Surface-reacted calcium carbonate as extrusion aid

Abstract

A method is described of using a surface-reacted calcium carbonate as an extrusion aid for the production of a puffed polysaccharide-based material, excluding fibrillated cellulose-containing materials. In embodiments, the surface-reacted calcium carbonate is a reaction product of ground natural calcium carbonate (GNCC) or precipitated calcium carbonate (PCC) with carbon dioxide.

Claims

1. A process for the production of a puffed polysaccharide-based material, the process comprising the following steps: (a) providing at least one polysaccharide-containing ground material, excluding fibrillated cellulose-containing materials; (b) providing at least one extrusion aid; (c) combining the polysaccharide-containing ground material provided in step (a) and the extrusion aid provided in step (b) to obtain a mixture; and (d) puffing the mixture obtained in step (c) by means of an extruder to obtain a puffed polysaccharide-based extrudate; wherein the extrusion aid provided in step (b) is a surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is a reaction product of ground natural calcium carbonate (GNCC) or precipitated calcium carbonate (PCC) treated with CO.sub.2 and one or more H.sub.3O.sup.+ ion donors and wherein the CO.sub.2 is formed in situ by the H.sub.3O.sup.+ ion donors treatment and/or is supplied from an external source wherein the extrusion aid has a specific surface area of from 15 m.sup.2/g measured using nitrogen and the BET method according to ISO 9277:1995.

2. The process according to claim 1, wherein: (i) the polysaccharide is a homopolysaccharide; and/or ii) the polysaccharide-containing ground material provided in step (a) comprises barley, corn (maize), oats, rice, rye, spelt, wheat, amaranth, quinoa, millet or mixtures thereof.

3. The process according to claim 1, wherein the one or more H.sub.3O.sup.+ ion donors are selected from the group consisting of: (i) strong acids having a pK.sub.a of 0 or less at 20° C.; and/or (ii) medium-strong acids having a pK.sub.a value from 0 to 2.5 at 20° C.; and/or (iii) weak acids having a pK.sub.a of greater than 2.5 and less than or equal to 7 at 20° C., associated with the ionization of its first available hydrogen, wherein a corresponding anion is formed on loss of this first available hydrogen capable of forming a water-soluble calcium salt, and wherein at least one water-soluble salt, which in the case of a hydrogen-containing salt has a pK.sub.a of greater than 7 at 20° C., associated with the ionization of the first available hydrogen, and the salt anion of which is capable of forming water-insoluble calcium salts, is additionally provided.

4. The process according to claim 1, wherein the surface-reacted calcium carbonate is obtained by a process comprising the following steps: (a) providing a suspension of ground natural calcium carbonate (GNCC) or precipitated calcium carbonate (PCC); (b) adding at least one acid having a pK.sub.a value of 0 or less at 20° C., or having a pK.sub.a value from 0 to 2.5 at 20° C. to the suspension provided in step (a); and (c) treating the suspension provided in step (a) with CO.sub.2 before, during or after step (b).

5. The process according to claim 1, wherein the surface-reacted calcium carbonate is obtained by a process comprising the following steps: (a) providing ground natural calcium carbonate (GNCC) or precipitated calcium carbonate (PCC); (b) providing at least one water-soluble acid; (c) providing gaseous CO.sub.2; and (d) contacting said GNCC or PCC provided in step (a), the at least one acid provided in step (b) and the gaseous CO.sub.2 provided in step (c); wherein (i) the at least one acid provided in step (b) has a pK.sub.a of greater than 2.5 and less than or equal to 7 at 20° C., associated with the ionization of its first available hydrogen, and a corresponding anion is formed on loss of this first available hydrogen capable of forming a water-soluble calcium salt; and (ii) following contacting the at least one water-soluble acid provided in step (b) and the GNCC or PCC provided in step (a), at least one water-soluble salt, which in the case of a hydrogen-containing salt has a pK.sub.a of greater than 7 at 20° C., associated with the ionization of the first available hydrogen, and the salt anion of which is capable of forming water-insoluble calcium salts, is additionally provided.

6. The process according to claim 1, wherein: (i) the natural calcium carbonate is selected from the group consisting of marble, chalk, dolomite, limestone and mixtures thereof; and/or (ii) the precipitated calcium carbonate comprises aragonitic, vateritic or calcitic mineralogical crystal forms or mixtures thereof.

