropwise to the mixture and stirring and heating was then continued for another 10 minutes at 120° C. (1000 rpm). After that time, the mixture was allowed to cool and the treated CCC 2 was collected

Poly- and/or Perfluorinated Compound Treated Calcium Carbonates (Inventive)

[0169] FCCC 3

[0170] FCCC 3 was prepared in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) by surface-treating CC 1. For that purpose, CC 1 (1 kg) was first conditioned in the high speed mixer by stirring for 5 minutes at 80° C. (1000 rpm). After that time, treatment agent A (0.5 wt % relative to the calcium carbonate amount) was added dropwise to the mixture and stirring and heating was then continued for another 10 minutes at 80° C. (1000 rpm). After that time, the mixture was allowed to cool and treated FCCC 3 was collected.

[0171] FCCC4

[0172] FCCC 4 was prepared in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) by surface-treating CC 1. For that purpose, CC 1 (1 kg) was first conditioned in the high speed mixer by stirring for 5 minutes at 80° C. (1000 rpm). After that time, treatment agent A (1 wt % relative to the calcium carbonate amount) was added dropwise to the mixture and stirring and heating was then continued for another 10 minutes at 80° C. (1000 rpm). After that time, the mixture was allowed to cool and treated FCCC 4 was collected.

[0173] FCCC 5

[0174] FCCC 5 was prepared in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) by surface-treating CC 1. For that purpose, CC 1 (1 kg) was first conditioned in the high speed mixer by stirring for 5 minutes at room temperature (1000 rpm). After that time, treatment agent A (1 wt % relative to the calcium carbonate amount) was added dropwise to the mixture and stirring was then continued for another 10 minutes at room temperature (1000 rpm).

[0175] After that time, treated FCCC 5 was collected.

[0176] FCCC 6

[0177] FCCC 6 was prepared in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) by surface-treating CC 1. For that purpose, CC 1 (1 kg) was first conditioned in the high speed mixer by stirring for 5 minutes at 120° C. (1000 rpm). After that time, treatment agent A (0.5 wt % relative to the calcium carbonate amount) and treatment agent F (0.5 wt % relative to the amount of calcium carbonate) was added dropwise to the mixture and stirring and heating was then continued for another 10 minutes at 120° C. (1000 rpm). After that time, the mixture was allowed to cool and the treated FCCC 6 was collected.

[0178] FCCC 7

[0179] FCCC 7 was prepared in a 10 l batch reactor by surface treatment of CC 1. For that purpose, a suspension of CC 1 (2.5 kg) in deionized water (5 l) was prepared at room temperature. After that, under strong stirring, treatment agent A (0.5 wt % relative to the calcium carbonate amount) was added and stirring was continued for 2 h. The slurry was then dried overnight in the oven (110° C.) and deagglomerated 2 times on Retsch SR300 rotor beater mill (9000 rpm), from Retsch GmbH, Germany.

[0180] FCCC 8

[0181] FCCC 8 was prepared in a 10 l batch reactor by surface treatment of CC 1. For that purpose, a suspension of CC 1 (2.5 kg) in deionized water (5 l) was prepared at room temperature. After that, under strong stirring, treatment agent A (1 wt % relative to the calcium carbonate amount) was added and stirring was continued for 2 h. The slurry was then dried overnight in the oven (110° C.) and deagglomerated 2 times on Retsch SR300 rotor beater mill (9000 rpm), from Retsch GmbH, Germany.

[0182] FCCC 9

[0183] 1 kg of CC 3 was placed in a high speed mixer (MTI Mixer, MTI Mischtechnik International GmbH, Germany), and conditioned by stirring for 10 minutes (3000 rpm, 120° C.). After that, treatment agent B (2 wt % relative to the amount of calcium carbonate) was introduced and stirring was continued for another 20 minutes (120° C., 3000 rpm). After that time, the treated powder was taken out (FCCC 9).

[0184] FCCC10

[0185] 1 kg of CC 2 was placed in a high speed mixer (MTI Mixer, MTI Mischtechnik International GmbH, Germany), and conditioned by stirring for 10 minutes (3000 rpm, 120° C.). After that, treatment agent B (1.1 wt % relative to the amount of calcium carbonate) was introduced and stirring was continued for another 20 minutes (120° C., 3000 rpm). After that time, the treated powder was taken out (FCCC 10).

