JP2022180230A - Method for increasing the purity of iron(iii) chloride - Google Patents
Method for increasing the purity of iron(iii) chloride Download PDFInfo
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- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 title claims abstract description 169
- 229910021578 Iron(III) chloride Inorganic materials 0.000 title claims abstract description 85
- 238000000034 method Methods 0.000 title claims abstract description 26
- MSNWSDPPULHLDL-UHFFFAOYSA-K ferric hydroxide Chemical compound [OH-].[OH-].[OH-].[Fe+3] MSNWSDPPULHLDL-UHFFFAOYSA-K 0.000 claims abstract description 53
- 239000007788 liquid Substances 0.000 claims abstract description 44
- 239000002244 precipitate Substances 0.000 claims abstract description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 5
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 41
- 239000002002 slurry Substances 0.000 claims description 30
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000005530 etching Methods 0.000 claims description 12
- 239000002699 waste material Substances 0.000 claims description 12
- 238000000746 purification Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 abstract description 12
- 239000003513 alkali Substances 0.000 abstract description 2
- 238000000967 suction filtration Methods 0.000 description 40
- 239000000706 filtrate Substances 0.000 description 32
- 239000007864 aqueous solution Substances 0.000 description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 13
- 229910052791 calcium Inorganic materials 0.000 description 13
- 239000011575 calcium Substances 0.000 description 13
- 239000011572 manganese Substances 0.000 description 13
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 12
- 229910052748 manganese Inorganic materials 0.000 description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
本発明は、塩化鉄（ＩＩＩ）の高純度化方法に関する。 The present invention relates to a method for highly purifying iron(III) chloride.
プリント配線板やＩＣ、ＬＳＩ用のリードフレームなどは、塩化鉄（ＩＩＩ）を含むエッチング液で部分的に腐食処理することにより製造されている。
エッチング処理によって、エッチング液に含まれる塩化鉄（ＩＩＩ）が還元されて塩化鉄（ＩＩ）になり、塩化鉄（ＩＩＩ）の濃度が低下してエッチング効率が悪くなるので、定期的にエッチング液の交換が行われている。
Printed wiring boards, ICs, lead frames for LSIs, etc. are manufactured by partially corroding with an etchant containing iron (III) chloride.
During the etching process, the iron (III) chloride contained in the etching solution is reduced to become iron (II) chloride, and the concentration of iron (III) chloride decreases, resulting in poor etching efficiency. exchange is taking place.
なお、特許文献１には、鋼材酸洗廃液より高純度の酸化鉄を製造するための酸洗廃液の精製方法が記載されている。 Patent document 1 describes a method for purifying a pickling waste liquid for producing high-purity iron oxide from the steel pickling waste liquid.
エッチング処理後の廃液であるエッチング廃液は銅成分、ニッケル成分を多量に含んでいる。そこで鉄粉を加えることでイオン化傾向の差により銅粉、ニッケル粉を液中から取り出す還元処理がなされている。還元後の塩化鉄（ＩＩ）は酸化処理され、塩化鉄（ＩＩＩ）となり、エッチング液として再びリサイクルされるが、プロセス上、余剰に塩化鉄（ＩＩＩ）を含む溶液が生成され、廃棄されているのが現状である。 Etching waste liquid, which is a waste liquid after etching processing, contains a large amount of copper component and nickel component. Therefore, by adding iron powder, a reduction treatment is performed in which the copper powder and the nickel powder are removed from the liquid due to the difference in ionization tendency. Iron (II) chloride after reduction is oxidized to become iron (III) chloride, which is recycled as an etchant again. is the current situation.
廃棄される塩化鉄（ＩＩＩ）を含む溶液を再利用することができれば、資源の有効利用の観点、及び廃棄物の減少による環境負荷の低減の観点から望ましい。
しかしながら、還元処理工程において銅成分、ニッケル成分が除去されても完全に除去されるわけではなく、また、鉄粉を加えても還元されない成分も種々液中には含まれる。塩化鉄（ＩＩＩ）を含む溶液中の不純物成分としては、典型元素であるカルシウムや亜鉛、遷移元素である銅、ニッケル、マンガン、コバルト等が挙げられる。これらの不純物が含まれる結果、塩化鉄（ＩＩＩ）の純度が低いため、様々な用途（例えば、リン酸鉄リチウムイオンバッテリーの正極材料や顔料の原料など）に再利用することが難しいという問題があった。
If the solution containing iron (III) chloride to be discarded can be reused, it is desirable from the viewpoint of effective utilization of resources and reduction of environmental load due to reduction of waste.
However, even if the copper component and the nickel component are removed in the reduction treatment process, they are not completely removed, and the liquid contains various components that are not reduced even when iron powder is added. Impurity components in a solution containing iron (III) chloride include typical elements such as calcium and zinc, and transition elements such as copper, nickel, manganese and cobalt. As a result of containing these impurities, the purity of iron (III) chloride is low, so there is a problem that it is difficult to reuse it for various purposes (for example, positive electrode materials for lithium iron phosphate batteries and raw materials for pigments). there were.
特許文献１には、塩化第二鉄溶液にアルカリを添加し、ｐＨを３～４に制御することが記載されている。
しかしながら、特許文献１に記載された条件では、得られる沈殿物の固液分離性に劣り、処理時間が長くなり、効率が低い。また、得られた沈殿物を濾過した場合、不純物を含む濾液が付着しているため、沈殿物を水洗する場合があるが、特許文献１に記載された条件では沈殿物が水洗中に溶解してしまうため、純度を高めることは難しい。また、特許文献１ではＦｅ３＋のモル濃度について記載されておらず、固液分離性の効率についても記載されていない。
Patent Document 1 describes adding an alkali to a ferric chloride solution to control the pH to 3-4.
However, under the conditions described in Patent Document 1, the solid-liquid separability of the resulting precipitate is poor, the treatment time is long, and the efficiency is low. In addition, when the obtained precipitate is filtered, it may be washed with water because the filtrate containing impurities is attached, but under the conditions described in Patent Document 1, the precipitate is dissolved during washing. Therefore, it is difficult to increase the purity. Moreover, Patent Document 1 does not describe the molar concentration of Fe 3+ , nor does it describe the efficiency of solid-liquid separation.
