CN103849775B - 一种从高温合金废料中回收镍和钴的方法 - Google Patents
一种从高温合金废料中回收镍和钴的方法 Download PDFInfo
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- CN103849775B CN103849775B CN201410114670.6A CN201410114670A CN103849775B CN 103849775 B CN103849775 B CN 103849775B CN 201410114670 A CN201410114670 A CN 201410114670A CN 103849775 B CN103849775 B CN 103849775B
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000000953 sodium hydroxide Substances 0.000 claims abstract description 14
- 229910052500 inorganic minerals Inorganic materials 0.000 claims description 38
- 239000011707 minerals Substances 0.000 claims description 38
- 241001081830 Degeneriaceae Species 0.000 claims description 36
- 239000012047 saturated solutions Substances 0.000 claims description 32
- 239000007788 liquids Substances 0.000 claims description 24
- NBIIXXVUZAFLBC-UHFFFAOYSA-K [O-]P([O-])([O-])=O Chemical compound 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[O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 20
- 239000010452 phosphate Substances 0.000 claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound 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OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixtures Substances 0.000 claims description 18
- 239000011977 sulfuric acid Substances 0.000 claims description 18
- 239000000243 solutions Substances 0.000 claims description 15
- 229910001856 sodium hydroxide Inorganic materials 0.000 claims description 13
- 239000000126 substances Substances 0.000 claims description 11
- LWIHDJKSTIGBAC-UHFFFAOYSA-K Tripotassium phosphate Chemical compound 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[K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 6