[0186] FCCC 11

[0187] 1 kg of CC 2 was placed in a high speed mixer (MTI Mixer, MTI Mischtechnik International GmbH, Germany), and conditioned by stirring for 10 minutes (3000 rpm, 120° C.). After that, treatment agent C (1.1 wt % relative to the amount of calcium carbonate) was introduced and stirring was continued for another 20 minutes (120° C., 3000 rpm). After that time, the treated powder was taken out (FCCC 11).

[0188] FCCC 12

[0189] 0.7 kg of CC 2 was placed in a high speed mixer (MTI Mixer, MTI Mischtechnik International GmbH, Germany), and conditioned by stirring for 10 minutes (3000 rpm, 140° C.). After that, treatment agent D (1.1 wt % relative to the amount of calcium carbonate) was introduced and stirring was continued for another 20 minutes (140° C., 3000 rpm). After that time, the treated powder was allowed to cool down and taken out of the mixer (FCCC 12).

[0190] FCCC 13

[0191] 0.7 kg of CC 2 was placed in a high speed mixer (MTI Mixer, MTI Mischtechnik International GmbH, Germany), and conditioned by stirring for 10 minutes (3000 rpm, 90° C.). After that, treatment agent E (0.9 wt % relative to the amount of calcium carbonate) was introduced and stirring was continued for another 20 minutes (90° C., 3000 rpm). After that time, the treated powder was taken out (FCCC 13).

[0192] FCCC14

[0193] FCCC 14 was prepared in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) by surface-treating CC 1. For that purpose, CC 1 (0.5 kg) was first conditioned in the high speed mixer by stirring for 5 minutes at 80° C. (1000 rpm). After that time, Treatment agent A (3 wt % relative to the calcium carbonate amount) was added dropwise to the mixture and stirring and heating was then continued for another 10 minutes at 80° C. (1000 rpm). After that time, the mixture was allowed to cool and the treated FCCC 14 was collected.

[0194] FCCC 15

[0195] FCCC 15 was prepared in a 10 l batch reactor by surface treatment of CC 1. For that purpose, a suspension of CC 1 (2 kg) in deionized water (5 l) was prepared at room temperature. After that, under strong stirring (1000 rpm), treatment agent A (0.5 wt % relative to the calcium carbonate amount), which has been mixed with deionized water at a mass concentration of 1:20 was added dropwise and stirring was continued for 40 min. The slurry was then spray dried at 200° C. and two times deagglomerated in an ultra-centrifugal mill ZM200 from Retsch GmbH, Germany.

[0196] FCCC 16

[0197] FCCC 16 was prepared in a 10 l batch reactor by surface treatment of CC 1. For that purpose, a suspension of CC 1 (2 kg) in deionized water (5 l) was prepared at room temperature. After that, under strong stirring (1000 rpm), treatment agent A (0.5 wt % relative to the calcium carbonate amount), which has been mixed with deionized water at a mass concentration of 1:20 was added dropwise and stirring was continued for 40 min. The slurry was then filter pressed at 2-2.5 bar and dried overnight in an oven (160° C.) and deagglomerated two times in an ultra-centrifugal mill ZM200 from Retsch GmbH, Germany.

[0198] FCCC 17

[0199] FCCC 17 is CC 4 treated with treatment agent A. FCCC 17 was prepared in a high speed mixer (Somakon MP-LB Mixer, Somakon Verfahrenstechnik, Germany) by surface-treating CC 4. For that purpose, CC 4 (2 kg) was first conditioned in the high speed mixer by stirring for 5 minutes at 100° C. (600 rpm). After that time, treatment agent A (2 wt % relative to the calcium carbonate amount) was added dropwise to the mixture and stirring and heating was then continued for another 10 minutes at 100° C. (600 rpm). After that time, the mixture was allowed to cool and the treated FCCC 17 was collected.

