CN102268550A - Recovering method of zinc in waste circuit board - Google Patents
Recovering method of zinc in waste circuit board Download PDFInfo
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- CN102268550A CN102268550A CN2011102115307A CN201110211530A CN102268550A CN 102268550 A CN102268550 A CN 102268550A CN 2011102115307 A CN2011102115307 A CN 2011102115307A CN 201110211530 A CN201110211530 A CN 201110211530A CN 102268550 A CN102268550 A CN 102268550A
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Abstract
The invention relates to a recovering method of zinc in a waste circuit board. The method comprises the following steps: firstly, smashing the waste circuit board to the grain size of 0.08-1.2mm, so that metal substances (copper, zinc and the like) in the circuit board are mutually dissociated with nonmetallic substances; then carrying out high-voltage electrostatic separation on a mixed material obtained by smashing so that the metal part is separated from the nonmetal part so as to obtain a mixed metal concentrate; carrying out zinc evaporation on the obtained zinc-containing mixed metal concentrate which is used as a raw material in a vacuum furnace; and finally, condensing zinc steam on a condenser. By using the method, the recovery rate of zinc reaches above 90%, the purity of zinc reaches above 99%, and the content of copper in the mixed metal is increased to above 98%, thus zinc is separated out of the mixed metal; and simultaneously, the purity of copper is improved. The method has the characteristics of low cost, high efficiency, no pollution and the like.
Description
Technical field
The present invention relates to waste and old circuit board, the recovery method of zinc in particularly a kind of waste and old circuit board.
Background technology
Infant industry waste-electron wastes appears in the high speed development along with electronic information industry: comprise electronic instrument that various waste computers, signal equipment, televisor, refrigerator, washing machine and unit eliminate etc.Estimate that according to the expert surplus the electrical equipment about 2800 such as the refrigerator that China scraps present every year, washing machine, computer, air-conditioning ten thousand, depleted electronic apparatus total amount reaches 1,000,000 tons.
In electron wastes, the content of metal is up to about 60%, and the rich ore metal content of occurring in nature only 3～5%.Waste printed circuit board is a kind of in the electron wastes, and the metal that wherein contains is tens times even a hundred times of natural mineral reserve, and domestic annual treatment capacity is approximately 5～80,000 tons.Circuit card is the mixture of glass fiber-reinforced resin and multiple metal, and wherein metal and nonmetal combining closely are separated difficulty, are the most complicated in the electron wastes, the most unmanageable.Therefore, require during processing with high content of technology.
Present waste and old circuit board resource treatment technique mainly contains hydrometallurgy, pyrometallurgy, mechanical treatment or several treatment technology and combines, because mechanical treatment is easily realized through engineering approaches, can't produce secondary pollution, and this method is favourably welcome.Chinese invention patent " a kind of hybrid metal reclaims the method for valuable material " (Wang Wenbin, the patent No. 98105592.3) with waste and old hybrid metal successively through shredding, pulverize, bang, efflorescence and in tank gravitational segregation, realize separating of metal and non-metallic material.Chinese invention patent " process for breaking, separating and recovering and the equipment used thereof of useless hybrid metal " (Shen Zhigang etc., the patent No. 99102862.7) waste and old hybrid metal is broken, carefully breaks through thick successively, pass through vibrosieve then, adopt airflow separator then, the realization metal separates with nonmetallic substance.Separate with nonmetallic though above method can realize metal, what obtain after separating is mixed metal particles, must carry out the separation of hybrid metal and purify, and the metal of recovery just can reach resource utilization.Document " reclaiming the research of gold and copper from printed circuit board waste material " (Zhu Ping etc., " rare metal " 2002 the 3rd phases) has been introduced the employing hydrometallurgical technology and has been reclaimed metallic element in the printed circuit board waste material.But the subject matter that exists is that chemical consumption is big, the processing of waste liquid will cause secondary pollution, document " electron wastes present situation and resource technology thereof both at home and abroad " (Wei Jinxiu etc., " Donghua University's journal " the 3rd phase in 2005) has been introduced and has been adopted electrolytic process to carry out the separation of hybrid metal.But, in electrolytic process, produce problems such as obnoxious flavoures such as hydrogen fluoride, carbon monoxide, sulfurous gas and waste electrolyte serious environment pollution.And these methods mainly lay particular emphasis on and extract precious metal and rare metal from circuit cards.And along with the raising of production level, the improvement of production technique, the content of precious metal, rare metal reduces relatively gradually in the circuit card, thereby how effectively to separate and reclaim other non-ferrous metals (for example zinc) and seem especially important.
