CN101649394A - Ag-SnO2废料回收循环利用的方法 - Google Patents
Ag-SnO2废料回收循环利用的方法 Download PDFInfo
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- CN101649394A CN101649394A CN200910055063A CN200910055063A CN101649394A CN 101649394 A CN101649394 A CN 101649394A CN 200910055063 A CN200910055063 A CN 200910055063A CN 200910055063 A CN200910055063 A CN 200910055063A CN 101649394 A CN101649394 A CN 101649394A
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- 239000002699 waste material Substances 0.000 title claims abstract description 22
- 238000004064 recycling Methods 0.000 title abstract description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials 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O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title abstract 5
- 229910017980 Ag—Sn Inorganic materials 0.000 claims abstract description 49
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 43
- 239000000956 alloy Substances 0.000 claims abstract description 43
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- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(II) oxide Inorganic materials 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- 229910006404 SnO 2 Inorganic materials 0.000 claims description 24
- 239000001257 hydrogen Substances 0.000 claims description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound data:image/svg+xml;base64,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 data:image/svg+xml;base64,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 [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical group 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[C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 229910002804 graphite Inorganic materials 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 11
- 230000001939 inductive effect Effects 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 230000002829 reduced Effects 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 8
- 239000007858 starting material Substances 0.000 claims description 7
- 238000003723 Smelting Methods 0.000 claims description 5
- 230000001351 cycling Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
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[Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 230000001131 transforming Effects 0.000 description 2
- 229910017750 AgSn Inorganic materials 0.000 description 1
