The method of preparation of nickel catalyst for hydrogenation of vegetable oils and fats

 

(57) Abstract:

Use: in the manufacture of the catalyst, in particular of Nickel catalyst for hydrogenation of vegetable oils and fats. The inventive method involves the precipitation of basic Nickel carbonate to silicate carrier at a ratio of 1 : 2.2 to 4 followed by filtration, washing and tabletting when the force of 4.5 - 5.5 kg/tablet. Then tablets restore in a stream of hydrogen and then Passepartout in a stream of nitrogen until the ratio of reduced and oxidized forms of Nickel, 0.5 to 4.5. The resulting product provides a high filtration capacity in a magnetic field. table 1.

The invention relates to the field of preparation of catalysts for hydrogenation of vegetable oils and fats.

Known method of preparing a Nickel catalyst brand GM-3 (TU 38102152-83), which consists in the precipitation of basic Nickel carbonate in the medium with subsequent separation of the catalyst mass in the drying, decomposition, the recovery current of hydrogen passivation in a stream of nitrogen mixed with oxygen.

The disadvantage of this method is to obtain a catalyst with a low filtration capacity in a magnetic field is celevoke catalyst by precipitation of basic Nickel carbonate to silicate carrier, filtering the resulting precipitate, wash it, mixing with graphite, pelletizing the obtained catalyst mass, reductive decomposition and passivating.

The disadvantage of this method is the low magnetic susceptibility of the obtained catalyst, the result is a low filtration capacity of the catalyst in a magnetic field.

The purpose of the invention is the preparation of the catalyst with increased filtration capacity in a magnetic field.

This objective is achieved in that in the method of preparation of Nickel catalyst for hydrogenation of vegetable oils and fats, which consists in the precipitation of basic Nickel carbonate to silicate carrier, filtering the resulting precipitate, washing, pelletizing, reductive decomposition and passivation, the precipitation of basic Nickel carbonate to silicate carrier is carried out at a ratio of Nickel:media 2,2-4,0, tableting is carried out at a pressing force of 4.5-5.5 kg/tablet, and reductive decomposition and passivation is carried out before the ratio of reduced and oxidized forms of Nickel, 0.5 to 4.5.

The significance of the distinctive features is that the proposed way is.

The method of preparation of Nickel catalyst is carried out as follows.

P R I m e R 1. A solution of Nickel sulfate with a concentration of 22.5 G. of Nickel ion/l, heated to 40aboutWith and with stirring, add the diatomaceous earth in an amount such that the ratio of the mass of a Nickel/diatomaceous earth in the resulting suspension was 2.2. Then the temperature in the reactor-the precipitator raised to 85-90aboutC and under stirring for 1 h, add 20% solution of sodium carbonate at a molar ratio of Nickel sulfate:sodium carbonate is 1: 1,1. The suspension is stirred for another 0.5 h, turn off the heating, and the resulting precipitate was separated and washed on the filter until a negative response to the sodium ion and sulfate ion. Washed of impurities precipitate is dried at 120aboutC to a residual moisture content of 3-5%. The precipitate basic Nickel carbonate on the diatomaceous earth is mixed with graphite and pressed into tablets in an effort to 5.5 kg per tablet. The obtained tablets are loaded into the reactor column type and restore in a stream of hydrogen at a speed of 1000 g-1at a temperature of 380-400aboutWith over 23,5 hours Later, the catalyst was cooled to 50aboutWith hydrogen substituted on the nitrogen and begin passivation increasing the oxygen concentration in the nitrogen the project in the process of hydrogenation of fats preformed catalyst is ground to a particle size of not more than 70 μm. When this mass fraction of particles with a size of 0.01 to 1.0 μm was 1.0%.

The resulting catalyst has the following chemical composition, wt.%: Nickel metal 45 Oxide and hydroxide of Nickel 9.4 Silicate Nickel 6.0 Nickel Sulfate 0.6 silica (diatomaceous earth) 33 Graphite 3,0 Crystallization water 3,0

The total mass fraction of Nickel in the catalyst 55%. The ratio of reduced and oxidized forms of Nickel 4,5. The catalyst is 80%. The selectivity of 99.7%.

High-gradient magnetic separation of hydrogenated fat containing catalyst 0,15 (Nickel) when the magnetic field of 1.0 T, the temperature of the hydrogenated fat 140aboutWith the duration of 3 allowed to separate 99% of the catalyst.

P R I m e R s 2-5. Preparation of the catalyst is carried out as in example 1 with the difference in technological modes listed in the table, which shows the composition and properties of the resulting catalysts.

As can be seen from table a catalyst containing metallic Nickel 20-45% and the ratio of reduced and oxidized forms of Nickel (Nio/Ni2+)0.5 to 4.5 has the activity and selectivity of not less than widely used in the present catalysts GM-3 and Nickel on kieselguhr brand "P", however, Breitnau separation. This allows to mechanize the process of separation of the catalyst from the fat and to abandon the traditional filtering techniques, leading to increased losses of fat and catalyst.

The economic effect from implementation of the proposed catalyst using the method of magnetic separation lines hydrogenation of fats capacity of 180 t/d is 210 thousand rubles per year (price 1990).

The METHOD of PREPARATION of NICKEL CATALYST FOR hydrogenation of VEGETABLE OILS AND FATS by precipitation of basic Nickel carbonate to silicate carrier, filtering the resulting precipitate, wash it, tabletting, reductive decomposition and passivating, characterized in that the precipitation of basic Nickel carbonate to silicate carrier is carried out at a ratio of Nickel / media 2,2 - 4,0, tableting is carried out at a pressing force of 4.5 - 5.5 kg/tablet, and reductive decomposition and passivation is carried out before the relationship restorative oxidized to form Nickel 0.5 to 4.5.

 

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