JPH054338B2 - - Google Patents
Info
- Publication number
- JPH054338B2 JPH054338B2 JP62311061A JP31106187A JPH054338B2 JP H054338 B2 JPH054338 B2 JP H054338B2 JP 62311061 A JP62311061 A JP 62311061A JP 31106187 A JP31106187 A JP 31106187A JP H054338 B2 JPH054338 B2 JP H054338B2
- Authority
- JP
- Japan
- Prior art keywords
- aluminum
- acid
- aluminum sulfate
- hydrochloric acid
- crystals
- 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.)
- Expired - Fee Related
Links
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 42
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 28
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 26
- 239000013078 crystal Substances 0.000 claims description 26
- 229910052782 aluminium Inorganic materials 0.000 claims description 23
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 22
- 239000002699 waste material Substances 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 12
- 239000012452 mother liquor Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 239000000701 coagulant Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/74—Sulfates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Removal Of Specific Substances (AREA)
Description
産業上の利用分野
本発明は、アルミニウムまたはアルミニウム合
金を塩酸または塩酸と硫酸の混酸で表面処理をす
る際に発生するアルミニウムを含む廃塩酸の処理
方法に関するものであつて、アルミニウム分を硫
酸アルミニウムの結晶として回収し母液は調製後
に再使用することができる方法に関するものであ
る。
従来の技術
従来、アルミニウムコンデンサーを製造してい
る電解箔工業関係の工場より排出される含アルミ
ニウム廃塩酸または含アルミニウム廃混酸は、中
和処理または製紙工場等の凝沈剤として利用され
る程度であつた。
発明が解決しようとする問題点
中和処理ではアルカリが多量に消費されるので
処理費が高く、その上水酸化アルミニウムを主成
分とするスラツジが発生し、これの処理が問題と
なつていた。廃酸を製紙工場等の凝沈剤として用
いる方法では、アルミニウム含量がAlとして１
〜２％で極めて少なく、遊離酸が多いために使用
時のPH低下が問題となつている。
さらに使用者側の消費量と廃酸の排出量がバラ
ンスしないため、大きな貯槽が必要で、その費用
は莫大なものになる。
本発明者は、先に日本国特許735107号、782728
号、830454号、830482号でアルミニウムまたはア
ルミニウム合金を陽極酸化処理した時の含アルミ
ニウム硫酸溶液より硫酸アルミニウム結晶を晶析
させ、硫酸を回収し再使用する方法を提案した。
そしてこれらの方法を含アルミニウム廃塩酸に適
用すべく鋭意検討した結果、(1)塩化アルミニウム
よりも硫酸アルミニウムの方が結晶がつくりやす
いこと、(2)アルミニウムを含む廃塩酸に硫酸を添
加すると硫酸アルミニウム結晶が優先的に晶析で
きること、(3)硫酸アルミニウムの種晶を添加する
とより効果的であること、(4)硫酸アルミニウムの
結晶が析出する濃度まで濃縮すると塩酸が回収さ
れること、(5)回収酸は再利用できること、(6)回収
される硫酸アルミニウム結晶は凝集剤として使用
できることなどを知見した。
問題点を解決するための手段及びその作用
本発明はこれらの知見に基づくものであつて、
アルミニウムを含む廃塩酸に硫酸を添加して
SO4／Alのモル比が３／２〜９／２の割合になる
ように調製する第１工程と、第１工程で得られる
混酸溶液中の硫酸アルミニウムが過飽和溶液にな
るように50〜60℃の温度で調製する第２工程と、
硫酸アルミニウムの種晶を添加して第２工程で得
られる過飽和溶液から硫酸アルミニウム結晶を晶
析する第３工程と、第３工程で得られる硫酸アル
ミニウム結晶を母液と分離する第４工程との結合
からなることを特徴とする含アルミニウム廃塩酸
の処理方法である。
本発明におけるアルミニウムを含む廃塩酸は、
硫酸との混酸である場合もある。この場合第１工
程のモル比調整には硫酸無添加の場合もあり得
る。本発明において、硫酸根（SO4）とアルミニ
ウム（Al）のモル比の値を３／２以上としたの
は硫酸アルミニウムの硫酸根とアルミニウムのモ
ル比の値が３／２であり、これ以上ないと硫酸ア
ルミニウム結晶が得られないためである。また第
１表に硫酸アルミニウム結晶が得られる硫酸根と
アルミニウムのモル比の値との関係を示した。こ
の表から判るように、硫酸根とアルミニウムのモ
ル比の値
INDUSTRIAL APPLICATION FIELD The present invention relates to a method for treating waste hydrochloric acid containing aluminum generated when surface treating aluminum or aluminum alloy with hydrochloric acid or a mixed acid of hydrochloric acid and sulfuric acid. It relates to a method in which the crystals are recovered and the mother liquor can be reused after preparation. Conventional technology Conventionally, aluminum-containing waste hydrochloric acid or aluminum-containing waste mixed acid discharged from factories related to the electrolytic foil industry that manufactures aluminum capacitors has been used only for neutralization treatment or as a coagulant in paper mills, etc. It was hot. Problems to be Solved by the Invention In neutralization treatment, a large amount of alkali is consumed, so the treatment cost is high, and in addition, sludge containing aluminum hydroxide as a main component is generated, and the treatment of this has been a problem. In the method of using waste acid as a coagulant in paper mills, etc., the aluminum content is 1 as Al.