- -1 AgSn is less Chemical class 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound 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OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010310 metallurgical process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000001473 noxious Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
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Classifications
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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
- 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
本发明公开一种Ag－SnO2废料回收循环利用的方法，采用还原剂对Ag－SnO2材料进行还原处理，然后得到Ag－Sn合金。最后将Ag－Sn合金作为原材料重新制备Ag－SnO2材料从而实现Ag－SnO2材料循环利用。这种方法能全部回收Ag－Sn合金、且工艺简单、操作方便、周期短、无工业三废污染、具有良好的社会和经济效益。
Description
Ag-Sn02废料回收循环利用的方法
技术领域
本发明涉及一种复合材料技术领域的回收利用方法，具体地说，涉及的是一 种Ag-Sn02废料回收循环利用的方法。 背景技术
复合材料的回收再利用一直以来是复合材料领域重点关注的方向。因为复合 材料中含有物理化学性质差异极大的各种增强相，较难回收。因此复合材料的回 收已经成为一个重要的研宄内容。由于Ag-Sn02材料中含有Ag基体、细小的高 烙点Sn02颗粒及各种不同含量的氧化物添加剂颗粒，从而使得Ag-Sn02材料的 回收成为一个难点。
国内外关于Ag废料回收方面的研究具体如下：
1) 萃取和回收银的方法CN1200407
2) 贵金属熔炼渣湿法冶金工艺CN1268580
3) 张钦发；龚竹青；含银废料中银的综合回收和利用工艺方法。有色金属 2004 (10)
现在对于Ag-Sn02废料的回收通常有两种办法： 一是采用湿法电解的方法 提取回收Ag;(文献1) -3)) 二是先采用熔炼去渣的方式先将硬质颗粒去除，然 后采用HN03溶解化学回收Ag金属。这两种方法存在污染大，回收率低，不可 循环利用等诸多缺点。
发明内容
本发明针对上述现有技术存在的不足和缺陷，提供一种Ag-Sn02废料回收 循环利用的方法，具有无污染、回收率高的优点。
为实现上述的目的，本发明采用的技术方案是：本发明采用还原剂（石墨粉 或氢气）对Ag-Sn02材料进行还原处理，然后得到Ag-Sn合金。最后将Ag-Sn 合金作为原材料重新制备Ag-Sn02材料，从而实现Ag-Sn02材料循环利用。
3本发明具体实现包括以下两种方案： 第一方案，以石墨为还原剂
首先将Ag-Sn02废料与石墨粉一起在中频感应加热炉中，熔炼气氛为惰性 气氛或真空，然后升温加热，温度在1000〜1300'C之间，保温时间15〜60分钟； 之后即可得到Ag-Sn合金，将其作为原材料重新制备成Ag-Sn02材料，实现循 环再利用的目的。Sn02与C重量比在l: 1~1: 5之间。 反应方程式：Sn02+C=Sn+C02
第二方案，以氢气为还原剂
首先将Ag-Sn02废料置于真空中频感应炉中，往熔炼炉中通氢气排除原有 空气后，开始升温熔炼，熔炼气氛保持为还原氢气气氛。熔炼温度1000〜130(TC 之间，保温时间0,5〜3小时；之后即可得到Ag-Sn合金，将其作为原材料重新 制备成Ag-Sn02材料，实现循环再利用的目的。 反应方程式：Sn02+2H2=Sn+2H20
本发明采用还原物质如石墨粉或还原性气体如氢气，在高温下实现Sn02颗 粒向Sn元素的转变，从而可以将Ag-Sn02废料成功转变成Ag-Sn合金，Ag-Sn 合金可以作为下次制备Ag-Sn02材料的原材料循环使用。通过上述方式能够全 部回收Ag-SnCb废料，实现Ag-Sn合金的循环再利用，由于采用此种方法不涉 及使用酸碱及有毒有害物质，因此无污染产生。并且由于高温操作过程时间较短， AgSn等金属挥发较少，损耗少，因而具有回收完全的优点。通过本发明，可以 有效解决以往AgSn02废料回收容易产生的污染严重、回收率低、回收工艺等问 题，可以真正实现循环利用的目的。
附图说明
图1为本发明采用石墨为还原剂的实施例流程图 图2为本发明采用氢气为还原剂的实施例流程图 具体实施方式
以下结合附图对本发明的技术方案作进一步的说明，以下描述只是用于理解 本发明，并不用于限定本发明的范围。
4实施例一
如图1所示，取重量5kgAg-Sn02 (10wt%)废料与250g石墨粉一起置于真 空中频感应炉中，然后抽真空，升温至IOOO'C，保温60分钟后，浇铸获得Ag-Sn 合金。最后以Ag-Sn合金为原料制备Ag-Sn02材料，该过程为：先将Ag-Sn合 金于1050。C熔炼15分钟，然后雾化制粉，获得Ag-Sn合金粉后在50(TC， lMPa 氧压下进行预氧化3h，之后将氧化后的Ag-Sn粉经500MPa等静压压制后在 90(TC烧结3h，将烧结后坯体50(TC热压，之后将热压获得的坯体在600"C下热 挤压等工序，获得的Ag-Sn02材料。
