JPS632810A - Method for recovering vanadium - Google Patents
Method for recovering vanadiumInfo
- Publication number
- JPS632810A JPS632810A JP61144792A JP14479286A JPS632810A JP S632810 A JPS632810 A JP S632810A JP 61144792 A JP61144792 A JP 61144792A JP 14479286 A JP14479286 A JP 14479286A JP S632810 A JPS632810 A JP S632810A
- Authority
- JP
- Japan
- Prior art keywords
- vanadium
- ammonium
- ammonium salt
- leachate
- mineral acid
- 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
- 229910052720 vanadium Inorganic materials 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims description 23
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 title claims description 19
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical class N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002253 acid Substances 0.000 claims abstract description 12
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 12
- 239000011707 mineral Substances 0.000 claims abstract description 12
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 11
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000002893 slag Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 4
- UPDATVKGFTVGQJ-UHFFFAOYSA-N sodium;azane Chemical compound N.[Na+] UPDATVKGFTVGQJ-UHFFFAOYSA-N 0.000 claims abstract 4
- 150000003863 ammonium salts Chemical class 0.000 claims description 15
- 239000011651 chromium Substances 0.000 claims description 11
- 238000011084 recovery Methods 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 3
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 3
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 3
- 238000010979 pH adjustment Methods 0.000 claims 3
- 239000010703 silicon Substances 0.000 claims 3
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 9
- 239000007858 starting material Substances 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract description 3
- 238000002386 leaching Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract 2
- -1 NH4Cl) Chemical class 0.000 abstract 1
- 238000013019 agitation Methods 0.000 abstract 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 abstract 1
- 229910003206 NH4VO3 Inorganic materials 0.000 description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 description 6
- 238000005185 salting out Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical class [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 125000004436 sodium atom Chemical group 0.000 description 1
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は硼素（Ｓｉ）、クロムＣＣｒ）及びバナジウ
ム（Ｖ）を多く含むスラグ、その他の産業副産物、廃棄
物の焙焼物質よりこれら元素を水で浸出させた３ｉ、Ｃ
ｒ及びＶを大量に含む浸出液より、ＶをＳｉ及びＣ「と
分離して回収する方法に関する。[Detailed Description of the Invention] [Industrial Application Field] The present invention is directed to the extraction of boron (Si), chromium (CCr), and vanadium (V) from slag, other industrial by-products, and roasted waste materials. 3i,C leached with water
This invention relates to a method for separating and recovering V from Si and C from a leachate containing a large amount of r and V.
従来バナジウム含有残滓をアルカリ焙焼抽出した浸出液
を脱シリカ、脱鉄処理し、硫酸アンモニアを大過剰に添
加し、鉱酸にてｐＨ５，２乃至５．４に調整し、８時間
攪拌して結晶化したナトリウムア単にＳ、Ａ、Ｖと云う
〕を結晶化して沈澱させる方法が特開昭６０−１６６２
２８号特許公開公報に如られている。Conventionally, the leachate obtained by roasting and extracting the vanadium-containing residue with alkali is desilicated and deironated, a large excess of ammonia sulfate is added, the pH is adjusted to 5.2 to 5.4 with mineral acid, and the mixture is stirred for 8 hours to form crystals. A method for crystallizing and precipitating the converted sodium atoms (simply referred to as S, A, and V) was disclosed in Japanese Patent Application Laid-Open No. 1662-1983.
It is mentioned in the Patent Publication No. 28.
またバナジン酸ソーダ溶液な鉱酸添加し、７５乃至９５
′ｃで脱シリカし、その後ｐＨ３，５乃至５．５に調整
し、塩化アンモニア（ＮＨ４Ｃｌ ）を添加し、田を４
．６乃至４．８に調整してＳ、Ａ、Ｖを回収する方法が
英国特許、１−１２６９６３９号明細書によって知られ
ている。In addition, a mineral acid such as a sodium vanadate solution is added, and 75 to 95
The pH was adjusted to 3.5 to 5.5, and ammonia chloride (NH4Cl) was added to the rice.
