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Method for preparing high-purity silver nitrate from photovoltaic waste silver paste

A technology of silver nitrate and silver paste, which is applied in chemical instruments and methods, silver compounds, silver compounds, etc., can solve the problems of limited high-purity yield, high production cost, and long process flow, and achieve uniform silver chloride particles, Improved purity and yield, low production cost

Active Publication Date: 2018-06-22
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] Patent CN103214022A, after nitric acid dissolves crude silver, add pure water to adjust the solution specific gravity, use nitrate containing Al, Fe, Zn, Sn, Bi, Ti as impurity remover, will certainly introduce new impurities, make the final metal ion content very high Difficult to reach below 10PPb
[0011] Patent CN102660684A uses silver-containing waste water in the production process of rhinestones, and after sedimentation, the sediment is sintered with borax, sodium salt, etc. to obtain silver ingots. Activated carbon is not effective in adsorbing impurities
[0012] In Cai Lianbing's paper "Preparation Research and Production Practice of High-Purity Silver Nitrate", the process of "synthesis-removal-crystallization-recrystallization" is used to produce high-purity silver nitrate. The process can produce silver nitrate with different purities, but the process is relatively long , the high-purity yield is limited, the production cost is higher, and it is not beneficial to expand the production of high-purity silver nitrate

Method used

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  • Method for preparing high-purity silver nitrate from photovoltaic waste silver paste

Examples

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Comparison scheme
Effect test

Embodiment 1

[0052] Such as figure 1 Shown, the method for preparing high-purity silver nitrate from photovoltaic waste silver paste, its concrete steps are as follows:

[0053] Step 1. Take 10Kg of photovoltaic waste silver paste (from a positive silver paste factory, the main components of photovoltaic waste silver paste are: silver powder 85%, glass powder (SiO 2 、 Bi 2 o 3 , PbO, MnO 2 、Al 2 o 3 etc.) 10%, organic matter 5%) at 100°C for 2 hours and ball milled for 2 hours to obtain powder;

[0054] Step 2, add pure water to the powder obtained in step 1 according to the mass ratio of 1:1.5 and heat to boiling, then add nitric acid solution with a concentration of 60wt%, the amount of nitric acid solution added is 1.0 times the mass of the powder (add in 4 times , add a total of 9.5kg), heat until the powder is completely dissolved to obtain a solution;

[0055] Step 3. Cool the solution obtained in step 2 to 30°C and filter, dilute the filtrate with water to contain 40g / L of si...

Embodiment 2

[0062] Such as figure 1 Shown, the method for preparing high-purity silver nitrate from photovoltaic waste silver paste, its concrete steps are as follows:

[0063] Step 1. Take 14Kg of photovoltaic waste silver paste (from a positive silver paste factory, the main components of photovoltaic waste silver paste are: silver powder 83%, glass powder (SiO 2 、 Bi 2 o 3 , PbO, Al 2 o 3 etc.) 5%, organic matter 10%) to obtain powder after drying at 100°C for 3 hours and ball milling for 3 hours;

[0064] Step 2, add pure water to the powder obtained in step 1 according to the mass ratio of 1:1.5 and heat it to boiling, then add nitric acid solution with a concentration of 60wt%, the amount of nitric acid solution added is 1.4 times the mass of the powder (add in 12 times , add a total of 18kg), heat until the powder is completely dissolved to obtain a solution;

[0065] Step 3. Cool the solution obtained in step 2 to 40°C and filter, dilute the filtrate with water to contain 50...

Embodiment 3

[0072] Such as figure 1 Shown, the method for preparing high-purity silver nitrate from photovoltaic waste silver paste, its concrete steps are as follows:

[0073]Step 1. Take 16.74Kg of photovoltaic waste silver paste (from a positive silver paste factory, the main components of photovoltaic waste silver paste are: 70% silver powder, glass powder (SiO 2 、 Bi 2 o 3 , PbO, Al 2 o 3 etc.) 3%, organic matter 15%) to obtain powder after drying at 100°C for 3 hours and ball milling for 3 hours;

[0074] Step 2. Add pure water to the powder obtained in step 1 according to the mass ratio of 1:1.5 and heat it to boiling, then add nitric acid solution with a concentration of 63wt%, and the amount of nitric acid solution added is 1.1 times the mass of the powder (add in 12 times) , add a total of 13.4kg), heat until the powder is completely dissolved to obtain a solution;

[0075] Step 3. Cool the solution obtained in step 2 to 40°C and filter, dilute the filtrate with water to c...

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Abstract

The invention relates to a method for preparing high-purity silver nitrate from photovoltaic waste silver paste, and belongs to the technical field of silver nitrate preparation. The method comprisesthe following steps: drying photovoltaic waste silver paste, carrying out ball milling to obtain powder; adding pure water, carrying out heating to boiling, then adding a nitric acid solution, and carrying out heating until the powder completely dissolves; carrying out cooling to 30-40 DEG C for filtering, adjusting the solution concentration, and adding a sodium chloride solution for precipitating silver; adding the obtained silver chloride filter cake in ammonia water for dissolution to obtain a silver-ammonia solution, adding hydrochloric acid into the silver-ammonia solution, and carryingout mechanical stirring for precipitating silver again; directly reducing the obtained silver chloride filter cake with hydrazine hydrate or a formaldehyde solution to obtain coarse silver powder, andsintering the silver powder; adding the silver powder into nitric acid of 40wt%-50wt% for dissolution, adding a regulator, and pouring the obtained solution into a rotary evaporator, and carrying outvacuum concentration until a small amount of crystals appear; and pouring the solution into a crystallizer for crystallization, filtering the remaining small amount of liquid during the crystallization, and drying the obtained crystals to obtain the high-purity silver nitrate. The method has high recovery rate, simple process, short recovery period and low cost, and is suitable for laboratories and industrial popularization.

Description

technical field [0001] The invention relates to a method for preparing high-purity silver nitrate from photovoltaic waste silver paste, and belongs to the technical field of silver nitrate preparation. Background technique [0002] The development of industry has improved people's living standards, but it has also seriously polluted the natural environment on which they live. Excessive extraction of resources has caused people to face energy depletion, and the growth of population has increased the consumption of energy. The development and utilization of new energy is imminent, and the green renewable resource solar power has developed rapidly in recent years. Silver paste is the most important conductive electrode in solar cells. It is prepared by superfine silver powder and screen-printed on the battery sheet, and finally sintered. At present, the annual consumption of silver paste in my country is about 3,000 tons, and it is on the rise every year, and the silver conten...

Claims

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Application Information

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IPC IPC(8): C01G5/00
CPCC01G5/00C01P2006/80
Inventor 苏绍晶胡劲冯旭王玉天王开军段云彪张维均傅强吴煦
Owner KUNMING UNIV OF SCI & TECH
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