CN114031386B - 一种绿色环保的资源回收利用方法 - Google Patents
一种绿色环保的资源回收利用方法 Download PDFInfo
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- 238000004064 recycling Methods 0.000 title claims abstract description 14
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- 239000002699 waste material Substances 0.000 claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 38
- 239000010802 sludge Substances 0.000 claims abstract description 32
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000011812 mixed powder Substances 0.000 claims abstract description 7
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 30
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 30
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 claims description 22
- PGTXKIZLOWULDJ-UHFFFAOYSA-N [Mg].[Zn] Chemical compound [Mg].[Zn] PGTXKIZLOWULDJ-UHFFFAOYSA-N 0.000 claims description 22
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 claims description 22
- 229910001308 Zinc ferrite Inorganic materials 0.000 claims description 19
- 239000011787 zinc oxide Substances 0.000 claims description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
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- 238000013461 design Methods 0.000 claims description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- 239000000395 magnesium oxide Substances 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 239000000654 additive Substances 0.000 claims description 7
- 230000000996 additive effect Effects 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- 238000003801 milling Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000428 dust Substances 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000010902 jet-milling Methods 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 239000011572 manganese Substances 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 238000011085 pressure filtration Methods 0.000 claims 1
- 229910052596 spinel Inorganic materials 0.000 claims 1
- 239000011029 spinel Substances 0.000 claims 1
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 17
- 239000002994 raw material Substances 0.000 description 12
- 230000004907 flux Effects 0.000 description 4
- WJZHMLNIAZSFDO-UHFFFAOYSA-N manganese zinc Chemical compound [Mn].[Zn] WJZHMLNIAZSFDO-UHFFFAOYSA-N 0.000 description 4
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- 238000012360 testing method Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002902 ferrimagnetic material Substances 0.000 description 2
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- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 description 1
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- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种绿色环保的资源回收利用方法，包括以下步骤：(1)将沉降池内的废淤泥料压滤后晾晒干燥；(2)将干燥后的粉料进行破碎和气流磨粉碎；(3)将粉碎后的粉料混匀，进行取样检测，得到主要元素质量比；(4)将混匀的粉料作为主料，再加入辅料进行球磨混料，混合均匀后进行预烧；(5)将预烧后的粉料进行砂磨、喷雾造粒和烧结，得到软磁铁氧体材料。本发明通过重复利用工厂沉降池中废淤泥料，降低了软磁铁氧体的生产成本，解决了粉料生产工厂废料处理的环保问题，所得材料完全符合抗信号干扰软磁铁氧体磁环的使用要求。
Description
技术领域
本发明属于亚铁磁性材料领域，更具体地说是涉及一种绿色环保的资源回收利用方法。
背景技术
软磁铁氧体属于亚铁磁性材料，主要包括锰锌铁氧体、镁锌铁氧体和镍锌铁氧体，其中应用量最大的为锰锌铁氧体，约占市场份额的70％。随着科技的发展和进步，铁氧体材料被广泛应用于车载电子、电子变压器等不同领域，与此同时，作为主材的氧化铁、氧化锌、氧化锰、氧化镁、氧化镍等原材料的价格也飞速上涨，同时原料的供给也供不应求，导致铁氧体生产困难重重。随着国家对环保问题的愈加重视，铁氧体生产厂家的废料浆处理成本日益增加，每年产生的地面废料和淤泥超过千吨，均摊成本很高，因此对于地面废料带来的厂内污水池淤泥处理和重新利用便尤为重要。
目前，申请公布号CN 102557606A的发明专利公开了一种使用废旧镁锌铁氧体磁芯制作镁锌软磁铁氧体材料的方法，能够有效降低生产成本。但废旧的镁锌铁氧体磁芯价格越来越高，加上处理投入与新材料投入相差并不大，并且重利用的过程中必然还会带来地面废料，经过冲洗和沉降后变为工厂内污水池中的淤泥。申请公布号CN109912301A的发明专利公开了一种利用锰锌研磨泥制造铁氧体的方法及铁氧体，能够对磁芯的磨泥进行重复利用，但对工厂内的污水池内淤泥的堆积和处理没有提供良好的建议。申请公布号CN101412623A的发明专利公开了一种用锰锌铁氧体废料生产锰锌铁氧体颗粒料的方法，能够将废旧磁芯经过硫酸强化浸出进行重复利用，但此处理方法本就成本较高，不利于降低成本，并且在处理过程产生废液是强污染物，不符合环保生产的要求。因此急需一种环境友好、降低生产成本、可重复利用淤泥废料的软磁铁氧体制备方法。
发明内容
有鉴于此，本发明提供了一种绿色环保的资源回收利用方法，可重复利用工厂沉降池中废淤泥料，降低铁氧体生产成本并解决粉料生产工厂废料处理的环保问题。
为了实现上述目的，本发明采用如下技术方案：
