SU1328404A1 - Method of producing univalent copper sulfide - Google Patents

Abstract

The invention relates to methods for producing copper (I) sulphide from sulphate solution by electrolysis and allows to simplify the process and improve the working conditions. The method relates to the production of sulfide from a sulfate solution containing bivalent copper sulfate, moreover, the deposition is carried out by electrolysis in a cell with a copper anode and a titanium cathode at a cathode current density of 200-400 A / m. A sulphate solution containing bivalent copper sulphate and sodium sulphite is used at a ratio of (0.5-1.5) :( 0.8-12.0). 3 tab. o (l

Description

The invention relates to methods for producing copper (I) sulfide from sulphate solutions by electrolysis.

The aim of the invention is to simplify the process and improve working conditions. .

An example. To the electrolyte containing 150 g / l of sulfuric acid, 1 g / l 5, ka-tri sulfite is introduced in the amount of 1.0 g / l. The electrolysis is carried out at koinatnoy temperature with stirring for two hours. The cathode density is 300 A / m. Copper anode, titanium cathode. At the end of the electrolysis, the copper (I) sulfide is separated from the copper, washing the precipitate with a 15% solution of ammonium chloride,. Current output 69.86%, copper weight 0.0573 g.

The distinctive features of the proposed process are as follows.

The combined reduction of sulfite ion and copper (II) ion at the cathode according to the following reactions :;

2m. Si I

S024S + 6Н S ° + ЗН „0.

Freshly formed active and highly dispersed copper and sulfur, due to chemical means, instantly form copper (I) sulfide:

2Ci ° + S

C, S.

To avoid the formation of a mixture of Cu, .S + CuS, the process must be carried out strictly in the proposed conditions.

The choice of electrodes. Copper was chosen as an anode in order that the electrolyte was constantly replenished with ions of divalent copper.

C ° - 2yo

 Si

The choice of the cathode material is due to the fact that titanium is stable in sulfuric acid solutions (does not dissolve and does not contaminate the electrolyte), and also because the electrolysis product (one sulfide) of copper) does not adhere to its surface. allows to obtain copper (I) sulphide in powder form.

The resulting electrolysis products: single-lithium copper sulphide and partly formed fine copper powder are filtered, washed from the electrolyte residues to neutral

0

five

0

five

0

five

0

five

0

five

medium (determined by litmus paper) and dried in air at room temperature. The fine copper in the washing process is immediately oxidized to nitrous oxide, which is separated off with a 15% solution of ammonium chloride.

The structure of monovalent copper sulphide is confirmed by X-ray phase and chemical analyzes.

In tab. Figure 1 shows the effect of current density on the formation of copper sulphide (Cu (ll) 1 g / l, 10 g / l, 150 g / l, t 25 ° C), in Table. 2 — the effect of the initial copper (I) concentration on the formation of copper (I) sulfide (D 300 A / m, 10 g / l, 150 g / l, t 25 ° C), in a table. 3 - the effect of sodium sulfite concentration on the output of monovalent copper sulfide (DI 300 A / m, Cu (II) 1 g / l, H, SO 150 g / l, t 25 ° С).

As can be seen from the table. 1-3, the optimal parameters for carrying out the process are as follows: the ratio C (0.5-1.5): (B, 0-12.0) g / l (preferably 1.0-10.0). The cathode current density is 200-400 A / m (preferably 300 A / m2). Current output 69-86%. Copper weight 0.0573 g

At current densities below 200 A / m, a compact copper precipitate forms on the ktode, the formation of copper (I) sulfide drops to a minimum. At current densities above 400 A / m, hydrogen evolution is enhanced, resulting in the formation of hydrogen sulphide, which reduces the current output Cuj S.

At copper (II) concentrations above 1.5 g / l, copper powder is formed in the electrolyte. At concentrations below 0.5 g / l, the speed of the process decreases, and as a result, the yield of the target product, copper (I) sulfide.

When the content of sodium sulfite is below 8 g / l, a deficit of sulfite ions is observed in the electrolyte, which leads to the formation of metallic copper. At a concentration above 12 g / l, fine-dispersed elemental sulfur is formed - a non-target product.

The optimum concentration of sulfuric acid is 150 g / l. In this case, the solution has a maximum specific electrical conductivity.

Thus, the advantage of the proposed method for the production of sulfide

Claims (1)

Claim method for producing monovalent copper sulfide by precipitation from sulphate solution containing sul 1328404 monovalent copper from sulphate applied process is environmentally safe solutions compared to the known. The fact is that there is no need to prepare a special mixture of gases, in addition, the instrumentation is simplified - no complicated hermetic equipment, special heating of bivalent copper, special heat sinks are needed to create high temperatures the fact that, for the purpose of control, and the process is carried out at room Q a process and improve the conditions of the temperature of labor, precipitation is carried out by electrolysis in a copper anode electrolyzer and The absence of precipitating into the atmosphere a titanium cathode at cathodic hydrogen sulphide eliminates the need for a current of 200–400 A / m and using special rooms or a sulphate solution containing complex devices for trapping bivalent copper sulfate and sulphite gases, and therefore, contributes to a ratio of copper ( Ii): reduce material costs for sewage treatment plants, which makes pre- (8.0-12.0). sodium sulfite, equal to (0.5-1.5): D.. I A / m2 100 I 200 T 300 D 400 1 500 | 600 L1IIIL11 CujS weight, r .0.1617 0.3970 0.63010.7375 6.8881 -0.9797 BTC,% 50.04 67.44 69.86.64.65 61.2654.32 Weight C, g 0.0843 0.0650 0.05309.1984 0.2733 0.5297 Table 2 Cu (ll), g / l0, 51,0I 1,52,02,5 CujS weight, g 0.2106 0.5831 0.6301 0.5302 0.4885 0.3269 WTC CujS,% 23.27 64.42 69.86 59.00 54.36.336.38 Weight C, g 0 , 0129 0.0226 0.0573 0.0704 0.1023 0.1926  Education is only due to the dissolution of the copper anode. Table 3 NajSOjj g / l I 6,08,010,012,014,016,0 Weight GujS, g 0.3358 0.5895 0.6301 0.5858 0.5569 0.5143 BTC,% 36.74 64.69 69.86 64.09 60.93 56., 44 Weight C, g 0, 3027 0.0755 0.0573 0.0662 0.0802 0.0946 DETAILED DESCRIPTION A method for producing monovalent copper sulfide by precipitation from a sulphate solution containing the sullagable process is environmentally safe. copper of divalent copper, that is, so that, in order to simplify the process and improve working conditions, precipitation is carried out by electrolysis a titanium cathode with a cathode current area of 200-400 A / m and using a sulfate solution containing bivalent copper sulfate and sodium sulfate at a ratio of copper (II): sodium sulfite, equal to (0.5-1.5): Table 1