．． A method for recovering S, A, and V by adjusting the concentration between 6 and 4.8 is known from British Patent No. 1-1269639.
また−般的な方法として、前記浸出液を脱シリカし、鉱
酸にてｐＨ２，５乃至３．０ としてアンモニア水にて
ｐＨ８，０乃至８．５に調整後塩化アンモニアの添加に
よりメクバナジン酸アンモン（ＮＨ４ＶＯ３）を回収す
る方法が知られている。In addition, as a general method, the leachate is desilicated, adjusted to pH 2.5 to 3.0 with mineral acid and pH 8.0 to 8.5 with aqueous ammonia, and then ammonium mecvanadate is added by adding ammonium chloride. Methods for recovering NH4VO3) are known.
しかしながら、前述の何れの方法においても、■と他の
不純物との分離が充分でなく、回収したＶの純度が光分
なものが得られず、その品位に問題があった。However, in any of the above-mentioned methods, the separation of (1) and other impurities was insufficient, and the recovered V could not be of optical purity, resulting in a problem with its quality.
この発明ｆ！Ｓｉ、Ｃｒなどの不純物と共にＶを含む浸
出液より、ＶをＳ、Ａ、Ｖの形態で結晶として析出させ
ることによって、Ｓｉ、Ｃｒなとの不純物と効率よ（充
分に除去し、■の回収率の向上及びその品質の向上と回
収コストの低減をはかることを目的とする。This invention f! By precipitating V as crystals in the form of S, A, and V from the leachate containing V together with impurities such as Si and Cr, impurities such as Si and Cr can be removed efficiently (with a recovery rate of 1). The purpose is to improve the quality of the products and reduce the collection costs.
この発明はＳｉ、Ｃｒおよび■を含む焙焼物質乃至はこ
れら元素を含むスラグより浸出させた前記各元素を含む
浸出液にこれに俗存する■とのモル比でアンモニアとし
て１．０乃至２倍となるアンモニウム塩を添加し、この
アンモニウム塩添加と相前後して、鉱酸または／および
アルカリ水としてＮＨ４ＯＨ又はＮａＯＨを添加して、
ｐＨ５，０乃至６．０の範囲に保ち、最終的にｐＨ５，
０乃至５．２ に調整し、次に冷却攪拌してＳ、尤Ｖ
、を結晶として析出させ、これを残りの溶液と分離して
、Ｓｉ、ＣｒとＶを分離することを特徴とするバナジウ
ム回収方法とすることによって問題点を解決した。This invention provides a leachate containing the above-mentioned elements leached from a roasted material containing Si, Cr and Adding an ammonium salt of
Maintain the pH in the range of 5.0 to 6.0, and finally adjust the pH to 5.0 to 6.0.
Adjust to 0 to 5.2, then cool and stir to
The problem was solved by a vanadium recovery method characterized by precipitating , as crystals, and separating this from the rest of the solution to separate Si, Cr, and V.
また他の発明は、前記の方法により分離したＳ。Another invention provides S separated by the method described above.
ＡＮを再び温水に洛解させ、この溶液ｐＨを８．０乃至
９．ＯＫアンモニア水を加えて調整し、次に塩化アンモ
ニアまたは／および硫酸アンモニアを添加して、冷却攪
拌してＮＨ４ＶＯ３を結晶析出させて、これを回収する
ことを特徴とするＶ回収方法とすることＫよって問題点
を解決した。The AN was again dissolved in warm water and the pH of the solution was adjusted to 8.0-9. A V recovery method characterized by adding OK ammonia water for adjustment, then adding ammonia chloride or/and ammonia sulfate, cooling and stirring to precipitate crystals of NH4VO3, and recovering the same.K Therefore, the problem was solved.
今この発明を具体的に説明する。This invention will now be explained in detail.
