CN1158904A - Recovering method of platinum and lead in anode sludge from electrolytic hydrogen peroxide solution production - Google Patents

Abstract

The present invention features that after anode sludge is NaOH-soaked and digested, coarse lead is recovered from soaked liquor through electrical deposition, gypsum is recovered from mother liquor through lime regeneration, pure platinum product is obtained from soaked slag through aqua regia dissolution, sulfuric acid eliminating of residual lead and routine purification, and the filteration liquid returns for NaOH soaking after testing and replenishing concentration. Being simple and no pollution to environment, the said method has good lead-eliminating effect and can obtain pure platinum product with 99.9% purity.

Description

Reclaim platinum and plumbous method from the anode sludge of electrolytic hydrogen peroxide solution production

The wet method that the present invention relates to precious metal is refined, and particularly the anode sludge from electrolytic hydrogen peroxide solution production reclaims platinum and lead.

Reclaim platinum and lead from the anode sludge of electrolytic hydrogen peroxide solution production, traditional extracting method is with anode sludge melting lead 2-base alloy, with enrichment platinum, will extract platinum behind the alloy ash stripping lead again, consumes greatly, and environmental pollution is serious.

" precious metal ", 1992,13 (2), P.30-34 reported a kind of " the high pressure dearsenification of the lead anode slurry of the low gold and silver of high arsenic " technology.This article is a raw material with the low gold and silver lead anode slurry of high arsenic, adopts pressurization to leach dearsenification; Dearsenification slag nitration mixture leaches antimony, bismuth, copper, lead; Leached mud melting, electrolysis get finished product silver; Silver anode slime is carried gold.Leach in the operation in pressurization, this article NaOH digestion (concentration 30-80g/L is good with 50g/L), digestion temperature 110-150 ℃ (150 ℃ is good), and time 2-4 hour (2 hours is good), oxygen is pressed 6kg/cm ², stagnation pressure 6.8kg/cm ²。The arsenic extrusion rate of this article is at 73.4-94.14%, takes off the gold and silver alloy of output purity-99% behind the antimony bismuth copper-lead.This technology purpose is to leach dearsenification, and lead is stayed and soaked in the slag, and this technology needs high-tension apparatus, operates not too safe.

The objective of the invention is to overcome the weak point that prior art exists, provide a kind of from the anode sludge of electrolytic hydrogen peroxide solution production the wet high-effective deleading, reclaim platinum and plumbous method with prior art then.Use the inventive method, environment do not polluted, and consume low, direct output lead bullion, and obtain pure platinum product very soon.

Technical scheme of the present invention is with the NaOH digestion anode sludge, with efficient deleading, uses prior art then and reclaims platinum and lead.

The inventive method comprises with the NaOH digestion anode sludge, it is characterized in that having following concrete operation:

A, at solid-liquid than (be the solid/liquid ratio, unit is g/mL or kg/L)=1: 8-25, in the 100-300g/L NaOH solution, under the temperature 20-95 ℃ of condition, the said anode sludge 1-4 of agitation leach hour;

B, leach liquor be at 1-3V, 100-300A/cm ²The direct current electrodeposition is 6-20 hour under the current density, and output also reclaims lead bullion;

C, electrodeposition mother liquor add 0.1-0.5 times of heavy lime of anode pug or milk of lime, under the 60-95 ℃ of condition, stir the output gypsum deposition and the NaOH that regenerates 1-4 hour;

D, the regeneration NaOH solution that removes gypsum return NaOH digestion operation A through calibrating concentration, after replenishing loss;

E, NaOH digestion slag add H through aqua regia dissolution, after catching up with nitre ₂SO ₄, be PbSO to precipitate residual lead ₄

Solution behind f, the deleading is purified and the pure platinum of output with ordinary method.

Compare with prior art, the present invention has following advantage:

1, the inventive method is free from environmental pollution, obvious social benefit;

2, NaOH can regenerate, so consume low;

3, can attached product lead bullion;

4, device simple, simple to operate;

5, the pure platinum product of very fast acquisition is good in economic efficiency.

