Edible fat powders

Abstract

The invention relates to an edible fat powder comprising at least two natural fats wherein the natural fat has a N10 of at least 10% and wherein the fat powder is a co-crystallized fat powder. The invention further relates to the use of said fat powder to prepare a fat containing emulsion. The invention also relates to a process for the preparation of said edible fat powder wherein the edible fat powder is prepared from a molten mixture comprising at least two natural fats.

Claims

1. Process for the preparation of an edible fat powder, which process comprises the steps of: Preparing a mixture of at least two fats which have not been interesterifed with each other having a N10 of at least 10%, each fat being present in an amount of at least 20%; and spraying a CO2-melt mixture of the fats having dissolved CO2 into a vessel to form the fat powder.

Description

(1) FIG. 1 is a schematic representation of the set up for the batch wise production of edible fat powder as used for the preparation of fat powder examples 1 to 14. The comparative fat powders were blended from these powders.

(2) The set-up consists of an autoclave (6) with a content of 600 ml (Premex Reactor AG HPM-PT-060, Wno. 14571, Art no. PT.060.462.45, ex Premex, CH) equipped with a mechanical stirrer (7) (six blade propeller stirrer, length 10.6 cm, 1 cm1 cm blades of 1.5 mm thick). The autoclave has connections at the top and at the bottom. The top connection (8) was used to pressurize the system with CO2. The mixture from the vessel is expelled from the bottom of the autoclave via tube (10) through valve (9) over nozzle (2) (orifice 0.34 mm SIA80/core SKA16/cap CPP37729-SS, ex Spraying Systems, Ridderkerk, NL) to about atmospheric pressure in an expansion vessel (1) (main section: height 26.1 cm and diameter 60 cm, conical bottom part: height 37 cm and diameter from 60 cm to 15 cm). The dimensions of the tube between the bottom of the autoclave and the nozzle are (3 cm vertical, 20 cm horizontal, 3 cm vertical, 4 mm inner diameter, 6 mm outer diameter).

(3) The autoclave is heated with an oil bath with heat transfer fluid. Tube (10) and nozzle (2) are kept at the desired temperature by heating tape (1.5 meters/5 mm wide Isopad SiS-10 CE/SN:02401022774/PN:328552-000, from Isopad BV/Tyco Thermal, Wijk bij Duurstede, NL) using a Thyristor to adjust the temperature of the heating tape.

(4) The expansion vessel is cooled with additional CO2 over inlet (3). A small barrel (5) (15 liters, model 729348-90, from Vink, Lisse, NL) for collection of the sprayed powder is mounted at the bottom of the expansion vessel. The gas in the expansion vessel leaves the vessel via a tube shaped membrane filter (4) (polypropylene, length 25.5 cm, outer diameter 6 cm, inner diameter 2.5 cm) thereby keeping the pressure inside the expansion vessel at atmospheric pressure.

(5) Preparation of Fat Powders

(6) The system (i.e. autoclave) was adjusted to the desired temperature and pressure. The temperature of tube (10) and nozzle (2) was set at a temperature above the melting temperature of the fat mixture using the Thyristor. The fat mixture (300 gram) was melted and the melted fat mixture was then poured into the autoclave. The autoclave was closed and the mixture was stirred with the mechanical stirrer at the desired speed. Liquid CO2 was added over connection (8) in steps of 30 bar till the desired working pressure is reached and the system was left till a steady state condition was reached (i.e. constant pressure and temperature, see Table 2). The expansion vessel was cooled to the desired temperature with CO2 gas over inlet (3). The CO2-melt mixture was expanded (i.e. sprayed) over nozzle (2) to atmospheric pressure in expansion vessel (1) and external CO2 gas (3) at the top of the expansion vessel was used for additional cooling to keep the expansion vessel at the desired temperature. Upon expansion of the CO2-melt mixture into the expansion vessel the evaporation of dissolved CO2 and the entrainment of CO2 into the spray caused crash-cooling conditions, which lead to very rapid solidification. The resulting powder was collected in barrel (5) below the expansion vessel and stored at a temperature of minus 20 degrees Celsius. The gas left the expansion vessel via membrane filter (4). The temperature and the pressure as measured in the autoclave dropped upon expansion (as mentioned in Table 2).

