CN111850565A - 一种从蚀刻废液中回收金和碘的方法 - Google Patents
一种从蚀刻废液中回收金和碘的方法 Download PDFInfo
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- CN111850565A CN111850565A CN202010686351.8A CN202010686351A CN111850565A CN 111850565 A CN111850565 A CN 111850565A CN 202010686351 A CN202010686351 A CN 202010686351A CN 111850565 A CN111850565 A CN 111850565A
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- 239000010931 gold Substances 0.000 title claims abstract description 65
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 65
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 239000007788 liquid Substances 0.000 title claims abstract description 33
- 239000002699 waste material Substances 0.000 title claims abstract description 25
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052740 iodine Inorganic materials 0.000 title claims abstract description 23
- 239000011630 iodine Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000005530 etching Methods 0.000 title claims abstract description 19
- 238000011084 recovery Methods 0.000 claims abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 claims description 24
- 239000000706 filtrate Substances 0.000 claims description 20
- 239000011347 resin Substances 0.000 claims description 18
- 229920005989 resin Polymers 0.000 claims description 18
- 239000002244 precipitate Substances 0.000 claims description 13
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical group [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 235000010265 sodium sulphite Nutrition 0.000 claims description 6
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910021595 Copper(I) iodide Inorganic materials 0.000 claims description 4
- LSXDOTMGLUJQCM-UHFFFAOYSA-M copper(i) iodide Chemical compound I[Cu] LSXDOTMGLUJQCM-UHFFFAOYSA-M 0.000 claims description 4
- 238000003723 Smelting Methods 0.000 claims description 3
- 150000001879 copper Chemical class 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 239000000779 smoke Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- 238000006722 reduction reaction Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- -1 gold ions Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229910003771 Gold(I) chloride Inorganic materials 0.000 description 1
- 239000007832 Na2SO4 Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/46—Regeneration of etching compositions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/13—Iodine; Hydrogen iodide
- C01B7/14—Iodine
-
- 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
- C22B11/00—Obtaining noble metals
- C22B11/02—Obtaining noble metals by dry processes
- C22B11/021—Recovery of noble metals from waste materials
- C22B11/025—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper, or baths
-
- 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
- C22B11/00—Obtaining noble metals
- C22B11/04—Obtaining noble metals by wet processes
- C22B11/042—Recovery of noble metals from waste materials
- C22B11/046—Recovery of noble metals from waste materials from manufactured products, e.g. from printed circuit boards, from photographic films, paper or baths
-
- 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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Metallurgy (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Removal Of Specific Substances (AREA)