TABLE-US-00001 TABLE 1 Treatment Treatment Dry or wet T ° of Powder CaCO.sub.3 agent 1 (wt %)* agent 2 (wt %)* treatment treatment CCC 1 CC 1 G (1.1%) — CCC 2 CC 2 G (0.6%) — FCCC 3 CC 1 A (0.5%) — dry  80° C. FCCC 4 CC 1 A (1%) — dry  80° C. FCCC 5 CC 1 A (1%) — dry room temp. FCCC 6 CC 1 A (0.5%) F (0.5%) dry 120° C. FCCC 7 CC 1 A (0.5%) — wet room temp. FCCC 8 CC 1 A (1%) — wet room temp. FCCC 9 CC 3 B (2%) — dry 120° C. FCCC 10 CC 2 B (1.1%) — dry 120° C. FCCC 11 CC 2 C (1.1%) — dry 120° C. FCCC 12 CC 2 D (1.1%) — dry 140° C. FCCC 13 CC 2 E (0.9%) — dry  90° C. FCCC 14 CC 1 A (3%) — dry  80° C. FCCC 15 CC 1 A (0.5%) — wet room temp. FCCC 16 CC 1 A (0.5%) — wet room temp. FCCC 17 CC 4 A (2%) — dry 100° C. *relative to the amount of calcium carbonate
Resins I Polymers to be filled

[0200] PA66: Rhodia Technyl A 205F Natural: an unreinforced polyamide 66 for injection moulding

[0201] PC: Polycarbonate: Resinex PC Calibre 201-22, from Trinseo LLC, United States

[0202] PET: Polyethylene terephthalate: T-209 serie

[0203] PC/PBT: Polycarbonate/Polybutylene terephthalate: Albis Pocan B7616

Other Compounds

[0204] PTFE: Polytetrafluoroethylene: Compound RTP 300 TEE 10, 15 and 20

[0205] Baryte: Barium sulfate: CAS 7727-43-7

[0206] Silicone: Compound RTP305 TFE13 S12

[0207] GE: Glass Eibre: Resinex Sikoclar E51.20, 30

Compounding

[0208] For evaluating the effects of the inventive fluorinated compound treated calcium carbonate fillers, the above described samples were introduced into several types of polymers by compounding.

[0209] Buss Compounding: 50% wt. CaCO.sub.3

[0210] Compounder: Co-rotating twin-screw, Type: Clextral, Evolum HT32

[0211] Screw: 32 mm, L/D ratio: 44, Output: 10-40 kg/hr, max. 100 kg/hr

[0212] Temperature: PBT: 260° C., PA66: 280° C., PC: 290° C.

Moulding

[0213] “Primitive” Injection molding on TSI PO Netstal—T: 290° C.

[0214] Technology: Injection molding, Type: Engel EM440/150

[0215] Sschliesskraft: 1500 KN, Screw diameter: 35 mm

[0216] Volume injected max.: 168 cm3, Pressure max.: 2800 bar

[0217] Temperature: PBT: 260° C., PA66: 280° C., PC: 290° C.

3. Treatment Effects

3.1. Powder Flowability

[0218] Powder flowability tests are summarized in table 2.

TABLE-US-00002 TABLE 2 BFE, CBD, Powder [mJ] [g/ml] CC 1 87.88 0.50 FCCC 3 82.64 0.55 FCCC 4 78.65 0.58 FCCC 14 48.74 0.58

[0219] It can be seen that the treatment with the perfluorinated additive improves powder flowability (lower BFE values) and increases bulk density (higher CBD values). This can be an advantage for processing and shipping.

3.2. Moisture Pickup

[0220] The moisture pickup of some of the poly- and/or perfluorinated compound treated calcium carbonates described above was investigated.

[0221] As can be seen from table 3, the inventive samples show reduced moisture pick-up compared to the corresponding untreated references, which is an advantageous effect in view of their use as fillers in polymers.