(7) Fat powder examples 1 to 8 are co-crystallized fat powders made from a mixture of two fats (see Table 2). Fat powder examples 9 to 14 are single crystallized fat powders made from a single fat (see Table 2). Fat powders 9 to 14 were used to blend fat powder comparative examples C1 to C7 (containing two fats, but not co-crystallized) (see Table 3).

(8) TABLE-US-00002 TABLE 2 Prepared fat powders Ex. Fat Mix A B C D E 1 35 wt % mfPOs/ 350, 57, 180 379 243, 21.8 84 1026 65 wt % PK 2 50 wt % mfPOs/ 350, 64, 180 285 Nm nm 1087 50 wt % PK 3 65 wt % mfPOs/ 350, 65, 180 337 Nm nm 1058 35 wt % PK 4 20 wt % full 350, 60, 180 367 234, 22.3 90 929 hydro PO/ 80 wt % full hydro PK 5 50 wt % dfPOs/ 350, 51, 180 361 232, 21.2 92 1165 50 wt % PK 6 50 wt % indfPOs/ 350, 51, 180 399 232, 23.2 94 1014 50 wt % PK 7 40 wt % full 350, 51, 180 375 235, 21.4 93 987 hydro PO/ 60 wt % full hydro PK 8 35 wt % mfPOs/ 350, 67, 180 355 220, 23.7 88 844 65 wt % dfPKs 9 dfPOs 350, 62, 183 337 232, 21.6 97 966 10 PK 350, 51, 180 392 234, 22.4 92 1130 11 indfPOs 350, 57, 183 376 230, 22.2 88 928 12 Full hydro PO 350, 62, 180 330 255, 21.2 63 959 13 Full hydro PK 350, 49, 180 368 242, 22.7 89 1035 14 mfPOs 350, 62, 183 328 243, 22.2 62 903 mfPOsmulti-fractionated palm oil stearin (top fraction of a multi-stage fractionation process); PKPalm kernel oil; Full hydro POfully hydrogenated palm oil; Full hydro PKfully hydrogenated palm kernel oil; dfPOsdry fractionated palm oil stearin (top fraction of a palm oil fractionation process); indfPOsinteresterified dry fractionated palm oil stearin; dfPKs: top fraction of palm kernel oil from a dry fractionation process AAutoclave: mixing speed (rpm), temperature (degrees Celsius), pressure (bar) BMass flow CO2 to autoclave (gram) CSpray time (min-sec), temperature of expansion vessel (degrees Celsius) DPowder yield (obtained powder/used fat, wt %) ETotal mass flow CO2 for autoclave plus cooling (gram)

(9) TABLE-US-00003 TABLE 3 Comparative fat powder examples TAG's (wt %) Reference as in G1 + G4 + Ex. Blend of prepared fat powder Table 2 G3 G7 P/S C1 35 wt % mfPOs + 65 wt % PK 14 + 10 28 18 11 C2 50 wt % mfPOs + 50 wt % PK 14 + 10 38 18 13 C3 65 wt % mfPOs + 35 wt % PK 14 + 10 50 18 15 C4 20 wt % fully hydro PO + 80 wt 12 + 13 33 33 1 % fully hydro PK C5 50 wt % dfPOs + 50 wt % PK 9 + 10 22 30 8 C6 50 wt % indfPOs + 50 wt % PK 11 + 10 18 31 8 C7 40 wt % fully hydro PO + 60 wt 12 + 13 49 25 1 % fully hydro PK

(10) The P over S ratio represents the Palmitic over Stearic fatty acid content in the TAG's. The TAG's of the corresponding blends of the fat powder examples 1 to 8 in Table 2 are identical to the comparative fat powder examples in Table 3 having the same fat blend composition.