Embodiment 1

A kind of anode sludge of electrolytic hydrogen peroxide solution production gained, its main component is: Pb56.87 (weight %), Pt423.5g/t. get the said anode sludge of 200 grams, at solid-liquid than 1: 15, in the 200g/L NaOH solution, 90 ℃ of following agitation leachs 2 hours.Filtrate and wash water are under normal temperature (20 ℃), at 3V, 150A/cm ²The direct current electrodeposition is 8 hours under the condition, and output contains the lead bullion of 70%Pb.Leached mud slag rate only 4%.

The electrodeposition mother liquor adds 100 gram lime, and 80 ℃ were stirred the output gypsum 2 hours down.Mother liquor returns next time through calibrating concentration and after replenishing 7%NaOH and leaches.NaOH digestion slag adds H through aqua regia dissolution, after catching up with nitre ₂SO ₄, be PbSO to precipitate residual lead ₄Solution behind the deleading is purified and the pure platinum of output with precipitation ammonium chloroplatinate method.Product purity 99.9%, the rate of recovery 97% of platinum.

Embodiment 2

Get the said anode sludge 100 grams of embodiment 1,, obtain 6 gram leached muds in agitation leach 4 hours in 120g/L NaOH2.5L solution under 23 ℃.The latter adds H through aqua regia dissolution, after catching up with nitre ₂SO ₄, be PbSO to precipitate residual lead ₄, obtain platiniferous solution.The NaOH leached mud is through 23 ℃, 3V, 100A/cm ²Electrodeposition reclaimed plumbous in 15 hours, and the electrodeposition mother liquor adds 20 gram lime, and 80 ℃ were stirred 2 hours down, output gypsum, and regeneration NaOH.Platiniferous solution is purified and the pure platinum of output with precipitation ammonium chloroplatinate method.Product purity 99.9%, the rate of recovery 97% of platinum.

Embodiment 3

The described anode sludge 100 grams of embodiment 1, than 1: 10, agitation leach 4 hours in regenerated NaOH (concentration adds to 280g/L) 1L solution obtains 20 and restrains leached muds under 80 ℃ at solid-liquid.Latter's agitation leach 2 hours in regenerated NaOH (concentration adds to 280g/L) 0.4L solution obtains 10 gram leached muds.The agitation leach 2 hours in regenerated NaOH (concentration adds to 280g/L) 0.4L solution again of this leached mud obtains 4 gram leached muds.Latter's enrichment whole platinum.

Three leach liquors are pressed method electrodeposition recovery lead bullion and the lime regeneration NaOH of embodiment 1.The method of enriched substance embodiment 1 obtains pure platinum product through the aqua regia dissolution platinum of purifying.

Claims (2)

1, a kind of anode sludge from electrolytic hydrogen peroxide solution production reclaims platinum and plumbous method, comprises with the NaOH digestion anode sludge, it is characterized in that having following concrete operation:

A, at solid-liquid than (be the solid/liquid ratio, unit is g/mL or kg/L)=1: 8-25, in the 100-300g/L NaOH solution, under the temperature 20-95 ℃ of condition, the said anode sludge 1-4 of agitation leach hour;

B, leach liquor be at 1-3V, 100-300A/cm ²The direct current electrodeposition is 6-20 hour under the current density, and output also reclaims lead bullion;

C, electrodeposition mother liquor add 0.1-0.5 times of heavy lime of anode pug or milk of lime, under 60～95 ℃ of conditions, stir the output gypsum deposition and the NaOH that regenerates 1-4 hour;

D, the regeneration NaOH solution that removes gypsum return NaOH and leach and boil preface A through calibrating concentration, after replenishing loss;

E, NaOH digestion slag add H through aqua regia dissolution, after catching up with nitre ₂SO ₄, be PbSO to precipitate residual lead ₄

Solution behind f, the deleading is purified and the pure platinum of output with ordinary method.

2, according to the method for claim 1, it is characterized in that the solid-liquid ratio in operation A is 15-20, the concentration of NaOH is 180-200g/L.