TABLE-US-00003 TABLE 3 Moisture Pickup Powder (mg/g) Compare with CC 1 2.4 — CC 2 2 — CC 3 1.5 — CC 4 2.9 — FCCC 5 1.8 CC 1 Inventive FCCC 7 1.2 CC 1 Inventive FCCC 8 1.6 CC 1 Inventive FCCC 9 1.1 CC 3 Inventive FCCC 10 1.2 CC 2 Inventive FCCC 11 1.7 CC 2 Inventive FCCC 12 1 CC 2 Inventive FCCC 13 1.6 CC 2 Inventive FCCC 17 2.3 CC 4 Inventive

3.2. Contact Angles and Surface Energy (Hydrophobicity and Lipophobicity)

[0222] Contact Angles of poly- and/or perfluorinated compound treated calcium carbonate To evaluate the hydrophobicity and lipophobicity of the poly- and/or perfluorinated compound treated calcium carbonates, tablets were prepared by compaction.

[0223] Tablet Preparation:

[0224] Tablets were prepared on a Herzog press TP40/2D (from HERZOG Maschinenfabrik GmbH & Co. KG, Germany) manually operated hydraulic press with 11 g of powder, which were compressed at 300 kN for 1 minute. The hydraulic pump is operated by a hand lever. A threaded spindle serves as a counter-bearing surface to provide a stable bed for the sample against the compacting pressure and to reduce the no-load stroke. The tablet was left in the metal cup used for tablet preparation.

[0225] For contact angle measurements, 3 tablets were prepared for the materials mentioned in table 4.

[0226] Contact Angles on Powder Tablets

[0227] Contact angles were measured by image analysis using images taken with a Canon EOS 600D and EF 1:2.8 MP-E 65 mm 1-5× macro-lens on a Kaiser stand and daylight illumination.

[0228] For each samples 5 microdroplets (5 μl) of each test liquids (water and hexadecane) were deposited on the tablets.

[0229] Images were taken 20 s after applying the droplets. Contact angle and height and

[0230] width were measured manually with the measuring module of the ImageAccess database Image Access Version 8.

[0231] For some of the comparative examples, it was not possible to measure contact angles (values too low). The results are summarized in table 4.

TABLE-US-00004 TABLE 4 Water Hexadecane Measured Calculated Measured Calculated contact angle contact angle contact angle contact angle Sample (°) f(circle) (°) (°) f(circle) (°) CC 2 <10 (not <10 (not <10 (not <10 (not Comparative measured) measured) measured) measured) CCC 2 142 +/− 3 134 +/− 2  21 +/− 4  10 +/− 1 Comparative FCCC 12 109 +/− 4 100 +/− 2 105 +/− 4 100 +/− 2 Inventive FCCC 13  84 +/− 9  82 +/− 1  87 +/− 1  82 +/− 1 Inventive

[0232] Table 3 shows that the inventive powders have both a hydrophobic and a lipophobic character, while the untreated powder is neither hydrophobic nor lipophobic, and the state-of-the art fatty acid treated reference is hydrophobic, but not lipophobic, as seen by the low contact angle with hexadecane.

[0233] Contact Angles on Coated Films

[0234] Coating colors were prepared with selected poly- and/or perfluorinated compound treated calcium carbonates and coated on superYUPO® foils from Fischer Papier AG, Switzerland (thickness 80 μm, size: 18×26 cm, 62 g/m.sup.2, polypropylene) with a table coater. The composition of the coating colours and contact angles with hexadecane are summarized in table 5 below.

TABLE-US-00005 TABLE 5 Coating colour composition Measured Dispersing Styronal contact agent.sup.a) D628 Solid angle with CaCO.sub.3 [parts, [parts, content.sup.b) hexadecane Example Powder [parts] dry/dry] dry/dry] [wt %] (°) Pap-1 CC 3 100 0.23 6 27.4 <10 Pap-2 FCCC 9 100 0.23 6 27.4   88 .sup.a)Sodium-neutralised polyacrylate (M.sub.w = 3500 g/mole, pH = 8) was used as dispersing agent. .sup.b)Solid content was adjusted with deionized water.

[0235] It can be seen from table 4 that the treatment of calcium carbonate with a functionalized poly- and/or perfluorinated compound additive significantly increases contact angles with non-polar solvents (lipophobicity).

[0236] Contact Angles on Resins Filled with Poly- and/or Perfluorinated Compound Treated Calcium Carbonates

[0237] Resins were filled with some of the above inventive poly- and/or perfluorinated compound treated calcium carbonates by compounding and further investigated as regards their surface properties. The results are shown in tables 6 to 9.

