CN113199033A - 一种高纯铑粉的制备方法 - Google Patents
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- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910052703 rhodium Inorganic materials 0.000 claims abstract description 54
- 239000010948 rhodium Substances 0.000 claims abstract description 54
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 230000009467 reduction Effects 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 15
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 12
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims abstract description 12
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 11
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 11
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 11
- 230000000536 complexating effect Effects 0.000 claims abstract description 10
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- ZJRXSAYFZMGQFP-UHFFFAOYSA-N barium peroxide Chemical compound [Ba+2].[O-][O-] ZJRXSAYFZMGQFP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 7
- 239000010953 base metal Substances 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 230000001376 precipitating effect Effects 0.000 claims abstract description 7
- 235000010288 sodium nitrite Nutrition 0.000 claims abstract description 6
- 238000010668 complexation reaction Methods 0.000 claims abstract description 4
- 239000003456 ion exchange resin Substances 0.000 claims abstract description 4
- 229920003303 ion-exchange polymer Polymers 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 7
- 239000003729 cation exchange resin Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims 2
- 159000000000 sodium salts Chemical class 0.000 claims 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 22
- 229910052697 platinum Inorganic materials 0.000 abstract description 10
- 238000001556 precipitation Methods 0.000 abstract description 6
- 229910000510 noble metal Inorganic materials 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 3
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- -1 platinum group metals Chemical class 0.000 description 1
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- HSSMNYDDDSNUKH-UHFFFAOYSA-K trichlororhodium;hydrate Chemical compound O.Cl[Rh](Cl)Cl HSSMNYDDDSNUKH-UHFFFAOYSA-K 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
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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
- 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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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
本发明公开了一种高纯铑粉的制备方法,其步骤包括:(1)焙烧;(2)溶解;(3)铵盐还原除杂;(4)络合;(5)沉淀铑;(6)铑液制取;(7)水合肼还原;(8)氢还原。本发明将含铑残渣与过氧化钡熔融后,将贵金属铂、铑氧化成可溶解的氧化物,用盐酸溶解,然后用氯化铵沉淀法分离铂和铑,然后将含铑的滤液用亚硝酸钠溶液络合后调节PH,用氯化铵沉淀法沉淀铑,得铑液,再用离子交换树脂去除贱金属,最后水合肼还原、氢还原得铑粉,该方法具有工艺简单,提纯周期短,操作方便,等优点,而且废气废物排放少,有利于保护环境,并且对设备要求简单。
Description