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 6
- 229940093916 potassium phosphate Drugs 0.000 claims description 6
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 6
- 235000019798 tripotassium phosphate Nutrition 0.000 claims description 6
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical group 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[Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 6
- 229910052751 metals Inorganic materials 0.000 abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 abstract description 7
- 229910052804 chromium Inorganic materials 0.000 abstract description 7
- 239000011651 chromium Substances 0.000 abstract description 7
- 229910052742 iron Inorganic materials 0.000 abstract description 7
- 239000011514 iron Substances 0.000 abstract description 7
- 238000004064 recycling Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract description 3
- 230000001105 regulatory Effects 0.000 abstract 1
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- 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
Abstract
本发明提供了一种从高温合金废料中回收镍和钴的方法,包括以下步骤:一、对高温合金废料进行一段浸出处理,得到一段浸出渣和一段浸出液;二、对一段浸出渣和一段浸出液分别进行处理,一段浸出渣的处理过程为:211、进行二段浸出处理,得到二段浸出液和二段浸出渣;212、调节二段浸出液的酸值,然后作为一段浸出剂重复利用;一段浸出液的处理过程为:221、对一段浸出液进行初步沉淀除杂;222、用氢氧化钠调节溶液的pH值,然后进行深度沉淀除杂;223、采用萃取分离法实现镍与钴的分离。本发明采用湿法工艺实现了Ni、Co主金属元素与Cr、Al、Fe等杂质元素的有效分离,工艺简单,回收率高,具有广泛的工业化应用前景。
Description
技术领域
[0001] 本发明属于湿法冶金技术领域,具体涉及一种从高温合金废料中回收镍和钴的方法。
背景技术
[0002] 废旧高温合金中含有大量价值昂贵的主金属元素,其主要来源于:(1)高温合金制备过程中产生的冒口、刨肩、车肩等;(2)高温合金构件、零部件等铸造与锻造加工产生废料;(3)到达使用期限的高温合金构件、零部件。2010年,国内产生的高温合金废料在7000吨以上,由于缺乏专业回收网络、回收技术以及相应管理水平的废料回收企业,大部分废料被堆存或降级使用,造成大量战略性金属被浪费;只有少量回炉用于高温合金制备,但由于废料处理手段不完善,造成夹杂等有害物增加,常常影响高温合金性能和使用寿命。