[0238] It can be seen from the given results that the treatment of calcium carbonate with poly- and/or perfluorinated compounds increases hydrophobicity of the resin filled therewith, wherein the surface energy is significantly decreased. This is especially important in view of the moulding properties of the resins, especially as regards problems of stickiness upon removal of the resin from the mould, which may be reduced.

[0239] This effect can be observed compared with the unfilled resin, as well as in comparison with resins filled with PTFE, as well as in combination with glass fibres.

TABLE-US-00006 TABLE 6 Contact Angle (°) Surface Energy Compound Diiodo- (mN .Math. m.sup.−1) Resin (wt %)* Water methane Total Dispersive Polar PC 85.6 30.0 45.5 44.2 1.3  + 10% FCCC 4 86.0 35.0 43.5 42.1 1.5  (x2)** 50% FCCC 3 98.4 47.5 35.7 35.7 0.2  (x2)** 50% FCCC 4 102.2 41.5 38.9 38.9 0.01 (x2)** + 10% CC 1 78.9 34.4 45.7 42.3 3.3  (x2)** + 10% PTFE 83.0 21.7 48.7 47.3 1.5  15% PTFE 84.3 30.3 45.7 44.1 1.6  13% PTFE + 88.9 27.3 45.9 45.3 0.6  2% Silicone 10% PTFE + 89.2 33.8 43.4 42.6 0.8  5% FCCC 3 (x2)** + 30% GF 83.9 30.0 44.4 42.4 2.0  30% GF + 83.1 35.0 40.7 37.8 2.8  10% FCCC 3 30% GF + 89.3 34.4 41.0 39.9 1.1  10% FCCC 4 30% GF + 15% 87.0 21.7 40.2 38.5 1.7  PTFE 30% GF + 94.5 33.8 40.7 40.4 0.8  10% PTFE + 5% FCCC 3 30% GF + 13% 90.5 27.3 39.7 38.8 1.0  PTFE + 2% Silicone *wt % based on the total amount of resin **x2 means two times compounded

TABLE-US-00007 TABLE 7 Compound Contact Angle (°) Total Surface Resin (wt %)* Water Diiodomethane Energy (mN .Math. m.sup.−1) PA66 — 73.7 40.6 42.5 +10% FCCC 3 73.8 +15% FCCC 3 72.3 +30% FCCC 3 69.5 +30% FCCC 4 70.5 +50% FCCC 3 78.7 56.5 41.1 +50% FCCC 4 73.8 +60% FCCC 3 67.1 59.4 38.8 +70% FCCC 3 71.9 61.6 37.1 +30% CC1 73.7 +50% CC1 82.2 60.7 38.4 +10% PTFE 68.3 43.9 41.6 +20% PTFE 69.7 41.4 43.2 +10% CC1 67.7 +10% PTFE +30% CC1 68.4 +10% PTFE +50% CC1 74.2 +10% PTFE +30% GF 69.6 +30% GF 77.1 +15% PTFE *wt % based on the total amount of resin

TABLE-US-00008 TABLE 8 Compound Contact Angle (°) Total Surface Resin (wt %)* Water Diiodomethane Energy (mN .Math. m.sup.−1) PET +25% CC1 74.6 40.0 42.4 +25% CCC1 69.0 49.2 40.9 +25% FCCC 3 92.7 34.0 44.2 +15% GF 79.3 43.6 37.2 +25% FCCC 3 *wt % based on the total amount of resin

TABLE-US-00009 TABLE 9 Contact Angle (°) Surface Energy Compound Diiodo- (mN .Math. m.sup.−1) Resin (wt %)* Water methane Total Dispersive Polar PC/PBT 15% GF 82.8 30.0 45.8 43.8 2.0 15% GF + 84.6 27.5 46.6 45.2 1.4 10% FCCC 4 (x2)** *wt % based on the total amount of resin **x2 means two times compounded

3.2. Physical and Mechanical Properties

[0240] As regards the impact on the mechanical properties of resins filled with inventive poly- and/or perfluorinated compound treated calcium carbonates as fillers, a number of experiments was made with different resins, and in comparison with other conventional fillers, as well as mixtures thereof. In this respect, PC (Polycarbonate) is especially interesting, as it is not trivial to use calcium carbonate fillers in polycarbonate resins.