本発明の課題は、塩化鉄（ＩＩＩ）の純度を高くすることができ、かつ効率に優れる塩化鉄（ＩＩＩ）の高純度化方法を提供することにある。 An object of the present invention is to provide a highly efficient method for highly purifying iron (III) chloride, which can increase the purity of iron (III) chloride.
上記課題は下記手段により達成することができる。
〔１〕
塩化鉄（ＩＩＩ）を含む溶液とアルカリ剤とを混合し、混合液中で水酸化鉄（ＩＩＩ）を含む沈殿物を得る工程（Ａ）と、
前記沈殿物を回収する工程（Ｂ）と、
回収された前記沈殿物と塩酸とを混合して、塩化鉄（ＩＩＩ）を含む溶液を得る工程（Ｃ）とを含み、
前記工程（Ａ）の前記混合液のｐＨをｐＨＡとし、下記式（１）で表されるｐＨの理論値をｐＨＴとし、Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００である、塩化鉄（ＩＩＩ）の高純度化方法。
ただし、Ｋｓｐは水酸化物溶解度積であり、Ｍｎ＋は金属イオンであり、［Ｍｎ＋］はＭｎ＋のモル濃度であり、ｎは価数であり、Ｋｗは水のイオン積である。
〔２〕
前記Ｄが、３．６７≦Ｄ≦６．０５である、〔１〕に記載の塩化鉄（ＩＩＩ）の高純度化方法。
〔３〕
前記工程（Ａ）で得られる前記混合液中のＦｅ３＋のモル濃度が、０．０５ｍｏｌ／Ｌ～２ｍｏｌ／Ｌである、〔１〕又は〔２〕に記載の塩化鉄（ＩＩＩ）の高純度化方法。
〔４〕
前記工程（Ａ）で用いられる前記塩化鉄（ＩＩＩ）を含む溶液が、エッチング廃液に由来する溶液である、〔１〕～〔３〕のいずれか１つに記載の塩化鉄（ＩＩＩ）の高純度化方法。
〔５〕
前記工程（Ｂ）が、前記沈殿物を含むスラリーを濾過する工程を含む、〔１〕～〔４〕のいずれか１つに記載の塩化鉄（ＩＩＩ）の高純度化方法。
〔６〕
前記工程（Ｂ）と前記工程（Ｃ）の間に、前記工程（Ｂ）で回収された沈殿物を水洗する工程を含む、〔１〕～〔５〕のいずれか１つに記載の塩化鉄（ＩＩＩ）の高純度化方法。
The above problems can be achieved by the following means.
[1]
A step (A) of mixing a solution containing iron (III) chloride with an alkaline agent to obtain a precipitate containing iron (III) hydroxide in the mixed solution;
a step (B) of recovering the precipitate;
a step (C) of mixing the recovered precipitate with hydrochloric acid to obtain a solution containing iron (III) chloride;
Let pH A be the pH of the mixed solution in step (A), pH T be the theoretical value of the pH represented by the following formula (1), and D = pH A - pH T , where 3.00 ≤ D A method for the purification of iron(III) chloride, wherein ≦7.00.
where K sp is the hydroxide solubility product, M n+ is the metal ion, [M n+ ] is the molar concentration of M n+ , n is the valence, and K w is the ionic product of water. .
[2]
The method for highly purifying iron (III) chloride according to [1], wherein D is 3.67≦D≦6.05.
[3]
High-purity iron(III) chloride according to [1] or [2], wherein the molar concentration of Fe 3+ in the mixed solution obtained in the step (A) is 0.05 mol/L to 2 mol/L. conversion method.
[4]
The iron (III) chloride-rich solution according to any one of [1] to [3], wherein the solution containing iron (III) chloride used in the step (A) is a solution derived from an etching waste liquid. purification method.
[5]
The method for highly purifying iron (III) chloride according to any one of [1] to [4], wherein the step (B) includes filtering the slurry containing the precipitate.
[6]
The iron chloride according to any one of [1] to [5], including a step of washing the precipitate collected in the step (B) with water between the step (B) and the step (C). (III) high purification method.
本発明によれば、塩化鉄（ＩＩＩ）の純度を高くすることができ、かつ効率に優れる塩化鉄（ＩＩＩ）の高純度化方法を提供することにある。 An object of the present invention is to provide a highly efficient method for increasing the purity of iron (III) chloride, which can increase the purity of iron (III) chloride.
本発明の塩化鉄（ＩＩＩ）の高純度化方法は、
塩化鉄（ＩＩＩ）を含む溶液とアルカリ剤とを混合し、混合液中で水酸化鉄（ＩＩＩ）を含む沈殿物を得る工程（Ａ）と、
前記沈殿物を回収する工程（Ｂ）と、
回収された前記沈殿物と塩酸とを混合して、塩化鉄（ＩＩＩ）を含む溶液を得る工程（Ｃ）とを含み、
前記工程（Ａ）の前記混合液のｐＨをｐＨＡとし、下記式（１）で表されるｐＨの理論値をｐＨＴとし、Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００である、塩化鉄（ＩＩＩ）の高純度化方法である。
The method for highly purifying iron (III) chloride of the present invention comprises:
A step (A) of mixing a solution containing iron (III) chloride with an alkaline agent to obtain a precipitate containing iron (III) hydroxide in the mixed solution;
a step (B) of recovering the precipitate;
a step (C) of mixing the recovered precipitate with hydrochloric acid to obtain a solution containing iron (III) chloride;
Let pH A be the pH of the mixed solution in step (A), pH T be the theoretical value of the pH represented by the following formula (1), and D = pH A - pH T , where 3.00 ≤ D A method for the high purification of iron(III) chloride, wherein ≦7.00.
ただし、Ｋｓｐは水酸化物溶解度積であり、Ｍｎ＋は金属イオンであり、［Ｍｎ＋］はＭｎ＋のモル濃度であり、ｎは価数であり、Ｋｗは水のイオン積である。 where K sp is the hydroxide solubility product, M n+ is the metal ion, [M n+ ] is the molar concentration of M n+ , n is the valence, and K w is the ionic product of water. .
