CH627778A5 - Process for accelerating the solidification of fats or fat-containing compositions - Google Patents

Description

The invention relates to a process for accelerating the solidification of fats or fat-containing preparations, which is characterized in that at least one finely powdered monoacid triglyceride or symmetrical triglyceride of saturated fatty acids of chain length Ciò to C20 is used as the solidification accelerator as substances remaining in solid form without melting or redissolving in the still molten fat melt before it forms its own fat crystals.

After the solidification accelerator has been added, the conditions for the solidification of the fats or fat-containing preparation are generally observed, which are carried out by the manufacturer for the respective products. B. static solidification below the solidification temperature at a constant or falling temperature or cooling at a constant or falling temperature or cooling at a constant or falling temperature with stirring, kneading, etc.

In addition to the substantial acceleration of solidification, the process also achieves improved solidification and products that are stable in storage. It is essential that when carrying out the process and the subsequent solidification, the conditions are selected for the respective product under which there is no or no significant melting, melting of the accelerators or their dissolution in the product.

It has been shown that the triglycerides mentioned, added under process conditions, have a very low solubility in the solidification of the products and, in a striking manner, approximately the same low solubility.

Since the melting temperatures of the products are different and accordingly the solidification is carried out at different temperatures, it is advisable to select such solidification accelerators whose melting point is 20 ° C. or more above the solidification temperature of the product.

The known melting points of the ß-forms or ß-rich forms can serve as a guide in the selection, so

627 778

that tricaprine with col. 29 to 29.8 and trilamine with col. 43 to 43.7 especially for very low melting, trimyristin with col. 53 to 53.5 and especially tripalmitin with col. 61 to 62.0 and tristearin with Sp. 67 to 67.9 are appropriate for higher melting but also for lower melting fats. As a result, the solidification accelerators added as finely divided solid bodies are coexistent in the still liquid melt. They are therefore able to immediately initiate the solidification crystallization of the fat melt, ie at a point in time when there are still no fat crystals from the actual melt.

Since, regardless of the particle size, each individual triglyceride crystal emits an inoculation pulse, the smaller the particle size, the greater the effect of a given additional amount (amount by weight), because the number of particles is inversely related to its size.

Products which are solid or predominantly solid at room temperature and which contain fats and / or oils which inhibit crystallizers or delay solidification, which are typical of lipids, are suitable as fats or preparations containing fat.

In the field of food, examples are chocolate, icing, couverture and the like. a. Dietary fats such as coconut and palm fats, shortenings, fatty lecithin preparations, etc., in the medical field fatty or coated tablets, suppositories and the like. a. in the field of feed, certain milk exchange feed, fattening feed and many others.

The shortening of the solidification time can be demonstrated by various methods. In addition to a generally customary examination of the consistency as a function of time by penetration measurements, the measurement method described below is well suited for a quantitative statement about the mode of action of the solidification accelerators to be used according to the invention. Here, the fat melt is first pretreated under defined conditions (both thermally and mechanically) and then cooled to a preselected solidification temperature in a measuring kneader with completely uniform stirring. Any resistance that the kneading blades find in the fat melt to be examined or its preparation manifests itself as a reactive force in the housing of the drive motor, which tries to rotate in the opposite direction to the direction of rotation of the motor. These torques are transferred to a writing device via a lever system and registered as a force / time diagram (Brabender-Farinograph measuring trough S 300 N). In this way, it is possible to determine the time it takes for a fat melt at a given solidification temperature to assume a defined degree of solidification, which is expressed as an increase in torque in the dimension meter-pond (mp).

This device, which was developed for another purpose, namely for measuring the consistency and toughness of batter, therefore allows - after increasing and refining the measuring range of the registration device - a meaningful and reproducible measurement that was not previously available in practice.

This test procedure allows an objective tracking and assessment of the solidification process of fat melts and thus also a quantitative evaluation of all additives that influence the solidification process.