[0241] The compounding of the resins was carried out as described above, the results of the tests are summarized in tables 10 to 15.

[0242] First of all, it can be seen from tables 10 and 11 that it is possible to fill the resin with a rather high amount of poly- and/or perfluorinated compound treated calcium carbonate of up to 50 wt % based on the total weight of resin to be filled. This is not possible with untreated calcium carbonate.

[0243] Density

[0244] As regards the density of the filled PC resin, it may be taken from tables 10 and 11 that there is nearly no density increase by the treatment of calcium carbonate with poly- and/or perfluorinated compounds, contrary to, e.g. baryte filled resins, or the additional filling with glass fibres, at comparable properties.

[0245] Heat Deflection Temperature (HDT)

[0246] The HDT of poly- and/or perfluorinated compound treated calcium carbonates is essentially the same as in untreated PC and in PC filled with untreated calcium carbonate or PTFE, and it is significantly lower than in glass fibre filled PC. Accordingly, there is no negative impact on the HDT by the filler treatment (cf. tables 10 and 11).

[0247] Tensile Properties

[0248] It can be observed that the filling with poly- and/or perfluorinated compound treated calcium carbonate has a positive impact on the tensile properties of the tested resins compared with other conventional fillers.

[0249] For example, the E-modulus of PC filled with poly- and/or perfluorinated compound treated calcium carbonate is higher than the one of unfilled PC, and only slightly lower than the one of PC filled with untreated calcium carbonate, wherein a higher treatment degree leads to a higher E-modulus. This is especially remarkable as PC filled with PTFE has lower E-modulus values, i.e. the increase of the E-modulus, appears to be due to a synergistic effect between calcium carbonate and poly- and/or perfluorinated compound.

[0250] Also, an admixture of poly- and/or perfluorinated compound treated calcium carbonate to other filler leads to an increase of the E-modulus, stronger than with the admixture of PTFE, as can be seen from the combination of baryte with PTFE and FCCC 3 (cf. table 10).

[0251] At a higher filler degree, it is even comparable to products filled with glass fibres (cf. table 11).

[0252] As regards the tensile strength, it can be seen that PC filled with untreated calcium carbonate is subjected to a decrease at filler loads of 30 wt %. In contrast to this, PC filled with poly- and/or perfluorinated compound treated calcium carbonate shows a tensile strength comparable with the one of unfilled PC even at a filler load of up to 30 wt %. Only at 50 wt % poly- and/or perfluorinated compound treated calcium carbonate, the tensile strength decreases.

[0253] Anyway, compared with other fillers such as PTFE or baryte, it can be seen that the tensile strength of PC filled with poly- and/or perfluorinated compound treated calcium carbonate is generally higher, except for 50 wt % baryte filler loads.

[0254] In combination with glass fibres, it can be observed that the tensile strength of PTFE filled PC and poly- and/or perfluorinated compound treated calcium carbonate filled PC is comparable.

[0255] Looking at the yield stress, the same tendencies can be observed.

[0256] The elongation at break of calcium carbonate filled PC may be significantly increased by the poly- and/or perfluorinated compound treatment as can be seen from the comparison of the corresponding values.

[0257] Furthermore, in combination with glass fibres, it can be observed that the elongation at break of poly- and/or perfluorinated compound treated calcium carbonate filled PC is higher than the one of PTFE filled PC.

