Process for the production of a composite polymer material with increased filler content

Abstract

An inventive process for the production of a composite polymer material is provided allowing for the preparation of a composite polymer material with high filler content which may be used as a masterbatch.

Claims

1. A composite polymer material obtained by a process comprising the steps of: (a) providing a mineral filler material; (b) providing a polymer material; (c) conveying the mineral filler material of step (a) and the polymer material of step (b) to a compounder; (d) forming a composite polymer material in said compounder; wherein the mineral filler material of step (a) is added to the polymer material of step (b) in an amount so that the mineral filler content of the resulting composite polymer material is in the range from 60 to 900 phr and wherein the mineral filler material of step (a) is added to the polymer material of step (b) by use of direct addition technology, said technology comprising the addition and mixing of said mineral filler material to said polymer material in a direct addition device in direct connection to the compounding section of the compounder so that no pneumatic conveying of the resulting mixture to the compounding section is involved and wherein said compounder is an extruder.

2. The composite polymer material according to claim 1, wherein the mineral filler content of the resulting composite polymer material ranges from 150 to 800 phr.

3. The composite polymer material according to claim 1, wherein the composite polymer material in step (d) is produced in a form of a granulate having an average grain size ranging from 2 to 8 mm.

4. The composite polymer material according to claim 1, wherein the obtained composite polymer material is micronized to yield an average grain size of less than 4 mm.

5. The composite polymer material according to claim 1, wherein the polymer material provided in step (b) comprises a mineral filler material.

6. The composite polymer material according to claim 1, wherein the polymer material provided in step (b) comprises a recycled polymer material.

7. The composite polymer material according to claim 1, wherein the temperature of the polymer melt is kept below 205 C.

8. The composite polymer material according to claim 1, wherein the mineral filler material is selected from the group consisting of calcium carbonate, chalk, limestone, marble, dolomite, titanium dioxide, barium sulphate, talc, clay, mica, and any mixture thereof.

9. The composite polymer material according to claim 1, wherein the mineral filler material is selected from ground dolomite, ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), modified calcium carbonate (MCC), and any mixture thereof.

10. The composite polymer material according to claim 1, wherein the polymer material comprises a polymer selected from the group consisting of vinyl polymers, vinyl copolymers, acryl polymers, acryl copolymers, chlorinated polyethylenes, and any mixture thereof.

11. The composite polymer material according to claim 1, wherein the mineral filler material is calcium carbonate and/or dolomite.

12. A composite polymer material comprising a mineral filler material and a polymer material, wherein the composite polymer material is in the form of grains having an average grain size of less than 4 mm, and wherein the filler content in the composite polymer material is in the range from 60 to 900 phr.

13. The composite polymer material according to claim 12, characterized in that the mineral filler content of the composite polymer material is in the range from 150 to 800 phr.

14. A polymer product comprising the composite polymer material of claim 1.

15. A masterbatch or polymer product comprising the composite polymer material according to claim 13.

Description

EXAMPLES

(1) The scope and interest of the invention may be better understood based on the following examples which are intended to illustrate certain embodiments of the present invention and are non-limitative.

(2) Measurements

(3) K-Value

(4) A measure of the molecular weight of a polymer based on measurements of viscosity of a polymer solution and is defined as follows:

(5) $\frac{\log \left(N_S/N_0\right)}{c}=\frac{75K^2}{1+1.5\mathrm{Kc}}+K$

(6) In general, k-values for a particular polymer may be requested from the polymer producer or may be taken on the packaging or the accompanying technical data sheet.

(7) Particle Size of the Mineral Filler Material

(8) The particle size distribution of the filler material may be measured using a Sedigraph 5120 from the company Micromeritics, USA. The method and the instruments are known to the skilled person and are commonly used to determine grain size of fillers and pigments. The measurement may be carried out in an aqueous solution comprising 0.1 wt.-% Na.sub.4P.sub.2O.sub.7. The samples were dispersed using a high speed stirrer and supersonics.

(9) Average Grain Size of the Composite Polymer Material

(10) The average grain size of the composite polymer material is the weight median grain size, i.e. 50 wt.-% of all grains are bigger or smaller than this average grain size. The grain size is determined by sieving according to ISO 3310-1:2000 (E).

(11) General Procedure

(12) Amounts and specifications of components used herein can be taken from the table given for examples 1-4.

(13) The corresponding polymer material may be provided in a hot-mixer. Stabilizer (S), lubricant (L), optional plasticizer (P), optional co-stabilizer (C), an optional processing additive (A) and/or calcium carbonate (F1) may be added and mixed until a temperature of about 120 C. is reached. The mixture then may be cooled down to about 50 C. in a cold-mixer. The mixture may be conveyed to a compounder. By use of direct addition technology further calcium carbonate (F2) as mineral filler material may be added and the resulting mixture may be fed into the compounding section of an extruder, preferably by use of a co-rotating double screw combined with a stuffing device. Optionally, the obtained granulate may be micronized e.g. by using a Pallmann mill to yield an average grain size of less than 2 mm.

