JPH07116479A - Method for recovering phosphoric acid - Google Patents
Method for recovering phosphoric acidInfo
- Publication number
- JPH07116479A JPH07116479A JP26498293A JP26498293A JPH07116479A JP H07116479 A JPH07116479 A JP H07116479A JP 26498293 A JP26498293 A JP 26498293A JP 26498293 A JP26498293 A JP 26498293A JP H07116479 A JPH07116479 A JP H07116479A
- Authority
- JP
- Japan
- Prior art keywords
- phosphoric acid
- advance
- dialysate
- hydrochloric acid
- ion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 11
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims description 40
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 11
- 239000003011 anion exchange membrane Substances 0.000 claims abstract description 11
- 150000001768 cations Chemical class 0.000 claims abstract description 11
- 238000011084 recovery Methods 0.000 claims abstract description 9
- 238000000502 dialysis Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000011550 stock solution Substances 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- 239000012466 permeate Substances 0.000 claims description 8
- 125000000129 anionic group Chemical group 0.000 claims description 3
- 150000001450 anions Chemical class 0.000 abstract description 13
- 229940085991 phosphate ion Drugs 0.000 abstract description 12
- 239000007788 liquid Substances 0.000 abstract 2
- 229910021645 metal ion Inorganic materials 0.000 abstract 2
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000002253 acid Substances 0.000 description 7
- 238000005530 etching Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- -1 sulphate Chemical class 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000005349 anion exchange Methods 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 239000003014 ion exchange membrane Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- MGQIWUQTCOJGJU-UHFFFAOYSA-N [AlH3].Cl Chemical compound [AlH3].Cl MGQIWUQTCOJGJU-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/36—Regeneration of waste pickling liquors
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- ing And Chemical Polishing (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は種々のイオン種を含有す
る混合溶液から陰イオン交換膜を介して燐酸イオンを選
択的に透過させ回収する燐酸回収法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a phosphoric acid recovery method for selectively permeating and recovering phosphate ions from a mixed solution containing various ionic species through an anion exchange membrane.
【０００２】[0002]
【従来の技術】金属の酸による洗浄、エッチング等の工
程においては、通常塩酸、硫酸、硝酸、フッ酸等のよう
な酸が使用されるが、この工程の速度等を制御するため
に燐酸等も添加される場合が少なくない。かかる場合、
酸洗いやエッチング排液は種々の酸の混合物を多量含有
しており、そこから酸を回収する場合、塩酸は揮発性で
あるため容易に回収できるが、酸の中でも格段に高価な
燐酸が回収困難で、通常は産業廃棄物として廃棄のため
の費用までかけて処理している。2. Description of the Prior Art Acids such as hydrochloric acid, sulfuric acid, nitric acid, and hydrofluoric acid are usually used in the steps such as cleaning and etching of metals with acid, and phosphoric acid and the like are used to control the speed of this step. Is often added. In such cases,
The pickling and etching effluent contains a large amount of a mixture of various acids, and when recovering acid from it, hydrochloric acid can be easily recovered because it is volatile, but phosphoric acid, which is much more expensive than other acids, is recovered. Difficult and usually dispose of as industrial waste at a cost for disposal.
【０００３】従ってこのような混合物から燐酸を効率的
に回収できれば燐酸を有効に再利用できるのみならず、
廃棄物処理費も節約できるのでそのような回収方法の開
発が望まれていた。Therefore, if phosphoric acid can be efficiently recovered from such a mixture, not only can phosphoric acid be effectively reused,
Since the waste treatment cost can be saved, the development of such a recovery method has been desired.
【０００４】[0004]
【発明が解決しようとする課題】しかしこのような金属
陽イオン種および２種以上の種々の陰イオン種を含有す
る水溶液を陰イオン交換膜を介して純水中に透過させる
と、透過速度の大きい１価の陰イオン例えば塩素イオ
ン、硝酸イオン等が最初に透過され、次に２価の陰イオ
ン例えば硫酸イオンが透過され、燐酸イオンのような３
価の陰イオンは透過しにくいので最後に透過することと
なる。However, when an aqueous solution containing such a metal cation species and two or more kinds of various anion species is permeated into pure water through an anion exchange membrane, the permeation rate is increased. Large monovalent anions such as chloride and nitrate are permeated first, followed by divalent anions such as sulphate, and phosphate such as phosphate.
Valuate anions are difficult to permeate, so they will permeate last.