7. The process according to claim 1, wherein the extrusion aid has: (i) a volume median grain diameter d.sub.50(vol) of from 1 μm to 75 μm; and/or (ii) a volume grain diameter d.sub.98(vol) of from 2 μm to 150 μm.

8. The process according to claim 1, wherein the mixture obtained in step (c) comprises from 0.01 wt.-% to 10 wt.-% of the extrusion aid provided in step (b), based on the total dry weight of said mixture.

9. The process according to claim 1, wherein in step (d): (i) the mixture obtained in step (c) is heated to from 100° C. to 150° C.; and/or (ii) the extruder operates at a minimum pressure of 0.5 MPa; and/or (iii) the extruder operates at a maximum pressure of 10 MPa.

10. The process according to claim 1, wherein the mixture obtained in step (c) further comprises the following additives: (i) water; and/or (ii) whole grains; and/or (iii) sucrose; and/or (iv) sodium chloride; each based on the total dry weight of said mixture.

11. The process according to claim 1, wherein the process further comprises step (e) of processing the puffed polysaccharide-based extrudate obtained in step (d) into: (i) a food product for human consumption; or (ii) a food product for animal consumption; or (iii) a packaging material.

12. An extrusion aid comprising an effective amount of a surface-reacted calcium carbonate for the production of a puffed polysaccharide-based material, excluding fibrillated cellulose-containing materials, wherein the surface-reacted calcium carbonate is a reaction product of ground natural calcium carbonate (GNCC) or precipitated calcium carbonate (PCC) treated with CO.sub.2 and one or more H.sub.3O.sup.+ ion donors and wherein the CO.sub.2 is formed in situ by the H.sub.3O.sup.+ ion donors treatment and/or is supplied from an external source wherein the extrusion aid has a specific surface area of from 15 m.sup.2/g measured using nitrogen and the BET method according to ISO 9277:1995.

13. The extrusion aid according to claim 12, wherein the aid has: (i) a volume median grain diameter d.sub.50(vol) of from 1 μm to 75 μm; and/or (ii) a volume grain diameter d.sub.98(vol) of from 2 μm to 150 μm.

14. A puffed polysaccharide-based material, excluding fibrillated cellulose-containing materials, wherein the puffed polysaccharide-based material is prepared by a process comprising the following steps: (a) providing at least one polysaccharide-containing ground material, excluding fibrillated cellulose-containing materials; (b) providing at least one extrusion aid; (c) combining the polysaccharide-containing ground material provided in step (a) and the extrusion aid provided in step (b) to obtain a mixture; and (d) puffing the mixture obtained in step (c) by means of an extruder to obtain a puffed polysaccharide-based extrudate; wherein the extrusion aid provided in step (b) is a surface-reacted calcium carbonate, wherein the surface-reacted calcium carbonate is a reaction product of ground natural calcium carbonate (GNCC) or precipitated calcium carbonate (PCC) treated with CO.sub.2 and one or more H.sub.3O.sup.+ ion donors, wherein the CO.sub.2 is formed in situ by the H.sub.3O.sup.+ ion donors treatment and/or is supplied from an external source, and wherein the extrusion aid has a specific surface area of from 15 m.sup.2/g to 200 m.sup.2/g measured using nitrogen and the BET method according to ISO 9277:1995.

15. The puffed polysaccharide-based material according to claim 14, wherein the material provides: (i) an expansion index F of from 5 to 30; and/or (ii) a crispness of from 25 N to 50 N measured on a TA.HDplus Texture Analyser from Stable Micro Systems equipped with a Kramer Shear cell with 10 blades.

16. The process according to claim 7, wherein: (i) the volume medium grain diameter d.sub.50(vol) is in a range selected from the group consisting of 1.5 μm to 50 μm, 2 μm to 40 μm, and 2.5 μm to 7.0 μm; and/or (ii) the volume grain diameter d.sub.98(vol) is in a range selected from the group consisting of 4 μm to 100 μm, 6 μm to 80 μm, 8 μm to 60 μm and 10 μm to 30 μm.

17. The process according to claim 1, wherein the specific surface area is in a range selected from the group consisting of 27 m.sup.2/g to 180 m.sup.2/g, 30 m.sup.2/g to 160 m.sup.2/g, 45 m.sup.2/g to 150 m.sup.2/g and 48 m.sup.2/g to 140 m.sup.2/g.