この、ＩＦ１番目発明１の出発物質としては、Ｖ、Ｓｉ
、及びＣｒなどを含む浸出液を用〜・る。この浸出液と
しては石油煤煙或は高炉スラグより浸出させたもの若く
は産業廃棄物の焙焼物質より浸出させたものなどが含ま
れる。The starting materials of IF 1st invention 1 include V, Si
A leachate containing , Cr, etc. is used. This leachate includes those leached from petroleum soot or blast furnace slag, and those leached from roasted materials of industrial waste.
先ずこの浸出液に鉱酸として硫酸又は塩酸を添加して、
ｐＨ５，５乃至６．０に調整する。First, sulfuric acid or hydrochloric acid is added as a mineral acid to this leachate,
Adjust the pH to 5.5 to 6.0.
次にアンモニウム塩を浸出液に溶存するＶに対シ、モル
比でＮＨ４として１．０倍以上好ましくは、１．０乃至
２倍添加する。Next, ammonium salt is added to V dissolved in the leachate at a molar ratio of 1.0 times or more as NH4, preferably 1.0 to 2 times.
而して、前記アンモニウム塩添加中乃至添加後にアンモ
ニア水又は鉱酸を用いてｐＨ５，０乃至５．２調整する
。Then, during or after the addition of the ammonium salt, the pH is adjusted to 5.0 to 5.2 using aqueous ammonia or a mineral acid.
この液を冷却攪拌を約１時間継続し、Ｓ、尤Ｖを析出さ
せ、残余の液と適宜の固液分離法によって例えば篩別す
る。This liquid is cooled and stirred for about 1 hour to precipitate S and V, which are then separated from the remaining liquid by an appropriate solid-liquid separation method, for example, by sieving.
、ＮＨ２番目の発明としては、前記の才１番目の方法発
明を前処理とし、この前処理によって得られたＳ、Ａ、
Ｖを７０°乃至９０℃の温水に溶解する。この場合７０
′Ｃの条件にお〜・てＶ濃度に換算して４７Ｆ！／ｌま
で浴解する。, NH The second invention uses the first method invention as a pretreatment, and the S, A,
Dissolve V in warm water at 70° to 90°C. In this case 70
Converting to V concentration under the conditions of 'C ~ 47F! Dissolve in bath up to /l.
次にアンモニア水を前記Ｓ、Ａ、Ｖｉ液のｐＨを８．０
乃至９．０になるまで加える。Next, add ammonia water to the pH of the S, A, and Vi solutions to 8.0.
Add until it reaches 9.0 to 9.0.
而して、塩化アンモニアおよび／または硫酸アンモニア
を１０乃至１５ｙ／ノ添加し塩析し、更に冷却撹拌して
ＮＨ４ＶＯ３を析出させる。Then, 10 to 15 y/min of ammonia chloride and/or ammonia sulfate are added to effect salting out, and the mixture is further cooled and stirred to precipitate NH4VO3.
前記、１７１香目及び才２番目の発明に用いるアンモニ
ウム塩としては、塩化アンモニウム、硫酸アンモニウム
、硝酸アンモニウムのうちの一種又は混合物を用いる。The ammonium salt used in the 171st invention and the second invention is one or a mixture of ammonium chloride, ammonium sulfate, and ammonium nitrate.
Ｖｌｌｏ、１６％、５ｔｉ７．８％、Ｃｒｔ １．３６
％、Ｆｅｉ：３４．８７％、ＰｉＯ，０５％、ん’ｉ
１．１７％を含む鉱滓なソーダ塩４００ｆ／ｋｇを混合
し、酸化焙焼後４．０１／〜の水を加え浸出した浸出液
の組成は下記懺１に示す通りであった。Vllo, 16%, 5ti7.8%, Crt 1.36
%, Fei: 34.87%, PiO, 05%, n'i
The composition of the leachate obtained by mixing 400 f/kg of slag soda salt containing 1.17% and oxidizing roasting and adding 4.01/kg of water was as shown in Table 1 below.