［工程（Ａ）］
工程（Ａ）は、塩化鉄（ＩＩＩ）を含む溶液とアルカリ剤とを混合し、混合液中で水酸化鉄（ＩＩＩ）を含む沈殿物を得る工程である。
工程（Ａ）で用いられる塩化鉄（ＩＩＩ）を含む溶液は、塩化鉄（ＩＩＩ）を含む水溶液であることが好ましく、エッチング廃液に由来する溶液であることがより好ましい。エッチング廃液に由来する溶液とは、エッチング廃液又はエッチング廃液に対して何らかの処理（例えば酸化処理や還元処理）を行った後の溶液である。エッチング廃液に由来する溶液は通常は鉄以外の金属などの不純物を含有しており、本発明の方法を適用した際に本発明の効果が顕著に現れる。
工程（Ａ）で用いられる塩化鉄（ＩＩＩ）を含む溶液は、鉄以外の金属を含むものであることが好ましく、カルシウム、亜鉛、マンガン、コバルト、銅、ニッケル少なくとも１種を含むものであることがより好ましく、カルシウム及びマンガンの少なくとも１種を含むことが更に好ましい。
工程（Ａ）で用いられる塩化鉄（ＩＩＩ）を含む溶液は、例えば、塩化鉄（ＩＩＩ）を１～５０質量％、カルシウムを５０～３０００ｐｐｍ、マンガンを５０～３０００ｐｐｍ含むものであってもよい。「ｐｐｍ」は「ｐａｒｔｓ ｐｅｒ ｍｉｌｌｉｏｎ」の略であり、質量基準（「質量ｐｐｍ」）である。
[Step (A)]
Step (A) is a step of mixing a solution containing iron(III) chloride and an alkaline agent to obtain a precipitate containing iron(III) hydroxide in the mixed solution.
The solution containing iron (III) chloride used in step (A) is preferably an aqueous solution containing iron (III) chloride, and more preferably a solution derived from an etching waste liquid. The solution derived from the etching waste liquid is the etching waste liquid or the solution after the etching waste liquid is subjected to some treatment (for example, oxidation treatment or reduction treatment). A solution derived from an etching waste liquid usually contains impurities such as metals other than iron, and the effect of the present invention appears remarkably when the method of the present invention is applied.
The solution containing iron (III) chloride used in step (A) preferably contains a metal other than iron, and more preferably contains at least one of calcium, zinc, manganese, cobalt, copper, and nickel. More preferably, it contains at least one of calcium and manganese.
The solution containing iron (III) chloride used in step (A) may contain, for example, 1 to 50% by mass of iron (III) chloride, 50 to 3000 ppm of calcium, and 50 to 3000 ppm of manganese. "ppm" is an abbreviation for "parts per million" and is based on mass ("mass ppm").
工程（Ａ）で用いるアルカリ剤は特に限定されない。アルカリ剤としては、例えば、アンモニア水溶液、水酸化ナトリウム水溶液等が挙げられる。 The alkaline agent used in step (A) is not particularly limited. Examples of alkaline agents include an aqueous ammonia solution and an aqueous sodium hydroxide solution.
工程（Ａ）では、塩化鉄（ＩＩＩ）を含む溶液とアルカリ剤とを混合し、得られた混合液中で水酸化鉄（ＩＩＩ）を含む沈殿物を得る。
塩化鉄（ＩＩＩ）を含む溶液とアルカリ剤との混合比は特に限定されない。
In step (A), a solution containing iron (III) chloride and an alkaline agent are mixed to obtain a precipitate containing iron (III) hydroxide in the resulting mixed solution.
The mixing ratio of the solution containing iron (III) chloride and the alkaline agent is not particularly limited.
工程（Ａ）で得られる混合液のｐＨをｐＨＡとし、下記式（１）で表されるｐＨの理論値をｐＨＴとし、Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００である。 Let pH A be the pH of the mixed solution obtained in step (A), pH T be the theoretical value of the pH represented by the following formula (1), and D = pH A - pH T , where 3.00 ≤ D ≦7.00.
ただし、Ｋｓｐは水酸化物溶解度積であり、Ｍｎ＋は金属イオンであり、［Ｍｎ＋］はＭｎ＋のモル濃度であり、ｎは価数であり、Ｋｗは水のイオン積である。 where K sp is the hydroxide solubility product, M n+ is the metal ion, [M n+ ] is the molar concentration of M n+ , n is the valence, and K w is the ionic product of water. .
なお、ｐＨは温度によって変動するが、例えば１０～５０℃のｐＨとすることができ、１５～４０℃のｐＨとすることが好ましい。 Although the pH varies depending on the temperature, the pH can be, for example, 10 to 50°C, preferably 15 to 40°C.
上記式（１）において、Ｋｓｐは具体的には、水酸化鉄（ＩＩＩ）の溶解度積であり、１８～２５℃における値は、７．１×１０－４０である。Ｍｎ＋はＦｅ３＋である。Ｋｗは２５℃では１×１０－１４である。 In the above formula (1), K sp is specifically the solubility product of iron(III) hydroxide, and its value at 18 to 25° C. is 7.1×10 −40 . Mn + is Fe3 + . The K w is 1×10 −14 at 25°C.
Ｄが、３．６７≦Ｄ≦６．０５であることが特に好ましい。 It is particularly preferred that D is 3.67≤D≤6.05.
工程（Ａ）で得られる混合液中のＦｅ３＋のモル濃度は、０．０５ｍｏｌ／Ｌ～２ｍｏｌ／Ｌであることが好ましく、０．０７５ｍｏｌ／Ｌ～１ｍｏｌ／Ｌであることがより好ましい。 The molar concentration of Fe 3+ in the mixed solution obtained in step (A) is preferably 0.05 mol/L to 2 mol/L, more preferably 0.075 mol/L to 1 mol/L.