Example 1 (comparison)

500 g cocoa mass of the varieties "Ghana", "Arriba", "Trinidad" and "Bahia" were melted in the measuring mixer S 300 N (Bra-bender) at 55 ° C (thermostat 1.60 minutes), then the mixer was kneaded switched on, and stirred for 60 minutes while maintaining the temperature (TI = 55 ° C). After that was

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switched to the thermostat 11, which cools the kneader to the preselected solidification temperature of exactly 28.0 ° C and keeps this temperature constant for the duration of the actual measurement. After a slight increase in torque at the beginning of the cooling phase, the force-time diagram initially runs horizontally as a result of the cooling. Depending on the quality of the cocoa mass, due to the different solidification properties of the cocoa fat contained in it ("solidification joy"), after a slight increase in the kneading resistance, which indicates the first crystals, there is a progressive increase in the kneading resistance, i.e. the torque, as soon as massive solidification and solidification starts. The initially easy flowing melt becomes plastic and solid. Both the course of solidification and the quantitative evaluation of the test results can be seen clearly from the diagram in FIG. 1.

1 illustrates the solidification process of the cocoa masses mentioned, as it appears under the test conditions described without the use of a solidification accelerator.

Example 2

If 1% by weight of microcrystalline tristearin in powder form is added to the cocoa mass melts according to Example 1 immediately after the start of the cooling phase (ie at time “0”, the diagram), the cocoa mass solidifies much more quickly. The course of solidification of these cocoa mass melts treated with a solidification accelerator is illustrated in FIG. 2.

In the following Table I, the result of Examples 1 and 2 are the solidification times of the four cocoa masses compared in comparison to the corresponding measured values for masses treated with microcrystalline tristearin as a crystallization accelerator. The strength that constitutes a torque of 100 mp under the specified conditions was used as the reference parameter for the solidification state.

Example 4

The setting time of 400 g of uncured, commercially available coconut oil was tested under the test conditions described in Examples 1 and 2. Without the solidification accelerator, the solidification was 43 minutes based on 20 mp, with the accelerator (1% microcrystalline tristearin) the solidification time was reduced to 28 minutes.

Example 5

A fat containing predominantly glycerol tricaprinate (melting point approx. 30.0 ° C.) was examined according to the test conditions of Examples 1 to 3 with regard to the setting time. Without a crystallization accelerator, the melt needed 172 minutes to reach the solidification state of 20 mp, with tristearin as the crystallization accelerator the solidification time was reduced to 80 minutes.

Example 6

A chocolate coupon 70-30-40 was treated in accordance with Example 1 and the solidification times were determined when various monoacid triglycerides (ETG) of myristic acid (Cm), palmitic acid (Ciò) and stearic acid (Cm) were added.

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Table II

% By weight

ETG art

Solidification time 60 mp / 28 ° C

0

control

162 min

1

ETG-Cm

102 min

1

ETG-Cie

82 min

1

ETG cis

73 min

Table I

Cocoa mass variety

Solidification time EZ / 28.0 ° C / D = 100 mp Arriba Trinidad Ghana Bahia

K = control attempt

115 '

125 '

155 '

190 '

without addition

B Add 1% tristearin

52 '

60 '

62 '

81 '

Shortening the

Solidification time in min.

63 '

65 '

93 '

109 '

Solidification time in%

55%

52%

60%

57%

Shortening the

Solidification time to%

45

49

40

43

35 Example 7

The chocolate couverture of Example 6 was first set at 55 ° C in the measuring device according to Example 1, then solidified at 28.0 ° C. The control test (100 mp) had solidified after 102 min.

The ETG-Cis used as a solidification accelerator was used in the finely crystalline, loosened and sieved form of the microcrystalline crystals. 1% by weight of additive gave a solidification time (EZ) of 67 minutes, 0.5% by weight of additive gave a EZ of 75 minutes, 0.25% by weight gave a EZ of 87 minutes and 0.05% by weight. % even reached a single room of 92 min.