一种绿色环保的资源回收利用方法，包括以下步骤：
S1：将软磁铁氧体生产场地的沉降池沉降后的废淤泥料进行压滤、晾晒干燥，得到粉料；
S2：将干燥后的粉料采用振磨机或球磨机破碎，再进行气流磨粉碎；
S3：将粉碎后的粉料投入锥混机中混合均匀，使用荧光分析仪进行成分检测，得到主要元素质量比；
S4：将混合均匀的粉料作为主料，根据设计配方，加入辅料进行球磨混料，混合均匀后进行预烧；
S5：将预烧后的粉料加入添加剂进行砂磨，然后加入粘结剂，喷雾造粒得到平均粒度为3-35um的颗粒料，烧结，得到软磁铁氧体材料。
优选地，所述软磁铁氧体材料包括尖晶石结构的锰锌铁氧体材料和镁锌铁氧体材料。
优选地，步骤S1中所述废淤泥料为生产过程中地面废料、地沟废料、除尘器沉积料和生产过程中的不合格料。
优选地，步骤S1中压滤后的废淤泥料含水量为5-20wt％，晾晒干燥后的粉料含水量低于5wt％。
优选地，步骤S2中气流磨前后设有筛网，筛网目数为50目、100目、200目或400目。
优选地，步骤S2中气流磨粉碎后的粉料粒度为0.5-5um。
优选地，步骤S3中混合均匀的粉料所含元素包括铁、锰、锌，其中铁元素质量比含量为65-75％。
优选地，步骤S3中，制备锰锌铁氧体材料时，所述设计配方为Fe2O3：MnO：ZnO的质量比为70.7：21.1：8.2；制备镁锌铁氧体材料时，所述设计配方为Fe2O3：MnO：MgO：ZnO的质量比为64.2：15.2：3：15。
优选地，步骤S4中，制备锰锌铁氧体材料时，所述辅料为质量分别占主料1-10wt％的氧化铁和1-8wt％的氧化锌；制备镁锌铁氧体材料时，所述辅料为质量分别占主料5-20wt％的氧化铁、1-15wt％的氧化镁和1-15wt％的氧化锌。
优选地，步骤S4中预烧时间为0.5-2h；制备锰锌铁氧体时，预烧温度为800-1000℃；制备镁锌铁氧体时，预烧温度为900-1150℃。
优选地，步骤S5中砂磨时间为1-5h；制备锰锌铁氧体时，所述添加剂选自Bi2O3、V2O5、CaCO3和Nb2O5中的一种或几种，添加量为预烧后粉料的0-5wt％；制备镁锌铁氧体时，所述添加剂选自SiO2、CaCO3、V2O5和Bi2O3中的一种或几种，添加量为预烧后粉料的0-5wt％。
CaCO3可在后续烧结时形成CaO，起到稳定晶界的作用，增加材料的Bs和电阻率，进一步降低材料的功耗。Nb2O5可起到助烧剂的作用，降低烧结温度，细化烧结后磁芯晶粒，降低功耗，使其达到此种材料所需要的性能。
优选地，步骤S5中，制备锰锌铁氧体时，所述粘结剂为占预烧后粉料0.8-1.2wt％的聚乙烯醇；制备镁锌铁氧体时，所述粘结剂为占预烧后粉料1-1.5wt％的聚乙烯醇。
后续压制磁芯时需要颗粒粉料具有粘性，聚乙烯醇起到粘结的作用。镁锌材料的压制密度要求更高，且磁芯多需要磨削，因此对磁芯的毛坯强度有要求，需要更多的聚乙烯醇。
本发明的优点在于，合理利用了软磁铁氧体生产过程中产生的废淤泥料，既解决了淤泥料处理难以处理的环保问题，又降低了粉料生产过程中的原料成本，生产出的软磁铁氧体材料完全符合相关性能要求。
本发明实施后，可实现废淤泥料100％重复利用，使工厂生产过程中的废料实现循环，符合绿色工厂的理念。同时，生产锰锌铁氧体的原料成本为74wt％氧化铁、23wt％氧化锰，目前氧化铁的价格为2万/吨，氧化锰的价格为1.2万/吨，现有的软磁铁氧体生产线每月会产生废淤泥料20吨以上，而废淤泥料中存在70wt％左右的氧化铁和20wt％左右的氧化锰，采用本发明的技术方案，每吨废淤泥料可以节约1.64万元。
具体实施方式
下面将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。
实施例1
利用锰锌铁氧体产线产生的废淤泥料制备锰锌铁氧体的方法
(1)将沉降池中的锰锌废淤泥料进行压滤处理，形成滤饼后进行晾晒干燥处理，检测粉料含水量为2wt％。
(2)将干燥的粉料加入到振磨机中振磨3h，测试粒度为10um，后将粗破碎的粉料投入到气流磨机中，细粉碎至粒度为1um。
(3)将粉碎后的粉料投入到锥混机中搅拌30min，混合均匀后使用荧光分析仪进行材料的成分检测，检测结果与原料检测结果对比如表1所示：
表1成分检测结果
| 原料 | Fe<sub>2</sub>O<sub>3</sub> | MnO | ZnO | NiO | SiO<sub>2</sub> | CaO | P<sub>2</sub>O<sub>5</sub> | Al<sub>2</sub>O<sub>3</sub> | Cr<sub>2</sub>O<sub>3</sub> | MgO | CuO |