The amount is extremely low at ~2%, and because of the large amount of free acid, a drop in pH during use has become a problem. Furthermore, since there is no balance between the amount consumed by users and the amount of waste acid discharged, a large storage tank is required, and the cost becomes enormous. The present inventor previously obtained Japanese patent Nos. 735107 and 782728.
No. 830454 and No. 830482 proposed a method in which aluminum sulfate crystals are crystallized from an aluminum-containing sulfuric acid solution when aluminum or aluminum alloy is anodized, and the sulfuric acid is recovered and reused.
As a result of intensive studies to apply these methods to aluminum-containing waste hydrochloric acid, we found that (1) crystals form more easily in aluminum sulfate than in aluminum chloride; (2) when sulfuric acid is added to aluminum-containing waste hydrochloric acid, sulfuric acid (3) adding aluminum sulfate seed crystals is more effective; (4) hydrochloric acid is recovered when concentrated to a concentration at which aluminum sulfate crystals precipitate; We found that 5) the recovered acid can be reused, and (6) the recovered aluminum sulfate crystals can be used as a flocculant. Means for solving the problems and their effects The present invention is based on these findings,
Adding sulfuric acid to waste hydrochloric acid containing aluminum
The first step is to adjust the molar ratio of SO 4 /Al to a ratio of 3/2 to 9/2, and the first step is to adjust the molar ratio of SO 4 /Al to 50 to 60 so that the aluminum sulfate in the mixed acid solution obtained in the first step becomes a supersaturated solution. a second step of preparing at a temperature of °C;
Combining the third step of adding aluminum sulfate seed crystals to crystallize aluminum sulfate crystals from the supersaturated solution obtained in the second step, and the fourth step of separating the aluminum sulfate crystals obtained in the third step from the mother liquor. A method for treating aluminum-containing waste hydrochloric acid, characterized by comprising the following steps: The waste hydrochloric acid containing aluminum in the present invention is
Sometimes it is a mixed acid with sulfuric acid. In this case, sulfuric acid may not be added to adjust the molar ratio in the first step. In the present invention, the value of the molar ratio of sulfate radicals (SO 4 ) to aluminum (Al) is set to 3/2 or more because the value of the molar ratio of sulfate radicals of aluminum sulfate to aluminum is 3/2. This is because without it, aluminum sulfate crystals cannot be obtained. Furthermore, Table 1 shows the relationship between the molar ratio of sulfate radicals and aluminum from which aluminum sulfate crystals are obtained. As can be seen from this table, the value of the molar ratio of sulfate radicals and aluminum
【表】【table】
【表】
が９／２以下では硫酸アルミニウム結晶が得られ
るが、10／２以上では酸性塩の結晶となる。この
酸性塩の結晶は結晶性が悪く母液との分離が困難
となる。つぎに第２工程の混酸溶液を硫酸アルミ
ニウムの過飽和溶液に調製する方法は、減圧濃縮
法、蒸発濃縮法、冷却濃縮法などのいずれでもよ
い。
ここで硫酸アルミニウムの過飽和溶液の意味は
晶析温度に対して過飽和の意味で、その温度は60
℃以下好ましくは55℃以下である。60℃以上では
晶析する硫酸アルミニウムの濃度が高く、晶析速
度が速いためにのり状になりやすいからである。
第３工程の硫酸アルミニウムの晶析は、過飽和
溶液の温度を上げ下げして温度履歴を与えて行な
うこともできる。硫酸アルミニウムの種晶を５〜
30％添加して行なうことで、温度制御の煩わしさ
を解消することができる。
第４工程の結晶と母液の分離は通常の遠心分離
法などが用いられる。そして分離した母液は調整
後再使用できる。また本発明の廃塩酸、硫酸と塩
酸の廃塩酸には硝酸とリン酸が含まれていてもよ
い。
実施例
(1) アルミニウム箔を電解処理した廃塩酸
（Al15g／、Cl95g／）10に95％硫酸を
1.7Kg添加し、減圧濃縮してAlが51g／ｌ、
H2SO4が550g／ｌ、Cl60g／ｌの混酸溶液を３
得た。
この溶液を65℃より３℃／Hrの割合で冷却