［工程（Ｂ）］
工程（Ｂ）は、工程（Ａ）で得られた水酸化鉄（ＩＩＩ）を含む沈殿物を回収する工程である。
工程（Ｂ）は、公知の手段（固液分離工程）により行うことができる。
工程（Ｂ）は、沈殿物を含むスラリーを濾過する工程を含むことが好ましく、沈殿物を含むスラリーを吸引濾過する工程を含むことがより好ましい。
[Step (B)]
Step (B) is a step of recovering the precipitate containing iron (III) hydroxide obtained in step (A).
The step (B) can be performed by known means (solid-liquid separation step).
The step (B) preferably includes a step of filtering the slurry containing the precipitate, more preferably a step of suction filtering the slurry containing the precipitate.
［工程（Ｃ）］
工程（Ｃ）は、回収された沈殿物と塩酸とを混合して、塩化鉄（ＩＩＩ）を含む溶液を得る工程である。
工程（Ｃ）で得られる塩化鉄（ＩＩＩ）を含む溶液は、塩化鉄（ＩＩＩ）を含む水溶液であることが好ましい。
工程（Ｃ）で得られる塩化鉄（ＩＩＩ）を含む溶液は、前述の工程（Ａ）で用いた塩化鉄（ＩＩＩ）を含む溶液よりも塩化鉄（ＩＩＩ）の純度が高くなっている。
工程（Ｃ）で用いる塩酸の濃度は特に限定されない。
[Step (C)]
Step (C) is a step of mixing the collected precipitate with hydrochloric acid to obtain a solution containing iron (III) chloride.
The solution containing iron(III) chloride obtained in step (C) is preferably an aqueous solution containing iron(III) chloride.
The solution containing iron (III) chloride obtained in step (C) has a higher purity of iron (III) chloride than the solution containing iron (III) chloride used in step (A).
The concentration of hydrochloric acid used in step (C) is not particularly limited.
［その他の工程］
本発明の塩化鉄（ＩＩＩ）の高純度化方法は、前述の工程（Ａ）と工程（Ｂ）と工程（Ｃ）に加え、更にその他の工程を含むことができる。
その他の工程は特に限定されないが、本発明の塩化鉄（ＩＩ）の高純度化方法は、工程（Ｂ）と工程（Ｃ）の間に、工程（Ｂ）で回収された沈殿物を水洗する工程を含むことが好ましい。
[Other processes]
The method for highly purifying iron (III) chloride of the present invention can further include other steps in addition to the above steps (A), (B) and (C).
Other steps are not particularly limited, but in the method for highly purifying iron (II) chloride of the present invention, the precipitate recovered in step (B) is washed with water between step (B) and step (C). It is preferable to include steps.
以下、本発明を実施例により具体的に説明するが、本発明は以下の実施例に限定されるものではない。 EXAMPLES Hereinafter, the present invention will be specifically described with reference to examples, but the present invention is not limited to the following examples.
実施例及び比較例で使用した塩化鉄（ＩＩＩ）水溶液Ａ～Ｃは、下記表１に示す成分を表１に示す含有量で含む塩化鉄（ＩＩＩ）水溶液である。 Iron (III) chloride aqueous solutions A to C used in Examples and Comparative Examples are iron (III) chloride aqueous solutions containing the components shown in Table 1 below in the contents shown in Table 1.
（実施例１）
塩化鉄（ＩＩＩ）水溶液Ａ４０ｍＬに希釈アンモニア水を１２０ｍＬ添加して混合液を得た。混合液中に水酸化鉄（ＩＩＩ）を含む沈殿物を得た。３０℃における混合液のｐＨ（ｐＨＡ）は５．００であり、混合液中のＦｅ３＋のモル濃度は０．８７（ｍｏｌ／Ｌ）であった。式（１）より算出したｐＨの理論値（ｐＨＴ）は０．９７であった。Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００を満たしているので、そのまま得られたスラリーを吸引濾過（この吸引濾過に要した時間をＴ１とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を８０ｇ得た。得られた水酸化鉄（ＩＩＩ）を含む濾物と純水２００ｍＬをビーカーに入れ攪拌し、スラリーを作成した。得られたスラリーを再び吸引濾過（この吸引濾過に要した時間をＴ２とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を得た。それぞれの吸引濾過に要した時間（Ｔ１及びＴ２）を表３に示す。水洗済みの水酸化鉄（ＩＩＩ）を含む濾物を塩酸にて溶解し、塩化鉄（ＩＩＩ）水溶液を得た。得られた塩化鉄（ＩＩＩ）水溶液の成分分析を行い、表４に結果を示した。また、カルシウム及びマンガンの除去率を表４に記載した。カルシウム及びマンガンの除去率が高いと、相対的に塩化鉄（ＩＩＩ）の純度が高くなるため、高純度化の効果が優れる。
(Example 1)
120 mL of diluted ammonia water was added to 40 mL of iron (III) chloride aqueous solution A to obtain a mixed liquid. A precipitate containing iron (III) hydroxide in the mixture was obtained. The pH (pH A ) of the mixed liquid at 30° C. was 5.00, and the molar concentration of Fe 3+ in the mixed liquid was 0.87 (mol/L). The theoretical pH value (pH T ) calculated from the formula (1) was 0.97. When D = pH A - pH T , since 3.00 ≤ D ≤ 7.00 is satisfied, the slurry obtained as it is is subjected to suction filtration (the time required for this suction filtration is T1 ). 80 g of a filtrate containing iron(III) hydroxide was obtained. The obtained filtrate containing iron (III) hydroxide and 200 mL of pure water were placed in a beaker and stirred to prepare a slurry. The slurry thus obtained was subjected to suction filtration again (the time required for this suction filtration is defined as T2 ) to obtain a filtrate containing iron (III) hydroxide. Table 3 shows the time required for each suction filtration (T 1 and T 2 ). The filtrate containing iron (III) hydroxide washed with water was dissolved in hydrochloric acid to obtain an aqueous iron (III) chloride solution. The component analysis of the obtained iron (III) chloride aqueous solution was performed, and the results are shown in Table 4. Table 4 also shows the removal rates of calcium and manganese. When the removal rate of calcium and manganese is high, the purity of iron (III) chloride is relatively high, so the effect of high purification is excellent.