40

45

Example 3

400 g of commercial cocoa butter were tested for the solidification process according to the procedure described in Example 1, both without and with 1% microcrystalline tristearin as the crystallization accelerator. At a cooling temperature of 28.0 ° C (= measuring temperature) there was no tendency to solidify after 10 hours, while the melt with the crystallization accelerator reached the degree of solidification of 40 mp after 207 minutes. The same cocoa butter solidified at 26.0 ° C in 496 minutes, on the other hand with the crystallization accelerator in 54 minutes, thus in about 10% of the original time.

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Example 8

For each 500 g of melted couverture 70-3044, 0.1% by weight, 0.25% by weight, 0.5% by weight was added under the conditions mentioned in Example 1 immediately at the beginning of the cooling phase (at 28.0 ° C) .-% and 1.0 wt .-% a microcrystalline mixture of about 80 wt .-% l, 3-distearoyl-2-palmitoyl-glycerin and l, 3-dipalmitoyl-2-stearoyl-glycerin and about 20 wt .-% tristearin and tripalmitin added. The measured solidification times, based on the solidification state 100 mp, are given in the table below in comparison to the solidification time which was determined for the untreated couverture melt.

Without addition

Additional quantities of the mixture

EZjoomp /

119 min

0.1 0.25 0.5 l, 0% by weight

28.0 ° C

106 98 93 90 min o

1 sheet of drawings

Claims (9)

