Total recycling method of PCB (printed circuit board) nitric acid type tin-lead stripping waste liquid

An all-resource, tin stripping technology, applied in chemical instruments and methods, ferric sulfate, process efficiency improvement, etc., can solve the problems of high energy consumption, high cost, low recovery rate, etc., achieve good sedimentation effect, low cost, The effect of less impurities

Inactive Publication Date: 2011-07-06
SOUTH CHINA UNIV OF TECH
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  • Summary
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  • Application Information

AI Technical Summary

Problems solved by technology

Although the added value of tin products has been improved, the cost is also high, and the recovery rate of tin, lead and copper is still low; metals are extracted by heavy catchers or sodium sulfide, because WSP contains a large amount of high iron and strong oxidant nitric acid, resulting in a great loss of reagents , and the follow-up treatment of each metal in the mixed sediment is extremely difficult, and it is even more difficult to make the waste water harmless; adding sulfuric acid to WSP can improve the extraction of lead, but the decomposition of nitric acid and the acid dissolution of stannic acid are intensified, which not only deteriorates the operating environment, Moreover, the load and difficulty of subsequent water treatment are greatly increased; the nitric acid is first distilled from WSP by distillation process, and then tin, lead and copper are separated by chemical precipitation process. The resource utilization rate of WSP has been greatly improved, but the equipment investment Large, high energy consumption, high overall cost, harsh operating environment, and serious pollution
Based on the research and development status of the past two decades at home and abroad and the current industrial reality, considering that WSP mainly includes tin-lead salts, copper salts, iron salts, nitric acid (salts) and additives (corrosion inhibitors\complexing agents, etc.), these components As a resource, it has high value, but as a pollutant, it is a hazardous waste, which requires high treatment costs and has potential safety hazards such as secondary pollution.

Method used

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  • Total recycling method of PCB (printed circuit board) nitric acid type tin-lead stripping waste liquid
  • Total recycling method of PCB (printed circuit board) nitric acid type tin-lead stripping waste liquid
  • Total recycling method of PCB (printed circuit board) nitric acid type tin-lead stripping waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The composition analysis of WSP is shown in Table 1:

[0038] Table 1

[0039]

[0040] Introduce 25368kg of the above WSP into the 30m with stirring (7.5kW, 16rpm) 3 Buried type reaction tank, add 2400kg concentration under agitation condition and be the ferrous sulfate heptahydrate solution of 50wt%, finish adding in 1 hour, continue to stir, react 0.5 hour to obtain reaction solution, reaction solution is filtered and separated solid by plate-and-frame filter Liquid phase, the obtained filter cake is washed with 1000kg of clear water, and the filtrate and cleaning solution are combined into mother liquor, and the filter cake is tin-lead mud. The total amount of tin-lead mud is 12294kg, containing 9.839wt% of tin and 6.619wt% of lead (the extraction rates of corresponding tin and lead are respectively 99.38% and 99.93%); The mother liquor of wt%) is moved into the buffer tank, fills up the contact reactor with 1000kg iron shavings, then starts the acid-resistant ...

Embodiment 2

[0043] Implementation method and step are with embodiment 1, wherein in WSP, continue to stir after adding ferrous sulfate heptahydrate solution for 1 hour, the component analysis of WSP is as shown in table 2:

[0044] Table 2

[0045]

[0046] Wherein WSP is 24983kg, 50wt% ferrous sulfate heptahydrate solution 3600kg, tin-lead mud total amount 14408kg, wherein contains tin 9.958wt%, contains lead 6.237wt% (the extraction rate of tin, lead is respectively 99.67% and 99.97%); The total amount of mother liquor is 15672kg, which contains 0.6423wt% copper and 4.591wt% iron. The total iron consumption in the copper extraction process is 1135kg, the sponge copper is 113.8kg, and contains 88.01wt% copper (copper extraction rate is 99.50%); the total amount of raffinate is 15540kg, which contains 11.93wt% iron. Adding 11,550kg of ferrous sulfate heptahydrate and 2,000kg of concentrated sulfuric acid to the system can produce about 29,000kg of modified polyiron, with an iron conte...

Embodiment 3

[0048] Implementation method and step are with embodiment 1, wherein continue to stir 2 hours after adding ferrous sulfate heptahydrate solution in WSP, the component analysis of WSP is as shown in table 3:

[0049] table 3

[0050]

[0051] WSP is 25143kg, 50wt% ferrous sulfate heptahydrate solution 5300kg, extracts tin-lead mud total amount 13542kg, wherein contains tin 10.79wt%, contains lead 5.395wt% (the extraction rate of tin is 99.92%, the extraction rate of lead is 99.99%); The total amount of mother liquor after extracting the tin-lead mud is 18506kg, which contains 0.4992wt% copper and 4.369wt% iron. The total iron consumption in the copper extraction process is 1048kg, the sponge copper is 122.2kg, and the copper content is 75.10wt% (copper extraction rate is 99.35%); the total amount of residual liquid after copper extraction is 19387kg, and the iron content is 9.575wt%. Add 5,000kg of ferrous sulfate heptahydrate and 1,500kg of concentrated sulfuric acid to th...

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Abstract

The invention provides a total recycling method of a PCB (printed circuit board) nitric acid type tin-lead stripping waste liquid. Ferrous sulfate is used as a reaction agent and a settling agent to react with the nitric acid type tin-lead stripping waste liquid; a filter cake is acquired from a reaction liquid through filtering separation, and is cleaned for the extraction of solid-phase tin-lead mud; a filter liquid and a cleaning liquid are merged to serve as a mother liquid; then iron is used as a reducing agent and a displacing agent to extract sponge copper from the mother liquid until the residual copper content in the mother liquid is lower than 1mg/L; the sponge copper is rinsed by clear water; after the sponge copper is extracted, the iron content of the residual mother liquid containing a large quantity of ion and acid is regulated through ferric salt or ferrous salt, and the acid content is regulated through acid; and after the residual mother liquid is continuously aerated through air or oxygen gas, ferrous iron is oxidized, hydrolyzed and polymerized, so as to prepare modified polymeric iron which serves as a water purifying agent. Through the method, the nitric acidtype tin-lead stripping waste liquid is totally recycled, the extraction rates of tin, lead and copper respectively exceed 99.3 percent, 99.9 percent and 99.0 percent, the yield of the modified polymeric iron reaches 100 percent, and three wastes and efflux are avoided, so that the environment is protected, and sustainable development of the PCB industry is achieved.

Description

technical field [0001] The invention relates to a treatment and comprehensive utilization method of PCB nitric acid-type tin-lead stripping waste liquid, in particular to a full-resource method for PCB nitric acid-type tin-lead stripping waste liquid. Background technique [0002] With the continuous deepening of my country's reform and opening up and the steady development of the economy, the IT industry has become an important pillar industry in our country. With the vigorous rise of the IT industry, the printed circuit board (referred to as PCB) manufacturing industry is also growing rapidly at an alarming rate. As of 2005, there were more than 3,500 PCB companies of different sizes in my country, and the total output of PCB exceeded 1.05×10 8 m 2 , has become one of the most important PCB manufacturing centers in the world. [0003] In the PCB manufacturing process, processes such as tin-lead plating, pattern etching, and tin-lead stripping need to discharge a variety...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23F1/46C02F1/62C22B7/00C22B3/46C22B13/00C22B15/00C22B25/00C01G49/14
CPCY02P10/20
Inventor 阮复昌张立志
Owner SOUTH CHINA UNIV OF TECH
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