| 废淤泥料 | 71.71 | 21.89 | 5.74 | 0.14 | 0.055 | 0.12 | 0.0024 | 0.0196 | 0.0272 | 0.032 | 0.05 |
| 氧化铁 | 99.4 | 0.2745 | - | 0.008 | 0.03 | 0.065 | 0.015 | 0.005 | - | 0.01 | - |
| 氧化锰 | 0.04 | 98.84 | - | - | 0.01 | 0.03 | 0.002 | - | - | 0.026 | - |
| 氧化锌 | 0.001 | - | 97.4 | - | 0.003 | 0.002 | 0.002 | - | - | - | - |
(4)按设计配方为Fe2O3：MnO：ZnO＝70.7：21.1：8.2的质量比进行振磨机混料，首先进行计算废淤泥料与设计配方之间的差异，后将差异进行原料添加，其中废淤泥料的使用量占总量的90wt％以上。
依照氧化锰原料占比百分比计算，需要21.1/21.89＝96.4％，因此需要加入处理后废淤泥料96.4wt％，此时等同于加入21.1wt％氧化锰和71.71*96.4wt％＝69.13wt％的氧化铁，还需要加入1.57wt％(70.7-69.13＝1.57wt％)的氧化铁，同样还需加入2.67wt％(8.2-5.74*96.4％＝2.67wt％)的氧化锌。
考虑到废淤泥料中存在少量的锰锌添加剂，需要根据最后的配方矫正加入0.05wt％Nb2O5。
(5)将混合好的粉料通过回转窑进行预烧结，烧结温度为850℃，时间为1.5h。
(6)将预烧后的物料通过振磨机粗破碎后将粉料投入到砂磨机中，根据荧光检测结果，在淤泥料中包含0.12wt％CaO，0.05wt％Nb2O5需要单独添加后砂磨1h。
(7)将砂磨好的料浆加入0.8wt％的聚乙烯醇，混合均匀后进行喷雾造粒，调节颗粒为5um，烧结得到锰锌铁氧体材料。
此款锰锌铁氧体材料主要关注两个指标，饱和磁通密度Bs需要大于490mT，常温25℃功耗需要低于700mW/cc。经过测试，按照本发明方法生产的铁氧体材料Bs可达到510mT，功耗可以达到450mW/cc，性能完全满足相关要求。
实施例2
利用锰锌铁氧体产线产生的废淤泥料制备镁锌铁氧体的方法：
(1)将沉降池中的镁锌废淤泥料进行压滤处理，形成滤饼后进行晾晒干燥处理，检测粉料含水量为2wt％。
(2)将干燥的粉料加入振磨机中振磨3h，测试粒度为10um，后将粗破碎的粉料投入到气流磨机中，细粉碎至粒度为1um。
(3)将粉碎后的粉料投入锥混机中进行搅拌混合30min，使用荧光分析仪进行材料的成分检测，检测结果与原料检测结果对比如表2所示：
表2成分检测结果
| 原料 | Fe<sub>2</sub>O<sub>3</sub> | MnO | ZnO | NiO | SiO<sub>2</sub> | CaO | P<sub>2</sub>O<sub>5</sub> | Al<sub>2</sub>O<sub>3</sub> | Cr<sub>2</sub>O<sub>3</sub> | MgO | CuO |
| 废淤泥料 | 71.71 | 21.89 | 5.74 | 0.14 | 0.055 | 0.12 | 0.0024 | 0.0196 | 0.0272 | 0.032 | 0.05 |
| 氧化铁 | 99.4 | 0.2745 | - | 0.008 | 0.03 | 0.065 | 0.015 | 0.005 | - | 0.01 | - |
| 氧化镁 | 0.08 | 0.01 | 0.04 | 0.06 | 0.02 | 0.04 | 0.004 | 0.15 | - | 98.5 | - |
| 氧化锌 | 0.001 | - | 97.4 | - | 0.003 | 0.002 | 0.002 | - | - | - | - |
(4)按设计配方为Fe2O3：MnO：MgO：ZnO＝64.2：15.2：3：15的质量比进行振磨机混料，首先进行计算废淤泥料与设计配方之间的差异，然后将差异进行原料添加。
