CN102465330A - 去除助溶剂中铁离子的方法 - Google Patents
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- CN102465330A CN102465330A CN2011101923918A CN201110192391A CN102465330A CN 102465330 A CN102465330 A CN 102465330A CN 2011101923918 A CN2011101923918 A CN 2011101923918A CN 201110192391 A CN201110192391 A CN 201110192391A CN 102465330 A CN102465330 A CN 102465330A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 62
- -1 iron ions Chemical class 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000006184 cosolvent Substances 0.000 title abstract 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 34
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 26
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 17
- 239000011592 zinc chloride Substances 0.000 claims abstract description 17
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 17
- 238000009736 wetting Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 9
- 206010058490 Hyperoxia Diseases 0.000 claims description 8
- 230000000222 hyperoxic effect Effects 0.000 claims description 8
- 239000004575 stone Substances 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- OMBRFUXPXNIUCZ-UHFFFAOYSA-N dioxidonitrogen(1+) Chemical compound O=[N+]=O OMBRFUXPXNIUCZ-UHFFFAOYSA-N 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 7
- 238000001914 filtration Methods 0.000 abstract description 4
- 230000001590 oxidative effect Effects 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 238000002791 soaking Methods 0.000 abstract 3
- 229910000831 Steel Inorganic materials 0.000 abstract 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- 239000010959 steel Substances 0.000 abstract 1
- 230000001502 supplementing effect Effects 0.000 abstract 1
- KFZAUHNPPZCSCR-UHFFFAOYSA-N iron zinc Chemical compound [Fe].[Zn] KFZAUHNPPZCSCR-UHFFFAOYSA-N 0.000 description 6
- 229910000640 Fe alloy Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 210000005056 cell body Anatomy 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1617—Purification and regeneration of coating baths
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1635—Composition of the substrate
- C23C18/1637—Composition of the substrate metallic substrate
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/54—Contact plating, i.e. electroless electrochemical plating
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Electrochemistry (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
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Abstract
一种去除助溶剂中铁离子的方法,用以润湿铁材对象的表面,该方法包括:以溶剂、氯化锌及氯化铵而在配制槽中配制助溶剂并送至处理槽;浸泡铁材对象于助溶剂中以溶出表面的部分铁并产生润湿作用;加入高氧化性气体以氧化助溶剂中的铁离子,形成氧化铁而沉淀;抽取出助溶剂并利用多层滤网过滤出已沉淀的氧化铁;以及将过滤后的助溶剂回流至处理槽中,并重复上述的铁材对象浸泡处理,以持续去除铁材对象浸泡处理中所产生的铁离子。本方法可维持助溶剂中氯化锌及氯化铵的浓度,确保钢铁表面上的润湿作用,而不需额外补充氯化锌及氯化铵。
Description
技术领域
本发明涉及一种去除助溶剂中铁离子的方法,尤其是注入高氧化性气体而不影响助溶剂中氯化锌及氯化铵的浓度并使铁离子形成氧化铁而沉淀。
背景技术
利用助溶剂进行润湿处理以润湿铁材对象的表面,是一般镀锌工序中常用的前期处理,以方便在后续的镀锌处理中形成具高度耐蚀性的高质量锌铁合金层,进而保护铁材物件。
在润湿处理中,铁材对象的表面会部分溶于助溶剂,而在后续的镀锌处理中使锌液产生锌渣,导致铁材对象的锌铁合金层质量不良,降低防蚀性。因此,在现有技术中,常须检验助溶剂的铁离子含量并加以过滤清除,而一般传统技术人员的实际做法是添加双氧水到助溶剂中,使铁离子反应而沉淀,再进行过滤以去除氧化铁,而达到去除助溶剂中铁离子的目的。
然而,上述的铁离子去除效率只有40%至60%之间,且助溶剂中的氯化锌及氯化铵浓度会因加入水溶液的双氧水而大幅度降低,所以必须添加大量的氯化锌及氯化铵以维持铁材对象的润湿作用,因而增加处理成本。因此,需要一种不影响氯化锌及氯化铵浓度以去除助溶剂中铁离子的方法,以解决上述现有技术的问题。
发明内容