表 １
この浸出液を出発物質として、４扉を用いこれに硫酸を
添加して、ｐＨ５，５とし、塩化アンモニウム１３６
Ｉｃｇ（ＮＨ４／Ｖ モｖ比”Ｃ” １．３ Ｋ相当）
ヲ添加する。Table 1 Using this leachate as a starting material, sulfuric acid was added to it using a 4-door to adjust the pH to 5.5, and ammonium chloride 136
Icg (NH4/V mov ratio "C" equivalent to 1.3 K)
Add wo.
塩化アンモニアの添加によりｐＨ３，９に低下するがア
ンモニア水を添加してｐＨ５，１とする。Addition of ammonia chloride lowers the pH to 3.9, but aqueous ammonia is added to bring the pH to 5.1.
その後約１時間冷却攪拌し、結晶析出したＳ。Thereafter, the S was cooled and stirred for about 1 hour to precipitate crystals.
Ａ、Ｖを２４４ｋｇ回収シタ、 コノＳ、Ａ、Ｖ （７
） ｍ成ｔ”！ 次の聚２に示す通りであった。この場
合のＶの収率は９７乃至９８％であった。Collected 244kg of A, V, Kono S, A, V (7
) m formation t"! It was as shown in the following 2. The yield of V in this case was 97 to 98%.
弐 ２
次に矛２発明の実施例としては前記の実施例により得ら
れたＳ、んＶ２４４ｋｇを温水２．５コに投入るまで添
加し、塩化アンモニアは１５ ｆｌ／ｌの割合で添加し
、ＮＨ４ＶＯ３を塩析する。2. Next, as an example of the second invention, 244 kg of S, N V obtained in the above example was added to 2.5 cups of hot water, and ammonia chloride was added at a rate of 15 fl/l. Salting out NH4VO3.
而して濾過及び少量の水で水洗し、ＮＨ４ＶＯ５を回収
する。得られたＮＨ４ＶＯ３の分析結果は以下の表３の
通りであった。Then, NH4VO5 is recovered by filtration and washing with a small amount of water. The analysis results of the obtained NH4VO3 were as shown in Table 3 below.
表 ３
このようにして得られた浸出液のＶの収率は９７％であ
った。Table 3 The yield of V in the leachate thus obtained was 97%.
実施例と同じ浸出敷を出発物質とし、これを７０℃に加
温し硫酸を添加し、ｐＨを２．５としてアンモニア水を
加えｐＨを８．５とした後、塩化アンモニウム５０ノ／
ｌの割合で添加し、ＮＨ４ＶＯ３を塩析し室温まで冷却
し、少量の水で水洗を行いｆ別し、得られたＮＨ４ＶＯ
５ｔの分析値は以下の表４に示す通りであった。Using the same leaching bed as in the example as a starting material, it was heated to 70°C, sulfuric acid was added, the pH was adjusted to 2.5, aqueous ammonia was added to adjust the pH to 8.5, and then ammonium chloride was added at 50°C.
NH4VO3 was salted out, cooled to room temperature, washed with a small amount of water and separated, and the obtained NH4VO
The analytical values for 5t were as shown in Table 4 below.
表 ４
このように、この比較例ではＳｉとＣｒの不純物が本件
発明の方法とは、オーダが一桁又は二桁多い。Table 4 As shown, in this comparative example, the Si and Cr impurities are one or two orders of magnitude higher than in the method of the present invention.
叙上のように第１番目の発明においては、簡単なｐＨの
調整を行い、特にアンモニウム塩添加時のｐ渣５．０乃
至６．０の範囲とし、最終的にｐＨ５，０乃至５．２と
して塩析させることになってＳ、Ａ、Ｖを結晶析出させ
ることができ、■と他の不純物の８１、Ｃｒなどとの分
離率が極めて高くなる。As mentioned above, in the first invention, the pH was simply adjusted, especially when the ammonium salt was added, so that the pH range was 5.0 to 6.0, and the final pH was 5.0 to 5.2. As a result, S, A, and V can be crystallized by salting out as a result of salting out, and the separation rate between ■ and other impurities such as 81 and Cr is extremely high.
