SU716583A1 - Cyclohexanol-to-cyclohexanone dehydrogenation catalyst - Google Patents

Description

(54) CATALYST FOR DEHYDROGENATION OF CYCLOGOXANOL TO CYCLOHEXANE

hydrogenation). Cataly: the congestion for a long time maintains stable and catalytic activity, does not require regeneration, retains a high mechanical strength, on average kg / mm .. - ..

Nickel phosphides are obtained by the method of reactive precipitation from an aqueous solution of nickel chloride with a solution of sodium hypophosphite in the presence of palladium chloride at a temperature in an acidic medium. The precipitate is a mixture of nickel phosphides .P2 -NiaP of general composition, wt.% Nickel 80-85, phosphorus 15-20.- v ,, .-,

PRI p 1. To 500 ml of 0.5 M rastor N1 CB, poured. :; 1000 ml bM sodium hypophosphite solution. Concentrated HCE to pH 2 is added dropwise. 0.005 g of palladium chloride is added to seed the reaction. The resulting mixture solution is heated to a temperature. Re, precipitation reduction action. lasts for 7 hours. The precipitate formed is filtered off (yrb)) with distilled water until a negative reaction occurs for the CE and PO ions and then dried at a temperature of H5t5 ° C to a constant weight. g of precipitate is poured over with 30 ml of a 1.5% aqueous solution of NaOH, stirred thoroughly, dried at b, then finally dried at 7 hours). The catalyst is tabulated under a pressure of 100 kg / cm into 0.5 cm diameter cylindrical tablets, which are crushed into granules, with a size of 0.2 mm,

The composition of the resulting cat or zatszra, wt.%: Nickel 4.505, nickel phosphide 92.95, sodium hydroxide 3. Specific surface 31, bulk density 1.98 g / cm, mechanical hi564, ndity 1.78 kg / 1F1. ...... and ..-.: ....

The catalyst prepared in the manner described above loads into kLL -,;:. quality of 1 ml (1.98 g) in-roe; ktOr of the laboratory unit 1Н | эо с 6чйбШ 1РГГШ and heating in a stream of nitrogen for 4 hours at a temperature of 2 80iio C. Nitrogen feed rate 3000 reaction zone using mic; c)) 5Ж yayosh iifiK cst

4.3 ml / h. At a temperature output It has 75% selectivity of 97%,

When carrying out the reaction under the same other conditions, the cyclohexanron yield is 77%, the selectivity is 94%,

EXAMPLE 2 Process as described in Example 1. Concentrated hydrochloric acid is added to a mixture of nickel chloride and sodium hypophosphite to a mixture of pH 3, and the precipitate is poured with a solution of sodium hydroxide for 15 g of precipitate with 30 ml of 2% NaOH. The subsequent steps; and preparation of the catalyst as in Example 1. The composition of the catalyst obtained, weight% nickel 4.0, nickel phosphide 92.0, sodium hydroxide 4, surface area 26, bulk density 1.72 g / cm, mechanical strength 1 , 83 kg / mm,

The catalyst / prepared as described is loaded in the amount of 1 ml (1.72 g) into the reactor of a flow type laboratory installation. The test of the catalyst is carried out as in example 1. At the reaction temperature of 2 ° C, the yield of cyclohexanone is 53% 1 three selectivity 95%.

At the reaction temperature, the yield of cyclohexanone is 69%, the selectivity is 95.5%,

 temperature, cyclohexanone yield 80%, selectivity 97.5%.

 At a temperature of 320 C, the yield of cyclohexanone is 72%, the selectivity is 85%,

PRI and measures 3. The process is carried out analogously to example 2, sodium hydrrkis is introduced into the sediment based on 15 g of sediment 30 ml of a 2.5% tiapH solution. The subsequent steps for preparing the catalyst are as S. Example 1, Composition of the obtained catalyst, wt.%: nickel 4.1b, nickel phosphides 91.04, sodium hydroxide 4.8, Surface area 28 m / g, bulk density 1.9 g / cm, mechanical strength 1.67

; These congestion reactions for cyclhexanol ehydration are determined as described in example 1 and 2. At a reaction temperature of 280 ° C, the yield of cyclohexanone is 56% with a selectivity of 80%. . ,

At a temperature, the yield of Cyclohexanone is 62%, selectivity of 77%,:

At a temperature, the yield of cyclrhexanone is 52%, the selectivity is 71%,

In the table below, the results of the study of stability, actinity and, gejifuivnn, type of catalyst prepared according to example E, at a temperature of 300 ° С,. .

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Claims (3)

E5 HEY; Sgrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrrr test: (a): As can be seen from the above data, a catalyst based on nickel phosphides promoted with 3-4% sodium hydroxide, has high catalytic activity, selectivity and. stability in the cyclohexanol dehydrogenation reaction in cyclohec non. The invention The catalyst for the dehydrogenation of cyclohexanol to cyclohexanone, including nickel and the sodium compound promoter, is olympic so that, in order to increase the activity and selectivity of the catalyst, it additionally contains nickel phosphides, and in Loghexanone, including nickel and a promoter, a sodium compound, characterized in that, in order to increase the activity and selectivity of the catalyst, it is additionally;. , nickel feeds, and, as a sodium compound, sodium hydroxide with the following content of components, wt.%: Nickel 4,0-4,17 Sodium hydroxide 3.0-4.8 nickel phosphides Remaining Sources of information taken into account during the examination 1. The patent of Great Britain 1111416, cl. H (1) p, pub. 1969. 2. The patent of CMA 2970172, cl. 260-586, publ. 1962. 3. Patent CWk 2588359, cl. 252-440, published. 1952 (prototype) ..