【０００５】陰イオン交換膜は金属陽イオンは透過させ
ないが、プロトンは透過させるので実質的には酸の透過
が進行することとなり、残留する陰イオン当量が金属陽
イオン当量に等しくなるまで減少して透過が停止する。
従って、透過が遅い燐酸イオンが原液側に残留し、酸の
中では格段に高価な燐酸の実質的回収がほとんど不可能
となっていた。その上、原液から酸性成分が透過により
透析液側に移行して酸性度が低下すると、燐酸の金属塩
が不溶性となる場合が多く、しばしば膜面に析出して陰
イオン交換操作を妨害していた。The anion exchange membrane does not allow the permeation of metal cations, but allows the permeation of protons, so that the permeation of acid progresses substantially, and the remaining anion equivalent is reduced until it becomes equal to the metal cation equivalent. Transmission stops.
Therefore, phosphate ions, which have slow permeation, remain on the side of the undiluted solution, and it is almost impossible to recover phosphoric acid, which is much more expensive in the acid. In addition, when acidic components from the stock solution permeate to the dialysate side due to permeation and the acidity decreases, the metal salts of phosphoric acid often become insoluble, often precipitating on the membrane surface and interfering with the anion exchange operation. It was
【０００６】従って、本発明は、これまでイオン交換膜
での透過による分離回収が困難だった燐酸を選択的に透
過させて効率的に回収できる方法を模索探究した結果開
発されたものである。エッチング排液のような、金属陽
イオン種および２種以上の陰イオン種例えば塩素イオ
ン、硝酸イオン、硫酸イオン、燐酸イオン、フッ素イオ
ン等を含有する混合溶液を陰イオン交換膜にかけた場
合、透析原液中に存在する塩酸を透析液にも添加するこ
とは、燐酸を選択的に透過させて回収をはかるという本
願発明の目的と一見矛盾する。しかし、原液と透析液と
の間の塩素イオン濃度の差を小さくすることにより、実
質的に塩素イオンの透過を抑制でき、目的とする燐酸イ
オンの選択的透過を高めることができるという効果を奏
することができる上、たとえ透析液中で目的とする燐酸
に塩酸が混入していても、回収した燐酸を再びエッチン
グ液として使用する場合には塩酸を添加する必要がある
ので、透析液に塩酸が存在することに何の不都合もな
く、むしろ好都合である。Therefore, the present invention was developed as a result of searching for a method for selectively permeating and efficiently recovering phosphoric acid, which has been difficult to separate and recover by permeation through an ion exchange membrane. When a mixed solution containing a metal cation species and two or more anion species such as an etching drainage solution such as chloride ion, nitrate ion, sulfate ion, phosphate ion, and fluorine ion is applied to the anion exchange membrane, dialysis The addition of hydrochloric acid present in the stock solution to the dialysate is seemingly contradictory to the purpose of the present invention to selectively permeate phosphoric acid for recovery. However, by reducing the difference in chlorine ion concentration between the stock solution and the dialysate, it is possible to substantially suppress the permeation of chlorine ions and to enhance the selective permeation of target phosphate ions. In addition, even if hydrochloric acid is mixed with the target phosphoric acid in the dialysate, it is necessary to add hydrochloric acid when using the recovered phosphoric acid again as an etching solution. There is no inconvenience to being there, but rather an advantage.
【０００７】また、透析原液中に存在する透過を意図し
ない陰イオン種の当量の総和がプロトン以外の陽イオン
種の当量の総和よりも低い場合には、透過の進行につれ
て透過回収を意図する陰イオン種である燐酸イオンが塩
を構成する陰イオンとして原液側に残り、それ以上透過
が進行しなくなる事実があった。このような場合に、透
過を意図しない陰イオン種好ましくは塩酸を陽イオン種
の当量の総和以上となるように透析原液に予め添加した
場合は、透過を意図する燐酸イオンの原液側への残留を
抑制し、透過を促進させることができ、それと同時にま
た原液のpHの上昇に起因する燐酸塩の結晶の析出等の問
題をも防ぐことができることをも見出した。本発明はこ
れら上記した知見に基づくものである。If the total equivalents of anion species not intended to permeate present in the dialysis stock solution is lower than the total equivalents of cation species other than protons, the anions intended to be permeated as the permeation proceeds. There was a fact that phosphate ion, which is an ionic species, remained on the undiluted solution side as an anion constituting a salt, and the permeation did not proceed any further. In such a case, when anion species not intended to be permeated, preferably hydrochloric acid, is added to the dialysis stock solution in advance such that the total amount of equivalents of the cationic species is equal to or more than the total amount, the phosphate ions intended to be permeated remain on the stock side. It was also found that it is possible to suppress the above-mentioned problems and promote the permeation, and at the same time, to prevent the problems such as the precipitation of phosphate crystals due to the increase of the pH of the stock solution. The present invention is based on these findings described above.