依照氧化锰原料占比百分比计算，需要15.2/21.89＝69.43％，因此需要加入处理后废淤泥料69.43wt％，此时等同于加入15.2wt％氧化锰和71.71*69.43wt％＝49.78wt％的氧化铁，还需要加入14.42wt％(64.2-49.78＝14.42wt％)的氧化铁，同样计算得还需要加入11.00wt％(15-5.74*69.43％＝11.00wt％)的氧化锌。因为锰锌废淤泥料中氧化镁的含量极少，混料过程暂不考虑，后续从待喷池做调整，此时需要完全添加新原料，直接加入3wt％氧化镁。
(5)将混合好的粉料通过回转窑进行预烧结，烧结温度为1050℃，时间为1h。
(6)将预烧后的物料通过振磨机粗破碎后将粉料投入到砂磨机中，砂磨1h，并在过程中加入0.25wt％Bi2O3和0.12wt％CaCO3。
(7)将砂磨好的料浆加入1.5wt％的聚乙烯醇，混合均匀后进行喷雾造粒，调节颗粒为3um，烧结得到镁锌铁氧体材料。
此款镁锌铁氧体可应用于制作抗信号干扰磁环，主要关注三个指标，初始磁导率需要大于400，饱和磁通密度Bs需要大于250mT，居里温度需要大于125℃，此方法生产的铁氧体性能初始磁导率为420，饱和磁通密度Bs为260mT，居里温度Tc为128℃，完全满足此款产品的要求。如果用纯原料制备的镁锌铁氧体，初始磁导率为430，饱和磁通密度Bs为265mT，居里温度Tc为130℃，与本发明指标接近。
本说明书中各个实施例采用递进的方式描述，每个实施例重点说明的都是与其他实施例的不同之处，各个实施例之间相同相似部分互相参见即可。对于实施例公开的装置而言，由于其与实施例公开的方法相对应，所以描述的比较简单，相关之处参见方法部分说明即可。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (6)
1.一种绿色环保的资源回收利用方法，其特征在于，包括以下步骤：
S1：将软磁铁氧体生产场地的沉降池沉降后的废淤泥料进行压滤、晾晒干燥，得到粉料；
S2：将干燥后的粉料采用振磨机或球磨机破碎，再进行气流磨粉碎；
S3：将粉碎后的粉料投入锥混机中混合均匀，使用荧光分析仪进行成分检测，得到主要元素质量比；
S4：将混合均匀的粉料作为主料，根据设计配方，加入辅料进行球磨混料，混合均匀后进行预烧；
S5：将预烧后的粉料加入添加剂进行砂磨，然后加入粘结剂，喷雾造粒得到平均粒度为3-35um的颗粒料，烧结，得到软磁铁氧体材料；
所述软磁铁氧体材料包括尖晶石结构的锰锌铁氧体材料和镁锌铁氧体材料；
步骤S4中，制备锰锌铁氧体材料时，所述设计配方为Fe2O3：MnO：ZnO的质量比为70.7：21.1：8.2；制备镁锌铁氧体材料时，所述设计配方为Fe2O3：MnO：MgO：ZnO的质量比为64.2：15.2：3：15；
步骤S4中，制备锰锌铁氧体材料时，所述辅料为质量分别占主料1-10wt％的氧化铁和1-8wt％的氧化锌；制备镁锌铁氧体材料时，所述辅料为质量分别占主料5-20wt％的氧化铁、1-15wt％的氧化镁和1-15wt％的氧化锌；
步骤S4中预烧时间为0.5-2h；制备锰锌铁氧体时，预烧温度为800-1000℃；制备镁锌铁氧体时，预烧温度为900-1150℃；
步骤S5中砂磨时间为1-5h；制备锰锌铁氧体时，所述添加剂选自Bi2O3、V2O5、CaCO3和Nb2O5中的一种或几种，添加量为预烧后粉料的0-5wt％；制备镁锌铁氧体时，所述添加剂选自SiO2、CaCO3、V2O5和Bi2O3中的一种或几种，添加量为预烧后粉料的0-5wt％。
2.根据权利要求1所述的绿色环保的资源回收利用方法，其特征在于，步骤S1中所述废淤泥料为生产过程中地面废料、地沟废料、除尘器沉积料和生产过程中的不合格料。
3.根据权利要求1所述的绿色环保的资源回收利用方法，其特征在于，步骤S1中压滤后的废淤泥料含水量为5-20wt％，晾晒干燥后的粉料含水量低于5wt％。
4.根据权利要求1所述的绿色环保的资源回收利用方法，其特征在于，步骤S2中气流磨粉碎后的粉料粒度为0.5-5um。
5.根据权利要求1所述的绿色环保的资源回收利用方法，其特征在于，步骤S3中混合均匀的粉料所含元素包括铁、锰、锌，其中铁元素质量比含量为65-75％。
6.根据权利要求1所述的绿色环保的资源回收利用方法，其特征在于，步骤S5中，制备锰锌铁氧体时，所述粘结剂为占预烧后粉料0.8-1.2wt％的聚乙烯醇；制备镁锌铁氧体时，所述粘结剂为占预烧后粉料1-1.5wt％的聚乙烯醇。
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