除去率（％）＝１００×［｛用いた塩化鉄（ＩＩＩ）水溶液中の不純物量（ｐｐｍ）－水酸化鉄（ＩＩＩ）溶解後の不純物量（ｐｐｍ）｝／用いた塩化鉄（ＩＩＩ）水溶液中の不純物量（ｐｐｍ）］ Removal rate (%) = 100 × [{amount of impurities (ppm) in iron (III) chloride aqueous solution used - amount of impurities (ppm) after dissolution of iron (III) hydroxide} / iron (III) chloride aqueous solution used Amount of impurities in (ppm)]
（実施例２）
塩化鉄（ＩＩＩ）水溶液Ａ４０ｍＬに希釈アンモニア水を１２０ｍＬ添加して混合液を得た。混合液中に水酸化鉄（ＩＩＩ）を含む沈殿物を得た。２８℃における混合液のｐＨ（ｐＨＡ）は７．００であり、混合液中のＦｅ３＋のモル濃度は０．８７（ｍｏｌ／Ｌ）であった。式（１）より算出したｐＨの理論値（ｐＨＴ）は０．９７であった。Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００を満たしているので、そのまま得られたスラリーを吸引濾過（この吸引濾過に要した時間をＴ１とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を８０ｇ得た。得られた水酸化鉄（ＩＩＩ）を含む濾物と純水２００ｍＬをビーカーに入れ攪拌し、スラリーを作成した。得られたスラリーを再び吸引濾過（この吸引濾過に要した時間をＴ２とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を得た。それぞれの吸引濾過に要した時間（Ｔ１及びＴ２）を表３に示す。水洗済みの水酸化鉄（ＩＩＩ）を含む濾物を塩酸にて溶解し、塩化鉄（ＩＩＩ）水溶液を得た。得られた塩化鉄（ＩＩＩ）水溶液の成分分析を行い、表４に結果を示した。また、カルシウム及びマンガンの除去率を表４に記載した。
(Example 2)
120 mL of diluted ammonia water was added to 40 mL of iron (III) chloride aqueous solution A to obtain a mixed liquid. A precipitate containing iron (III) hydroxide in the mixture was obtained. The pH (pH A ) of the mixed liquid at 28° C. was 7.00, and the molar concentration of Fe 3+ in the mixed liquid was 0.87 (mol/L). The theoretical pH value (pH T ) calculated from the formula (1) was 0.97. When D = pH A - pH T , since 3.00 ≤ D ≤ 7.00 is satisfied, the slurry obtained as it is is subjected to suction filtration (the time required for this suction filtration is T1 ). 80 g of a filtrate containing iron(III) hydroxide was obtained. The obtained filtrate containing iron (III) hydroxide and 200 mL of pure water were placed in a beaker and stirred to prepare a slurry. The slurry thus obtained was subjected to suction filtration again (the time required for this suction filtration is defined as T2 ) to obtain a filtrate containing iron (III) hydroxide. Table 3 shows the time required for each suction filtration (T 1 and T 2 ). The filtrate containing iron (III) hydroxide washed with water was dissolved in hydrochloric acid to obtain an aqueous iron (III) chloride solution. The component analysis of the obtained iron (III) chloride aqueous solution was performed, and the results are shown in Table 4. Table 4 also shows the removal rates of calcium and manganese.
（実施例３）
塩化鉄（ＩＩＩ）水溶液Ｂ２２０ｍＬに希釈アンモニア水を６５０ｍＬ添加して混合液を得た。混合液中に水酸化鉄（ＩＩＩ）を含む沈殿物を得た。２５℃における混合液のｐＨ（ｐＨＡ）は５．００であり、混合液中のＦｅ３＋のモル濃度は０．０８（ｍｏｌ／Ｌ）であった。式（１）より算出したｐＨの理論値（ｐＨＴ）は１．３２であった。Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００を満たしているので、そのまま得られたスラリーを吸引濾過（この吸引濾過に要した時間をＴ１とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を５０ｇ得た。得られた水酸化鉄（ＩＩＩ）を含む濾物と純水２００ｍＬをビーカーに入れ攪拌し、スラリーを作成した。得られたスラリーを再び吸引濾過（この吸引濾過に要した時間をＴ２とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を得た。それぞれの吸引濾過に要した時間（Ｔ１及びＴ２）を表３に示す。水洗済みの水酸化鉄（ＩＩＩ）を含む濾物を塩酸にて溶解し、塩化鉄（ＩＩＩ）水溶液を得た。得られた塩化鉄（ＩＩＩ）水溶液の成分分析を行い、表４に結果を示した。また、カルシウム及びマンガンの除去率を表４に記載した。
(Example 3)
650 mL of diluted ammonia water was added to 220 mL of the iron (III) chloride aqueous solution B to obtain a mixed liquid. A precipitate containing iron (III) hydroxide in the mixture was obtained. The pH (pH A ) of the mixed liquid at 25° C. was 5.00, and the molar concentration of Fe 3+ in the mixed liquid was 0.08 (mol/L). The theoretical pH value (pH T ) calculated from the formula (1) was 1.32. When D = pH A - pH T , since 3.00 ≤ D ≤ 7.00 is satisfied, the slurry obtained as it is is subjected to suction filtration (the time required for this suction filtration is T1 ). , 50 g of a filtrate containing iron(III) hydroxide was obtained. The obtained filtrate containing iron (III) hydroxide and 200 mL of pure water were placed in a beaker and stirred to prepare a slurry. The slurry thus obtained was subjected to suction filtration again (the time required for this suction filtration is defined as T2 ) to obtain a filtrate containing iron (III) hydroxide. Table 3 shows the time required for each suction filtration (T 1 and T 2 ). The filtrate containing iron (III) hydroxide washed with water was dissolved in hydrochloric acid to obtain an aqueous iron (III) chloride solution. The component analysis of the obtained iron (III) chloride aqueous solution was performed, and the results are shown in Table 4. Table 4 also shows the removal rates of calcium and manganese.
