CS215175B1 - Method of hydrogenation of non-saturated fatty acids and glycerides thereof - Google Patents

Description

The invention relates to a process for the hydrogenation of unsaturated fatty acids and their glycerides to the corresponding partially or fully saturated compounds,

Hydrogenation of unsaturated fatty acids bound in vegetable oils and animal fats, resp. Free unsaturated fatty acids are one of the most important processes in the food industry. More than 4.10® tons of oils and fats are hydrogenated worldwide for further processing into food or technical products. This fact and the effort to maximize the use of all food sources forces the manufacturer to improve the technological management of hydrogenation, where besides achieving the desired optimum economic effect, the requirement is also required for its selective course.

Due to . the boiling point of the processed materials, the hydrogenation process is carried out in the liquid phase at an elevated temperature. and the pressure under the heterogeneous catalyst and thus constitutes a relatively complex three-phase liquid-gas-solids system. In addition to the technological parameters of the apparatus, such as discontinuous or continuous process execution, solution of mass and heat transport in the system, etc., the quality of the catalyst used is essential. From the point of view of the maximum utilization of the device, economics, it is desirable to obtain a high reaction rate of hydrogenation in obtaining the saturated matic acids and their yields, which is due to the high activity of the catalyst. In view of the possibility of partial hydrogenation, it is possible to obtain a product of the desired composition containing selected esters of the fatty acids. For example, in the hydrogenation of vegetable oils (rapeseed, soybean) containing glycerides of linolenic acid, it is desirable, in order to increase the taste and aromatic aromatic acid constant, to substantially or completely eliminate it with minimal loss of glycerin acid. 1: 0: 10 ^ associated with minimal seearovl glyceride content in the oil. The desired degree of zhydrogrnovia of the fatty acids may therefore be varied and is judged by the iodine value, the melting point - or the determination of the fatty acid content by the gas-liquid gas.

In technical practice, nickel catalysts protected by the preparation and composition (content of active ingredient, activator, admixtures, etc.) are used for many oils, animal fats and free fatty acids for the use of Uydrogens®. they are not concurrently achieved in their activity and selectivity. Usually, only one of the aforementioned ylasenoots dominates. In some cases, for example, when copper is present as the second active component to increase the selectivity of the nickel catalyst, it may dissolve and degrade the fat. Also, the Usmosern catalysts did not achieve better activity and selectivity parameters compared to heterogeneous ones, bearing in mind the difficulty of adopting hydrogenation technology and separating these catalyst systems from the product.

The foregoing considerably reduces the process of the present invention, which is a process for hydrating unsaturated fatty acids and their glycerides to form partially or fully saturated compounds. The present invention is based on a process in which Uydrsgrnacr is carried out in a temperature range of 80 to 240 ° C and a pressure of 1,013.10 to 2.7.10 Pa with a catalyst having a total content of 10 to 65% by weight of nickel, of which 40 up to 99% by weight is the proportion of deduced nickel in the form of metal and further comprises 0.05 to 6.7% by weight of bound boron, the amount of catalyst being in the range of 0.01 to 2% by weight of active metal, based on the treated and the conversion time is governed by the fatty acid composition required in the product. The above hydrogenation process can be carried out in both batch and continuous operating modes.

In the selective process control to partially hydrogenated vegetable oils, the hydrogenation is usually terminated at a content of 0 to 30% by weight of the original amount of linolenic acid, i.e. in the processing of rapeseed oil in minimized erucic acid content starting at 115 The linoleic acid ester content decreases to 50-80% by weight of the original amount under the specified conditions. · The oils thus processed are then suitable for further production of salad oils, mayonnaise, shortening, etc. ·

Due to the selective properties of the catalyst used, a relatively high yield of oleic acid can also be achieved in the hydrogenation of vegetable oils. For example, when processing rapeseed oil and minimized erucic acid content, the maximum oleic acid ester content of the product is about 83% and the product obtained can be further processed for technical purposes.