【０００８】[0008]
【課題を解決するための手段】すなわち本発明は、燐酸
イオン、塩素イオン及び金属陽イオン種を含有する混合
溶液から陰イオン交換膜を介して燐酸イオンを選択的に
透過させ回収するにあたり、塩酸を透析液に予め添加す
ることを特徴とする燐酸回収法に関する。本発明はま
た、燐酸イオン、塩素イオン及び金属陽イオン種を含有
する混合溶液から陰イオン交換膜を介して燐酸イオンを
選択的に透過させ回収するにあたり、塩酸を透析液に予
め添加し、かつ透過を意図しない陰イオン種をプロトン
以外の陽イオン種の当量の総和以上となるように透析原
液中に予め添加することを特徴とする燐酸回収法にも関
する。Means for Solving the Problems That is, according to the present invention, when the phosphate ion is selectively permeated and recovered from the mixed solution containing the phosphate ion, the chlorine ion and the metal cation species through the anion exchange membrane, To a dialysate in advance, and relates to a method for recovering phosphoric acid. In the present invention, in selectively permeating and recovering phosphate ions from a mixed solution containing phosphate ions, chloride ions and metal cation species through the anion exchange membrane, hydrochloric acid is added to the dialysate in advance, and It also relates to a phosphoric acid recovery method characterized in that anionic species not intended to be permeated are added in advance to the dialysis stock solution so as to be equal to or more than the total equivalent amount of cationic species other than protons.
【０００９】本発明において透析液に予め添加される塩
酸の量は、原液中に存在する塩素イオン濃度とほぼ等し
くなるまでとするのが好適である。本発明で好適に使用
される陰イオン交換膜をあげればネオセプタ（徳山ソー
ダ製）その他である。In the present invention, it is preferable that the amount of hydrochloric acid added to the dialysate in advance be substantially equal to the concentration of chloride ions present in the stock solution. Examples of the anion exchange membrane preferably used in the present invention include Neoceptor (manufactured by Tokuyama Soda) and others.
【００１０】[0010]
【実施例】以下の実施例により本発明を詳細に説明す
る。 実施例１ 下記組成： Al+3 1.5ｇモル／1000mL Cl- 4 ｇモル／1000mL PO4 -3 0.5ｇモル／1000mL を有する、アルミの塩酸によるエッチング装置からの排
水を陰イオン交換膜を介して処理した。未処理排水は燐
酸イオンが除去された場合、残る塩素イオンだけでは陽
イオンであるアルミニウムイオン濃度に比較して当量が
不足するので、原液に塩酸を加えてCl- 濃度が4.5gモル
／1000mLとなるように調整した。また透析液である水に
は塩酸をその濃度が4.5gモル／1000mLとなるまで添加し
た。原液と透析液はイオン交換膜ネオセプタ（徳山ソー
ダ製）を介して向流に流して拡散透析を行った。The present invention will be described in detail with reference to the following examples. Example 1 Waste water from an aluminum hydrochloric acid etching apparatus having the following composition: Al +3 1.5 gmol / 1000 mL Cl − 4 gmol / 1000 mL PO 4 -3 0.5 gmol / 1000 mL was passed through an anion exchange membrane. Processed. If untreated wastewater that phosphate ions are removed, only the remaining chloride ions because insufficient equivalents compared to the aluminum ion concentration is a cation, by adding hydrochloric acid to the stock solution Cl - concentration and 4.5g mol / 1000 mL I adjusted it so that. Hydrochloric acid was added to water as a dialysate until the concentration reached 4.5 gmol / 1000 mL. Diffusion dialysis was performed by flowing the stock solution and the dialysate countercurrently through an ion exchange membrane Neoceptor (manufactured by Tokuyama Soda).
