SU1701633A1 - Method of producing mixed copper and copper oxide powders - Google Patents

Abstract

The invention relates to the chemical industry and makes it possible to obtain a copper oxide powder containing 3-80% copper oxide by partially oxidizing metallic copper for 10-120 minutes at 300-400 ° C and subsequent reduction of copper oxides to the non-oxidized part of metallic copper. at 400-500 ° C for 40 min in inert gas in a fluidized bed. 3 tab.

Description

The invention relates to processes for the preparation of copper oxide powders used as catalysts in the direct synthesis of organochlorosilanes, the oxidative dehydrogenation of alcohols, the oxidation of olefins, etc.

The aim of the invention is to simplify the process of obtaining copper-oxide powders containing from 3 to 80% copper oxide (1) and reducing environmental pollution,

PRI me R 1. 8 vertical reactor (20 mm, I 400 mm) placed 40 g of copper powder (FR. 71-315 μm), and the reactor is placed in a tube furnace. By supplying an inert gas to the reactor, an inert medium is created and the heating is switched on. After reaching a temperature of 400 ° C, inert gas is replaced by supplying air to the lower part of the reactor, creating a fluidized bed of powder, and oxidation is carried out for 30 minutes. The oxidized powder contains wt.%: Cu 74.5, Cu 20 15.7 and CuO 9.9.

After the end of the oxidation process, the air supply is again replaced with inert air.

gas (while retaining the fluidized bed of the powder), increase the temperature of the reactor to 450 ° C, and maintain the powder for 40 minutes. Then turn off the heat and cool to room temperature without air. After thermal diffusion, the composition of the powder: Cu 66.7%, Cu2033.3%, sintering degree 1.3%.

PRI mme R 2. Under similar conditions at 400 ° C, copper powder was oxidized for 120 min (fr. 5–40 µm). The obtained powder contained Cu 35.3%, SizO 45.1% and CuO 19.6%.

Similarly, the process of thermal diffusion is also carried out, only at 500 ° C, the powder is kept for 40 minutes in an inert atmosphere and cooled without air access. The composition of the obtained powder Cu 19.6%, CuaO 804%, the degree of sintering 5.6%,

At the request of the industry (Dankov Chemical Plant, GNIIHTEOS), as well as according to the temporary technological regulation, the content of copper oxide (2) should not exceed 0.5 wt.%. And the content of copper (I) oxide is required in the range of 3-80 wt.%.

sl C

-h oh

s

about with

00

Sintering powder pains)% leads to a violation of the process technology.

The rationale for the necessary and sufficient time and temperature for the oxidation of metallic copper are given in Table. one.

The diameter of the reactor is 20 mm, the height is 400 mm, the mass of copper powder is 40 g, the speed under air is 4-6 l / min.

As follows from Table 1, the substantiation of the temperature and time of oxidation depends both on the degree of sintering of the powder and on the amount of copper formed by OXIDOR.

Oxidized powders containing more than 64-65% of CuO and CuO, after thermal diffusion (reduction) contain 1-3% of CuO, which is unacceptable at the request of the industry.

The quality of the target product depends on the time and temperature of the sanding process, which is confirmed by the examples.

In tab. 2 shows the dependence of the composition of the copper oxide powder on the time of thermal diffusion.

In tab. 3 shows the dependence of the composition of the copper oxide powder on the temperature of thermal diffusion.

As follows from the data table. 2 and 3, all oxidized powders containing up to 10% of copper oxides (regardless of oxidation temperature) at 350 ° C are reduced in 10-40 minutes, t, i.e., the method is carried out. And powders containing more than "2-15%

0

five

0

five

0

copper oxides, for 40 minutes to recover with no success. Powders containing up to 64.7% of copper oxides at 400-500 ° C are reduced within 40 minutes.

Thus, at 350 ° C, the process is partially carried out, and in the temperature range of 400-500 ° C, the reduction of oxidized powders containing up to 64.7% of copper oxides (regardless of the oxidation temperature) ends in 40 minutes.

In the known method, poisonous carbon monoxide is used as a reducing agent for copper (2) oxide to copper oxide (1), the use of which is associated with the complexity of the technological design of the process and with the pollution of the environment. In the proposed method, these shortcomings are eliminated.

Claims (1)

The invention The method of obtaining - a mixture of powders of copper and copper oxide containing from 3 to 80% copper oxide (1) for the manufacture of catalysts, including the partial oxidation of metallic copper to copper oxide (2), followed by its reduction to copper oxide (1), characterized in that, in order to simplify the process and reduce the zgr count of the environment, partial oxidation of the wire is carried out with air during 10-120 MK.I — three 300–400 ° C, and the reduction of the lead1 in an inert gas in a fluidized bed is / w 40 min at 400-500С ° s № p / p Temperature, ° С 400 Same 400 Same Table 1 table 2 T a b n i c a 3