技术领域
本发明涉及贵金属制备方法技术领域,具体为一种高纯铑粉的制备方法。
背景技术
铑是极其重要的贵金属元素,最大特点是其催化活性和选择性高。据统计,世界上90%以上的铑都用于汽车尾气净化催化剂;同时, 铑在化工、 航空航天、电子等行业中也占有重要的地位。铑在溶液中的化学性质十分复杂, 与其他贵金属的分离一直是铂族金属提取精炼和化学分析中的难题。自然界中,铑存在于铂矿中,且纯度较低,含有大量其他杂志贱金属。
专利CN102557155 A公开了一种从含铑废液中回收铑制备水合三氯化铑的方法,采用水合肼将铑废液中含有的铑沉淀出来,减压过滤、洗涤,沉淀用盐酸、过氧化氢处理转化为较纯的氯铑酸溶液。
专利CN101275184 B、CN100308707 C、CN100410395 C公开了铑的回收方法,都是从六铑氯酸铵水溶液中添加甲酸,以铑黑的形式还原回收铑后, 将铑黑在氢气氛中700~900°C烧结,得到海绵铑。
在资源缺乏的情况下,充分利用国内铂族金属矿产资源及二次资源回收就显得越来越重要。铂铑的制备方法可以从铂族金属矿产资源经过层层提炼获得,也可以回收提纯应用中失效的铂铑制品。由于矿产资源非常稀少,目前主要采用回收提纯应用中失效的铂铑制品,因此我们需要将纯铑从铂矿中分离提纯。为此我们提出一种高纯铑粉的制备方法用于解决上述问题。
发明内容
本发明的目的在于提供一种高纯铑粉的制备方法,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:一种高纯铑粉的制备方法,包括以下步骤:
(1)焙烧:将含铑残渣与过氧化钡混合均匀,进行焙烧;
(2)溶解:将焙烧后的混合物进行冷却,加入盐酸溶解并稀释;
(3)铵盐还原除杂:往铑溶液中加入铵盐,将还原生成的黑色粉末过滤,得到滤液,滤液加水稀释;
(4)络合:将步骤(3)中稀释的滤液加热,用亚硝酸钠溶液络合,调节PH,冷却后过滤;
(5)沉淀铑:将过滤的络合液放入冰浴中冷却,加入氯化铵沉淀铑,得到白色沉淀物,用5%-10%的氯化铵溶液洗涤;
(6)铑液制取:将上述得到的白色沉淀用盐酸溶解;
(7)水合肼还原:将上述溶液过滤后用氢氧化钠调节溶液PH至1-3.5,去除溶液中的贱金属,通过阳离子交换树脂除杂,加入水合肼煮沸还原得到铑黑;
(8)氢还原:将上述所得到的铑黑在氢还原炉中还原,碾碎得到纯铑粉。
与现有技术相比,本发明的有益效果是:本发明将含铑残渣与过氧化钡熔融后,将贵金属铂、铑氧化成可溶解的氧化物,用盐酸溶解, 然后用氯化铵沉淀法分离铂和铑,然后将含铑的滤液用亚硝酸钠溶液络合后调节PH,用氯化铵沉淀法沉淀铑,得铑液,再用离子交换树脂去除贱金属,最后水合肼还原、氢还原得铑粉,该方法具有工艺简单,提纯周期短,操作方便,等优点,而且废气废物排放少,有利于保护环境,并且对设备要求简单。
附图说明
图1为本发明工艺流程示意图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
在本发明的描述中,需要理解的是,术语“上”、“下”、“顶”、“底”、“内”、“外”、“前”、“后”、“左”、“右”等指示的方位或位置关系为基于附图1所示的方位或位置关系,仅是为了便于描述本发明和简化描述,而不是指示或暗示所指的装置或结构必须具有的特定方位、以特定的方位构造和操作,因此不能理解为对本发明的限制。
请参阅图1,本发明提供一种技术方案:一种高纯铑粉的制备方法,包括(1)焙烧:将含铑残渣与过氧化钡混合均匀,进行焙烧,含铑残渣与过氧化钡按照1∶4.2-6.5的重量比充分混合均匀,然后将混合物在800-950°C焙烧;(2)溶解:将焙烧后的混合物进行冷却,加入盐酸溶解,溶解后加入0.6-0.7倍的氯化钠溶液稀释;(3)铵盐还原除杂:往铑溶液中加入铵盐,将还原生成的黑色粉末过滤,得到滤液,滤液加水稀释;(4)络合:将上述稀释的滤液加热,加热温度为80-90℃,用亚硝酸钠溶液络合,调节PH至5-6,冷却后过滤;(5)沉淀铑:将过滤的络合液放入冰浴中冷却,加入氯化铵沉淀铑,得到白色沉淀物,用5%-10%的氯化铵溶液洗涤;(6)铑液制取:将上述得到的白色沉淀用盐酸溶解;(7)水合肼还原:将上述溶液过滤后用氢氧化钠调节溶液PH至1-3.5,去除溶液中的贱金属,通过阳离子交换树脂除杂,离子交换树脂为强酸性阳离子交换树脂,优选001×7强酸性苯乙烯系阳离子交换树脂,加入水合肼煮沸还原得到铑黑;(8)氢还原:将上述所得到的铑黑在氢还原炉中还原,碾碎得到纯铑粉。
用该方法具有工艺简单,提纯周期短,操作方便,等优点,而且废气废物排放少,有利于保护环境,并且对设备要求简单。
工作原理:本发明将含铑残渣与过氧化钡熔融后,将贵金属铂、铑氧化成可溶解的氧化物,用盐酸溶解, 然后用氯化铵沉淀法分离铂和铑,然后将含铑的滤液用亚硝酸钠溶液络合后调节PH,用氯化铵沉淀法沉淀铑,得铑液,再用离子交换树脂去除贱金属,最后水合肼还原、氢还原得铑粉。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。
Claims (5)
1.一种高纯铑粉的制备方法,其特征在于按以下步骤完成:
(1)焙烧:将含铑残渣与过氧化钡混合均匀,进行焙烧;
(2)溶解:将焙烧后的混合物进行冷却,加入盐酸溶解并稀释;
(3)铵盐还原除杂:往铑溶液中加入铵盐,将还原生成的黑色粉末过滤,得到滤液,滤液加水稀释;
(4)络合:将步骤(3)中稀释的滤液加热,用亚硝酸钠溶液络合,调节PH,冷却后过滤;
(5)沉淀铑:将过滤的络合液放入冰浴中冷却,加入氯化铵沉淀铑,得到白色沉淀物,用5%-10%的氯化铵溶液洗涤;
(6)铑液制取:将上述得到的白色沉淀用盐酸溶解;
(7)水合肼还原:将上述溶液过滤后用氢氧化钠调节溶液PH至1-3.5,去除溶液中的贱金属,通过阳离子交换树脂除杂,加入水合肼煮沸还原得到铑黑;
(8)氢还原:将上述所得到的铑黑在氢还原炉中还原,碾碎得到纯铑粉。
2.根据权利要求1所述的一种高纯铑粉的制备方法,其特征在于:步骤(1)中含铑残渣与过氧化钡按照1∶4.2-6.5的重量比充分混合均匀,然后将混合物在800-950°C焙烧。
3.根据权利要求1所述的一种高纯铑粉的制备方法,其特征在于:步骤(2)中溶解后加入0.6-0.7倍的钠盐稀释,钠盐优选氯化钠。
4.根据权利要求1所述的一种高纯铑粉的制备方法,其特征在于:步骤(4)中加热温度为80-90℃,络合后调节PH至5-6。
5.根据权利要求1所述的一种高纯铑粉的制备方法,其特征在于:步骤(7)中的离子交换树脂为强酸性阳离子交换树脂,优选001×7强酸性苯乙烯系阳离子交换树脂。
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