CN113884359A - 一种镍阳极泥少量样品脱硫方法 - Google Patents
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
Abstract
本发明涉及一种镍阳极泥少量样品脱硫方法,包括:(1)取适量镍阳极泥样品进行低温烘干或室温晾干,干透的样品碾压并磨细至200目以下,混匀并缩分一定量;(2)将缩分好的样品加入一定体积的纯水,在室温下振荡洗涤、过滤,直至流出液为中性;(3)在低温下烘干纯水洗涤后的滤渣,然后碾细、混匀,加入一定体积的X溶剂,室温搅拌洗涤,真空快速抽滤;(4)将X溶剂洗涤后的滤渣依次用无水乙醇、纯水洗涤,过滤,反复多次,最后得到的滤渣经低温烘干后可用于物质组成检测分析。本发明简单易行,方便快捷,单质硫脱除率高,可为镍阳极泥物质组成检测提供适合的样品。
Description
技术领域
本发明涉及镍阳极泥脱硫技术领域,尤其涉及一种镍阳极泥少量样品脱硫方法。
背景技术
镍阳极泥是镍电解精炼中附着于阳极基体表面或沉淀于电解槽底或悬浮于电解液中的泥状物。镍阳极泥的成分随产地不同差异很大,其组分通常以硫、镍、铜、铁为主,还含碳、硅酸盐炉渣等,铂族金属和金、银的品位仅0.01%~10%。其中,粗镍电解精炼的阳极泥产率小(2%~5%),贵金属富集倍数高,阳极泥含硫低(8%~10%),含铜(40%~60%),还含二氧化硅和碳(约20%~30%),贵金属品位可达1%~10%。而硫化镍电解精炼的阳极泥产率大(约25%),贵金属富集程度低,阳极泥含硫高(70%~96%),含铜镍低(1%~15%),贵金属品位仅0.01%~1%。因此,镍阳极泥的处理需根据其组成不同选择各种不同方法来处理回收有价金属。镍阳极泥中的硫,60%-80%是单质硫,少量是硫酸盐(NiSO4、Fe2(SO4)3、CuSO4)及硫化物(硫化镍、硫化铁、硫化铜)。
金川公司镍冶炼厂镍电解车间随着产量的不断加大,每年产生的镍阳极泥可达上万吨,这些阳极泥是采用硫化镍电解精炼产生的,含有很高的单质硫和少量有价金属,为了查明镍阳极泥中的物质成分,需要对其进行物质组成检测分析,而镍阳极泥中单质硫含量较高,会对设备造成损坏,需要在做物质组成检测前进行脱硫处理。
传统的脱除镍阳极泥中单质硫的方法主要有两种:一种是将阳极泥加热至130℃~145℃熔化,在保温状态下热过滤,滤出不溶残渣,液态单质硫冷却回收,但是这种方法适合大规模生产,对于样品的物质组成检测方面,由于样品量少,不容易操作;另一种是采用将样品在马弗炉加热至120℃~135℃,单质硫可以挥发去除,这种方法适合含有少量硫的样品,但是这种方法处理周期长,而且加热过程产生的刺激性烟气污染环境。
鉴于此,亟需一种适合少量样品脱除镍阳极泥中单质硫的方法,为镍阳极泥物质组成检测提供一种方便、快捷的脱硫方法。
发明内容
本发明所要解决的技术问题是提供一种方便、快捷的镍阳极泥少量样品脱硫方法。
为解决上述问题,本发明所述的一种镍阳极泥少量样品脱硫方法包括:
(1)取适量镍阳极泥样品进行低温烘干或室温晾干,干透的样品碾压并磨细至200目以下,混匀并缩分一定量;
(2)将缩分好的样品加入一定体积的纯水,在室温下振荡洗涤、过滤,直至流出液为中性;
(3)在低温下烘干纯水洗涤后的滤渣,然后碾细、混匀,加入一定体积的X溶剂,室温搅拌洗涤,真空快速抽滤;
(4)将X溶剂洗涤后的滤渣依次用无水乙醇、纯水洗涤,过滤,反复多次,最后得到的滤渣经低温烘干后可用于物质组成检测分析。
优选地,还包括:将步骤(3)中得到的滤液用于结晶析出单质硫。
优选地,步骤(1)和步骤(3)中低温烘干指在80℃以下烘箱中烘干。
优选地,步骤(1)中缩分采用四分法。
优选地,步骤(3)中X溶剂为二硫化碳溶剂。
本发明与现有技术相比具有以下优点:
本发明中,先将镍阳极泥洗涤,分离水溶性物质,然后将不溶性物质在一定条件下加入一定量溶剂,过滤,洗涤,溶液回收溶剂用于结晶析出单质硫,滤渣进行物质组成检测,简单易行,方便快捷,单质硫脱除率高,可为镍阳极泥物质组成检测提供适合的样品。
具体实施方式
镍阳极泥1#
一种镍阳极泥少量样品脱硫方法,可为镍阳极泥物质组成检测提供适合的样品,该方法具体包括如下内容:
(1)将湿的镍阳极泥在室温下晾干,缩分500g在磨样机中磨细(200目以下),并缩分100g样品。
(2)将步骤(1)缩分好的样品加入到锥形瓶中,并量取200ml纯水加入到锥形瓶中,在室温下振荡洗涤30min,过滤,纯水洗涤至流出液为中性(pH =7)。