【００１１】透析処理済みの原液中における燐酸イオン
濃度は0.1gモル／1000mLまで低下しており、そして透析
液側燐酸イオン濃度は0.4gモル／1000mLで、80％の燐酸
が回収されていた。 比較例１ 実施例１におけると同様の組成を有するエッチング装置
からの排水を、透析液に塩酸を添加しない以外は実施例
１と同様にして陰イオン交換処理した。燐酸はほとんど
透過せず、実質的には燐酸の回収はできなかった。The phosphate ion concentration in the dialyzed stock solution had dropped to 0.1 gmol / 1000 mL, and the phosphate ion concentration on the dialysate side was 0.4 gmol / 1000 mL, and 80% of the phosphoric acid had been recovered. Comparative Example 1 Wastewater from an etching apparatus having the same composition as in Example 1 was subjected to anion exchange treatment in the same manner as in Example 1 except that hydrochloric acid was not added to the dialysate. Phosphoric acid was hardly permeated, and phosphoric acid could not be substantially recovered.
【００１２】[0012]
【発明の効果】以上説明したとおり、本発明の燐酸回収
法によれば、塩酸を透析液に予め添加することにより、
目的とする燐酸イオンを選択的かつ効率的に透過させる
ことができ、また塩酸を透析液に予め添加することに加
え、透過を意図しない陰イオン種を透析原液に予め添加
することにより、燐酸イオンを選択的かつ効率的に透過
させることができる。As described above, according to the phosphoric acid recovery method of the present invention, by adding hydrochloric acid to the dialysate in advance,
The target phosphate ion can be selectively and efficiently permeated, and in addition to adding hydrochloric acid to the dialysate in advance, anion species not intended to permeate are added to the dialysate stock solution in advance. Can be selectively and efficiently transmitted.
Claims (2)
ン種を含有する混合溶液から陰イオン交換膜を介して燐
酸イオンを選択的に透過させ回収するにあたり、塩酸を
透析液に予め添加することを特徴とする燐酸回収法。1. To selectively permeate and recover phosphate ions from a mixed solution containing phosphate ions, chloride ions and metal cation species through an anion exchange membrane, it is necessary to add hydrochloric acid to a dialysate in advance. Characteristic phosphoric acid recovery method.
ン種を含有する混合溶液から陰イオン交換膜を介して燐
酸イオンを選択的に透過させ回収するにあたり、塩酸を
透析液に予め添加し、かつ透過を意図しない陰イオン種
をプロトン以外の陽イオン種の当量の総和以上となるよ
うに透析原液中に予め添加することを特徴とする燐酸回
収法。2. To selectively permeate and recover phosphate ions from a mixed solution containing phosphate ions, chloride ions and metal cation species through an anion exchange membrane, hydrochloric acid is added to a dialysate in advance, and A method for recovering phosphoric acid, characterized in that anionic species not intended to be permeated are added in advance to the dialysis stock solution so that the total amount of the anionic species other than protons becomes equal to or more than the total equivalent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26498293A JPH07116479A (en) | 1993-10-22 | 1993-10-22 | Method for recovering phosphoric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26498293A JPH07116479A (en) | 1993-10-22 | 1993-10-22 | Method for recovering phosphoric acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH07116479A true JPH07116479A (en) | 1995-05-09 |
Family
ID=17410923
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26498293A Pending JPH07116479A (en) | 1993-10-22 | 1993-10-22 | Method for recovering phosphoric acid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07116479A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000050343A3 (en) * | 1999-02-23 | 2000-12-07 | Bio Con As | Treatment of solutions comprising metals, phosphorous and heavy metals obtained from dissolution of combusted waste materials in order to recover metals and phosphorous |
| US7030070B2 (en) | 2002-08-13 | 2006-04-18 | Takasago International Corporation | Composition for hard article surface cleaning liquid |
| KR101079069B1 (en) * | 2004-08-10 | 2011-11-02 | 가부시키가이샤 신꼬오 간쿄우 솔루션 | Method of treating wastewater and apparatus for treating wastewater |
| WO2025028268A1 (en) * | 2023-08-03 | 2025-02-06 | ラサ工業株式会社 | Etching liquid regeneration method |
-
1993
- 1993-10-22 JP JP26498293A patent/JPH07116479A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000050343A3 (en) * | 1999-02-23 | 2000-12-07 | Bio Con As | Treatment of solutions comprising metals, phosphorous and heavy metals obtained from dissolution of combusted waste materials in order to recover metals and phosphorous |
| US7030070B2 (en) | 2002-08-13 | 2006-04-18 | Takasago International Corporation | Composition for hard article surface cleaning liquid |
| KR101079069B1 (en) * | 2004-08-10 | 2011-11-02 | 가부시키가이샤 신꼬오 간쿄우 솔루션 | Method of treating wastewater and apparatus for treating wastewater |
| WO2025028268A1 (en) * | 2023-08-03 | 2025-02-06 | ラサ工業株式会社 | Etching liquid regeneration method |
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