18. The process according to claim 8, wherein the amount of the extrusion aid is in a range selected from the group consisting of 0.05 wt.-% to 5 wt.-%, 0.1 wt.-% to 2 wt.-% and 0.2 wt.-% to 1.8 wt.-%.

19. The process according to claim 9, wherein: (i) the mixture obtained in step (c) is heated to a temperature selected from the group consisting of: 105° C. to 140° C., 110° C. to 135° C. and 115° C. to 130° C.; and/or (ii) the extruder operates at a minimum pressure selected from the group consisting of 2.5 MPa, 3.5 MPa, 5 MPa, 5.5 MPa and 6 MPa; and/or (iii) the extruder operates at a maximum pressure selected from the group consisting of 8 MPa, 7.5 MPa, 6 MPa and 5 MPa.

20. The process according to claim 10, wherein: (i) the water is present in an amount selected from the group consisting of 0.01 wt.-% to 15 wt.-%, 0.1 wt.-% to 10 wt.-% and 0.2 wt.-% to 5 wt.-%; and/or (ii) the whole grains are present in an amount selected from the group consisting of 0.1 wt.-% to 30 wt.-%, 0.5 wt.-% to 20 wt.-% and 1 wt.-% to 15 wt.-%; and/or (iii) the amount of sucrose is selected from the group consisting of 0.01 wt.-% to 20 wt.-%, 0.1 wt.-% to 10 wt.-% and 0.2 wt.-% to 5 wt.-%; and/or (iv) the amount of sodium chloride is selected from the group consisting of 0.001 wt.-% to 5 wt.-%, 0.01 wt.-% to 2 wt.-% and 0.1 wt.-% to 1 wt.-%.

21. The extrusion aid according to claim 13, wherein: (i) the volume medium grain diameter d.sub.50(vol) is selected from the group consisting of 1.5 μm to 50 μm, 2 μm to 40 μm, and 2.5 μm to 7.0 μm; and/or (ii) the volume grain diameter d.sub.98(vol) is selected from the group consisting of 4 μm to 100 μm, 6 μm to 60 μm, 8 μm to 60 μm and 10 μm to 30 μm.

22. The extrusion aid according to claim 12, wherein the specific surface area is selected from the group consisting of 27 m.sup.2/g to 180 m.sup.2/g, 30 m.sup.2/g to 160 m.sup.2/g, 45 m.sup.2/g to 150 m.sup.2/g and 48 m.sup.2/g to 140 m.sup.2/g.

23. The puffed polysaccharide-based material according to claim 15, wherein: (i) the expansion index F is selected from the group consisting of 8 to 25, 10 to 20, and 12 to 18; and/or (ii) the crispness is selected from the group consisting of 30 N to 48 N, 32 N to 45 N and 35 N to 40 N.

Description

DESCRIPTION OF THE FIGURES

(1) FIG. 1: Diameter of the extrudate (snacks)

(2) FIG. 2: Diameter of the extrudate (cereals)

(3) FIG. 3: Expansion index (snacks)

(4) FIG. 4: Expansion index (cereals)

(5) FIG. 5: Crispness (snacks)

(6) FIG. 6: Photograph of extrudate (standard cereal)

(7) FIG. 7: Photograph of extrudate (cereals prepared with 0.5% of SRCC2)

(8) FIG. 8: Stereo microscope (SM) image of the cross section of extrudate (standard snack)

(9) FIG. 9: Stereo microscope (SM) image of the cross section of extrudate (cereals prepared with 0.5% of SRCC3)

EXAMPLES

(10) The scope and interest of the invention may be better understood on basis of the following examples which are intended to illustrate embodiments of the present invention. However, they are not to be construed to limit the scope of the claims in any manner whatsoever.

(11) (a) Measuring Methods

(12) In the following, the measuring methods for the parameters defined in the present application and used in the following examples are described.

(13) Particle Size Distribution

(14) The volume determined median particle size d.sub.50 (vol) and the volume determined top cut particle size d.sub.98 (vol) were evaluated using a Malvern Mastersizer 2000 Laser Diffraction System (Malvern Instruments Plc., Great Britain). The raw data obtained by the measurement was analysed using the Fraunhofer theory without specified refractive index, with an absorption index of 0.005. The methods and instruments are known to the skilled person and are commonly used to determine particle size distributions of fillers and pigments.