し、60℃で150gの種晶を添加し、25℃まで冷
却した後に遠心分離機で硫酸アルミニウム結晶
を1.33Kg得た。この時の母液は2.45で、Alが
27.8g／ｌ、H2SO4が310g／ｌ、HClが72g／ｌ
であつた。
(2) Alが17.0g／ｌ、H2SO4が120g／ｌ、HClが
136g／ｌの廃塩酸10を減圧濃縮してAlが
51g／、H2SO4360g／、HCl70g／の混
酸溶液を3.3得た。これを60℃より３℃／Hr
の割合で冷却し、58℃で硫酸アルミニウム結晶
の種晶を150g添加し、25℃まで冷却した後に
遠心分離機で硫酸アルミニウム結晶を母液と分
離した。
硫酸アルミニウム結晶は1.3Kg、母液は2.8で
分析の結果硫酸アルミニウム結晶はAlが7.5％、
SO4が42.6％であつた。また母液はAlが27.8g／
ｌ、H2SO4300g／、HCl72g／であつた。
発明の効果
本発明によれば回収された廃酸は調整後に再使
用することができるし、有用な硫酸アルミニウム
の結晶が得られるので実用上の価値は大である。[Table] When the ratio is 9/2 or less, aluminum sulfate crystals are obtained, but when it is 10/2 or more, acid salt crystals are obtained. Crystals of this acid salt have poor crystallinity and are difficult to separate from the mother liquor. Next, the method for preparing the mixed acid solution in the second step into a supersaturated solution of aluminum sulfate may be any of a vacuum concentration method, an evaporation concentration method, a cooling concentration method, and the like. Here, a supersaturated solution of aluminum sulfate means supersaturated with respect to the crystallization temperature, and the temperature is 60
℃ or lower, preferably 55℃ or lower. This is because at temperatures above 60°C, the concentration of aluminum sulfate that crystallizes is high and the crystallization rate is fast, so that it tends to become glue-like. The crystallization of aluminum sulfate in the third step can also be carried out by raising and lowering the temperature of the supersaturated solution to give a temperature history. 5~5 seeds of aluminum sulfate
By adding 30%, the trouble of temperature control can be eliminated. For the separation of the crystals and the mother liquor in the fourth step, a conventional centrifugation method or the like is used. The separated mother liquor can then be reused after adjustment. Further, the waste hydrochloric acid of the present invention, the waste hydrochloric acid of sulfuric acid and hydrochloric acid, may contain nitric acid and phosphoric acid. Example (1) 95% sulfuric acid was added to waste hydrochloric acid (Al15g/, Cl95g/)10 obtained by electrolytically treating aluminum foil.
Added 1.7Kg and concentrated under reduced pressure to have Al of 51g/L.
A mixed acid solution containing 550 g/l of H 2 SO 4 and 60 g/l of Cl
Obtained. This solution was cooled from 65°C at a rate of 3°C/Hr, 150g of seed crystals were added at 60°C, and after cooling to 25°C, 1.33kg of aluminum sulfate crystals were obtained using a centrifuge. The mother liquor at this time was 2.45, and Al was
27.8g/l, H 2 SO 4 310g/l, HCl 72g/l
It was hot. (2) Al: 17.0g/l, H 2 SO 4 : 120g/l, HCl:
136g/l of waste hydrochloric acid 10 was concentrated under reduced pressure to remove Al.
3.3 mixed acid solutions of 51 g/, H 2 SO 4 360 g/, and HCl 70 g/ were obtained. 3℃/Hr from 60℃
150 g of aluminum sulfate crystal seed crystals were added at 58°C, and after cooling to 25°C, the aluminum sulfate crystals were separated from the mother liquor using a centrifuge. The aluminum sulfate crystal is 1.3 kg, the mother liquor is 2.8 kg, and the analysis results show that the aluminum sulfate crystal contains 7.5% Al.
SO4 was 42.6%. In addition, the mother liquor contains 27.8g/Al
1, H 2 SO 4 300g/, HCl 72g/. Effects of the Invention According to the present invention, recovered waste acid can be reused after adjustment, and useful aluminum sulfate crystals can be obtained, so the present invention has great practical value.