(11) TABLE-US-00004 TABLE 4 Physical data of edible fat powder examples 1 to 14 and comparative fat powder examples C1 to C7 Ex. FWHM 1 0.576 2 0.555 3 0.516 4 0.671 5 0.507 6 0.474 7 0.874 8 0.532 9 0.387 10 0.412 11 0.387 12 0.458 13 0.554 14 0.411 C1 2-peak C2 2-peak C3 2-peak C4 2-peak C5 2-peak C6 2-peak C7 2-peak
Preparation of Spreads

(12) Spreads with a composition as in Table 5 were made according to the methods as described below using the edible fat powders of examples 1 to 8 and comparative fat powder examples C-1 to C-7 (see Table 6).

(13) TABLE-US-00005 TABLE 5 Spreads compositions Composition A1 Composition A2 Composition B (parts) (parts) (parts) AQUEOUS PHASE Tap water 66.440 66.429 54.606 Starch 4.000 4.000 Buttermilk 0.100 0.100 0.150 powder NaCl 1.000 1.000 0.015 Potassium 0.130 0.130 0.090 sorbate dfPOfIV55 1.400 1.400 Sunflower oil 1.600 1.600 1.500 Dimodan HP 0.300 0.300 0.100 TOTAL 74.97 74.959 56.461 citric acid 0.030 (pH 5.20) 0.030 (pH 5.20) 0.022 (pH 5.14) FAT PHASE Sunflower oil 20.369 22.153 37.490 Fat powder 4.471 2.794 5.850 Colorant 0.144 0.048 0.166 Flavor 0.016 0.016 0.011 TOTAL 25 25.011 43.517 Starch: Merigel 341, modified pre-gelled waxy corn starch (hydroxypropyl distarch) ex Tate & Lyle Europe (pre-gelled starch, needs to be dispersed at 40 to 50 degrees Celsius at low shear) Dimodan HP: molecularly distilled mono/diacylglyceride mixture derived from fully hardened palm oil (90% monoglyceride) ex Danisco, DK dfPOfIV55: fractionated Palm Oil with iodine value of 55

(14) TABLE-US-00006 TABLE 6 Spreads and fat powders used Spread example Fat power used Composition used 1 1 Composition B 2 2 Composition B 3 3 Composition B 4 4 Composition B 5 5 Composition A1 6 6 Composition A1 7 7 Composition A2 8 4 Composition A2 9 8 Composition A2 C1 C1 Composition B C2 C2 Composition B C3 C3 Composition B C4 C4 Composition B C5 C5 Composition A1 C6 C6 Composition A1 C7 C7 Composition A2

Spreads Examples 1 to 4 and Comparative Spreads Examples C1-C4

(15) First 24.489 parts (538.76 g) of hot water (80 degrees Celsius) was mixed with 0.150 parts (3.30 g) of butter milk powder, 0.015 parts (0.33 g) of salt and 0.090 parts (1.98 g) of K-sorbate by dispersing the ingredients in the water using the Ultra-turrax.

(16) Then 1.5 parts (33 g) of oil was weighed and together with 0.1 parts (2.20 g) of the emulsifier (Dimodan HP) gently heated to 75 degrees Celsius in a steel can while stirring, followed by adding this blend to the hot water phase part, while using the turrax. The mixture was homogenised and pasteurised using the turrax for 5 to 10 minutes.

(17) The remaining cold part of the water 30.117 parts (662.57 g) was added to the hot water phase while using the turrax, ending up at about 30 degrees Celsius and the pH was adjusted to about 5.2 by slowly adding citric acid.

(18) 37.490 parts (824.78 g) of cold oil was mixed with 0.166 parts (3.65 g) of -carotene (0.4% dispersion) and 0.011 parts (0.24 g) of flavour and added as a fourth step to the emulsion while using the turrax resulting in a homogenous oil in water emulsion.

