CN114703369A - 一种深度脱除铜阳极泥预处理渣中铅、铋、碲的方法 - Google Patents
一种深度脱除铜阳极泥预处理渣中铅、铋、碲的方法 Download PDFInfo
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- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 38
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 31
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 20
- 239000010949 copper Substances 0.000 title claims abstract description 20
- 239000002893 slag Substances 0.000 title claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 30
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 25
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 23
- 238000002386 leaching Methods 0.000 claims abstract description 20
- 230000001698 pyrogenic effect Effects 0.000 claims abstract description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 12
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 20
- 238000003825 pressing Methods 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 16
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- 239000003513 alkali Substances 0.000 claims description 13
- 239000000706 filtrate Substances 0.000 claims description 13
- 238000006386 neutralization reaction Methods 0.000 claims description 13
- 229910045601 alloy Inorganic materials 0.000 claims description 10
- 239000000956 alloy Substances 0.000 claims description 10
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 6
- 238000011085 pressure filtration Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical compound [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 2
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- 239000002699 waste material Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 18
- 239000012535 impurity Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 229910000510 noble metal Inorganic materials 0.000 abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 3
- 229910000978 Pb alloy Inorganic materials 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- 238000005272 metallurgy Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
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- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
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- C22B11/00—Obtaining noble metals
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
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Abstract
本发明提供了一种深度脱除铜阳极泥预处理渣中铅、铋、碲的方法,采用将加压脱铜料常压盐酸浸出‑碳酸钠中和改性‑醋酸浸出脱铅工艺,有效脱除铜阳极泥预处理渣中的铅、铋、碲,并将其一一进行回收,大大降低了火法处理入炉料中的铅、铋、碲杂质品位,提高了贵金属含量,减少火法处理入炉料的处理量,为火法生产提供了保障。
Description
技术领域
本发明属于冶金技术领域,涉及铜阳极泥处理的方法,特别涉及一种深度脱除铜阳极泥预处理渣中铅、铋、碲的新方法。
背景技术
在稀贵金属冶金工业中,常常采用加压浸出工艺脱除铜阳极泥中的铜、镍、碲,主要是利用中压蒸汽在加压釜中将体系升温至150~160℃,后通入氧气,进行氧压浸出。通过此种方法可有效脱除铜、镍及少量碲等杂质金属,但是其中的铅、铋以及约50%的碲仍留在渣中无法脱除,尤其是随着铜阳极泥原料供应的日趋紧张,其贵金属含量进一步降低,杂质品位尤其是铅、铋、碲含量逐年上升,使得火法处理难度日益增大。
发明内容