前記塩析させるときのｐＨが５．２以上では、Ｓｉを溶
存する場合、＆Ａ、Ｖ析出後の上液中のＶ濃度が高＜ｐ
Ｈ５，５テ上記上ｉ中ノＶｙｊｋ度１．０８９ ／ ｌ
。When the pH at the time of salting out is 5.2 or higher, when Si is dissolved, the V concentration in the upper solution after &A and V precipitation is high < p
H5,5 te above i middle no Vyjk degree 1.089/l
.
ｐＨ６，０で■の濃度は２．Ｏｆ／７３で、それぞれｐ
Ｈ５，５トｐＨ６，０（１：） トきのｖの収率は９６
％及び９２％となり、■の回収率が低くなる。またｐＨ
６，０以上ｐＨ９，０までではＮＨ４ＶＯ３が沈澱し、
比較例に示したよ５ＫＣｒ及びＳｉの不純物が多量に混
入する。ま酸アンモン（レッドケーキ〕が析出し、純度
のよいＳ、Ａ、Ｖが得られなくなる。特にｐＨが２乃至
３のときは、レッドケーキが析出し、５ｉ０３”’−１
Ｃｒ０４２−と共沈し、不純物率が増大する。At pH 6.0, the concentration of ■ is 2. Of/73, each p
H5,5 pH6,0 (1:) Tokino v yield is 96
% and 92%, and the recovery rate of ■ becomes low. Also pH
At pH 6.0 to pH 9.0, NH4VO3 precipitates,
As shown in the comparative example, a large amount of 5KCr and Si impurities are mixed in. Ammonium chloride (red cake) precipitates, making it impossible to obtain S, A, and V with good purity.Especially when the pH is between 2 and 3, red cake precipitates and 5i03'''-1
Co-precipitates with Cr042-, increasing the impurity rate.
アンモニウム塩の添加は多い程バナジウムの回収率はよ
くなるが、コストの関係上、浸出液に溶存するバナジウ
ムとのモル比でアンモニアとして１乃至２倍で充分であ
る。The more ammonium salt is added, the better the recovery rate of vanadium will be, but for reasons of cost, a molar ratio of 1 to 2 times the amount of vanadium dissolved in the leachate as ammonia is sufficient.
矛２発明の発明の効果としては１，１−１番目の方法に
叙上の方法を加えた後処理を行うことによって、更Ｖｃ
ｖの回収率と他の不純物の分離効果を高め、高純度の■
が回収でき、■の収率は実施例においては９７％であっ
た。The effect of the invention of the second invention is that by performing post-processing by adding the above method to the method 1 and 1-1, it is possible to further improve Vc.
Enhance the recovery rate of v and the separation effect of other impurities, and achieve high purity.
could be recovered, and the yield of ■ was 97% in the example.