(19) This finely dispersed oil in water emulsion was then poured in to the Esco-Labor (ESCO-double wall Vacuum mixer processing plant Type EL3 with 4.5 liter vessel in pharmaceutical version, ex ESCO-Labor AG, CH) which was cooled at about 5 degrees Celsius using a cooling machine (Huber HS40 thermostated at 4 degrees Celsius), followed by deaeration for about ten minutes.

(20) Then 5.85 parts (128.70 g) of the edible fat powder was weighed using a pre-cooled (5 degrees Celsius) steel can and scoop and added to the oil in several steps via a funnel at the bottom of the Esco-Labor. The powder was sucked into the mixture using vacuum. After pouring the slurry into a pre-cooled can of 5 degrees Celsius, it was made homogeneous and smooth by applying the Ultra-turrax (T 50 basic ULTRA-TURRAX, ex IKA Werke GmbH & Co. KG, DE) for a few minutes at the lowest level of shear, ending at about 8 degrees Celsius.

(21) The mixture was poured into the feed tank of the spreads production line and product was finished by pumping the mixture at about 14 kg/h through a pin stirrer operating at 2400 rpm, with an internal volume of 75 ml and 4 rows of pins on the stator and on the rotor. The inlet temperature was about 13 degrees Celsius and the outlet temperature was about 16 degrees Celsius. The resulting thick and white water in oil emulsion was filled in 200 ccm tubs followed by storage at 5 degrees Celsius.

(22) TABLE-US-00007 TABLE 7 Spreads processing conditions for spreads examples 1 to 4 and comparative spreads examples C1 to C4 Example 1 2 3 4 C1 C2 C3 C4 Flow (kg/hr) 14.4 14.0 14.0 16.1 14.5 14.0 14.0 17.3 Line Pressure 0.8 2.4 3.0 2.0 1.0 2.3 2.6 1.9 (bar) Temp, inlet 14.6 13.4 12.6 14.8 13.3 12.9 12.8 14.6 mixer* ( C.) Temp, after 17.8 16.3 15.6 18.4 17.3 15.8 16.5 18.5 mixer* ( C.) *mixer is a 75 ml pin stirrer with 4 rows of pins on stator and on rotor

Examples 5 to 9 and Comparative Examples C5 to C7

Slurry Preparation

(23) First 1.8 kg of a slurry was made by dispersing the fat powder in cold sunflower oil of about 5 degrees Celsius, while degassing under vacuum.

(24) The oil was weighed and pre-cooled to 5 degrees Celsius in an Esco-Labor (ESCO-Vacuum mixer processing plant Type EL3 with 4.5 liter vessel in pharmaceutical version, ex ESCO-Labor AG, CH). The powder was weighed using a pre-cooled (5 degrees Celsius) vessel and scoop, and added to the oil in several steps via a funnel on top of the Esco-Labor. The powder was sucked stepwise into the oil using vacuum. After each step a valve under the funnel was closed and the pressure dropped significantly. The density of the final slurry was measured to check if the de-aeration process was completed. Sometimes lumps were formed. After pouring the slurry into a pre-cooled can of 5 degrees Celsius, it was made homogeneous and smooth by applying an Ultra-turrax (T 50 basic ULTRA-TURRAX, ex IKA Werke GmbH & Co. KG, DE) for a few minutes at the lowest level of shear.

(25) Slurry Phase

(26) Colorant and flavor were added to the slurry as prepared above and the slurry was brought into the fat feed tank of the spreads production line.

(27) The fat feed tank is a double walled stainless steel vessel with an internal diameter of 125 mm and a height of 310 mm, equipped with a ribbon stirrer, pushing the product downwards to the outlet opening in the bottom of the tank. The tank is thermo-stated at 5 degrees Celsius.

(28) Aqueous Phase

(29) The aqueous phase was prepared by mixing three phases (I), (II) and (III).