(3)在低温下烘干步骤(2)纯水洗涤后的滤渣(在80℃以下烘箱中进行),将烘干后的滤渣碾细、混匀,加入到锥形瓶中,并量取100ml二硫化碳溶剂加入到锥形瓶中,室温搅拌洗涤10min,真空快速抽滤。
该步骤中在进行少量二硫化碳溶剂洗涤、过滤后,滤液可以单独回收,在旋转蒸发仪蒸发溶剂,结晶析出的即为单质硫。
(4)将步骤(3)二硫化碳溶剂洗涤后的滤渣依次用无水乙醇(分析纯)、纯水洗涤,过滤,反复多次,最后得到的滤渣经低温烘干后可直接用于物质组成检测分析。
镍阳极泥2#
除步骤(1)中所用“湿的镍阳极泥”不同,其余步骤与镍阳极泥1#一致。1#是生产现场正常阳极泥,2#是试验阳极泥。
验证实验
为验证本发明脱硫方法的脱硫效果,申请人对镍阳极泥1#和2#制取过程中不同阶段样品分别进行了元素分析和失重率计算等试验,具体内容如下。
对步骤(1)缩分100g阳极泥样品进行元素分析,结果见表1。
表1 阳极泥元素分析结果/%
将步骤(2)中纯水洗涤后的溶液定容在250ml的容量瓶中,用原子吸收光谱仪测定其中的金属含量,分析水溶性物质的成分及含量。洗涤后的阳极泥在低温下烘干,称重,计算失重率。阳极泥洗涤条件及洗涤液分析结果见表2。
表2 阳极泥样品洗涤条件及结果
续表2 洗涤液中元素含量(g/l)及水溶性盐类金属含量(%)
由表可知,镍阳极泥1#的失重率为5.3%,说明1#阳极泥中约含有5%水溶性盐类。水溶性盐类含镍9.48%,含铜4.20%,阳极泥是在硫酸体系中产生的,因此,水溶性盐类镍以NiSO4计算,含量为24.99%,铜以CuSO4计算,含量为10.50%。
镍阳极泥2#的失重率为3.0%,说明2#阳极泥中约含有3%水溶性盐类。水溶性盐类含镍16.33%,含铜2.50%,阳极泥是在硫酸体系中产生的,因此,水溶性盐类镍以NiSO4计算,含量为43.05%,铜以CuSO4计算,含量为6.25%。
对步骤(2)纯水洗涤完成后样品进行元素分析,结果见表3。
表3 纯水洗涤后阳极泥元素分析/%
注:因为水洗后部分可溶性盐类去除了,总重减少,所以S元素百分含量相对变高。
对步骤(4)低温烘干后样品(最终成品)进行元素分析,结果见表4。
表4 脱硫后阳极泥元素分析/%
编号 | Ni | Cu | Fe | S |
1# | 13.18 | 32.90 | 5.51 | 23.80 |
2# | 26.33 | 4.70 | 13.28 | 25.50 |
对比表1和表4中单质硫的含量可见,本发明脱硫方法具有较高的单质硫脱除率。
以上对本发明所提供的技术方案进行了详细介绍。本文中应用了具体个例对本发明的原理及实施方式进行了阐述,以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求的保护范围内。
Claims (5)
1.一种镍阳极泥少量样品脱硫方法,该方法包括:
(1)取适量镍阳极泥样品进行低温烘干或室温晾干,干透的样品碾压并磨细至200目以下,混匀并缩分一定量;
(2)将缩分好的样品加入一定体积的纯水,在室温下振荡洗涤、过滤,直至流出液为中性;
(3)在低温下烘干纯水洗涤后的滤渣,然后碾细、混匀,加入一定体积的X溶剂,室温搅拌洗涤,真空快速抽滤;
(4)将X溶剂洗涤后的滤渣依次用无水乙醇、纯水洗涤,过滤,反复多次,最后得到的滤渣经低温烘干后可用于物质组成检测分析。
2.如权利要求1所述的方法,其特征在于,还包括:将步骤(3)中得到的滤液用于结晶析出单质硫。
3.如权利要求1所述的方法,其特征在于,步骤(1)和步骤(3)中低温烘干指在80℃以下烘箱中烘干。
4.如权利要求1所述的方法,其特征在于,步骤(1)中缩分采用四分法。
5.如权利要求1所述的方法,其特征在于,步骤(3)中X溶剂为二硫化碳溶剂。
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Cited By (2)
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CN114635034A (zh) * | 2022-03-29 | 2022-06-17 | 宁波大地化工环保有限公司 | 一种高硫阳极泥湿法循环脱硫工艺 |
CN115465903A (zh) * | 2022-08-29 | 2022-12-13 | 金川集团股份有限公司 | 一种洗涤含贵金属镍阳极泥的方法 |
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