SU1384329A1 - Method of preparing catalyst for hydrogenation of benzene - Google Patents

Abstract

This invention relates to catalytic chemistry, in particular to the preparation of a catalyst (CT) for the hydrogenation of benzene. The purpose of the invention is to increase the activity and stability of CT. Preparation of QDs is carried out by applying a promoter onto a flat metal carrier, for which zirconium and aluminum are used in a total amount of 5.95-6.19 g / cm in the following ratio of components, wt%: nickel 86.3-89.8; zirconium 0.3-4.2; aluminum opt al: noe. The resulting product is subjected to heat treatment at 500-600 seconds until the aluminum phase disappears and the NiAlj phase is formed. The resulting alloy is leached. The obtained CT scan is active by 2–5 times and exceeds the activity of the known CT scan after 5 hours of work by 2.5–6 times. 2 tab. with

Description

11384329

The invention relates to the production of skeletal nickel catalysts and can be used in the chemical industry.

The aim of the invention is to increase the activity and stability of the catalyst due to a certain sequence of deposition of alloy components on a metal surface in a certain ratio and annealing at a certain temperature range.

Example 1. A foil of 03 KP steel with a size of 7x7 mm is deposited using a vacuum condensate-diffusion method (printing at a residual pressure of 2, 2-10 mm Hg) nickel, zirconium, then aluminum in co

EXAMPLE 3 A catalyst is prepared analogously to Example 1, but nickel zirconium and aluminum are deposited in an amount of 6.13 mg / cm with the following ratio of may.%: Nickel 87.1, qi 3,3, aluminum 9.6 and leach.

The prepared catalyst was examined under the conditions of Example 1, but at 170 ° C and when the concentration of benzene vapor was 1.5–10 mol / ml.

15

The value of the activity of the catalyst are given in table.1.

Example 4. The catalyst is prepared analogously to example 1, but the deposition of zirconium and aluminum in the amount of 6.19 mg / cm in the following ratio.%: Nickel 86.3, zirconium 4

The amount of 5.95 mg / cm is as follows: co-aluminum 20.5, and also better target.

% by weight: nickel 89.8, zirconium 0.3, aluminum 9.9. The sample is annealed in a vacuum at 500 ° C for 1 hour. The absence of the aluminum phase and the formation of the NijAl phase are recorded 25 by X-ray phase analysis.

Next, take a 0.5 cm sample and treat with 25% sodium hydroxide solution at 100 ° C, then 5 and 2% sodium hydroxide solution at 100 ° C. After that, the sample is washed in alcohol and then in ether.

A hydrogen stream of 99.999% purity is fed into a catalytic reactor with a diameter of 15 mm, 0.5 cm is added.

The prepared catalyst was tested under the conditions of Example 1, but the benzene vapor concentration was 3.2 x X 10 mol / ml.

The value of the activity of the catalyst are given in table.1. It also shows the activity of a catalyst prepared in a known manner.

EXAMPLE 5 A foil of one hundred grade 12X18H10T with a size of 8 x 8 cm is applied in vacuum at 2.2 10 mm Hg. the condensate diffusion method is a layer of nickel, zirconium, then an aluminum layer in the amount of 5.95 mg / cm in the following ratio, wt.%: nickel 89.8, zirconium 0.3, aluminum 9.9.

lenny catalyst. Then the reactor is heated to a temperature of 90 ° C and hydrogen is fed, saturated with benzene vapor. The flow rate of hydrogen is 60 ml / min, the concentration of benzene vapor is 4.1-10 mol / ml. The analysis of the resulting cyclohexane is carried out chromatographically. The initial rate of hydrogenation of benzene is 9.5 to X 10 mol / h-cm. The rate of hydrogenation after 5 hours is 4.3–10 mol / h-cm.

Example 2. The catalyst is prepared analogously to example 1, but nickel, zirconium and aluminum are deposited in an amount of 6.06 mg / cm in the following ratio, wt%: nickel 88.1, zirconium 2.1, aluminum 9.8, and also explicable.

The activity of the prepared catalyst is examined under the conditions of Example 1 at a benzene concentration of 4.3 x 10 mol / ml.

The value of the activity of the catalyst are given in table.1.

EXAMPLE 3 A catalyst is prepared analogously to example 1, but nickel, zirconium and aluminum are deposited in an amount of 6.13 mg / cm in the following ratio in percent by weight: nickel 87.1, zirconium 3.3, aluminum 9 , 6 and leached.

The prepared catalyst is tested under the conditions of Example 1, but at 170 ° C and at a benzene vapor concentration of 1.5 × 10 mol / ml.

The value of the activity of the catalyst are given in table.1.

Example 4. The catalyst is prepared analogously to example 1, but nickel, zirconium and aluminum are deposited in an amount of 6.19 mg / cm with the following ratio:%: nickel 86.3, zirconium 4.2,

aluminum 9.5, and also better.

five

about

five

0

five

0

five

The prepared catalyst was tested under the conditions of Example 1, but with a benzene vapor concentration of 3.2 x 10 mol / ml.