Claims (1)
てSO4／Alのモル比が３／２〜９／２の割合にな
るように調製する第１工程と、第１工程で得られ
る混酸溶液中の硫酸アルミニウムが過飽和溶液に
なるように50〜60℃の温度で調製する第２工程
と、硫酸アルミニウムの種晶を添加して第２工程
で得られる過飽和溶液から硫酸アルミニウム結晶
を晶析する第３工程と、第３工程で得られる硫酸
アルミニウム結晶を母液と分離する第４工程との
結合からなることを特徴とする含アルミニウム廃
塩酸の処理方法。 ２ アルミニウムを含む廃塩酸が硫酸との混酸で
あつて、これに硫酸を添加又は無添加で、SO4／
Alのモル比が３／２〜９／２の割合になるよう
に調製する上記第１工程を有することを特徴とす
る特許請求の範囲第１項記載の含アルミニウム廃
塩酸の処理方法。[Claims] 1. A first step of adding sulfuric acid to waste hydrochloric acid containing aluminum to adjust the molar ratio of SO 4 /Al to a ratio of 3/2 to 9/2; The second step is to prepare the aluminum sulfate in the mixed acid solution obtained in the step at a temperature of 50 to 60 °C so that it becomes a supersaturated solution, and the aluminum sulfate is prepared from the supersaturated solution obtained in the second step by adding seed crystals of aluminum sulfate. A method for treating aluminum-containing waste hydrochloric acid, comprising a third step of crystallizing crystals and a fourth step of separating aluminum sulfate crystals obtained in the third step from the mother liquor. 2 Waste hydrochloric acid containing aluminum is a mixed acid with sulfuric acid, and it is mixed with SO 4 / with or without sulfuric acid.
2. The method for treating aluminum-containing waste hydrochloric acid according to claim 1, which comprises the first step of preparing the molar ratio of Al to be from 3/2 to 9/2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62311061A JPH01153517A (en) | 1987-12-10 | 1987-12-10 | Method for treating aluminum-containing waste hydrochloric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62311061A JPH01153517A (en) | 1987-12-10 | 1987-12-10 | Method for treating aluminum-containing waste hydrochloric acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01153517A JPH01153517A (en) | 1989-06-15 |
| JPH054338B2 true JPH054338B2 (en) | 1993-01-19 |
Family
ID=18012642
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62311061A Granted JPH01153517A (en) | 1987-12-10 | 1987-12-10 | Method for treating aluminum-containing waste hydrochloric acid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01153517A (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE523966C2 (en) * | 2001-06-07 | 2004-06-08 | Feralco Ab | Process for the purification of a metal salt from inorganic impurities in an aqueous solution |
| JP2007279442A (en) * | 2006-04-07 | 2007-10-25 | Victor Co Of Japan Ltd | Polygon mirror, polygon mirror motor and disk driving motor |
| JP5160215B2 (en) * | 2007-12-27 | 2013-03-13 | 株式会社ユニックス | Method for treating sodium hydroxide waste solution of aluminum material |
| CN103111272B (en) * | 2013-03-07 | 2015-04-08 | 西北师范大学 | Preparation and application of modified polyaniline-palygorskite composite adsorbent |
| CN106927490B (en) * | 2017-04-06 | 2018-05-15 | 南通三圣石墨设备科技股份有限公司 | Aluminium salt and the method for waste acid recovery are extracted in a kind of acid solution from aluminium containing salt |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4868496A (en) * | 1971-12-22 | 1973-09-18 | ||
| JPS50131861A (en) * | 1974-04-09 | 1975-10-18 | ||
| JPS54157792A (en) * | 1978-06-01 | 1979-12-12 | Sumitomo Aluminium Smelting Co | Method of manufacturing aluminum sulfate from aluminum sludge containing soluble silicic acid |
| JPS62275018A (en) * | 1986-05-23 | 1987-11-30 | Kimura Kakoki Kk | Method for recovering valuable metal and acid from acidic waste liquor |
-
1987
- 1987-12-10 JP JP62311061A patent/JPH01153517A/en active Granted
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4868496A (en) * | 1971-12-22 | 1973-09-18 | ||
| JPS50131861A (en) * | 1974-04-09 | 1975-10-18 | ||
| JPS54157792A (en) * | 1978-06-01 | 1979-12-12 | Sumitomo Aluminium Smelting Co | Method of manufacturing aluminum sulfate from aluminum sludge containing soluble silicic acid |
| JPS62275018A (en) * | 1986-05-23 | 1987-11-30 | Kimura Kakoki Kk | Method for recovering valuable metal and acid from acidic waste liquor |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01153517A (en) | 1989-06-15 |
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