SU1357362A1 - Method of extracting copper from used solutions of chemical copper plating - Google Patents

Description

The invention relates to the chemical metallization of dielectrics, in particular to spent chemical copper sulphide solutions for their disposal in front of C. PIV to sewage.

The purpose of the invention is to increase the degree of copper recovery from spent chemical copper solutions.

The method is carried out as follows.

A granulated adsorbent, such as activated carbon or talc, is introduced into the waste solution with a surface treated with a catalyst — copper hydride formed by treating the granular adsorbent with an aqueous solution containing 80-120 g / l of sulfuric copper, 80-120 g / l of hypophofite alkali metal and 150-200 ml / l of ammonia, followed by heat treatment of the adsorbent at 160-170 s with the following ratio of components to 1 l of the spent solution: Adsorbent, g 5-20 Catalyst (as solution), ml 2.5-10

The catalyst is a copper hydride obtained as follows.

A portion of the activated carbon 5, Ø or 20 g is washed with water from coal dust5, dried and introduced into an aqueous solution containing:

I

Copper sulfuric acid, g / l

Hypophosphite sodium, g / l

Ammonia (25%)

solution, ml. 200 -170 150

incubated in it for about an hour with occasional stirring, then removed by filtration and placed in a drying oven for heat treatment at 160-170 ° C for 2.5-3 hours until the weight of red-brown is obtained n-1 dry and copper without traces of greenery

In a similar manner, a mixture of talc in the amount of 5, 10 or 20 g is prepared, which is impregnated with ruta when mixed with a solution containing copper sulfate, alkali metal HIPOPOSPHIT and aMiviHaK of composition I, II or III, respectively 2.5; 5 or 10 ml and placed in a drying cabinet for heat treatment at 160-170 ° C for 2.5-3 hours to obtain a mass of red-brown copper hydride without traces of green

120

II 100

120,100

III 80 80

ten

20

25

thirty

-15

35

40

The catalytic activity of copper is associated with hydride formation. Copper hydride catalyzes the reduction reaction of copper from solution to metal.

The test results of the catalytic activity of the system with an initial copper concentration of 2.5 g / l are presented in Table. 1 and 2.

Example 1. The composition of the spent solution:

Copper sulfuric acid ,, g / l7

Trilon B, g / l25

Formalin (37% solution J, MP / L7

Sodium hydroxide, g / l 8

The cooled seed, talc, with a surface treated with copper hydride, is poured with waste solution heated to 45 ° C, formalin is introduced to 10 ml / l and alkali to 25 g / l. The solution is kept at this temperature for 3 hours until the copper is reduced from the solution and then at room temperature for 48 hours (2 days). The precipitate containing copper is removed from the solution by filtration. After that, the complexing agent (Trilon B) in the form of EDTA is isolated from the solution in a known manner, for which the pH of the solution is adjusted to a value of 1–2 with sulfuric acid, the solution is thoroughly mixed and left for 3 hours, to accelerate the reaction 1 g / l of trylon B. The precipitate is filtered off and reused in production. After removal of the copper and complexing agent, the solution is alkalinized to pH 6.5 and drained to the sewage system.

0

II p and m e r 2. The composition of the spent solution:

Copper sulfuric acid, g / l

Potassium sodium tartrate (segenetova

salt), g / l

Formalin (37%)

solution), g / l

Sodium hydroxide, g / l16

Extraction of copper from solution is performed as in the example activated carbon, copper hydride,

B Table 3 shows the data on the residual copper content in the spent solutions, obtained with is5

80.4 4.17

primed - processed

S1357362v

Tables AZ

creator Residual content of copper ions in spent solutions of chemical sinking before draining to sewer

Extraction of copper by the proposed Extraction of copper method, mg / l, after, h, settled by the known method, mg / l

36 h48 h

0.09 (I) 0.02 (I) 16 0.08 (II) 0.016 (11)

0.1 (III) 0.02 (III)

0.08 (I) 0.02 (I) 14.5 0.06 (II) 0.018 (II)

0.09 (III) 0.02 (III)

Claims (2)

1. METHOD FOR REMOVING COPPER FROM WORKED CHEMICAL COPPER SOLUTIONS by sorption on a granular adsorbent with a surface treated with a catalyst, characterized in that, in order to increase the degree of extraction, copper hydride is used as a catalyst. 2. The method according to claim 1, with the fact that the catalytic surface is formed by treating the granulated adsorbent with an aqueous solution containing 80-120 g / l of copper sulfate, 80-120 g / l of alkali metal hypophosphite and 150-200 mp / l ammonia, followed by heat treatment of the adsorbent at 160-170 C. g * "ω 57362