TABLE-US-00010 TABLE 10 Tensile Yield Elongation Resin + wt % Density HDT E-Modulus Strength stress @ break compound* (g/cm.sup.3) (° C.) (N/mm.sup.2) (N/mm.sup.2) (%) (%) PC 1.18 121 2200 63 6.3 142 PC + FCCC 10% FCCC 3 1.23 120 2400 61 5.7 55 10% FCCC 4 1.25 120 2620 61 5.3 25 30% FCCC 3 1.35 121 2920 60 4   6.1 30% FCCC 4 1.40 124 3620 60 3.3 3.7 50% FCCC 3 1.62 121 5280 34 0.7 50% FCCC 4 1.62 121 5880 32 0.6 PC + CC 10% CC 1 1.25 121 2600 63 5.5 16 30% CC 1 1.41 119 3740 33 0.9 50% CC 1 Not feasible PC + PTFE 10% PTFE 1.24 123 2000 57 6.1 92 15% PTFE 1.27 122 2070 54 5.9 73 13% PTFE + 1.24 121 1870 53 5.7 41 2% Silicone 10% PTFE + 1.26 121 2280 55 5.9 38 5% FCCC 3 (x2)** PC + Baryte 30% baryte 1.50 119 3180 52 4   10 30% baryte + 1.57 119 2970 45 4.3 13 10% PTFE (x2)** 30% baryte + 1.62 115 3820 34 0.9 10% FCCC 3 50% baryte 1.85 116 4140 43 1.6 *wt % based on the total amount of resin **x2 means two times compounded

TABLE-US-00011 TABLE 11 E- Tensile Yield Elongation Density HDT Modulus Strength stress @ break (g/cm.sup.3) (° C.) (N/mm.sup.2) (N/mm.sup.2) (%) (%) PC + 20% GF 1.32 135 5930 112 3.5 4   +10% PTFE 1.39 141 6320 100 2.6 +10% FCCC 1.39 130 5970  98 3.2 3.9 3 (x2)** +10% FCCC 1.39 130 5690  96 3.3 4   4 (x2)** +15% FCCC 1.42 135 5850  94 3.1 3.5 3 (x2)** +5% PTFE + 1.37 135 5480  92 3.4 4.4 5% FCCC 3 (x2)** PC + 30% GF 1.40 135 8170 135 3.1 +15% PTFE 1.53 141 9020 106 2   +15% FCCC 1.51 131 8050 111 2.5 3 (x2)** +10% PTFE + 1.52 137 8690 112 2.9 5% FCCC 3 (x2)** +15% FCCC 1.51 128 7950 107 2.1 4 (x2)** +13% PTFE + 1.51 141 8930 102 1.8 2% Silicone *wt % based on the total amount of resin **x2 means two times compounded

TABLE-US-00012 TABLE 12 E- Tensile Yield Elongation Density HDT Modulus Strength stress @ break (g/cm.sup.3) (° C.) (N/mm.sup.2) (N/mm.sup.2) (%) (%) PC/PBT + 1.35 91 4560 78 3.5 4.1 15% GF +10% FCCC 1.41 63 4540 67 2.9 4.3 4 (x2)** *wt % based on the total amount of resin **x2 means two times compounded

[0258] The PA66 resin filled with FCCC 15 and 20 as well as CC 1 were examined as regards the E-modulus, elongation at break and tensile strength, as well.

[0259] As can be taken from table 13, no negative impact of the treatment with poly- and/or perfluorinated compound on the E-modulus can be observed. For highly filled systems, the treatment of calcium carbonate filler with poly- and/or perfluorinated compound even allows an increase of tensile strength and elongation at break by improving the melt rheology and reducing the melt fracture.

TABLE-US-00013 TABLE 13 Tensile Elongation Resin + wt % E-Modulus Strength @ break compound* (N/mm.sup.2) (N/mm.sup.2) (%) PA66 1230 86 8.8 PA66 + FCCC 30% FCCC 15 1430 80 6.2 30% FCCC 16 1510 82 5.9 40% FCCC 15 1550 80 4.9 40% FCCC 16 1570 83 5.3 50% FCCC 15 1490 74 4.1 50% FCCC 16 1640 81 4.5 PA66 + CC 30% CC 1 1490 81 6.1 40% CC 1 1620 80 4.9 50% CC 1 1640 72 3.6 *wt % based on the total amount of resin

[0260] Furthermore the impact properties were investigated.

[0261] As can be taken from table 14, an increase of the impact strength of poly- and/or perfluorinated compound treated calcium carbonate filled PC can be observed compared with PC filled with untreated calcium carbonate.

[0262] Compared with PTFE and baryte filled PCs comparable results are obtained.

[0263] In admixtures with glass fibres the impact strength values of poly- and/or perfluorinated compound treated calcium carbonate filled PC are higher than those of merely PTFE filled PC (cf. table 15).