实施例二
如图2所示，取重量5kgAg-Sn02 (10wt%)废料置于真空中频感应炉中， 通氢排除炉中空气后，在氢气气氛下升温至1000°C，保温3h后获得Ag-Sn合金。 最后以Ag-Sn合金为原料制备Ag-Sn02材料，该过程为：先将Ag-Sn合金于 105(TC烙炼15分钟，然后雾化制粉，获得Ag-Sn合金粉后在500'C， lMPa氧 压下进行预氧化3h，之后将氧化后的Ag-Sn粉经500MPa等静压压制后在900°C 烧结3h，将烧结后坯体50(TC热压，之后将热压获得的坯体在60(TC下热挤压等 工序，获得的Ag-Sn02材料。
通过本实例获得的Ag-Sn合金，总重损失0.05%，由此制备的Ag-Sn02材 料中Sn02含量9.95wt。/0，强度为300MPa，导电率为2.2^X1。
实施例三
如图l所示，取重量5kgAg-Sn02 (10wt%)废料与50g石墨粉一起置于真 空中频感应炉中，然后充惰性气体排出空气后，在惰性气氛下升温至1300°C, 保温15分钟后浇铸获得Ag-Sn合金。最后以Ag-Sn合金为原料制备Ag-Sn02 材料，该过程为：先将Ag-Sn合金于105(TC熔炼15分钟，然后雾化制粉，获得 Ag-Sn合金粉后在500°C ， lMPa氧压下进行预氧化3h，之后将氧化后的Ag-Sn 粉经500MPa等静压压制后在90(TC烧结3h，将烧结后的坯体500'C热压，之后 将热压获得的坯体在60(TC下热挤压等工序，获得的Ag-Sn02材料。
通过本实例获得的Ag-Sn合金，总重损失0.1%,由此制备的Ag-Sn02材料中Sn02含量9.92wt。/0，强度为310MPa，导电率为2.15pa。实施例四
如图2所示，取重量5kgAg-Sn02 (10wt%)废料置于真空中频感应炉中，通氢排除炉中空气后，在氢气气氛下升温至1300。C，保温0.511后获得八8-811合金。最后以Ag-Sn合金为原料制备Ag-Sn02材料，该过程为：先将Ag-Sn合金于1050'C熔炼15分钟，然后雾化制粉，获得Ag-Sn合金粉后在500'C， lMPa氧压下进行预氧化3h，之后将氧化后的Ag-Sn粉经500MPa等静压压制后在900。C烧结3h，将烧结后坯体500'C热压，之后将热压获得的坯体在600'C下热挤压等工序，获得的Ag-Sn02材料。
通过本实例获得的Ag-Sn合金，总重损失0.1%，由此制备的Ag-Sn02材料中Sn02含量9.9wt。/。，强度为315MPa,导电率为2.2^.。
实施例五
如图2所示，取重量5kgAg-Sn02 (10wt%)废料置于真空中频感应炉中，通氢排除炉中空气后，在氢气气氛下升温至1100'C，保温L5h后获得Ag-Sn合金。最后以Ag-Sn合金为原料制备Ag-Sn02材料，该过程为：先将Ag-Sn合金于1050。C熔炼15分钟，然后雾化制粉，获得Ag-Sn合金粉后在500'C， lMPa氧压下进行预氧化3h，之后将氧化后的Ag-Sn粉经500MPa等静压压制后在卯0'C烧结3h，将烧结后的坯体50(TC热压，之后将热压获得的坯体在600'C下热挤压等工序，获得Ag-Sn02材料。
通过本实例获得的Ag-Sn合金，总重损失0.05%,由此制备的Ag-Sn02材料中Sn02含量9.95wt。/i，强度为295MPa，导电率为2.2^0.。
实施例六
如图1所示，取重量5kgAg-Sn02 (10wt%)废料与100g石墨粉一起置于真空中频感应炉中，然后充惰性气体排出空气后，在惰性气氛下升温至1100°C，保温45分钟后浇铸获得Ag-Sn合金。最后以Ag-Sn合金为原料制备Ag-Sn02材料，该过程为：先将Ag-Sn合金于1050'C熔炼15分钟，然后雾化制粉，获得Ag-Sn合金粉后在500°C， lMPa氧压下进行预氧化3h，之后将氧化后的Ag-Sn粉经500MPa等静压压制后在900'C烧结3h,将烧结后坯体500'C热压，之后将热压获得坯体在600'C下热挤压等工序，获得的Ag-Sn02材料。
通过本实例获得的Ag-Sn合金，总重损失0.06%，由此制备的Ag-Sn02材料中Sn02含量9.95wtn/。，强度为320MPa，导电率为2.12nQ.。
Claims (5)
1.一种Ag-SnO2废料循环再利用的方法，其特征在于，采用还原剂对Ag-SnO2材料进行还原处理，得到Ag-Sn合金，再将Ag-Sn合金作为原材料重新制备Ag-SnO2材料，从而实现Ag-SnO2材料循环利用；所述还原剂为石墨粉或氢气。
2. 根据权利要求l所述的Ag-Sn02废料循环再利用的方法，其特征在于，所述还原剂为石墨粉时，所述方法实现步骤如下：首先将Ag-Sn02废料与石墨粉一起在中频感应加热炉中，熔炼气氛为惰性气氛或真空；然后升温加热，温度在1000〜130(TC之间；之后即得到Ag-Sn合金，将其作为原材料重新制备成Ag-Sn02材料，实现循环再利用的目的。
3. 根据权利要求2所述的Ag-Sn02废料循环再利用的方法，其特征在于，所述加热，其保温时间15〜60分钟。
4. 根据权利要求l所述的Ag-Sn02废料循环再利用的方法，其特征在于，所述还原剂为氢气时，所述方法实现步骤如下：首先将Ag-Sn02废料置于中频感应炉中，往熔炼炉中通氢气将空气排出后，开始升温熔炼，熔炼温度1000〜1300'C之间，熔炼气氛为氢气；之后得到Ag-Sn合金，将其作为原材料重新制备成Ag-Sn02材料，实现循环再利用的目的。
5. 根据权利要求4所述的Ag-Sn02废料循环再利用的方法，其特征在于，所述熔炼，其保温时间0.5〜3小时。
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