[0003] 废旧高温合金的回收方法主要有火法工艺和湿法工艺两种。火法工艺回收废旧高温合金是将高温合金废料通过采用表面处理和真空吹氧脱碳技术(V0D)及特种渣系去夹杂物、高真空提纯等一系列技术,并结合真空感应炉、电渣炉等先进冶炼设备进行再生应用。湿法工艺是将废旧高温合金预处理后进行酸浸、碱浸,使有回收价值的元素以离子的形式进入溶液,再采用化学沉淀、电解沉积、有机溶剂萃取、置换法、离子交换法中的一种或几种分离方法将主金属元素元素分离出来的化学方法。火法技术设备要求高、投资大、能耗高,稀有金属回收率低,且分离效果不如湿法工艺。
发明内容
[0004] 本发明所要解决的技术问题在于针对上述现有技术的不足,提供一种从高温合金废料中回收镍和钴的方法。该方法采用湿法工艺能够实现N1、Co主金属元素与Cr、Al、Fe等杂质元素的有效分离。
[0005] 为解决上述技术问题,本发明采用的技术方案是:一种从高温合金废料中回收镍和钴的方法,其特征在于,该方法包括以下步骤:
[0006] 步骤一、采用H+浓度为3.6mol/L〜5.0mol/L的无机酸为一段浸出剂对高温合金废料进行一段浸出处理,得到一段浸出渣和一段浸出液;所述高温合金废料的化学成分按质量百分比计为:Ni40% 〜60%,Col5% 〜20%,Cr5% 〜10%,A15% 〜10%,Fe0.5% 〜2%,W3% 〜8%,Tal%〜5%,Hf 1%〜5% ;所述高温合金废料与一段浸出剂的固液比为1: (6〜10),所述一段浸出处理的温度为50°C〜100°C,所述一段浸出处理的时间为0.5h〜3h ;
[0007] 步骤二、对步骤一中所述一段浸出渣和一段浸出液分别进行处理:
[0008] 所述一段浸出渣的处理过程为:
[0009] 步骤211、采用H+浓度为8mol/L〜12mol/L的无机酸为二段浸出剂对一段浸出渣进行二段浸出处理,得到二段浸出液和二段浸出渣;所述一段浸出渣与二段浸出剂的固液比为1: (6〜10),所述二段浸出处理的温度为50°C〜100°C,所述二段浸出处理的时间为lh 〜5h ;
[0010] 步骤212、将步骤211中所述二段浸出液的H+浓度调节为3.6mol/L〜5.0mol/L,然后将H+浓度为3.6mol/L〜5.0mol/L的二段浸出液作为一段浸出剂重复利用;
[0011] 所述一段浸出液的处理过程为:
[0012] 步骤221、采用水溶性磷酸盐的饱和溶液为沉淀剂对一段浸出液进行初步沉淀除杂,直至使一段浸出液的pH为1.6〜2.0为止;
[0013] 步骤222、采用氢氧化钠溶液将步骤221中初步沉淀除杂后的一段浸出液的pH值调节至3.5〜5.5,然后将pH值为3.5〜5.5的一段浸出液在温度为50°C〜100°C的条件下搅拌0.5h〜3h进行深度沉淀除杂;
[0014] 步骤223、采用萃取分离的方法将步骤222中深度沉淀除杂后的一段浸出液中的镍与钴分呙。
[0015] 上述的一种从高温合金废料中回收镍和钴的方法,其特征在于,步骤一和步骤211中所述无机酸均为硫酸。
[0016] 上述的一种从高温合金废料中回收镍和钴的方法,其特征在于,步骤221中所述水溶性磷酸盐的饱和溶液为磷酸钠饱和溶液或磷酸钾饱和溶液。
[0017] 上述的一种从高温合金废料中回收镍和钴的方法,其特征在于,步骤222中所述氢氧化钠溶液的质量百分比浓度为5%〜40%。
[0018] 所述固液比是指固体质量与液体体积之比,其中固体的质量单位为g,液体的体积单位为mL。
[0019] 本发明主要采用“两段浸出一初步沉淀除杂一深度沉淀除杂”工艺实现N1、Co主金属元素与Cr、Al、Fe等杂质元素的有效分离。首先,进行一段低酸浸出,然后对一段浸出渣进行二段高酸浸出,二段浸出液调节酸值后作为一段浸出处理的浸出剂重复利用。两段浸出能够实现N1、Co、Cr、Al、Fe等与稀有金属W、Ta、Hf的有效分离,使得N1、Co、Cr、Al、Fe的浸出率达99%以上,而稀有金属W、Ta、Hf的浸出率不大于3% ;然后,采用化学沉淀法初步除杂,从而实现N1、Co与Cr、Al、Fe的分离;之后,采用深度水解沉淀法,使得99%以上的杂质元素水解沉淀,从而与主金属元素N1、Co分离,达到深度净化的目的;最后,采用常规的萃取分离法实现镍与钴的有效分离。