针对现有技术的缺陷,本发明的目的是提供一种深度脱除铜阳极泥预处理渣中铅、铋、碲的方法。
一种深度脱除铜阳极泥预处理渣中铅、铋、碲的方法,包括如下步骤:
(1)盐酸浸出:将铜阳极泥预处理渣和浓度为1~2mol/L的盐酸溶液按固液比1:3~4混合,升温至80~85℃,恒温2~3h后压滤;
(2)碳酸钠中和改性:将步骤(1)所得的滤渣与浓度为50~60g/L的碳酸钠溶液按照固液比1:3~4混合,升温至60~70℃,反应5~6h,压滤;
(3)醋酸酸浸脱铅:将步骤(2)所得的滤渣与水按照1:2.5~3的固液比混合后搅拌升温至70~80℃,缓慢加入浓醋酸进行中和反应,至无气泡产生后压滤,滤渣通过合金炉火法处理生产金银阳极板;
(4)废液处理回收铅、铋、碲:将步骤(1)所得滤液使用液碱进行中和,控制体系温度为70~80℃,中和终点为pH=5~6,压滤,滤渣通过碲精炼碱浸分离回收碲、铋;将步骤(2)、(3)所得滤液进行混合,至无白色沉淀生成后,进行压滤,得到主要成分为硫酸铅的滤渣,通过合金生产贵铅合金。
综上所述,本发明采用将加压脱铜料常压盐酸浸出-碳酸钠中和改性-醋酸浸出脱铅工艺,有效脱除铜阳极泥预处理渣中的铅、铋、碲,并将其一一进行回收,大大降低了火法处理合金炉入炉料中的铅、铋、碲杂质品位,提高了贵金属含量,减少火法处理合金炉入炉料的处理量,为火法生产提供了保障
附图说明
图1是本发明的工艺流程图。
具体实施方式
下面通过具体实施例对本发明作进一步详细的说明。
实施例1
(1)向反应槽内,按固液比1:3加入铜阳极泥预处理渣(加压脱铜料)以及浓度为1mol/L的盐酸溶液,升温至80℃,恒温2h后压滤。
(2)将盐酸浸出所得的滤渣与浓度为50g/L的碳酸钠溶液按照固液比1:3加入反应槽内,升温至60℃,反应5h,压滤。
(3)将碳酸钠改性所得的滤渣与水按照1:2.5的比例混合后搅拌升温至70℃,缓慢加入浓醋酸进行中和反应,至无气泡产生后(pH≤3)压滤,滤渣交合金炉火法处理生产金银阳极板;合金炉入炉料(脱铅滤渣)的铅、铋、碲含量分别为:19.54%、2.11%、0.82%。
(4)将步骤(1)中的盐酸浸出所得滤液使用液碱进行中和,控制体系温度为70℃,中和终点为pH=5,压滤,滤液交氯碱车间生产液氯和氢氧化钠,滤渣交碲精炼碱浸分离回收得到碲、铋回收料,碲、铋回收料中碲、铋含量分别为:0.24%、47.7%。将步骤(2)和步骤(3)压滤后所得滤液进行混合,至无白色沉淀生成后,进行压滤,得到主要成分为硫酸铅的滤渣,通过合金生产贵铅合金,滤液主要成分为醋酸钠交中间水处理沉淀重金属。硫酸铅滤渣中铅含量为40.99%。
实施例2
向反应槽内,按固液比1:3.5加入铜阳极泥预处理渣(加压脱铜料)以及浓度为1.5mol/L的盐酸溶液,升温至83℃,恒温2.5h后压滤。
(2)将盐酸浸出所得的滤渣与浓度为55g/L的碳酸钠溶液按照固液比1:3.5加入反应槽内,升温至65℃,反应5.5h,压滤。
(3)将碳酸钠改性所得的滤渣与水按照1:3的固液比混合后搅拌升温至75℃,缓慢加入浓醋酸进行中和反应,至无气泡产生后(pH≤3)压滤,滤渣交合金炉火法处理生产金银阳极板。合金炉入炉料(脱铅滤渣)的铅、铋、碲含量分别为:17.44%、1.93%、0.76%;
(4)将步骤(1)盐酸浸出所得滤液使用液碱进行中和,控制体系温度为75℃,中和终点为Ph=5.5,压滤,滤液交氯碱车间生产液氯和氢氧化钠,滤渣交碲精炼碱浸分离回收得到碲、铋回收料,碲、铋回收料中碲、铋含量分别为:0.22%、49.75%。将步骤(2)和步骤(3)所得滤液进行混合,至无白色沉淀生成后,进行压滤,得到硫酸铅滤渣,硫酸铅滤渣中铅含量为42.35%。
实施例3
(1)向反应槽内,按固液比1:4加入铜阳极泥预处理渣(加压脱铜料)以及浓度为2mol/L的盐酸溶液,升温至85℃,恒温3h后压滤。
(2)将盐酸浸出所得的滤渣与浓度为60g/L的碳酸钠溶液按照固液比1:4加入反应槽内,升温至70℃,反应6h,压滤。
(3)将碳酸钠改性所得的滤渣与水按照1:3的比例混合后搅拌升温至80℃,缓慢加入浓醋酸进行中和反应,至无气泡产生后(pH≤3)压滤,滤渣交合金炉火法处理生产金银阳极板。合金炉入炉料(脱铅滤渣)的铅、铋、碲含量分别为:13.84%、1.58%、0.74%。
(4)将步骤(1)盐酸浸出所得滤液使用液碱进行中和,控制体系温度为80℃,中和终点为Ph=6,压滤,滤液交氯碱车间生产液氯和氢氧化钠,滤渣交碲精炼碱浸分离回收得到碲、铋回收料,碲、铋回收料中碲、铋含量分别为:0.11%、52.75%。将步骤(2)和步骤(3)所得滤液进行混合,至无白色沉淀生成后,进行压滤,得到主硫酸铅滤渣,通过合金生产贵铅合金。硫酸铅滤渣中铅含量为43.1%。
Claims (1)
1.一种深度脱除铜阳极泥预处理渣中铅、铋、碲的方法,包括如下步骤:
(1)盐酸浸出:将铜阳极泥预处理渣和浓度为1~2mol/L的盐酸溶液按固液比1:3~4混合,升温至80~85℃,恒温2~3h后压滤;
(2)碳酸钠中和改性:将步骤(1)所得的滤渣与浓度为50~60g/L的碳酸钠溶液按照固液比1:3~4混合,升温至60~70℃,反应5~6h,压滤;
(3)醋酸酸浸脱铅:将步骤(2)所得的滤渣与水按照1:2.5~3的固液比混合后搅拌升温至70~80℃,缓慢加入浓醋酸进行中和反应,至无气泡产生后压滤,滤渣通过合金炉火法处理生产金银阳极板;
(4)废液处理回收铅、铋、碲:将步骤(1)所得滤液使用液碱进行中和,控制体系温度为70~80℃,中和终点为pH=5~6,压滤,滤渣通过碲精炼碱浸分离回收碲、铋;将步骤(2)、(3)所得滤液进行混合,至无白色沉淀生成后,进行压滤,得到硫酸铅滤渣。
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王俊娥;: "铜阳极泥综合回收技术研究", 矿产保护与利用, no. 05, pages 39 - 43 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115323187A (zh) * | 2022-08-19 | 2022-11-11 | 中南大学 | 一种去除富铂族金属的铜阳极泥中SnPbFe杂质的方法 |
CN115323187B (zh) * | 2022-08-19 | 2023-08-22 | 中南大学 | 一种去除富铂族金属的铜阳极泥中SnPbFe杂质的方法 |
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