The value of the activity of the catalyst are given in table.1. It also shows the activity of the catalyst prepared in a known manner.

PRI me R 5. A foil of steel, grade 12X18H10T, 8 x 8 cm in size, is applied under vacuum at 2.2 10 mm Hg, using a condensate diffusion method, a layer of nickel, zirconium, then an aluminum layer of 5.95 mg / cm in the following ratio, wt%: nickel 89.8, zirconium 0.3, aluminum 9.9.

The sample is annealed in vacuum at

within 3h The method of X-ray phase analysis revealed the presence of an aluminum phase and the absence of a phase,.

The plate of the prepared catalyst with a size of 0.5 cm is treated with a 25% sodium hydroxide solution at 100 ° C, then with a 5% and 2% sodium hydroxide solution at 100 ° C. After that, the sample is washed in alcohol and in ether. Then a stream of hydrogen of 99.999% purity is fed into a catalytic reactor with a diameter of 15 mm, 0.5 cm of the catalyst is introduced. After that, the reactor

they are heated to a temperature of 170 ° C and hydrogen is supplied, all of them with benzene vapor. The hydrogen flow rate is 60 ml / min. The analysis of the resulting cyclohexane is carried out chromatographically. Initial rate of hydrogenation of benzene

400 ° C

ten

and the speed after 5 hours is

1 o mol / h, see. Initial concentration

benzene vapor 4, 1 10 mol / min.

EXAMPLE 6 A catalyst prepared analogously to example 5 was annealed at 500 ° C for 0.5 h. The X-ray phase analysis shows the presence of an aluminum phase.

The prepared catalyst is targeted and examined under the conditions of Example 5. The initial activity in the hydrogenation of benzene and the activity after 5 hours is 10 mol / h-cm.

Example 7. The catalyst prepared in analogy to example 5 was annealed at 600 ° C for 2 hours, X-ray phase analysis showed the absence of an aluminum phase and the presence of a phase .20

The prepared catalyst is leached and examined under the conditions of Example 5.

Initial activity and activity after 5 hours are given in table 2, 25

In the example, the Catalyst prepared similarly to Example 5 is annealed at 700 ° C for 5 hours. The X-ray phase analysis shows the absence of aluminum phases and. ,,

The prepared catalyst is leached and tested under the conditions of Example 5,

Initial activity and activity after 5 hours are given in Table 2.

compared to the known, it is 2–5 times more active in a wide range of temperatures and concentrations of benzene. The method allows to obtain a catalyst also significantly higher in stability, as it exceeds the activity of a known catalyst after 5 hours of operation by 2.5-6 times. Furthermore, the method has wider possibilities, since it allows the introduction of other metals, for example zirconium, in order to increase the activity and stability of the catalyst,

Claims (1)

Invention Formula The method of preparation of the catalyst for the hydrogenation of benzene by carrying Nickel, Aluminum, and the promoter onto a flat metallic support, followed by heat treatment and pressing of the resulting alloy, which, in order to increase the activity and stability of the catalyst, is consistently applied to the support. Nickel, a promoter, in which quality zirconium and aluminum are used in a total amount of 5.95-6.19 g / cm with the following ratio of components, wt.%: Nickel - 86.3-89.8 Zirconium 0.3-4.2 Aluminum Else and the heat treatment is carried out at 500C. As can be seen from the tables, the catalyst, 600 ° C, until the aluminum phase disappears prepared by the proposed method, and the formation of the phase 0 0 , compared to the known, it is 2–5 times more active in a wide range of temperatures and concentrations of benzene. The method allows to obtain the catalyst also significantly higher in stability, since it exceeds the activity of a known catalyst after 5 hours of operation by 2.5-6 times. Furthermore, the method has wider possibilities, since it allows the introduction of other metals, for example zirconium, in order to increase the activity and stability of the catalyst, Invention Formula The method of preparing a catalyst for the hydrogenation of benzene by deposition of nickel, aluminum and a promoter on a flat metal carrier followed by heat treatment and higher. by melting the resulting alloy, it is about the fact that, in order to increase the activity and stability of the catalyst, nickel is successively deposited on the carrier, a promoter, which uses zirconium and aluminum in a total amount of 5.95-6.19 g / cm with the following ratio of components, wt.%: Nickel - 86,3-89,8 Zirconium 0,3-4,2 Aluminum Else and heat treatment is carried out at 500 to 600 ° C until the aluminum phase disappears and the phase is formed  Catalyst activity the famous  0 90 T70 230 90 four; 1-10 4.3-10 .-6 1.5-10 .-7 .-6 4,2.40 .-6 Table 1 9,5.-10 -S 4.3-10 -five 31,1- 10 ,-five 5.2-10 8.1 -10 ,-five 2.9-10 -g 4.610 , -6 2.0 -10 .-at 5.240 -S 0.87-10 -five The catalyst activity is initial even after 5 hours. 0.3 0.3 0.3 0.3 170 170 170 170 4.1 -10 g 4.1-10 , -b 4.1 -10 4.1 -10 .Table 2 .ten -T ten -7 1010 9.5--10 -five 4.3-10 -S -7 ten ten -7