（実施例４）
塩化鉄（ＩＩＩ）水溶液Ａ４０ｍＬに希釈水酸化ナトリウム溶液を１００ｍＬ添加して混合液を得た。混合液中に水酸化鉄（ＩＩＩ）を含む沈殿物を得た。３１℃における混合液のｐＨ（ｐＨＡ）は５．００であり、混合液中のＦｅ３＋のモル濃度は１（ｍｏｌ／Ｌ）であった。式（１）より算出したｐＨの理論値（ｐＨＴ）は０．９５であった。Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００を満たしているので、そのまま得られたスラリーを吸引濾過（この吸引濾過に要した時間をＴ１とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を８０ｇ得た。得られた水酸化鉄（ＩＩＩ）を含む濾物と純水２００ｍＬをビーカーに入れ攪拌し、スラリーを作成した。得られたスラリーを再び吸引濾過（この吸引濾過に要した時間をＴ２とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を得た。それぞれの吸引濾過に要した時間（Ｔ１及びＴ２）を表３に示す。水洗済みの水酸化鉄（ＩＩＩ）を含む濾物を塩酸にて溶解し、塩化鉄（ＩＩＩ）水溶液を得た。得られた塩化鉄（ＩＩＩ）水溶液の成分分析を行い、表４に結果を示した。また、カルシウム及びマンガンの除去率を表４に記載した。
(Example 4)
100 mL of diluted sodium hydroxide solution was added to 40 mL of iron (III) chloride aqueous solution A to obtain a mixed solution. A precipitate containing iron (III) hydroxide in the mixture was obtained. The pH (pH A ) of the mixed liquid at 31° C. was 5.00, and the molar concentration of Fe 3+ in the mixed liquid was 1 (mol/L). The theoretical pH value (pH T ) calculated from the formula (1) was 0.95. When D = pH A - pH T , since 3.00 ≤ D ≤ 7.00 is satisfied, the slurry obtained as it is is subjected to suction filtration (the time required for this suction filtration is T1 ). 80 g of a filtrate containing iron(III) hydroxide was obtained. The obtained filtrate containing iron (III) hydroxide and 200 mL of pure water were placed in a beaker and stirred to prepare a slurry. The slurry thus obtained was subjected to suction filtration again (the time required for this suction filtration is defined as T2 ) to obtain a filtrate containing iron (III) hydroxide. Table 3 shows the time required for each suction filtration (T 1 and T 2 ). The filtrate containing iron (III) hydroxide washed with water was dissolved in hydrochloric acid to obtain an aqueous iron (III) chloride solution. The component analysis of the obtained iron (III) chloride aqueous solution was performed, and the results are shown in Table 4. Table 4 also shows the removal rates of calcium and manganese.
（実施例５）
塩化鉄（ＩＩＩ）水溶液Ａ４０ｍＬに希釈水酸化ナトリウム溶液を１００ｍＬ添加して混合液を得た。混合液中に水酸化鉄（ＩＩＩ）を含む沈殿物を得た。３０℃における混合液のｐＨ（ｐＨＡ）は７．００であり、混合液中のＦｅ３＋のモル濃度は１（ｍｏｌ／Ｌ）であった。式（１）より算出したｐＨの理論値（ｐＨＴ）は０．９５であった。Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００を満たしているので、そのまま得られたスラリーを吸引濾過（この吸引濾過に要した時間をＴ１とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を８０ｇ得た。得られた水酸化鉄（ＩＩＩ）を含む濾物と純水２００ｍＬをビーカーに入れ攪拌し、スラリーを作成した。得られたスラリーを再び吸引濾過（この吸引濾過に要した時間をＴ２とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を得た。それぞれの吸引濾過に要した時間（Ｔ１及びＴ２）を表３に示す。水洗済みの水酸化鉄（ＩＩＩ）を含む濾物を塩酸にて溶解し、塩化鉄（ＩＩＩ）水溶液を得た。得られた塩化鉄（ＩＩＩ）水溶液の成分分析を行い、表４に結果を示した。また、カルシウム及びマンガンの除去率を表４に記載した。
(Example 5)
100 mL of diluted sodium hydroxide solution was added to 40 mL of iron (III) chloride aqueous solution A to obtain a mixed solution. A precipitate containing iron (III) hydroxide in the mixture was obtained. The pH (pH A ) of the mixed liquid at 30° C. was 7.00, and the molar concentration of Fe 3+ in the mixed liquid was 1 (mol/L). The theoretical pH value (pH T ) calculated from the formula (1) was 0.95. When D = pH A - pH T , since 3.00 ≤ D ≤ 7.00 is satisfied, the slurry obtained as it is is subjected to suction filtration (the time required for this suction filtration is T1 ). 80 g of a filtrate containing iron(III) hydroxide was obtained. The obtained filtrate containing iron (III) hydroxide and 200 mL of pure water were placed in a beaker and stirred to prepare a slurry. The slurry thus obtained was subjected to suction filtration again (the time required for this suction filtration is defined as T2 ) to obtain a filtrate containing iron (III) hydroxide. Table 3 shows the time required for each suction filtration (T 1 and T 2 ). The filtrate containing iron (III) hydroxide washed with water was dissolved in hydrochloric acid to obtain an aqueous iron (III) chloride solution. The component analysis of the obtained iron (III) chloride aqueous solution was performed, and the results are shown in Table 4. Table 4 also shows the removal rates of calcium and manganese.