(15) Particle Size Distribution

(16) The weight determined median particle size d.sub.50 (wt) was measured by the sedimentation method, which is an analysis of sedimentation behaviour in a gravimetric field. The measurement was made with a Sedigraph™ 5120 of Micromeritics Instrument Corporation, USA. The method and the instrument are known to the skilled person and are commonly used to determine particle size distributions 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 sonicated.

(17) Specific Surface Area (SSA)

(18) The specific surface area was measured via the BET method according to ISO 9277:1995 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 Buchner 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.

(19) Intra Particle Intruded Specific Pore Volume (in cm.sup.3/g)

(20) The specific pore volume was measured using a mercury intrusion porosimetry measurement using a Micromeritics Autopore V 9620 mercury porosimeter having a maximum applied pressure of mercury 414 MPa (60 000 psi), equivalent to a Laplace throat diameter of 0.004 μm. The equilibration time used at each pressure step was 20 seconds. The sample material was sealed in a 5 cm.sup.3 chamber powder penetrometer for analysis. The data were corrected for mercury compression, penetrometer expansion and sample material compression using the software Pore-Comp (Gane, P. A. C., Kettle, J. P., Matthews, G. P. and Ridgway, C. J., “Void Space Structure of Compressible Polymer Spheres and Consolidated Calcium Carbonate Paper-Coating Formulations”, Industrial and Engineering Chemistry Research, 35(5), 1996, pp. 1753-1764).

(21) Expansion Index

(22) The expansion index F is a measure to describe the cross-sectional expansion of an extrudate after passing the outlet of an extruder. The expansion index used herein is defined as:
F=(D.sub.E/D.sub.D).sup.2
wherein D.sub.E denotes the diameter of the extrudate and D.sub.D denotes the nozzle diameter or the corresponding hole diameter of the die at the extruder outlet. Extrudate diameters were measured using a caliper. A high expansion index thus indicates a higher porosity and a lower density of the extrudate.
Crispness (TA.HDplus Texture Analyser)

(23) Samples are weighed so that equally defined portions are obtained. The amount must be such that at least half of the Kramer shear cell is filled volumetrically. The Kramer shear cell simulates a single bite on a sample and thus provides information about bite-behaviour, crispness and consistency. The 10 blades are moved with constant velocity through the sample, compressing, shearing and extruding the sample through the slotted base plate. Measuring of multiple blades at the same time results in measuring at different places in the sample (resistance in Newtons) for levelling out local structural differences. Measuring parameters are set out in the table below.

(24) TABLE-US-00002 T.A. Settings & Parameters Type of test: pressure Velocity for: 10.00 mm/s Velocity test: 8.00 mm/s Velocity back: 10.00 mm/s Target parameter: strain Strength: 100.0 g Path: 5.000 mm Strain: 105.0% Release: AUTO (force) Release force: 5.0 g Tool: HDP/KS10; KRAMER SHEAR CELL 10 BLADE Charge: C-DP-0749-0.5% Measuring points per second: 500
(b) Extrusion Aids

(25) The following mineral materials are used as extrusion aids or as corresponding reference materials.

(26) Surface-Reacted Calcium Carbonate 1 (SRCC1)

(27) SRCC1 had a d.sub.50 (vol)=6.6 μm, d.sub.98 (vol)=15.1 μm, SSA=144 m.sup.2/g with an intra-particle intruded specific pore volume of 0.811 cm.sup.3/g (for the pore diameter range of 0.004 to 0.23 μm).

(28) SRCC1 was obtained by preparing 450 litres of an aqueous suspension of ground calcium carbonate in a mixing vessel by adjusting the solids content of a ground marble calcium carbonate from Hustadmarmor, Norway, having a mass based median particle size distribution of 90% less than 2 μm, as determined by sedimentation, such that a solids content of 16 wt.-%, based on the total weight of the aqueous suspension, is obtained.

(29) Whilst mixing the slurry, 47.1 kg phosphoric acid were added in form of an aqueous solution containing 30 wt.-% phosphoric acid to said suspension over a period of 15 minutes at a temperature of 70° C. After the addition of the acid, the slurry was stirred for additional 5 minutes, before removing it from the vessel and drying.

(30) Surface-Reacted Calcium Carbonate 2 (SRCC2)

(31) SRCC2 had a d.sub.50 (vol)=2.98 μm, d.sub.98 (vol)=10.64 μm, SSA=97.55 m.sup.2/g with an intra-particle intruded specific pore volume of 0.723 cm.sup.3/g (for the pore diameter range of 0.004 to 0.18 μm).