Summary of the invention
The objective of the invention is to deficiency at above-mentioned prior art existence, the recovery method of zinc in a kind of waste and old circuit board is provided, zinc is able to Separation and Recovery, purity with copper in the mixed metal particles improves simultaneously, realizes recovery, regeneration and recycling treatment to metallic zinc in the waste and old circuit board and copper.
For realizing this purpose, technical solution of the present invention is as follows:
The recovery method of zinc in a kind of waste and old circuit board, adopted fragmentation to dissociate-high pressure static electricity sorting enrichment-vacuum metallurgy method for separating and recovering, its principle is at first that zinciferous waste and old circuit board process is broken, particle diameter reaches 0.08-1.2mm, makes that the metallics (copper, zinc etc.) in the circuit card dissociates mutually with nonmetallic substance; With the mixture process high pressure static electricity sorting that obtains after the fragmentation, the metal part is separated with non-metallic part then, obtain the hybrid metal enrich body; At last, under same temperature, have different vapour pressures,, volatile metallic zinc is evaporated under suitable temperature, be separated from each other, thereby realize comprehensive utilization and reclaim with metal such as copper in a vacuum by evaporation and condensation based on each component of hybrid metal.
At the separation of zinc in the mixed metal particles, the present invention at first heats zinciferous hybrid metal enrich body (particle diameter 0.08-1.2mm) in vacuum oven, be 1 * 10 in vacuum tightness
-2～1 * 10
2Pa, temperature are to carry out the zinc evaporation under 600～850 ℃ of conditions, carry out zinc vapor condensation by condenser simultaneously, and condensing temperature is 100～400 ℃.Zinc is separated from hybrid metal thus.Specifically may further comprise the steps:
1, zinciferous waste and old circuit board being crushed to particle diameter is 0.08-1.2mm;
2, with the mixture process high pressure static electricity sorting that obtains after the fragmentation, the scope of its corona electrode voltage is 10kv～50kv, obtains containing the powder of zinc hybrid metal enrichment;
3, be raw material with the described powder that contains the enrichment of zinc hybrid metal, the crucible of putting into plumbago crucible or adopting high-temperature refractory to tie a knot is put into vacuum oven to crucible again;
4, startup vacuum system in vacuum oven sealing back is bled, and the pressure that makes vacuum oven is 1 * 10
-2～1 * 10
2Pa;
5, start the vacuum furnace power supply, raw material in the crucible is heated to 600～850 ℃, keep temperature-resistant then, make zinc evaporation in the raw material, evaporation time is 1～3 hour;
6, described zinc fume is able to condensation on condenser, and condensing temperature is 100～400 ℃, and zinc recovery reaches more than 90%, purity reaches more than 99%, the content of copper rises to more than 98% in the hybrid metal, and zinc is separated from hybrid metal thus, has improved the purity of copper simultaneously.
Compared with prior art, the recovery method of zinc is simple in the waste and old circuit board of the present invention, has characteristics such as cost is low, efficient, pollution-free, and the hybrid metal that vacuum separation finishes can continue on for next step pointed purification to be separated.Compare the method that methods such as adopting baked wheaten cake and pickling reclaims valuable metal in the waste metal, the present invention especially has advantage aspect the minimizing environmental pollution.
Description of drawings
Fig. 1 is the schema of the recovery method of zinc in the waste and old circuit board of the present invention.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is further described, but should limit protection scope of the present invention with this.
Please consult Fig. 1 earlier, figure is the schema of the recovery method of zinc in the waste and old circuit board of the present invention.As shown in the figure, the recovery method of zinc comprises the following steps: in the waste and old circuit board
The waste and old circuit board that at first will contain zinc obtains the mixture that particle diameter is 0.08-1.2mm through broken;
Then mixture is carried out the high pressure static electricity sorting, obtain containing the hybrid metal enrich body of zinc;
At last, will contain the hybrid metal enrich body of zinc, separate purification, under suitable operating parameters, obtain metallic zinc (purity＞99%) and metallic copper (purity＞98%) through the vacuum metallurgy partition method.