（実施例６）
塩化鉄（ＩＩＩ）水溶液Ｂ２００ｍＬに希釈水酸化ナトリウム溶液を６５０ｍＬ添加して混合液を得た。混合液中に水酸化鉄（ＩＩＩ）を含む沈殿物を得た。２４℃における混合液のｐＨ（ｐＨＡ）は５．００であり、混合液中のＦｅ３＋のモル濃度は０．０７５（ｍｏｌ／Ｌ）であった。式（１）より算出したｐＨの理論値（ｐＨＴ）は１．３３であった。Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００を満たしているので、そのまま得られたスラリーを吸引濾過（この吸引濾過に要した時間をＴ１とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を５０ｇ得た。得られた水酸化鉄（ＩＩＩ）を含む濾物と純水２００ｍＬをビーカーに入れ攪拌し、スラリーを作成した。得られたスラリーを再び吸引濾過（この吸引濾過に要した時間をＴ２とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を得た。それぞれの吸引濾過に要した時間（Ｔ１及びＴ２）を表３に示す。水洗済みの水酸化鉄（ＩＩＩ）を含む濾物を塩酸にて溶解し、塩化鉄（ＩＩＩ）水溶液を得た。得られた塩化鉄（ＩＩＩ）水溶液の成分分析を行い、表４に結果を示した。また、カルシウム及びマンガンの除去率を表４に記載した。
(Example 6)
A mixed solution was obtained by adding 650 mL of diluted sodium hydroxide solution to 200 mL of iron (III) chloride aqueous solution B. A precipitate containing iron (III) hydroxide in the mixture was obtained. The pH (pH A ) of the mixed liquid at 24° C. was 5.00, and the molar concentration of Fe 3+ in the mixed liquid was 0.075 (mol/L). The theoretical pH value (pH T ) calculated from the formula (1) was 1.33. When D = pH A - pH T , since 3.00 ≤ D ≤ 7.00 is satisfied, the slurry obtained as it is is subjected to suction filtration (the time required for this suction filtration is T1 ). , 50 g of a filtrate containing iron(III) hydroxide was obtained. The obtained filtrate containing iron (III) hydroxide and 200 mL of pure water were placed in a beaker and stirred to prepare a slurry. The slurry thus obtained was subjected to suction filtration again (the time required for this suction filtration is defined as T2 ) to obtain a filtrate containing iron (III) hydroxide. Table 3 shows the time required for each suction filtration (T 1 and T 2 ). The filtrate containing iron (III) hydroxide washed with water was dissolved in hydrochloric acid to obtain an aqueous iron (III) chloride solution. The component analysis of the obtained iron (III) chloride aqueous solution was performed, and the results are shown in Table 4. Table 4 also shows the removal rates of calcium and manganese.
（実施例７）
塩化鉄（ＩＩＩ）水溶液Ｃ４０ｍＬに希釈アンモニア水を１２０ｍＬ添加して混合液を得た。混合液中に水酸化鉄（ＩＩＩ）を含む沈殿物を得た。３０℃における混合液のｐＨ（ｐＨＡ）は５．００であり、混合液中のＦｅ３＋のモル濃度は０．８７（ｍｏｌ／Ｌ）であった。式（１）より算出したｐＨの理論値（ｐＨＴ）は０．９７であった。Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００を満たしているので、そのまま得られたスラリーを吸引濾過（この吸引濾過に要した時間をＴ１とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を８０ｇ得た。得られた水酸化鉄（ＩＩＩ）を含む濾物と純水２００ｍＬをビーカーに入れ攪拌し、スラリーを作成した。得られたスラリーを再び吸引濾過（この吸引濾過に要した時間をＴ２とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を得た。それぞれの吸引濾過に要した時間（Ｔ１及びＴ２）を表３に示す。水洗済みの水酸化鉄（ＩＩＩ）を含む濾物を塩酸にて溶解し、塩化鉄（ＩＩＩ）水溶液を得た。得られた塩化鉄（ＩＩＩ）水溶液の成分分析を行い、表４に結果を示した。また、カルシウム及びマンガンの除去率を表４に記載した。
(Example 7)
120 mL of diluted aqueous ammonia was added to 40 mL of the iron (III) chloride aqueous solution C to obtain a mixed liquid. A precipitate containing iron (III) hydroxide in the mixture was obtained. The pH (pH A ) of the mixed liquid at 30° C. was 5.00, and the molar concentration of Fe 3+ in the mixed liquid was 0.87 (mol/L). The theoretical pH value (pH T ) calculated from the formula (1) was 0.97. When D = pH A - pH T , since 3.00 ≤ D ≤ 7.00 is satisfied, the slurry obtained as it is is subjected to suction filtration (the time required for this suction filtration is T1 ). 80 g of a filtrate containing iron(III) hydroxide was obtained. The obtained filtrate containing iron (III) hydroxide and 200 mL of pure water were placed in a beaker and stirred to prepare a slurry. The slurry thus obtained was subjected to suction filtration again (the time required for this suction filtration is defined as T2 ) to obtain a filtrate containing iron (III) hydroxide. Table 3 shows the time required for each suction filtration (T 1 and T 2 ). The filtrate containing iron (III) hydroxide washed with water was dissolved in hydrochloric acid to obtain an aqueous iron (III) chloride solution. The component analysis of the obtained iron (III) chloride aqueous solution was performed, and the results are shown in Table 4. Table 4 also shows the removal rates of calcium and manganese.
（比較例１）
塩化鉄（ＩＩＩ）水溶液Ａ３５ｍＬに希釈アンモニア水を１００ｍＬ添加して混合液を得た。混合液中に水酸化鉄（ＩＩＩ）を含む沈殿物を得た。３４℃における混合液のｐＨ（ｐＨＡ）は３．００であり、混合液中のＦｅ３＋のモル濃度は０．９１（ｍｏｌ／Ｌ）であった。式（１）より算出したｐＨの理論値（ｐＨＴ）は０．９６であった。Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００を満たしていなかったが、そのまま得られたスラリーを吸引濾過（この吸引濾過に要した時間をＴ１とする。）し、水酸化鉄（ＩＩＩ）を含む濾物を７０ｇ得た。濾液を見ると茶色がかっており、完全に水酸化鉄（ＩＩＩ）になっていないことがわかった。得られた水酸化鉄（ＩＩＩ）を含む濾物と純水２００ｍＬをビーカーに入れ攪拌し、スラリーを作成した。得られたスラリーを再び吸引濾過したが水酸化鉄（ＩＩＩ）が溶出してしまったため中止した。
(Comparative example 1)
100 mL of diluted ammonia water was added to 35 mL of iron (III) chloride aqueous solution A to obtain a mixed liquid. A precipitate containing iron (III) hydroxide in the mixture was obtained. The pH (pH A ) of the mixed liquid at 34° C. was 3.00, and the molar concentration of Fe 3+ in the mixed liquid was 0.91 (mol/L). The theoretical pH value (pH T ) calculated from the formula (1) was 0.96. When D = pH A - pH T , 3.00 ≤ D ≤ 7.00 was not satisfied, but the slurry obtained as it was was subjected to suction filtration (the time required for this suction filtration is defined as T 1 ). 70 g of a filtrate containing iron (III) hydroxide was obtained. The filtrate was found to be brownish and not completely converted to iron(III) hydroxide. The obtained filtrate containing iron (III) hydroxide and 200 mL of pure water were placed in a beaker and stirred to prepare a slurry. The resulting slurry was suction filtered again, but the filtration was stopped because iron (III) hydroxide was eluted.