(32) SRCC2 was obtained by preparing 10 litres of an aqueous suspension of ground calcium carbonate in a mixing vessel by adjusting the solids content of a ground limestone calcium carbonate from Omya SAS, Orgon, having a mass based median particle size distribution of 90% less than 1 μm, as determined by sedimentation, such that a solids content of 10 wt.-%, based on the total weight of the aqueous suspension, is obtained.

(33) Whilst mixing the slurry, 2.7 kg phosphoric acid was added in form of an aqueous solution containing 20 wt.-% phosphoric acid to said suspension over a period of 44 minutes at a temperature of 70° C. After the addition of the acid, the slurry was stirred for additional 5 minutes, before removing it from the vessel and drying.

(34) Surface-Reacted Calcium Carbonate 3 (SRCC3)

(35) SRCC3 had a d.sub.50 (vol)=6.13 μm, d.sub.98 (vol)=15 μm, SSA=55.5 m.sup.2/g with an intra-particle intruded specific pore volume of 0.739 cm.sup.3/g (for the pore diameter range of 0.004 to 0.41 μm).

(36) Starting Material: Limestone

(37) A calcium carbonate suspension is prepared by adding water and undispersed limestone (ground under wet conditions in water, optionally in the presence of a food approved dispersing or grinding aid such as monopropyleneglycol (MPG)) having a d.sub.50 (wt) of 3 μm, wherein 33 wt.-% of particles have a diameter of less than 2 μm in a 20 L stainless steel reactor, such that the aqueous suspension obtained has a solids content corresponding to 16 wt.-% by dry weight relative to the total suspension weight. The temperature of this suspension is thereafter is brought to and maintained at 70° C. Under stirring at approximately 1 000 rpm such that an essential laminar flow is established, phosphoric acid in the form of a 30% solution is added to the calcium carbonate suspension through a separate funnel over a period of 10 minutes in an amount corresponding to 30% by weight on dry calcium carbonate weight. Following this addition, the suspension is stirred for an additional 5 minutes. The resulting suspension was allowed to settle overnight, and the SRCC had a specific surface area of 36 m.sup.2/g, a d.sub.50 (vol) of 9.3 μm (Malvern) and d.sub.98 (vol) of 23.5 μm (Malvern).

(38) Starting Material: Marble

(39) A calcium carbonate suspension is prepared by adding water and undispersed marble (ground under wet conditions in water, optionally in the presence of a food approved dispersing or grinding aid such as monopropyleneglycol (MPG)) having a d.sub.50 (wt) of 3.5 μm, wherein 33 wt.-% of particles have a diameter of less than 2 μm in a 20 L stainless steel reactor, such that the aqueous suspension obtained has a solids content corresponding to 16 wt.-% by dry weight relative to the total suspension weight. The temperature of this suspension is thereafter is brought to and maintained at 70° C. Under stirring at approximately 1 000 rpm such that an essential laminar flow is established, phosphoric acid in the form of a 30% solution is added to the calcium carbonate suspension through a separate funnel over a period of 10 minutes in an amount corresponding to 30% by weight on dry calcium carbonate weight. Following this addition, the suspension is stirred for an additional 5 minutes. The resulting suspension was allowed to settle overnight, and the SRCC had a specific surface area of 46 m.sup.2/g, a d.sub.50 (vol) of 9.5 μm (Malvern) and d.sub.98 (vol) of 18.9 μm (Malvern).

(40) Starting Material: Marble

(41) A calcium carbonate suspension is prepared by adding water and undispersed marble of (ground under wet conditions in water, optionally in the presence of a food approved dispersing or grinding aid such as monopropyleneglycol (MPG)) having a d.sub.50 (wt) of 2 μm in a 20 L stainless steel reactor, such that the aqueous suspension obtained has a solids content corresponding to 16 wt.-% by dry weight relative to the total suspension weight. The temperature of this suspension is thereafter is brought to and maintained at 70° C. Under stirring at approximately 1 000 rpm such that an essential laminar flow is established phosphoric acid in the form of a 30% solution is added to the calcium carbonate suspension through a separate funnel over a period of 10 minutes in an amount corresponding to 50% by weight on dry calcium carbonate weight. Following this addition, the suspension is stirred for an additional 5 minutes. The resulting suspension was allowed to settle overnight, and the SRCC had a specific surface area of 71 m.sup.2/g, a d.sub.50 (vol) of 10.6 μm (Malvern) and d.sub.98 (vol) of 21.8 μm (Malvern).