Abstract
本发明属于金属回收再生技术领域，涉及一种从蚀刻废液中回收金和碘的方法，步骤包括金还原、金吸附、金提纯、精炼和碘回收。本工艺处理的综合性好，能够比较彻底地回收蚀刻废液中的金元素和碘元素，效率高，成本低，污染小。
Description
技术领域
本发明涉及金属回收再生技术领域，特别涉及一种从蚀刻废液中回收金和碘的方法。
背景技术
半导体及光电产业制造工艺中均使用蚀刻法来经行蚀刻制造工艺，含有碘化钾的溶液为常见金蚀刻液。工艺生产中产生大量报废的蚀刻液,废液中含有300～700ppm金离子和2～17％含量的碘，具有很高的回收价值。
目前市场多采树脂直接吸附或还原回收。树脂吸附金同时也吸附大量碘，在回收焚化时产生大量碘废气，造成空气污染；还原回收后废液会残留＜10ppm金，造成贵金属浪费及回收率低。两种回收方法回收后废液中都含有大量碘，目前含碘废水大都与其他废水综合处理，处理成本高且低效率。
因此，有必要提供一种新的回收方法来解决上述问题。
发明内容
本发明的主要目的在于提供一种从蚀刻废液中回收金和碘的方法，能够更彻底地回收蚀刻液中的金元素和碘元素，节约成本，减少废气排放。
本发明通过如下技术方案实现上述目的：一种从蚀刻废液中回收金和碘的方法，其步骤包括：
(1)金还原:在含碘金蚀刻废液中加入碱液并搅拌，直至pH≥11，然后加入还原剂A还原至无沉淀析出，过滤得沉淀和滤液；
(2)金吸附：将步骤(1)所得滤液过树脂塔吸附至废液含金量为0，得到含金树脂A，将含金树脂A洗涤至pH＞5，得含金树脂B和水洗液；
(3)金提纯：将含金树脂B焚化成灰渣，将步骤(1)所得沉淀与灰渣都加入王水，搅拌溶解至无黄烟产生，过滤得滤液B，将滤液B脱硝后加入还原剂B还原至液体澄清，过滤得海绵金；
(4)精炼：将步骤(3)所得海绵金在高周波炉中熔炼得到金锭；
(5)碘回收:将步骤(2)所得废液和水洗液合并，搅拌加入铜盐和还原剂C，静置脱水得碘化亚铜沉淀和滤液C。
具体的，所述碱液为氢氧化钠溶液或碳酸钠溶液。
具体的，所述还原剂A为联氨。
具体的，所述还原剂B为亚硫酸钠。
具体的，所述还原剂C为亚硫酸钠。
采用上述技术方案，本发明技术方案的有益效果是：
本工艺处理的综合性好，能够比较彻底地回收蚀刻废液中的金元素和碘元素，效率高，成本低，污染小。
具体实施方式
下面结合具体实施例对本发明作进一步详细说明。
实施例：
本发明的一种从蚀刻废液中回收金和碘的方法，其步骤包括：
(1)金还原:在含碘金蚀刻废液中加入碱液并搅拌，直至pH≥11，然后加入还原剂A还原至无沉淀析出，过滤得沉淀和滤液。
碱液为氢氧化钠溶液或碳酸钠溶液。此类碱液碱性强，不引入杂质离子或者杂质离子去除容易。
还原剂A可用联氨。此处发生的反应为：4Au3++3N2H4+12OH-＝4Au↓+3N2↑+12H2O。所以反应能将金还原，所以沉淀以金为主，且副产物只会产生无污染的氮气和水。但是还原剂A也可以选用其他可以还原金的还原剂类型。
(2)金吸附：将步骤(1)所得滤液过树脂塔吸附至废液含金量为0，得到含金树脂A，将含金树脂A洗涤至pH＞5，得含金树脂B和水洗液。本步骤能让未完全反应的金离子吸附在树脂上。
(3)金提纯：将含金树脂B焚化成灰渣，将步骤(1)所得沉淀与灰渣都加入王水，搅拌溶解至无黄烟产生，过滤得滤液B，将滤液B脱硝后加入还原剂B还原至液体澄清，过滤得海绵金。本步骤能让前两个步骤分离的金元素重新溶解在王水中，随后再让金沉淀出来，提升纯度。
王水溶金的反应为：Au+4HCl+HNO3→H(AuCl4)+NO↑+2H2O。
还原剂B可用亚硫酸钠。获得海绵金的反应为：2H(AuCl4)+7Na2SO3＝2Au↓+3Na2SO4+8NaCl+4SO2↑+H2O。但是还原剂A也可以选用其他可以还原金的还原剂类型。
(4)精炼：将步骤(3)所得海绵金在高周波炉中熔炼得到金锭。此处高周波会让金以外的可燃固体杂质燃烧除去，提高金的纯度，并且让金变成块状。
(5)碘回收:将步骤(2)所得废液和水洗液合并，搅拌加入铜盐和还原剂C，静置脱水得碘化亚铜沉淀和滤液C。
还原剂C可以选用亚硫酸钠。还原反应为：I2+Na2SO3+H2O＝2HI+Na2SO4。但是还原剂A也可以选用其他可以还原碘的还原剂类型。
沉淀反应为：2I-+2Cu2+＝2Cu2I2↓。
碘化亚铜可用于回收碘。滤液C中的碘含量＜50ppm，可以排放至废水处理。
本工艺处理的综合性好，能够比较彻底地回收蚀刻废液中的金元素和碘元素，效率高，成本低，污染小。
以上所述的仅是本发明的一些实施方式。对于本领域的普通技术人员来说，在不脱离本发明创造构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。
Claims (5)
1.一种从蚀刻废液中回收金和碘的方法，其特征在于步骤包括：
(1)金还原:在含碘金蚀刻废液中加入碱液并搅拌，直至pH≥11，然后加入还原剂A还原至无沉淀析出，过滤得沉淀和滤液；
(2)金吸附：将步骤(1)所得滤液过树脂塔吸附至废液含金量为0，得到含金树脂A，将含金树脂A洗涤至pH＞5，得含金树脂B和水洗液；
(3)金提纯：将含金树脂B焚化成灰渣，将步骤(1)所得沉淀与灰渣都加入王水，搅拌溶解至无黄烟产生，过滤得滤液B，将滤液B脱硝后加入还原剂B还原至液体澄清，过滤得海绵金；
(4)金精炼：将步骤(3)所得海绵金在高周波炉中熔炼得到金锭；
(5)碘回收:将步骤(2)所得废液和水洗液合并，搅拌加入铜盐和还原剂C，静置脱水得碘化亚铜沉淀和滤液C。
2.根据权利要求1所述的方法，其特征在于：所述碱液为氢氧化钠溶液或碳酸钠溶液。
3.根据权利要求1所述的方法，其特征在于：所述还原剂A为联氨。
4.根据权利要求1所述的方法，其特征在于：所述还原剂B为亚硫酸钠。
5.根据权利要求1所述的方法，其特征在于：所述还原剂C为亚硫酸钠。
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| CN103343224A (zh) * | 2013-07-29 | 2013-10-09 | 沈少波 | 一种含金物料中金的快速提取方法 |
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| CN105965030A (zh) * | 2016-06-20 | 2016-09-28 | 昆山鸿福泰环保科技有限公司 | 一种碘化金废液中金回收工艺 |
| CN110983065A (zh) * | 2019-12-23 | 2020-04-10 | 昆山全亚冠环保科技有限公司 | 一种还原含碘废液中的金的方法 |
-
2020
- 2020-07-16 CN CN202010686351.8A patent/CN111850565A/zh active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5026420A (en) * | 1989-05-12 | 1991-06-25 | Susumu Kubo | Purification process for gold-bearing iodine lixiviant |
| JPH03166324A (ja) * | 1989-11-24 | 1991-07-18 | Tanaka Kikinzoku Kogyo Kk | 白金の回収方法 |
| KR101392179B1 (ko) * | 2013-02-08 | 2014-05-08 | 강희남 | 백금족 금속의 회수방법 및 이에 사용되는 백금족 금속의 회수장치 |
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