TABLE-US-00014 TABLE 14 Resin + wt % Impact Strength (N/mm.sup.2) compound* Charpy UN (4J) Charpy UN (5J) PC No break PC + FCCC 10% FCCC 3 No break 10% FCCC 4 No break 30% FCCC 3 69 65.0 30% FCCC 4 33 31.0 50% FCCC 3 5 5.0 50% FCCC 4 5 4.5 PC + CC 10% CC 1 No break 30% CC 1 10 10.0 50% CC 1 Not feasible PC + PTFE 10% PTFE No break 15% PTFE No break 13% PTFE + No break 2% Silicone 10% PTFE + 5% No break FCCC 3 (×2)** PC + Baryte 30% baryte 85 97.0 30% baryte + 10% 66 50.0 PTFE (×2)** 30% baryte + 10% 4 FCCC 3 50% baryte 9 *wt % based on the total amount of resin **×2 means two times compounded

TABLE-US-00015 TABLE 15 Resin + wt % Impact Strength (N/mm.sup.2) compound* Charpy UN (4J) PC + 20% GF 62 +10% PTFE 39 +10% FCCC 3 (×2)** 53 +10% FCCC 4 (×2)** 50 +15% FCCC 3 (×2)** 46 +5% PTFE 54 +5% FCCC 3 (×2)** PC + 30% GF 62 +15% PTFE 35 +15% FCCC 3 (×2)** 41 +10% PTFE 47 +5% FCCC 3 (×2)** +15% FCCC 4 (×2)** 37 +13% PTFE 31 +2% Silicone *wt % based on the total amount of resin *×2 means two times compounded

TABLE-US-00016 TABLE 16 Resin + wt % Impact Strength (N/mm.sup.2) compound* Charpy UN (4J) PC/PBT + 15% GF 38 +10% FCCC 4 (×2)** 41 *wt % based on the total amount of resin *×2 means two times compounded

[0264] Furthermore, as can be taken from table 17, there is no negative influence of poly- and/or perfluorinated compound treated calcium carbonate on the impact properties versus untreated calcium carbonate in PA66.

TABLE-US-00017 TABLE 17 Impact Strength (N/mm.sup.2) Resin + wt % Charpy notched compound* (N/mm.sup.2) PA66 6.6 PA66 + FCCC 30% FCCC 15 4.3 30% FCCC 16 3.1 40% FCCC 15 3.3 40% FCCC 16 3.2 50% FCCC 15 3.4 50% FCCC 16 3.4 PA66 + CC 30% CC 1 3.2 40% CC 1 3.2 50% CC 1 3.4 *wt % based on the total amount of resin

[0265] Thermal Conductivity

[0266] As can be seen from table 18, the poly- and/or perfluorinated compound treatment of calcium carbonate increases the axial and radial thermal conductivity of PA66, which is advantageous and allows for new application fields of PA66, and the replacement of otherwise applied additives such as copper powders, at an increased filler load.

TABLE-US-00018 TABLE 18 Thermal conductivity λ (W .Math. m.sup.−1 .Math. K.sup.−1) Compound axial radial Resin (wt %) 22° C. 155° C. 22° C. 155° C. PA66 +20% CC 1 0.40 0.34 0.44 0.44 +20% FCCC 3         Not measured +50% CC 1 0.59 0.54 0.65 0.59 +50% FCCC 3 0.66 0.61 0.72 0.66 +70% CC 1         Not feasible +70% FCCC 3 0.91 0.84 0.88 0.77

[0267] As regards the thermal conductivity of the PET/15% GE resin, it can be seen that the thermal conductivity is about the same in the treated and untreated calcium carbonate filled samples. However, due to the fact that the poly- and/or perfluorinated compound can be added at a higher filler load, the thermal conductivity can be increased (cf. table 19).

TABLE-US-00019 TABLE 19 Thermal conductivity λ (W .Math. m.sup.−1 .Math. K.sup.−1) Compound axial radial Resin (wt %) 22° C. 155° C. 22° C. 155° C. PET/ +40% CC 1 0.42 0.48 0.48 0.49 15% GF +40% FCCC 3 0.42 0.43 0.48 0.53 +40% CC 1 — — — — Not feasible +40% FCCC 3 0.54 0.57 0.60 0.66