The process according to the invention can also be successfully applied in the hydrogenation of vegetable oils to the melting point of 32-39 ° C of the product, which is then suitable for further processing into edible fats, diets, etc., and in total hydrogenation of vegetable oils or fatty acids. for purposes of iodine number 2 to 5, when high activity of catalyst is applied

The catalyst is prepared by a process comprising treating nickel hydroxide and / or basic nickel carbonate prepared by precipitation of a nickel salt with alkali at a temperature of 20 to 100 ° C and a pH of more than 10 with an alkali borohydride solution for 5 to 60 minutes, and After washing, drying and adjusting to the desired grain size, the mass obtained is reduced at 250 to 480 ° C to a reduction degree of 0.40 to 0.99. This catalyst can be applied for both batch (batch) and continuous operating modes, whereby the catalyst can be used. several times without regeneration.

The following are some examples of embodiments of the method of the invention.

Example 1

To a stainless steel autoclave equipped with a paddle stirrer was charged 80 g of refined rapeseed oil with minimized erucic acid content and a catalyst containing

3.8% by weight of bound boron and 27% by weight of nickel, of which 48% was in the form of metallic nickel in an amount of 0.04% by weight of nickel based on oil. Hydrogenation was carried out at 180 ° C under a hydrogen pressure of 1.52 bar. Changes in the composition of the product during the hydrogenation are shown in Table I, which shows high selectivity and catalyst activity. The products obtained were of a quality suitable for further processing as a part of salad oils, mayonnaise, diatoms, etc.

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Table I

Hydrogenation of maximized erucic acid rapeseed oil under the conditions of Example 1

time (min) iodine number Fatty acid content (% by weight) stearová 1 oil and lónolová ¹ __ ¹ Hnolenova L.. .. 0 115 2,6) 59.2 21.3 1 7.3 3 111 2.8 : 62.7 19,3 i i 5,7 5 104 2.9! i 66.7 16.7 4.0 7 98 3.1 70.2 14.8 2.3 9 95 3.3. 73.5 12.9 0.9 12 89 3.5 76.8 9.8 0 15 Dec ®5 3.7. 80.7 5.7 0 17 79 5.5 83.0 3.0 0 20 May 76 9.7 82.0 0 0 24 70 15.2 77.1 0 0 30 63 21.0 71.7 0 0 36 59 26.7 66.2 0 0 45 55 32.2 60.7 0 0

Example 2

80 g of sunflower oil of the following composition were hydrogenated on the same apparatus as in Example 1:

acid % wt. acid palmitová 6.73 arachová 0.54 гишаг ^ ё 0.14 gadolejová 0.76 stearová 3., 96 behenová 0.81 oil 20.28 eruková 4.95 lónolová 61.83

The iodine value determined by Wijs was 129. The catalyst was recovered in an amount of 0.03% by volume after filtration from the previous hydrogenation. Ni based on oil. The temperature was 140 ° C and the hydrogen pressure was 1.52 bar. After 160 minutes, the melting point of the product was 33.2 ° C while maintaining the consistent properties required for further processing in the shortening production.

Example 3

80 g of distilled fatty acids from animal fats having an iodine number of 56 were hydrogenated in a screened autoclave as in Example 1. The hydrogenation was carried out at 200 ° C and a pressure of 2.354 · 10 Pa, on a catalyst containing 0.25. % of bound boron and 45% of nickel, of which 87% was in the form of nickel metal. The amount of catalyst was 0.43% nickel based on fatty acid. After 90 minutes, an iodine value of 2.5 was reached.

Claims (2)

SUBJECT OF THE INVENTION Process for the hydrogenation of unsaturated fatty acids and their glycerides to the corresponding partially or fully saturated compounds, characterized in that the hydrogenation is carried out in a temperature range of 80 to 240 ° C and a hydrogen pressure of 1,013.10 to 2.7.10 ^ p _{and in the} presence of a total catalyst. content of 10 to 85% by weight of nickel, of which 40 to 99% is the proportion of reduced nickel in the form of metal, and further comprising 0.05 to 6.7% by weight of boron bound, the amount of catalyst being in the range of 0.01 up to 2% by weight of active metal, based on the feedstock to be processed, preferably 0.02 to 0.06% by weight, and the conversion time is 1 ^; It controls the fatty acid composition required in the product. 2. A method according to claim 1, wherein the hydrogenation is carried out in a batch or continuous operating mode.