[0020] 本发明与现有技术相比具有以下优点:
[0021] 1、本发明首先进行一段低酸浸出,然后对一段浸出渣进行二段高酸浸出,二段浸出液经过调节酸值后作为一段浸出处理的浸出剂重复利用。两段浸出不但可以得到符合后续工序所需的具有较高pH值的浸出液,而且实现了贱金属与稀有金属的有效的分离,同时明显提高了酸利用率。
[0022] 2、本发明采用磷酸盐进行初步除杂,有效地实现了主金属元素元素N1、Co与Cr、Al、Fe的分离。相比传统的直接水解沉淀法,本发明获得了易于过滤的液固混合体,解决了工业生产中过滤困难的问题。
[0023] 3、本发明采用氢氧化钠进行深度除杂,相比传统的萃取深度除杂法,本发明设备投入少,操作简单方便,效果好,水解沉淀渣可直接酸溶返回初步化学沉淀再利用,镍钴零损失,深度净化液可直接进行镍钴分离。
[0024] 综上所述,本发明采用全湿法处理废旧高温合金,不但回收率高,而且还可经过湿法提纯技术,获得纯度较高的单质金属或化工中间体产品。此外,本发明有很好的研究利用价值,思路新颖,且本发明涉及废旧资源再生利用,属于循环经济范畴,有很好的工业化应用前景。
[0025] 下面结合附图和实施例对本发明作进一步详细说明。
附图说明
[0026] 图1是本发明的工艺流程框图。
具体实施方式
[0027] 实施例1
[0028] 本实施例待处理的高温合金废料的化学成分按质量百分比计为:Ni60%,Co 15%,Cr5%,A15%,Fel%,W6%,Ta4%,Hf4%。结合图1,本实施例从高温合金废料中回收镍和钴的方法包括以下步骤:
[0029] 步骤一、称取高温合金废料,然后按照固液比1: 6量取H+浓度为3.6mol/L的无机酸作为一段浸出剂,之后将高温合金废料与一段浸出剂混合均匀,在温度为50°C的条件下搅拌0.5h进行一段浸出处理,得到一段浸出渣和一段浸出液;所述无机酸优选为硫酸;
[0030] 步骤二、对步骤一中所述一段浸出渣和一段浸出液分别进行处理:
[0031] 其中,一段浸出渣的处理过程为:
[0032] 步骤211、按照一段浸出渣与二段浸出剂的固液比1: 6量取H+浓度为8mol/L的无机酸作为二段浸出剂,之后将一段浸出渣与二段浸出剂混合均匀,在温度为50°C的条件下搅拌lh进行二段浸出处理,得到二段浸出液和二段浸出渣;所述无机酸优选为硫酸;
[0033] 步骤212、采用添加去离子水的方法将步骤211中所述二段浸出液的H+浓度调节为3.6mol/L,然后将H+浓度为3.6mol/L的二段浸出液作为一段浸出剂重复利用;
[0034] 一段浸出液的处理过程为:
[0035] 步骤221、采用水溶性磷酸盐的饱和溶液为沉淀剂对一段浸出液进行初步沉淀除杂,直至使一段浸出液的pH为1.6为止;所述水溶性磷酸盐的饱和溶液优选为磷酸钠饱和溶液;
[0036] 步骤222、采用质量百分比浓度为5%的氢氧化钠溶液将步骤221中初步沉淀除杂后的一段浸出液的pH值调节至3.5,然后将pH值为3.5的一段浸出液在温度为50°C的条件下搅拌0.5h进行深度沉淀除杂;
[0037] 步骤223、采用萃取分离的方法将步骤222中深度沉淀除杂后的一段浸出液中的镍与钴分呙。
[0038] 经本实施例处理后,镍和钴的回收率均高达99%以上。
[0039] 实施例2
[0040] 本实施例待处理的高温合金废料的化学成分按质量百分比计为:Ni40%%,Co20%,Crl0%,A110%,Fe2%,W8%,Ta5%,Hf5%。结合图1,本实施例从高温合金废料中回收镍和钴的方法包括以下步骤:
[0041] 步骤一、称取高温合金废料,然后按照固液比1: 7量取H+浓度为3.8mol/L的无机酸作为一段浸出剂,之后将高温合金废料与一段浸出剂混合均匀,在温度为60°C的条件下搅拌lh进行一段浸出处理,得到一段浸出渣和一段浸出液;所述无机酸优选为硫酸;
[0042] 步骤二、对步骤一中所述一段浸出渣和一段浸出液分别进行处理:
[0043] 其中,一段浸出渣的处理过程为:
[0044] 步骤211、按照一段浸出渣与二段浸出剂的固液比1: 7量取H+浓度为9mol/L的无机酸作为二段浸出剂,之后将一段浸出渣与二段浸出剂混合均匀,在温度为60°C的条件下搅拌1.5h进行二段浸出处理,得到二段浸出液和二段浸出渣;所述无机酸优选为硫酸;
[0045] 步骤212、采用添加去离子水的方法将步骤211中所述二段浸出液的H+浓度调节为3.8mol/L,然后将H+浓度为3.8mol/L的二段浸出液作为一段浸出剂重复利用;
[0046] 一段浸出液的处理过程为:
[0047] 步骤221、采用水溶性磷酸盐的饱和溶液为沉淀剂对一段浸出液进行初步沉淀除杂,直至使一段浸出液的pH为1.7为止;所述水溶性磷酸盐的饱和溶液优选为磷酸钾饱和溶液;
[0048] 步骤222、采用质量百分比浓度为10%的氢氧化钠溶液将步骤221中初步沉淀除杂后的一段浸出液的pH值调节至4,然后将pH值为4的一段浸出液在温度为60°C的条件下搅拌lh进行深度沉淀除杂;
[0049] 步骤223、采用萃取分离的方法将步骤222中深度沉淀除杂后的一段浸出液中的镍与钴分呙。
[0050] 经本实施例处理后,镍和钴的回收率均高达99%以上。
[0051] 实施例3
[0052] 本实施例待处理的高温合金废料的化学成分按质量百分比计为:Ni60%,Co 16%,Cr8%,A18%,Fe0.5%,W3%,Ta2%,Hf2%。结合图1,本实施例从高温合金废料中回收镍和钴的方法包括以下步骤:
[0053] 步骤一、称取高温合金废料,然后按照固液比1: 8量取H+浓度为4mol/L的无机酸作为一段浸出剂,之后将高温合金废料与一段浸出剂混合均匀,在温度为70°C的条件下搅拌1.5h进行一段浸出处理,得到一段浸出渣和一段浸出液;所述无机酸优选为硫酸;
[0054] 步骤二、对步骤一中所述一段浸出渣和一段浸出液分别进行处理:
[0055] 其中,一段浸出渣的处理过程为:
[0056] 步骤211、按照一段浸出渣与二段浸出剂的固液比1: 8,量取H+浓度为lOmol/L的无机酸作为二段浸出剂,之后将一段浸出渣与二段浸出剂混合均匀,在温度为70°C的条件下搅拌2h进行二段浸出处理,得到二段浸出液和二段浸出渣;所述无机酸优选为硫酸;
[0057] 步骤212、采用添加去离子水的方法将步骤211中所述二段浸出液的H+浓度调节为4mol/L,然后将H+浓度为4mol/L的二段浸出液作为一段浸出剂重复利用;
[0058] 一段浸出液的处理过程为:
[0059] 步骤221、采用水溶性磷酸盐的饱和溶液为沉淀剂对一段浸出液进行初步沉淀除杂,直至使一段浸出液的pH为1.8为止;所述水溶性磷酸盐的饱和溶液优选为磷酸钠饱和溶液;
[0060] 步骤222、采用质量百分比浓度为15%的氢氧化钠溶液将步骤221中初步沉淀除杂后的一段浸出液的pH值调节至4.5,然后将pH值为4.5的一段浸出液在温度为70°C的条件下搅拌1.5h进行深度沉淀除杂;
[0061] 步骤223、采用萃取分离的方法将步骤222中深度沉淀除杂后的一段浸出液中的镍与钴分呙。
[0062] 经本实施例处理后,镍和钴的回收率均高达99%以上。
[0063] 实施例4
[0064] 本实施例待处理的高温合金废料的化学成分按质量百分比计为:Ni57%,Co 18%,Crl0%,A16%,Fel%,W4%,Tal%,Hf3%。结合图1,本实施例从高温合金废料中回收镍和钴的方法包括以下步骤:
[0065] 步骤一、称取高温合金废料,然后按照固液比1: 9量取H+浓度为4.2mol/L的无机酸作为一段浸出剂,之后将高温合金废料与一段浸出剂混合均匀,在温度为80°C的条件下搅拌2h进行一段浸出处理,得到一段浸出渣和一段浸出液;所述无机酸优选为硫酸;