（比較例２）
塩化鉄（ＩＩＩ）水溶液Ｂ２２０ｍＬに希釈アンモニア水を６５０ｍＬ添加して混合液を得た。混合液中に水酸化鉄（ＩＩＩ）を含む沈殿物を得た。２７℃における混合液のｐＨ（ｐＨＡ）は３．００であり、混合液中のＦｅ３＋のモル濃度は０．０８（ｍｏｌ／Ｌ）であった。式（１）より算出したｐＨの理論値（ｐＨＴ）は１．３２であった。Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００を満たしていなかったが、そのまま得られたスラリーに対して吸引濾過を試みたところ、水酸化鉄（ＩＩＩ）はほとんど得ることができなかったため中止した。
(Comparative example 2)
650 mL of diluted ammonia water was added to 220 mL of the iron (III) chloride aqueous solution B to obtain a mixed liquid. A precipitate containing iron (III) hydroxide in the mixture was obtained. The pH (pH A ) of the mixed liquid at 27° C. was 3.00, and the molar concentration of Fe 3+ in the mixed liquid was 0.08 (mol/L). The theoretical pH value (pH T ) calculated from the formula (1) was 1.32. When D = pH A - pH T , 3.00 ≤ D ≤ 7.00 was not satisfied, but when suction filtration of the slurry obtained as it was tried, iron (III) hydroxide was almost I stopped because I couldn't get it.
（比較例３）
塩化鉄（ＩＩＩ）水溶液Ｂ２００ｍＬに希釈水酸化ナトリウム溶液を６５０ｍＬ添加して混合液を得た。混合液中に水酸化鉄（ＩＩＩ）を含む沈殿物を得た。２５℃における混合液のｐＨ（ｐＨＡ）は３．００であり、混合液中のＦｅ３＋のモル濃度は０．０７５（ｍｏｌ／Ｌ）であった。式（１）より算出したｐＨの理論値（ｐＨＴ）は１．３３であった。Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００を満たしていなかったが、そのまま得られたスラリーに対して吸引濾過を試みたところ、水酸化鉄（ＩＩＩ）はほとんど得ることができなかったため中止した。
(Comparative Example 3)
A mixed solution was obtained by adding 650 mL of diluted sodium hydroxide solution to 200 mL of iron (III) chloride aqueous solution B. A precipitate containing iron (III) hydroxide in the mixture was obtained. The pH (pH A ) of the mixed liquid at 25° C. was 3.00, and the molar concentration of Fe 3+ in the mixed liquid was 0.075 (mol/L). The theoretical pH value (pH T ) calculated from the formula (1) was 1.33. When D = pH A - pH T , 3.00 ≤ D ≤ 7.00 was not satisfied, but when suction filtration of the slurry obtained as it was tried, iron (III) hydroxide was almost I stopped because I couldn't get it.
実施例１～６、比較例１～３のｐＨＡ、ｐＨＴ、Ｄ（ｐＨＡ－ｐＨＴ）を下記表２にまとめた。 The pH A , pH T , and D (pH A −pH T ) of Examples 1 to 6 and Comparative Examples 1 to 3 are summarized in Table 2 below.
実施例１～７は、吸引濾過に要する時間が短く、効率に優れていた。 In Examples 1 to 7, the time required for suction filtration was short and the efficiency was excellent.
実施例１～７は、カルシウムとマンガンの含有率が低くなり（除去率が高く）、塩化鉄（ＩＩＩ）の純度を高くすることができた。
In Examples 1 to 7, the content of calcium and manganese was low (the removal rate was high), and the purity of iron (III) chloride could be increased.
Claims (6)
前記沈殿物を回収する工程（Ｂ）と、
回収された前記沈殿物と塩酸とを混合して、塩化鉄（ＩＩＩ）を含む溶液を得る工程（Ｃ）とを含み、
前記工程（Ａ）の前記混合液のｐＨをｐＨＡとし、下記式（１）で表されるｐＨの理論値をｐＨＴとし、Ｄ＝ｐＨＡ－ｐＨＴとした場合、３．００≦Ｄ≦７．００である、塩化鉄（ＩＩＩ）の高純度化方法。
ただし、Ｋｓｐは水酸化物溶解度積であり、Ｍｎ＋は金属イオンであり、［Ｍｎ＋］はＭｎ＋のモル濃度であり、ｎは価数であり、Ｋｗは水のイオン積である。 A step (A) of mixing a solution containing iron (III) chloride with an alkaline agent to obtain a precipitate containing iron (III) hydroxide in the mixed solution;
a step (B) of recovering the precipitate;
a step (C) of mixing the recovered precipitate with hydrochloric acid to obtain a solution containing iron (III) chloride;
Let pH A be the pH of the mixed solution in step (A), pH T be the theoretical value of the pH represented by the following formula (1), and D = pH A - pH T , where 3.00 ≤ D A method for the purification of iron(III) chloride, wherein ≦7.00.
where K sp is the hydroxide solubility product, M n+ is the metal ion, [M n+ ] is the molar concentration of M n+ , n is the valence, and K w is the ionic product of water. .
The iron(III) chloride according to any one of claims 1 to 5, comprising a step of washing the precipitate recovered in step (B) with water between step (B) and step (C). ) for high purification.
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