(42) Ground Natural Calcium Carbonate (GNCC1)

(43) GNCC1 was a food-grade high purity natural calcium carbonate, commercially available from Omya International AG, Switzerland, d.sub.50 (wt)=5.5 μm.

(44) (c) Examples: Snack and Cereal Extrusion

(45) For the purpose of the following examples, commercially available standard corn flour was purchased from Bäko eG, Germany. Roland Mehl Typ 550 and Grüner Roland Typ 1050 were used as wheat cereals and were purchased from Bremer Rolandmühle Erling GmbH & Co. KG, Germany.

(46) (i) Equipment

(47) Twin-screw extruder DNDL-44, from Bühler AG, Uzwil, Switzerland, with the following parts:

(48) Housing:

(49) Number of housings: 5 (where 4 D=0.176 m) Housings separately or connectedly heatable or coolable Heating medium: steam Cooling medium: water Processing length: 20 D (1 D=0.044 m)
Screw: Twin-screw Worm gear shaft rotating in the same direction Twin-screw diameter: 44 mm Twin-screw length (without coupling): 0.88 m (corresponds to 20 D) Screw speed: 60 to 450 rpm Standard screw configuration:

(50) TABLE-US-00003 Mix- Pres- Feeder ing Conv. sure Temp. Shear Zone Amount/ /// / \\ / /// /// // // \ / \ /// Dir. Gradient 66 44 poly 66 44 33 44 44 44 33 [°] Length 66 44 20 66 44 33 15 15 15 33 [mm] Offset [°] — — — —  0  0 90 90 90 90

(51) The feeder zone consisted of 3 elements DNDL 66/R66 and 1 element DNDL 44/R44, the mixing zone consisted of 2 elements of DNDL P45-4/L20, the conveying zone consisted of 1 element of DNDL 66/R66, the pressure zone consisted of 6 elements of DNDL 44/R44e, the temperature zone consisted of 4 elements of DNDL 33/R33, and the shear zone consisted of 6 elements: 1 element of DNDL 44/L14.7, 1 element of DNDL 44/R14.7, 1 element of DNDL 44/L14.7 and 3 elements of DNDL 33/L33.

(52) Cutting Device:

(53) Movable Cutter head with 4 blades
Extrusion Dies:

(54) TABLE-US-00004 Die Hole Cross-sect. Die Cross-sect. form diam. area form Hole diam. area 2 × 3.3 mm 17.1 mm.sup.2 1 × 3.0 mm 14.1 mm.sup.2 1-hole 2-hole 2 × 5.0 mm 39.2 mm.sup.2 1 × star shaped ca. 60 mm.sup.2  1-hole 2-hole 2 × 3.0 mm 84.8 mm.sup.2 6-hole 2 × 2.0 mm 62.8 mm.sup.2 1 × 3.0 mm  3.9 mm.sup.2 10-hole 2-hole 2.0 mm 2 × 1.0 mm 18.8 mm.sup.2 (tube) 12-hole
Feed (Product Feed): Twin-screw feed device Volumetric feed (metering unit with container)
(ii) Process and Product Parameters: Snacks Product: snacks Final screw: cone-shaped Die: 1×2-hole (diameter: 3 mm) Recipe:

(55) TABLE-US-00005 Ingredients Corn flour Sugar Salt SRCC Total Standard Amount % 98.00 1.00 1.00 0.00 100.00 Amount kg 29.40 0.30 0.30 0.00 30.00 SRCC Amount % 97.50 1.00 1.00 0.50 100.00 0.5% Amount kg 14.63 0.15 0.15 0.08 15.00 SRCC Amount % 96.50 1.00 1.00 1.50 100.00 1.5% Amount kg 14.48 0.15 0.15 0.23 15.00 SRCC Amount % 96.00 1.00 1.00 2.00 100.00 2.0% Amount kg 14.40 0.15 0.15 0.30 15.00 SRCC Amount % 93.00 1.00 1.00 5.00 100.00 5.0% Amount kg 13.95 0.15 0.15 0.75 15.00 SRCC Amount % 88.00 1.00 1.00 10.00 100.00 10.0% Amount kg 13.20 0.15 0.15 1.50 15.00 Process parameters:

(56) TABLE-US-00006 Sample No. SRCC1 SRCC1 SRCC2 SRCC2 Standard 0.5% 1.5% 0.5% 1.5% Torque [%] 44 46 52 47 47 Speed [%] 50 50 50 50 50 Blade speed 33 33 33 33 33 [%] H.sub.2O 3.9 3.9 3.9 3.9 3.9 addition [kg/h] Product 33 33 33 33 33 dosing [kg/h] Pressure 45-50 45-50 50 45-50 45-50 [bar] Temp. 100 100 100 100 100 module 2 [° C.] Temp. 110 110 110 110 110 module 3 [° C.] Temp. 125 125 125 125 125 module 4 [° C.] Temp. 125 125 125 125 125 module 5 [° C.] Sample No. SRCC3 SRCC3 SRCC3 SRCC3 SRCC3 0.5% 1.5% 2.0% 5.0% 10.0% Torque [%] 46 49 50 54 67 Speed [%] 50 50 50 50 50 Blade speed 33 33 33 33 33 [%] H.sub.2O 3.9 3.9 3.9 3.9 3.9 addition [kg/h] Product 33 33 33 33 33 dosing [kg/h] Pressure 45-50 50 51 51-55 30 [bar] Temp. 100 100 100 100 100 module 2 [° C.] Temp. 110 110 110 110 110 module 3 [° C.] Temp. 125 125 125 125 125 module 4 [° C.] Temp. 125 125 125 125 125 module 5 [° C.]
(iii) Process and Product Parameters: Cereals Product: cereals Final screw: cone-shaped Die: 1×2-hole (diameter: 3 mm) Recipe:

(57) TABLE-US-00007 Wheat Wheat whole Ingredients flour grain Sugar Salt SRCC Total Stan- Amount % 82.50 10.00 7.00 0.50 0.00 100.00 dard Amount 24.75 3.00 2.10 0.15 0.00 30.00 kg SRCC Amount % 82.00 10.00 7.00 0.50 0.50 100.00 0.5% Amount 12.30 1.50 1.05 0.08 0.08 15.00 kg SRCC Amount % 81.00 10.00 7.00 0.50 1.50 100.00 1.5% Amount 12.15 1.50 1.05 0.08 0.23 15.00 kg SRCC Amount % 80.50 10.00 7.00 0.50 2.00 100.00 2.0% Amount 12.08 1.50 1.05 0.08 0.30 15.00 kg SRCC Amount % 78.50 10.00 7.00 0.50 5.00 100.00 5.0% Amount 11.78 1.50 1.05 0.08 0.75 15.00 kg SRCC Amount % 72.78 10.00 7.00 0.50 10.00 100.00 10.0% Amount 10.88 1.50 1.05 0.08 1.50 15.00 kg Process parameters:

(58) TABLE-US-00008 Sample No. SRCC1 SRCC1 SRCC2 SRCC2 Standard 0.5% 1.5% 0.5% 1.5% Torque [%] 40 55 57 54 53 Speed [%] 52 52 52 52 52 Blade speed 34 34 34 34 34 [%] H.sub.2O 1.2 1.2 1.2 1.2 1.2 addition [kg/h] Product 35 35 35 35 35 dosing [kg/h] Pressure 41 53 55-60 55 55 [bar] Temp. 100 100 100 100 100 module 2 [° C.] Temp. 110 110 110 110 110 module 3 [° C.] Temp. 125 125 125 125 125 module 4 [° C.] Temp. 135 135 135 135 135 module 5 [° C.] Sample No. SRCC3 SRCC3 SRCC3 SRCC3 SRCC3 0.5% 1.5% 2.0% 5.0% 10.0% Torque [%] 46 51 54 56 54 Speed [%] 52 52 52 52 52 Blade speed 34 34 34 34 34 [%] H.sub.2O 1.2 1.2 1.2 1.2 1.2 addition [kg/h] Product 35 35 35 35 35 dosing [kg/h] Pressure 48 42 53 54 38 [bar] Temp. 100 100 100 100 100 module 2 [° C.] Temp. 110 110 110 110 110 module 3 [° C.] Temp. 125 125 125 125 125 module 4 [° C.] Temp. 135 135 135 135 135 module 5 [° C.]
(d) Results

(59) FIGS. 1 to 5 show the results for the diameter of the extrudate (FIG. 1: snacks, FIG. 2: cereals), the expansion index (FIG. 3: snacks, FIG. 4: cereals), and the crispness of snacks (FIG. 5).