本发明的主要目的在提供一种去除助溶剂中铁离子的方法,对铁材对象的表面进行润湿处理以方便后续镀锌处理时锌层的形成,该方法包括:以氯化锌及氯化铵并添加溶剂而在处理槽中配制助溶剂;将铁材对象浸泡于处理槽中的助溶剂以使铁材对象表面的铁溶于助溶剂中;在处理槽中的助溶剂中加入高氧化性气体,以使助溶剂中的铁离子氧化而形成不溶性的氧化铁并沉淀;抽出处理槽中的助溶剂并利用多层滤网过滤出已沉淀的氧化铁;以及将过滤后的助溶剂回流至处理槽中,并重复上述铁材对象的浸泡处理。
由于本发明的方法可持续去除助溶剂中因铁材对象浸泡所产生的铁离子,并且可维持助溶剂中氯化锌及氯化铵的浓度而不需补充氯化锌及氯化铵,因而能确保对铁材对象表面所产生的润湿作用,非常适合用于后续的镀锌工序,可帮助锌铁反应进行而形成具耐蚀性的锌铁合金层,进而保护铁材物件。
附图说明
图1为本发明去除助溶剂中铁离子的方法的操作流程示意图。
图2为本发明去除助溶剂中铁离子的方法的系统示意图。
具体实施方式
以下配合附图对本发明的实施方式做更详细的说明,使熟悉本技术领域的技术人员在阅读本说明书后能据以实施。
参考图1及图2,分别为本发明去除助溶剂中铁离子的方法的操作流程示意图及系统示意图。如图1及图2所示,本发明的方法首先由步骤S10开始,以氯化锌及氯化铵并添加溶剂而在配置槽10中配制第一助溶剂F1,并传送至处理槽20。
上述第一助溶剂F1的配制可利用搅拌装置以提高氯化锌及氯化铵的溶解速率,其中搅拌装置可包括多个搅拌棒或多个搅拌叶片,且搅拌装置可由塑料或陶瓷材料构成。氯化锌及氯化铵的混合重量比可为1∶1.05至1∶1.55之间。溶剂可为去离子水或纯水。
要注意的是,本发明的另一实施例可使用配置槽10当作处理槽20,即,上述的配置槽10及处理槽20可为同一槽体。
接着进入步骤S20,将铁材对象30浸泡于处理槽20所包含的第一助溶剂F1中,以使铁材对象30的表面的部分铁溶于第一助溶剂F1中而形成铁离子,进而达到对铁材对象30的表面的润湿作用。
在步骤S30中,在含有铁离子的第一助溶剂F1中加入高氧化性气体G,以使得第一助溶剂F1中的铁离子与高氧化性气体G产生氧化反应而形成不溶性的氧化铁并沉淀,进而形成包含氧化铁沉淀物的第二助溶剂F2。
高氧化性气体G可包括二氧化氮、三氧化氮、高纯度氧气或臭氧,其中高纯度氧气可为氧气纯度高于50%,且高氧化性气体G可经由处理槽20的底部以气泡上升的方式注入而与铁离子反应。此外,可利用混合装置(图中未显示),比如搅拌棒,以加强铁离子的氧化反应速率。
然后在步骤S40中,可用抽水马达(图中未示)以抽取出处理槽20中的第二助溶剂F2,并利用多层滤网40以过滤出第二助溶剂F2中的氧化铁沉淀物,并产生不含氧化铁沉淀物或包含低氧化铁含量的第三助溶剂F3。
最后进入步骤S50,将过滤后的第三助溶剂F3回流至处理槽20中,并回到步骤S20以重复上述的铁材对象浸泡处理。
上述本发明的特点在于,可维持助溶剂中氯化锌及氯化铵的浓度而不需补充氯化锌及氯化铵,能确保对铁材对象表面的润湿作用,很适合应用于后续的镀锌工序中,帮助进行锌铁反应以形成具耐蚀性的锌铁合金层,而达到保护铁材对象的目的。
以上所述仅是用以解释本发明的较佳实施例,并非企图据以对本发明做任何形式上的限制,因此,凡有在相同的发明精神下所作有关本发明的任何修饰或变更,皆仍应包括在本发明权利要求的范畴。
Claims (4)
1.一种去除助溶剂中铁离子的方法,其特征在于,本发明方法包括以下步骤:
以氯化锌及氯化铵并添加溶剂而在一配制槽中配制第一助溶剂,并传送至一处理槽;
将铁材对象浸泡于该第一助溶剂中,使得该铁材对象的表面的部分铁溶于该第一助溶剂中而形成铁离子,以润湿该铁材对象的表面;
加入高氧化性气体于该处理槽的第一助溶剂中,以使该第一助溶剂中的铁离子氧化而形成不溶性的氧化铁并沉淀,进而形成包含氧化铁的第二助溶剂;
抽取出该第二助溶剂,并利用多层滤网过滤出该第二助溶剂中已沉淀的氧化铁,并产生不含氧化铁或包含低氧化铁含量的第三助溶剂;以及
将该第三助溶剂回流至该处理槽中,并重复另一铁材对象的上述浸泡处理,以持续去除因铁材对象浸泡所产生的铁离子。
2.如权利要求1所述的方法,其特征在于,该助溶剂中的氯化锌及氯化铵的混合重量比为1∶1.05至1∶1.55之间,且该溶剂为去离子水或纯水。
3.如权利要求1所述的方法,其特征在于,该配制槽当作该处理槽使用。
4.如权利要求1所述是方法,其特征在于,该高氧化性气体包括二氧化氮、三氧化氮、高纯度氧气及臭氧的其中之一,且该高纯度氧气为氧气纯度高于50%的气体。
Priority Applications (3)
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PCT/CN2011/001509 WO2013006995A1 (zh) | 2011-07-11 | 2011-09-06 | 去除助溶剂中铁离子的方法 |
US14/232,049 US20140158544A1 (en) | 2010-11-18 | 2011-09-06 | Method for removing iron ions from galvanizing flux solution |
GB1400362.8A GB2510705A (en) | 2011-07-11 | 2011-09-06 | Method for removing iron ions in solubility promoter |
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TW99139845A TW201221481A (en) | 2010-11-18 | 2010-11-18 | Method of removing iron ion from flux |
TW099139845 | 2010-11-18 |
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CN102465330A true CN102465330A (zh) | 2012-05-23 |
CN102465330B CN102465330B (zh) | 2015-05-13 |
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CN104955990A (zh) * | 2013-02-05 | 2015-09-30 | 不二商事株式会社 | 镀液的再生方法 |
US10316400B1 (en) * | 2017-05-11 | 2019-06-11 | Beta Control Systems, Incorporated | Systems and methods for removing impurities from galvanizing flux solution |
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CN1974834A (zh) * | 2006-12-01 | 2007-06-06 | 华南理工大学 | 用于热镀锌生产线的助镀液综合处理方法及装置 |
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CN1974834A (zh) * | 2006-12-01 | 2007-06-06 | 华南理工大学 | 用于热镀锌生产线的助镀液综合处理方法及装置 |
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US20140158544A1 (en) | 2014-06-12 |
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