Embodiment 1
At first waste and old circuit board is broken into the mixture that particle diameter is 0.08-0.1mm, then, through the high pressure static electricity sorting, corona electrode voltage is 10kv, obtains containing zinc hybrid metal enrich body raw material 50g, and copper accounts for 95wt%, zinc accounts for 5wt%, puts into crucible, again crucible is put into vacuum oven.Vacuum oven sealing back starts vacuum system bleeds, and makes the vacuum tightness of vacuum oven be in 1. * 10
-2Pa; Start the heating member heating crucible in the vacuum oven, mixed metal particles in the crucible is heated to 600 ℃.Keep temperature-resistant then, make zinc evaporation in the raw material, evaporation time is 1 hour.Zinc fume is able to condensation on condenser, condensing temperature is 100 ℃, reclaims zinc 2.3g, and zinc recovery is 94.0%, and purity is 99.2%, and the content of copper rises to 98.3% in the hybrid metal.The hybrid metal that evaporates carries out next step and continues the separation of purifying.
Embodiment 2
At first waste and old circuit board is broken into the mixture that particle diameter is 1.0-1.2mm, then, through the high pressure static electricity sorting, corona electrode voltage is 50kv, obtains containing zinc hybrid metal enrich body raw material 5g, and copper accounts for 95wt%, zinc accounts for 5wt%, puts into crucible, again crucible is put into vacuum oven.Vacuum oven sealing back starts vacuum system bleeds, and makes the vacuum tightness of vacuum oven be in .1 * 10
2Between the Pa.Start the melting heating member heating crucible in the vacuum oven, hybrid metal in the crucible is heated to 850 ℃.Keep temperature-resistant then, make zinc evaporation in the raw material, evaporation time is 3 hours.Zinc fume is able to condensation on condenser, condensing temperature is 400 ℃, and zinc recovery is 95.7%, and purity is 99.4%, and the content of copper rises to 99.7% in the hybrid metal.The hybrid metal that evaporates carries out next step and continues the separation of purifying.
Embodiment 3
At first waste and old circuit board is broken into the mixture that particle diameter is 0.2-1.0m, then, through the high pressure static electricity sorting, corona electrode voltage obtains containing zinc hybrid metal enrich body raw material 8g at 20kv, and copper accounts for 95wt%, zinc accounts for 5wt%, puts into crucible, again crucible is put into vacuum oven.Vacuum oven sealing back starts vacuum system bleeds, and makes the vacuum tightness of vacuum oven be in 5.0 * 10
2Pa.Start the melting heating member heating crucible in the vacuum oven, hybrid metal in the crucible is heated to 750 ℃.Keep temperature-resistant then, make zinc evaporation in the raw material, evaporation time is 1.5 hours.Zinc fume is able to condensation on condenser, condensing temperature is 270 ℃, and zinc recovery is 92.2%, and purity is 99.0%, and the content of copper rises to 99.5% in the hybrid metal.The hybrid metal that evaporates carries out next step and continues the separation of purifying.
Embodiment 4
At first waste and old circuit board is broken into the mixture that particle diameter is 0.1-1.2mm, then, through the high pressure static electricity sorting, corona electrode voltage obtains containing zinc hybrid metal enrich body raw material 8g at 30kv, and copper accounts for 95wt%, zinc accounts for 3wt%, puts into crucible, again crucible is put into vacuum oven.Vacuum oven sealing back starts vacuum system bleeds, and makes the vacuum tightness of vacuum oven be in 1.6 * 10
1Pa.Start the melting heating member heating crucible in the vacuum oven, hybrid metal in the crucible is heated to 800 ℃.Keep temperature-resistant then, make zinc evaporation in the raw material, evaporation time is 2.5 hours.Zinc fume is able to condensation on condenser, condensing temperature is 346 ℃, and zinc recovery is 92.9%, and purity is 99.3%, and the content of copper rises to 98.8% in the hybrid metal.The hybrid metal that evaporates carries out next step and continues the separation of purifying.
Embodiment 5
At first waste and old circuit board is broken into the mixture that particle diameter is 1.0-1.2mm, then, through the high pressure static electricity sorting, corona electrode voltage obtains containing zinc hybrid metal enrich body raw material 8g at 45kv, and copper accounts for 95wt%, zinc accounts for 3wt%, puts into crucible, again crucible is put into vacuum oven.Vacuum oven sealing back starts vacuum system bleeds, and makes the vacuum tightness of vacuum oven be in 8 * 10
-2Pa.Start the melting heating member heating crucible in the vacuum oven, hybrid metal in the crucible is heated to 650 ℃.Keep temperature-resistant then, make zinc evaporation in the raw material, evaporation time is 2.5 hours.Zinc fume is able to condensation on condenser, condensing temperature is 150 ℃, and zinc recovery is 91.5%, and purity is 99.1%, and the content of copper rises to 98.2% in the hybrid metal.The hybrid metal that evaporates carries out next step and continues the separation of purifying.