(60) FIGS. 6 and 7 show photographs of standard cereals (FIG. 6) and of cereals prepared in the presence of 0.5% SRCC2 (FIG. 7).

(61) FIGS. 8 and 9 show stereo microscope (SM) images of the cross section of a standard snack (FIG. 8) and of a snack that was prepared in the presence of SRCC3-0.5% (FIG. 9). The images were made with a Leica MZ16A stereo microscope and a Leica DFC 320 camera and angled light illumination to show the structure of the samples.

(62) Organoleptic panel tests were carried out for the produced snacks as well as for the produced cereals. The organoleptic panel consisted of 6 persons, all trained according to DIN 10961. Tables 1 and 2 show the results obtained for snacks and cereals, respectively.

(63) TABLE-US-00009 TABLE 1 results of organoleptic panel test for snacks Colour Surface Crispness Bite Standard yellow hard very crispy fluffy, sharp-edged SRCC1 yellow slightly finer Crispy fluffy, 0.5% sharp-edged SRCC1 yellow finer crispy fluffy, 1.5% sharp-edged SRCC2 yellow coarser crispy fluffy, 0.5% sharp-edged SRCC2 yellow finer crispy fluffy 1.5% SRCC3 yellow coarser crispy fluffy 0.5% SRCC3 yellow coarser crispy fluffy 1.5% SRCC3 brighter finer less crispy less 2.0% sharp-edged SRCC3 brighter very fine not at all fast gone 5.0% crispy SRCC3 much brighter very fine not at all sticky, 10.0% crispy adherent Chewing Mouthfeel impression Taste Smell Standard sticky first airy, corn corn, neutral then sticky SRCC1 more sticky sticky corn corn, neutral 0.5% SRCC1 more sticky sticky corn corn, neutral 1.5% SRCC2 more sticky sticky corn corn, neutral 0.5% SRCC2 less sticky sticky, cross corn corn, neutral 1.5% SRCC3 sticky very airy corn corn, neutral 0.5% SRCC3 sticky airy, sticky corn corn, neutral 1.5% SRCC3 sticky less airy slightly salty corn, neutral 2.0% SRCC3 sticky floury corn corn, neutral 5.0% SRCC3 shrill sticky, neutral sweet 10.0% paste-like

(64) TABLE-US-00010 TABLE 2 results of organoleptic panel test for cereals Colour Surface Crispness Bite Standard slightly uneven crispy, fast gone brownish fast gone SRCC1 brighter more uniform more crispy faster gone 0.5% SRCC1 brighter more uniform more crispy faster gone 1.5% SRCC2 standard slightly crispy, more crispy 0.5% uneven fast gone SRCC2 brighter relatively fine more crispy 3 to 4 times 1.5% to chew SRCC3 standard uneven standard standard 0.5% SRCC3 brighter more uniform crispy, fast 1 to 2 times 1.5% gone to chew SRCC3 brighter more uniform no difference no difference 2.0% SRCC3 brighter uniformly crispy, fast gone 5.0% rough very fast gone SRCC3 very bright very fine crispy fast gone 10.0% pores Chewing Mouthfeel impression Taste Smell Standard sticky, sticky, whole grain roasty fast gone fast gone SRCC1 sticks at sticks at teeth whole grain no difference 0.5% teeth SRCC1 dryer dryer whole grain no difference 1.5% SRCC2 standard longer crispy whole grain no difference 0.5% SRCC2 hygroscopic hygroscopic no off-flavour no difference 1.5% SRCC3 standard crispy, no off-flavour no difference 0.5% fast gone SRCC3 slightly 1 to 2 times no off-flavour no difference 1.5% stickier to chew SRCC3 no difference fast gone no off-flavour no difference 2.0% SRCC3 fast gone fast gone no off-flavour no difference 5.0% SRCC3 very sticky, very sticky, like popcorn no difference 10.0% hard hard

(65) The results of the present examples indicate an increased expansion index (F) and improved crispness (TA.HDplus Texture Analyser) for the products prepared according to the inventive process compared with the samples prepared from standard calcium carbonate (GNCC1) which were prepared analogously (see FIGS. 1 to 5). Furthermore, the organoleptic panel test revealed improved surface textures and crispness (see the foregoing tables).