[0066] 步骤二、对步骤一中所述一段浸出渣和一段浸出液分别进行处理:
[0067] 其中,一段浸出渣的处理过程为:
[0068] 步骤211、按照一段浸出渣与二段浸出剂的固液比1: 9,量取H+浓度为llmol/L的无机酸作为二段浸出剂,之后将一段浸出渣与二段浸出剂混合均匀,在温度为80°C的条件下搅拌2.5h进行二段浸出处理,得到二段浸出液和二段浸出渣;所述无机酸优选为硫酸;
[0069] 步骤212、采用添加去离子水的方法将步骤211中所述二段浸出液的H+浓度调节为4.2mol/L,然后将H+浓度为4.2mol/L的二段浸出液作为一段浸出剂重复利用;
[0070] 一段浸出液的处理过程为:
[0071] 步骤221、采用水溶性磷酸盐的饱和溶液为沉淀剂对一段浸出液进行初步沉淀除杂,直至使一段浸出液的pH为1.9为止;所述水溶性磷酸盐的饱和溶液优选为磷酸钾饱和溶液;
[0072] 步骤222、采用质量百分比浓度为20%的氢氧化钠溶液将步骤221中初步沉淀除杂后的一段浸出液的pH值调节至5,然后将pH值为5的一段浸出液在温度为80°C的条件下搅拌2h进行深度沉淀除杂;
[0073] 步骤223、采用萃取分离的方法将步骤222中深度沉淀除杂后的一段浸出液中的镍与钴分呙。
[0074] 经本实施例处理后,镍和钴的回收率均高达99%以上。
[0075] 实施例5
[0076] 本实施例待处理的高温合金废料的化学成分按质量百分比计为:Ni59%,Co 16%,Cr6%,A110%,Fe2%,W3%,Ta3%,Hfl%。结合图1,本实施例从高温合金废料中回收镍和钴的方法包括以下步骤:
[0077] 步骤一、称取高温合金废料,然后按照固液比1: 10量取H+浓度为4.4mol/L的无机酸作为一段浸出剂,之后将高温合金废料与一段浸出剂混合均匀,在温度为90°C的条件下搅拌2.5h进行一段浸出处理,得到一段浸出渣和一段浸出液;所述无机酸优选为硫酸;
[0078] 步骤二、对步骤一中所述一段浸出渣和一段浸出液分别进行处理:
[0079] 其中,一段浸出渣的处理过程为:
[0080] 步骤211、按照一段浸出渣与二段浸出剂的固液比1: 10,量取H+浓度为12mol/L的无机酸作为二段浸出剂,之后将一段浸出渣与二段浸出剂混合均匀,在温度为90°C的条件下搅拌3h进行二段浸出处理,得到二段浸出液和二段浸出渣;所述无机酸优选为硫酸;
[0081] 步骤212、采用添加去离子水的方法将步骤211中所述二段浸出液的H+浓度调节为4.4mol/L,然后将H+浓度为4.4mol/L的二段浸出液作为一段浸出剂重复利用;
[0082] 一段浸出液的处理过程为:
[0083] 步骤221、采用水溶性磷酸盐的饱和溶液为沉淀剂对一段浸出液进行初步沉淀除杂,直至使一段浸出液的pH为2.0为止;所述水溶性磷酸盐的饱和溶液优选为磷酸钾饱和溶液;
[0084] 步骤222、采用质量百分比浓度为25%的氢氧化钠溶液将步骤221中初步沉淀除杂后的一段浸出液的pH值调节至5.5,然后将pH值为5.5的一段浸出液在温度为90°C的条件下搅拌3h进行深度沉淀除杂;
[0085] 步骤223、采用萃取分离的方法将步骤222中深度沉淀除杂后的一段浸出液中的镍与钴分呙。
[0086] 经本实施例处理后,镍和钴的回收率均高达99%以上。
[0087] 实施例6
[0088] 本实施例待处理的高温合金废料的化学成分按质量百分比计为:Ni51%,Co20%,Cr9%,A19%,Fel.5%,W5%,Ta2.5%,Hf2%。结合图1,本实施例从高温合金废料中回收镍和钴的方法包括以下步骤:
[0089] 步骤一、称取高温合金废料,然后按照固液比1: 10量取H+浓度为4.6mol/L的无机酸作为一段浸出剂,之后将高温合金废料与一段浸出剂混合均匀,在温度为100°c的条件下搅拌3h进行一段浸出处理,得到一段浸出渣和一段浸出液;所述无机酸优选为硫酸;
