SU1181702A1 - Catalyst for obtaining pyridine bases - Google Patents

Abstract

CATALYST, FOR THE PRODUCTION OF PYRIDINE BASES, including zinc oxide and alumina, which is characterized by the fact that, in order to increase the activity and selectivity of the catalyst, it additionally contains iron oxide at the following content, wt.%: Zinc oxide 5.0-10, 0 Oxide of iron 5,0-10,0 Oxide of aluminum Else JV

Description

one

This invention relates to catalysts for the preparation of pyridine bases.

The purpose of the invention is to increase the activity and selectivity of the catalyst due to the additional content of iron oxide in its composition and a certain ratio of components.

The invention is illustrated by the following examples.

Example 1. 127 g of aluminum hydroxide (33% loss on ignition) are treated with 60 ml of a 5% aqueous solution of hydrochloric acid and 70 mg of a 4% aqueous solution of hydrofluoric acid are added to 3.0 g of zinc oxide and 12.0 g of iron oxide (Id). The resulting mass is mixed and molded in the form of a macaron, 4 mm in diameter. The molded mass is dried at 25-30 ° C for 3 hours, and then, gradually, the temperature at 30 ° / h is dried for 5 hours and calcined at 430-450 C for 3 hours. After grinding, a catalyst of composition is obtained, wt.%:

Zinc Oxide 3.0

Iron oxide 12.0

Alumina Rest

Examples 2-5. Catalyst samples were prepared according to principle 1, adding to 127 g of alumina treated with hydrochloric and hydrofluoric acid, appropriate amounts of zinc oxide and iron oxide.

The compositions of the obtained catalyst samples are given in table. 1 and 2.

Catalyst samples are tested in the synthesis of pyridine bases from acetylene and ammonia, as well as from acetylene and ammonia in the presence of methanol. Experiments conducted in I

181702

flow conditions on a facility consisting of two metal reactors, 35x350 mm in size made of stainless steel, operating in parallel-in-series. Each reactor is charged with 100 ml of bulk catalyst. A mixture of acetylene and ammonia in a ratio of 1: 1 - 1: 2 mol is passed through a catalyst bed at 320-360 ° C with a bulk velocity of 120-150 hours. The resulting vapor-gas mixture is condensed in the receiver. After 12 hours of operation, the first reactor is shut off and the second reactor is turned on, and after 12 hours, the first reactor is again switched on. Under similar conditions, a mixture of acetylene, ammonia and methanol with a ratio of 1: 1: 1 1: 2: 0, 8 mol with a gas flow rate of 120-150 h and methanol 0.10 is passed through a 100 ml bulk volume of the catalyst at 390-440 ° C. 15 h. An organic layer is separated from the catalyzate formed by saturating it with solid KOH, followed by extraction with benzene. Analysis of the liquid reaction products is carried out by gas-liquid chromatography. The catalyst with the initial activity is operated for 47-55 hours and, after regeneration by air oxygen, fully restores its activity.

The results of the synthesis of 2- and 4-methylpyridines from acetylene and ammonia (T 320-360 ° C; 150 h) are given in Table. one .

The results of the synthesis of pyridine and methylpyridines from acetylene, ammonia and methanol (T 390-420 ° С; WCjyj +

+ NH 120-150h; Wch ,,)

uh

1 - I j h are given in table. 2,

Table 1

12.0

3.0

Rest

18.0 33.0

14.0

12.0

comparative data

table 2

Claims (1)

THE CATALYST OF THE DAY OF PRODUCTION OF THE PYRIDINE BASES, including zinc oxide and alumina, characterized in that, in order to increase the activity and selectivity of the catalyst, it additionally contains iron oxide with the following components, wt.%: Oxide zinc 5.0-10.0 Oxide gland 5.0-10.0 Oxide aluminum Rest