627778 PATENT CLAIMS 1. A process for accelerating the solidification of fats or preparations containing fat, characterized in that at least one finely powdered monoacid triglyceride or symmetrical triglyceride of saturated fatty acids of chain length Ciò to C20 is used as the solidification accelerator as substances remaining in the still liquid fat melt without melting or redissolving in solid form before it forms its own fat crystals. 2. The method according to claim 1, characterized in that the additional amount of solidification accelerator is 0.01 to 1.0 weight percent, based on the fats or fat-containing preparations. 3. The method according to claim 1, characterized in that the solidification accelerator is added before the solidification crystallization. 4. The method according to claim 1, characterized in that the addition takes place during or directly before the solidification temperature or cooling. 5. The method according to any one of the preceding claims, characterized in that the solidification accelerators are added and the solidification or tempering takes place at the temperature provided for this. 6. The method according to claim 1, characterized in that the solidification accelerators are in the β-modification. 7. The method according to claim 6, characterized in that the solidification accelerators are in microcrystalline form. 8. The method according to any one of claims 1,6 or 7, characterized in that the fatty acids have the chain length Ciò to Ci8. 9. Fats or fat-containing preparations produced by the process according to claim 1. Melted fats often solidify when they cool down, often only from the supercooled melt. Although the rate of solidification increases with the temperature gradient, this in particular favors the formation of the undesirable unstable fat modifications and there are numerous, sometimes unexplained, difficulties. For example, changes in structure and consistency occur, but also in u. a. Suppositories undesirable melting point increases, in chocolate, fat ripening and much more. Therefore, all known solidification processes aim to achieve as complete a solidification as possible as "solidification crystallization" during the cooling phase in order to a. to avoid later "crystallization of the bearing". This careful solidification crystallization, which sometimes takes several hours, attempts to avoid later difficulties and strives for complete solidification of the fats in a stable form. From the deliberately careful and slow execution of the solidification, it can be concluded that any shortening of the solidification time is considered dangerous and is followed by storage difficulties and quality defects. The use of seed crystals or crystallization accelerators - although they are successful in removing inhibition of crystallization of numerous chemical substances - has probably never been seriously considered in the field of fat preparations, especially since solidified or well crystallized fats of various kinds have proven to be ineffective or ineffective. In practice, various types of devices are used to cool fat melts or melted fat-containing preparations to such an extent that fat crystals form to an increasing extent, which in turn are active as crystallization nuclei for the not yet recrystallized parts of the melt. This process is generally referred to as “tempering” or “pre-crystallization”. In addition to purely mechanical cooling processes, processes are also known for adding high-melting fats to the warm liquid fats and dissolving them therein by melting, which then recrystallize first and thus promote the solidification crystallization of the actual fat melt. This measure is also to be regarded as a mere enrichment with better crystallizing fats or as a means of increasing the melting point of the products because of the comparatively large amounts added. It has been shown that the solidification of fat melts or melted fat-containing preparations by adding triglycerides of saturated fatty acids with chain lengths of at least C10 in the form of a crystal powder can be significantly favored and that the fat melts treated in this way solidify considerably faster. In particular, it was found that the common feature of effective saturated triglycerides is the stable, low-energy ß-form of the fats. This was surprising because it does not match the crystal form of the fats to be solidified and the fat-containing preparation, which usually do not predominantly form the stable form during production. Such triglycerides, which are able to crystallize in β-form, have chain lengths of 10 to 20 carbon atoms and are, for example, monoacid triglycerides, hence those with three identical fatty acid residues, furthermore also symmetrical triglycerides, in which the average fatty acid residue in the chain length of the two is the same external deviates, but also mixtures of several acid triglycerides with one another, or mixtures of one, also several acidic with a symmetrical triglyceride. There are no exaggerated requirements for purity, but a minimum content of 70 or better 80% by weight of acidic and symmetrical triglycerides appears to be a prerequisite for effectiveness. If individual monoacid or symmetrical triglycerides are used, their 90 or better 95% by weight purity is expedient. The solidification accelerators - insofar as they are chemically uniform substances - are substances with a sharp melting point and thus differ significantly from the usual fats. In general, additional amounts of 0.01 to 1% by weight, based on the respective fat mass, are already sufficient and have a considerably accelerating effect on the solidification. Such small quantities do not change the desired properties of the products. Smaller amounts can be achieved by using the above-mentioned triglycerides in microcrystalline form, or these further accelerate the solidification. Such microcrystalline triglycerides are accessible in various ways, for example by tempering or crystallization from solvents. The annealing can be done, for example, in such a way that the crystals are heated to alternating temperatures at very little, e.g. H. 1.5 to 0.5 ° C below their measured melting point and then to about 4-6 ° C below this melting point. As a result, virtually all crystallites are apparently in the stable β-shape, and the formation of the crystallites or crystal surfaces is also likely to be improved. Crystallization from solvents such as alcohols, especially ethanol, ether, low-boiling gasoline fractions etc. achieves the same. It is particularly advantageous to use these materials in mikro2 5 10th 15 20th 25th 30th 35 40 45 50 55 60 65 crystalline state to produce a finely crystalline, loosened form, of which even the smallest addition quantities already reduce the solidification time. For this purpose, the number of individual crystallites is increased and, if possible, the proportion of very small crystallites is increased by loosening the crystal apparatus by a type of grinding process and by subsequent sieving z. B. the desired small crystals can be obtained with sieves. This finely crystalline form is a very light crystal powder, has a chalky white appearance and has an enlarged inner surface compared to a regrind made of normally compact, translucent solidified fats. In the microscope, individual crystals that have not grown together with well-developed crystal surfaces are predominantly visible, which sizes from 0.5 to 20 yes. to have; the vast majority of the particles have sizes from 2 to 10 (j. and uniformly acting shape. Among the triglycerides with a trowel length of Ciò to C20, which contain only or most of the natural even-numbered fatty acid residues, some are more effective than the others. The chain length Ci6 and Cis is the most effective. Acidic triglycerides are more effective than symmetrical ones, but on the other hand, quite good effectiveness of mixtures with high, but not exclusive, contents of the acidic and additionally the symmetrical triglycerides is observed. For example, tristearin and tripalmitin are very effective, but so are the symmetrical triglycerides l, 3-distearoyl-2-pal-mitoyl-glycerol and l, 3-dipalmiloyl-2-stearoyl-glycerol and their mixtures with a predominant proportion of tripalmitin.