[0090] 步骤二、对步骤一中所述一段浸出渣和一段浸出液分别进行处理:
[0091] 其中,一段浸出渣的处理过程为:
[0092] 步骤211、按照一段浸出渣与二段浸出剂的固液比1:10,量取H+浓度为12mol/L的无机酸作为二段浸出剂,之后将一段浸出渣与二段浸出剂混合均匀,在温度为100°c的条件下搅拌3.5h进行二段浸出处理,得到二段浸出液和二段浸出渣;所述无机酸优选为硫酸;
[0093] 步骤212、采用添加去离子水的方法将步骤211中所述二段浸出液的H+浓度调节为4.6mol/L,然后将H+浓度为4.6mol/L的二段浸出液作为一段浸出剂重复利用;
[0094] 一段浸出液的处理过程为:
[0095] 步骤221、采用水溶性磷酸盐的饱和溶液为沉淀剂对一段浸出液进行初步沉淀除杂,直至使一段浸出液的pH为2.0为止;所述水溶性磷酸盐的饱和溶液优选为磷酸钠饱和溶液;
[0096] 步骤222、采用质量百分比浓度为30%的氢氧化钠溶液将步骤221中初步沉淀除杂后的一段浸出液的pH值调节至5.5,然后将pH值为5.5的一段浸出液在温度为100°C的条件下搅拌3h进行深度沉淀除杂;
[0097] 步骤223、采用萃取分离的方法将步骤222中深度沉淀除杂后的一段浸出液中的镍与钴分呙。
[0098] 经本实施例处理后,镍和钴的回收率均高达99%以上。
[0099] 实施例7
[0100] 本实施例待处理的高温合金废料的化学成分按质量百分比计为:Ni50%,Co20%,Crl0%,A18%,Fel%,W6.5%,Ta2%,Hf2.5%。结合图1,本实施例从高温合金废料中回收镍和钴的方法包括以下步骤:
[0101] 步骤一、称取高温合金废料,然后按照固液比1: 10量取H+浓度为4.8mol/L的无机酸作为一段浸出剂,之后将高温合金废料与一段浸出剂混合均匀,在温度为100°c的条件下搅拌3h进行一段浸出处理,得到一段浸出渣和一段浸出液;所述无机酸优选为硫酸;
[0102] 步骤二、对步骤一中所述一段浸出渣和一段浸出液分别进行处理:
[0103] 其中,一段浸出渣的处理过程为:
[0104] 步骤211、按照一段浸出渣与二段浸出剂的固液比1: 10,量取H+浓度为12mol/L的无机酸作为二段浸出剂,之后将一段浸出渣与二段浸出剂混合均匀,在温度为100°c的条件下搅拌4h进行二段浸出处理,得到二段浸出液和二段浸出渣;所述无机酸优选为硫酸;
[0105] 步骤212、采用添加去离子水的方法将步骤211中所述二段浸出液的H+浓度调节为4.8mol/L,然后将H+浓度为4.8mol/L的二段浸出液作为一段浸出剂重复利用;
[0106] 一段浸出液的处理过程为:
[0107] 步骤221、采用水溶性磷酸盐的饱和溶液为沉淀剂对一段浸出液进行初步沉淀除杂,直至使一段浸出液的pH为2.0为止;所述水溶性磷酸盐的饱和溶液优选为磷酸钾饱和溶液;
[0108] 步骤222、采用质量百分比浓度为35%的氢氧化钠溶液将步骤221中初步沉淀除杂后的一段浸出液的pH值调节至5.5,然后将pH值为5.5的一段浸出液在温度为100°C的条件下搅拌3h进行深度沉淀除杂;
[0109] 步骤223、采用萃取分离的方法将步骤222中深度沉淀除杂后的一段浸出液中的镍与钴分呙。
[0110] 经本实施例处理后,镍和钴的回收率均高达99%以上。
[0111] 实施例8
[0112] 本实施例待处理的高温合金废料的化学成分按质量百分比计为:Ni55%,Co 18%,Cr7%,A17%,Fe2%,W6%,Ta2.5%,Hf2.5%。结合图1,本实施例从高温合金废料中回收镍和钴的方法包括以下步骤:
[0113] 步骤一、称取高温合金废料,然后按照固液比1: 10量取H+浓度为5.0mol/L的无机酸作为一段浸出剂,之后将高温合金废料与一段浸出剂混合均匀,在温度为100°c的条件下搅拌3h进行一段浸出处理,得到一段浸出渣和一段浸出液;所述无机酸优选为硫酸;