(14) Materials

(15) Polymer Material: Polyvinyl Chloride (PVC)

(16) Vestolit P 1982 K, commercially available from Vestolit GmbH & Co. KG, Germany, k=65.

(17) Polymer Material: Polyvinyl Chloride (PVC)

(18) Vinnolit E 2059, commercially available from Vinnolit GmbH & Co. KG, Germany, k=59.

(19) Polymer Material: Polyvinyl Chloride (PVC)

(20) INEOS S 5730 Suspenion PVC, commercially available from INEOS Vinyls Deutschland GmbH, Germany, k=57.

(21) Polymer Material: Micronized Recycled Polyvinyl Chloride (R-PVC)

(22) Commercially available from Tonsmeier Kunststoffe, Germany. Average grain size: 0.5 to 1.0 mm.

(23) Co-Stabilizer: Epoxidized Soybean Oil (ESBO)

(24) Vikoflex 7170, commercially available from ARKEMA, France.

(25) Plasticizer: 1,2-Cyclohexane Dicarboxylic Acid Diisononyl Ester (DINCH)

(26) Hexamoll DINCH, commercially available from BASF SE, Germany.

(27) Filler Material: Hydrocarb 95T-OG

(28) Ground calcium carbonate, commercially available from Omya AG, Switzerland. Particle size d.sub.50: 0.8 m; top cut d.sub.98: 5.0 m.

(29) Filler Material: Omyalite 50H-OM

(30) Ground calcium carbonate, commercially available from Omya AG, Switzerland. Particle size d.sub.50: 2.0 m; top cut d.sub.98: 10 m.

(31) Filler Material: Omya BSH-OM

(32) Ground calcium carbonate, commercially available from Omya AG, Switzerland. Particle size d.sub.50: 2.4 m; top cut d.sub.98: 20 m.

(33) In the art and in particular in the field of polyvinyl chloride (PVC) processing mixtures comprising stabilizers and lubricants are available, also referred to as one packs. Typical stabilizers may comprise lead stabilizers, calcium-zink stabilizers, organic based stabilizers, calcium organic based stabilizers or tin stabilizers. Typical lubricants may comprise internal lubricants such as fatty alcohols, dicarboxylic acid esters or oxidized polyethylene waxes, external lubricants such as paraffin wax or polyethylene wax or lubricants with internal and external properties such as ester wax or fatty acid esters.

(34) For example, a preferred one pack comprises:

(35) TABLE-US-00001 3.5 phr calcium-zink stabilizer, 0.3 phr polyethylene wax, 0.25 phr paraffin wax, and 0.2 phr oxidized polyethylene wax.

Examples 1-4

(36) The following illustrative examples may be prepared according to the general procedure given above.

(37) TABLE-US-00002 1 2 3 4 polymer Vestolit Vinnolit INEOS R-PVC material P 1982 K E 2059 S 5730 (micronized) S, L One Pack One Pack One Pack One Pack (3 phr) (4 phr) (5 phr) (2 phr) P Hexamoll DINCH (4 phr) C Vikoflex 7170 (2 phr) F1 Hydrocarb Omyalite 95T-OG 50H-OM (20 phr) (10 phr) F2 Hydrocarb Omyalite Omyalite Omya 95T-OG 90T-OM 50H-OM BSH-OM (170 phr) (200 phr) (300 phr) (400 phr) F1 + 190 phr 200 phr 310 phr 400 phr F2

Examples 5-8

(38) S-PVC (INEOS S 5730, k=57) was dry blended with calcium carbonate (Omyalite 50H-OM), stabilizer (BAEROPAN R 91800 P/1-CC) and co-stabilizer (ESBO). The blend was charged into a Coperion ZSK 26/60 MC extruder, wherein additional calcium carbonate (Omyalite 50H-OM) was added by direct addition using an extra metering unit. Redispersion quality of the extrusion product was controlled via profile extrusion and visual inspection. The results of the different trials are listed in the table below.

(39) TABLE-US-00003 5 6 7 8 dry blend INEOS INEOS INEOS INEOS S 5730 S 5730 S 5730 S 5730 Omyalite Omyalite Omyalite Omyalite 50H-OM 50H-OM 50H-OM 50H-OM (30 phr) (30 phr) (30 phr) (30 phr) BAEROPAN BAEROPAN BAEROPAN BAEROPAN (3.4 phr) (3.4 phr) (3.4 phr) (3.4 phr) ESBO ESBO ESBO (0 phr) (0 phr) (0 phr) extruder 46.7 kg/h 48.7 kg/h 49.5 kg/h 54.5 kg/h output CaCO.sub.3 via 4.5 kg/h 3.5 kg/h 2.7 kg/h 2.4 kg/h dry blend (clcd.) CaCO.sub.3 via 26.5 kg/h 29.5 kg/h 34.5 kg/h 41.5 kg/h direct addition total 31.0 kg/h 33.0 kg/h 37.2 kg/h 43.9 kg/h CaCO.sub.3 filler content of 66.4 wt.-% 67.8 wt.-% 75.1 wt.-% 88.7 wt.-% the composite dispersion excellent excellent good acceptable, quality some small agglomerates