Claims (4)
1. the recovery method of zinc in the waste and old circuit board, comprise that the waste and old circuit board that will contain zinc is through break process, carry out the high pressure static electricity sorting process again, acquisition contains the hybrid metal enrich body of zinc, it is characterized in that the described hybrid metal enrich body that contains zinc is carried out the vacuum metallurgy separating treatment.
2. the recovery method of zinc in the waste and old circuit board as claimed in claim 1 is characterized in that described break process is to contain the waste and old circuit board fragmentation of zinc, obtains the mixture that particle size range is 0.08-1.2mm.
3. the separation and recovery method of zinc in the waste and old circuit board as claimed in claim 1 is characterized in that the voltage range of corona electrode is at 10kv-50kv in the described high pressure static electricity sorting process.
4. the recovery method of zinc in the waste and old circuit board as claimed in claim 1 is characterized in that described vacuum metallurgy separating treatment comprises the steps:
1. be raw material with the described hybrid metal enrich body that contains zinc, the crucible of putting into plumbago crucible or adopting high-temperature refractory to tie a knot is put into vacuum oven to crucible again;
2. the sealed vacuum stove starts vacuum system and bleeds, and the pressure that makes vacuum oven is 1 * 10
-2～1 * 10
2Pa;
3. start the vacuum oven power supply, mixed metal particles in the crucible is heated to 600～850 ℃, keep temperature-resistant then, make the zinc evaporation in the raw material, evaporation time is 1～3 hour;
4. zinc fume condensation on condenser, condensing temperature are 100～400 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102115307A CN102268550A (en) | 2011-07-27 | 2011-07-27 | Recovering method of zinc in waste circuit board |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102115307A CN102268550A (en) | 2011-07-27 | 2011-07-27 | Recovering method of zinc in waste circuit board |
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| CN102268550A true CN102268550A (en) | 2011-12-07 |
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|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104505525A (en) * | 2014-12-17 | 2015-04-08 | 华东师范大学 | Method for preparing nano zinc powder by using waste zinc-manganese battery |
| CN106834694A (en) * | 2017-01-03 | 2017-06-13 | 长沙汇聚环境技术有限公司 | A kind of recovery method of waste printed circuit board metals resources |
| CN112813266A (en) * | 2020-12-30 | 2021-05-18 | 重庆凯歌电子股份有限公司 | Waste treatment system for PCB |
| CN113321236A (en) * | 2020-07-31 | 2021-08-31 | 上海交通大学 | Method for preparing zinc sulfide ultrafine powder by using zinc skins of waste zinc-manganese battery |
| CN114574701A (en) * | 2022-02-24 | 2022-06-03 | 西南交通大学 | Recovery and extraction device and method for metal in circuit board |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1654124A (en) * | 2005-02-03 | 2005-08-17 | 上海交通大学 | Breaking and high tension electrostatic separating method for worn-out printed circuit board |
| CN1760384A (en) * | 2005-11-03 | 2006-04-19 | 上海交通大学 | Vacuum distillation method for separating zinc element from mixed metals in worn-out printing circuit board |
-
2011
- 2011-07-27 CN CN2011102115307A patent/CN102268550A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1654124A (en) * | 2005-02-03 | 2005-08-17 | 上海交通大学 | Breaking and high tension electrostatic separating method for worn-out printed circuit board |
| CN1760384A (en) * | 2005-11-03 | 2006-04-19 | 上海交通大学 | Vacuum distillation method for separating zinc element from mixed metals in worn-out printing circuit board |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104505525A (en) * | 2014-12-17 | 2015-04-08 | 华东师范大学 | Method for preparing nano zinc powder by using waste zinc-manganese battery |
| CN106834694A (en) * | 2017-01-03 | 2017-06-13 | 长沙汇聚环境技术有限公司 | A kind of recovery method of waste printed circuit board metals resources |
| CN106834694B (en) * | 2017-01-03 | 2019-05-21 | 大连易舜绿色科技有限公司 | A kind of recovery method of waste printed circuit board metal resource |
| CN113321236A (en) * | 2020-07-31 | 2021-08-31 | 上海交通大学 | Method for preparing zinc sulfide ultrafine powder by using zinc skins of waste zinc-manganese battery |
| CN112813266A (en) * | 2020-12-30 | 2021-05-18 | 重庆凯歌电子股份有限公司 | Waste treatment system for PCB |
| CN114574701A (en) * | 2022-02-24 | 2022-06-03 | 西南交通大学 | Recovery and extraction device and method for metal in circuit board |
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Application publication date: 20111207 |