[0114] 步骤二、对步骤一中所述一段浸出渣和一段浸出液分别进行处理:
[0115] 其中,一段浸出渣的处理过程为:
[0116] 步骤211、按照一段浸出渣与二段浸出剂的固液比1: 10,量取H+浓度为12mol/L的无机酸作为二段浸出剂,之后将一段浸出渣与二段浸出剂混合均匀,在温度为100°c的条件下搅拌5h进行二段浸出处理,得到二段浸出液和二段浸出渣;所述无机酸优选为硫酸;
[0117] 步骤212、采用添加去离子水的方法将步骤211中所述二段浸出液的H+浓度调节为5.0mol/L,然后将H+浓度为5.0mol/L的二段浸出液作为一段浸出剂重复利用;
[0118] 一段浸出液的处理过程为:
[0119] 步骤221、采用水溶性磷酸盐的饱和溶液为沉淀剂对一段浸出液进行初步沉淀除杂,直至使一段浸出液的pH为2.0为止;所述水溶性磷酸盐的饱和溶液优选为磷酸钠饱和溶液;
[0120] 步骤222、采用质量百分比浓度为40%的氢氧化钠溶液将步骤221中初步沉淀除杂后的一段浸出液的pH值调节至5.5,然后将pH值为5.5的一段浸出液在温度为100°C的条件下搅拌3h进行深度沉淀除杂;
[0121] 步骤223、采用萃取分离的方法将步骤222中深度沉淀除杂后的一段浸出液中的镍与钴分呙。
[0122] 经本实施例处理后,镍和钴的回收率均高达99%以上。
[0123] 以上所述,仅是本发明的较佳实施例,并非对本发明作任何限制。凡是根据发明技术实质对以上实施例所作的任何简单修改、变更以及等效变化,均仍属于本发明技术方案的保护范围内。
Claims (3)
1.一种从高温合金废料中回收镍和钴的方法,其特征在于,该方法包括以下步骤: 步骤一、采用H+浓度为3.6mol/L〜5.0mol/L的无机酸为一段浸出剂对高温合金废料进行一段浸出处理,得到一段浸出渣和一段浸出液;所述高温合金废料的化学成分按质量百分比计为:Ni40% 〜60%,Co 15% 〜20%,Cr5% 〜10%,A15% 〜10%,Fe0.5% 〜2%,W3% 〜8%,Tal%〜5%,Hf 1%〜5% ;所述高温合金废料与一段浸出剂的固液比为1: (6〜10),所述一段浸出处理的温度为50°C〜100°C,所述一段浸出处理的时间为0.5h〜3h ; 步骤二、对步骤一中所述一段浸出渣和一段浸出液分别进行处理: 所述一段浸出渣的处理过程为: 步骤211、采用H+浓度为8mol/L〜12mol/L的无机酸为二段浸出剂对一段浸出渣进行二段浸出处理,得到二段浸出液和二段浸出渣;所述一段浸出渣与二段浸出剂的固液比为1: (6〜10),所述二段浸出处理的温度为50°C〜100°C,所述二段浸出处理的时间为lh〜5h ; 步骤212、将步骤211中所述二段浸出液的H+浓度调节为3.6mol/L〜5.0mol/L,然后将H+浓度为3.6mol/L〜5.0mol/L的二段浸出液作为一段浸出剂重复利用; 所述一段浸出液的处理过程为: 步骤221、采用水溶性磷酸盐的饱和溶液为沉淀剂对一段浸出液进行初步沉淀除杂,直至使一段浸出液的pH为1.6〜2.0为止;所述水溶性磷酸盐的饱和溶液为磷酸钠饱和溶液或磷酸钾饱和溶液; 步骤222、采用氢氧化钠溶液将步骤221中初步沉淀除杂后的一段浸出液的pH值调节至3.5〜5.5,然后将pH值为3.5〜5.5的一段浸出液在温度为50°C〜100°C的条件下搅拌0.5h〜3h进行深度沉淀除杂; 步骤223、采用萃取分离的方法将步骤222中深度沉淀除杂后的一段浸出液中的镍与钴分呙。
2.根据权利要求1所述的一种从高温合金废料中回收镍和钴的方法,其特征在于,步骤一和步骤211中所述无机酸均为硫酸。
3.根据权利要求1所述的一种从高温合金废料中回收镍和钴的方法,其特征在于,步骤222中所述氢氧化钠溶液的质量百分比浓度为5%〜40%。
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