(30) Phase I being a mixture of about 70% of the water and the starch was prepared in the standard way and cooled to 60 degrees Celsius. Phase II being a mixture of the remainder of the water, Salt, Potassium Sorbate and Butter Milk Powder, was prepared at 75 degrees Celsius and subsequently pasteurized at 75 degrees for 10 minutes. Phase III being a mixture at 80 degrees Celsius of dfPOflV55, a small part of the oil and the emulsifier. The three phases were mixed and the pH adjusted to the desired pH with citric acid by using the Ultra Turrax operating at about 8000 rpm.

(31) Then the mixture was poured into the aqueous feed tank of the spreads production line. The aqueous feed tank is a double walled stainless steel vessel, equipped with an agitator, thermo-stated at 57 degrees Celsius.

(32) Spreads Production

(33) The spreads were made by pumping the content of the fat feed tank and of the aqueous phase feed tank via a junction in to a 75 ml double walled stainless steel pin stirrer, with two rows of 4 stator and rotor pins. The fat phase increasing in temperature up to about 16 degrees Celsius in line just before the junction point, due to heat generated in the fat pump and due to ambient conditions and length of feeding pipes. The aqueous phase being cooled inline down to about 8 degrees Celsius prior to mixing with the fat phase.

(34) Initially the fat phase was pumped into this system including the pin stirrer to fill it completely. Then both phases were pumped into the system at the required ratio using 2 gear pumps. After the junction point the mixture is pumped at about 16 kg/h, into the pin stirrer, which results in a residence time of 17 seconds in the stirrer. The pin stirrer is thermo-stated at 14 degrees Celsius and operated at 2800 rpm.

(35) The final product was filled into 150 ml plastic tubs and stored at 5 degrees Celsius.

(36) TABLE-US-00008 TABLE 8 Spreads processing conditions for examples 5 to 9 and comparative examples C5 to C7 Flow Flow Temp. Temp. Temp. Temp. Mois- fat aqueous fat aqueous pin pin ture phase phase phase # phase # stirrer stirrer content Ex. (kg/hr) (kg/hr) ( C.) ( C.) in ( C.) out ( C.) (wt %) 5 4 12 16.9 7.9 12.6 15.2 67.7 6 4 12 15.9 9.5 12.6 15.4 68.4 7 4 12 nm 8.6 12.5 15.2 67.3 8 4 12 21.5 8.8 10.8 15.9 67.7 9 4 12 19.5 9.0 11.0 15.5 67.6 C5 4 12 17.6 8.1 11.7 14.8 68.5 C6 4 12 15.9 8.8 13.0 15.1 67.6 C7 4 12 nm 8.9 11.9 15.0 66.2 # As measured at the junction point.
Results

(37) The hardness, spreadibility, free water and the droplet size (D3,3) after stabilization at 5 degrees Celsius as well as after a heat stability test at 30 degrees Celsius and re-stabilization at 5 degrees Celsius was determined for each of the spreads according to the methods as described above.

(38) TABLE-US-00009 TABLE 9 Spreads analyses Free D3,3 5 degrees D3,3 30/5 degrees Ex. Hardness Spreadibility water Celsius @ Celsius @@ 1 15 0.5 0.5 13 16 2 28 1 0 6 7 3 29 1 0 7 7 4 62 1 0 7 7 5 61 1 0 8 38 6 130 1.5 0.5 7 51 7 59 1 0 7 7 8 67 1 0 8 10 9 72 1 0 8 44 C1 Too soft Too soft 3 21 Free oil C2 18 1.5 0 8 9 C3 18 1 0.5 8 8 C4 74 1.5 0 7 7 C5 42 3.5 3.5 65 Free water C6 18 2.5 4 59 100 C7 58 1 0 7 7 @ D3,3 determined after stabilization at 5 degrees Celsius. @@ D3,3 determined after a heat stability test at 30 degrees Celsius and re-stabilization at 5 degrees Celsius.