Claims (1)
これら元素を含むスラグより浸出させた前記各元素を含
む浸出液に、これに溶存するバナジウムとのモル比でア
ンモニアとして１．０倍以上好ましくは１．０乃至２倍
となるアンモニウム塩を添加し、 このアンモニウム塩添加と相前後して、鉱酸または／お
よびアルカリ水を添加して、ｐＨ５．０乃至６．０の範
囲に保ち、最終的にｐＨ５．０乃至５．２に調整し次に
冷却攪拌して、ナトリウムアンモニウムバナジン酸塩を
結晶として析出させ、これを残りの溶液と分離して硅素
及びクロムとバナジウムを分離することを特徴とするバ
ナジウム回収方法。 ２）前記ｐＨの調整方法はアンモニウム塩を浸出液に添
加前に鉱酸によりｐＨ５．５乃至６．０とし、次にアン
モニウム塩の添加後に鉱酸または／およびアンモニア水
によりｐＨ５．０乃至５．２に調整する方法であること
を特徴とする特許請求の範囲第１項記載のバナジウム回
収方法。 ３）前記ｐＨの調整方法はアンモニウム塩の添加と同時
的に行うことを特徴とする特許請求の範囲第１項記載の
バナジウム回収方法。 ４）前記アンモニウム塩としては、塩化アンモニウム硫
酸アンモニウム硝酸アンモニウムのうちの１種又は２種
以上の混合物であることを特徴とする特許請求の範囲第
１項記載のバナジウム回収方法。 ５）前記ｐＨ調整に用いる鉱酸としては塩酸又は硫酸で
あることを特徴とする特許請求の範囲第１項、第２項又
は第３項記載のバナジウム回収方法６）硅素、クロム及
びバナジウムを含む焙焼物質乃至これら元素を含むスラ
グより浸出させた前記各元素を含む浸出液に、これに溶
存するバナジウムとのモル比でアンモニアとして１．０
乃至２．０倍となるアンモニウム塩を添加し、このアン
モニウム塩添加と相前後して、鉱酸または／およびアン
モニア水を添加してｐＨ５．０乃至６．０の範囲に保ち
、最終的にｐＨ５．０乃至５．２に調整し、次に冷却攪
拌して、ナトリウムアンモニウムバナジン酸塩を結晶と
して析出させ、これを残りの溶液より分離し、次にこの
ナトリウムアンモニウムバナジン酸塩を再び温水に溶解
させ、この溶液ｐＨを８．０乃至９．０にアンモニア水
を加えて調整し、次にアンモニウム塩を添加して、冷却
攪拌してメタバナジン酸アンモンを結晶析出させて、こ
れを回収することを特徴とするバナジウム回収方法。 ７）前記アンモニウム塩としては塩化アンモニウム、硫
酸アンモニウム、硝酸アンモニウムのうちの一種又は２
種以上の混合物であることを特徴とする特許請求の範囲
第６項記載のバナジウム回収方法。[Scope of Claims] 1) A leachate containing each of the above elements leached from a roasted material containing silicon, chromium and vanadium or a slag containing these elements is added as ammonia in a molar ratio of 1 to the vanadium dissolved therein. .0 times or more, preferably 1.0 to 2 times the ammonium salt, and before and after this addition of the ammonium salt, mineral acid or/and alkaline water are added to adjust the pH to 5.0 to 6.0. Finally, the pH is adjusted to 5.0 to 5.2, and then cooled and stirred to precipitate sodium ammonium vanadate as crystals, which are separated from the rest of the solution to remove silicon, chromium, and vanadium. A vanadium recovery method characterized by separation. 2) The pH adjustment method is to adjust the pH to 5.5 to 6.0 with mineral acid before adding the ammonium salt to the leachate, and then adjust the pH to 5.0 to 5.2 with mineral acid or/and aqueous ammonia after adding the ammonium salt. 2. The method for recovering vanadium according to claim 1, which is a method for adjusting vanadium. 3) The vanadium recovery method according to claim 1, wherein the pH adjustment method is carried out simultaneously with the addition of ammonium salt. 4) The vanadium recovery method according to claim 1, wherein the ammonium salt is one or a mixture of two or more of ammonium chloride, ammonium sulfate, and ammonium nitrate. 5) The vanadium recovery method according to claim 1, 2 or 3, wherein the mineral acid used for pH adjustment is hydrochloric acid or sulfuric acid. 6) Contains silicon, chromium and vanadium. The leachate containing the above-mentioned elements leached from the roasted material or slag containing these elements has a molar ratio of 1.0 as ammonia to the vanadium dissolved therein.
Add ammonium salt to a concentration of 2.0 to 2.0 times, add mineral acid or/and aqueous ammonia to maintain the pH in the range of 5.0 to 6.0, and finally adjust the pH to 5. .0 to 5.2, then cooled and stirred to precipitate sodium ammonium vanadate as crystals, which were separated from the rest of the solution, and then this sodium ammonium vanadate was redissolved in warm water. The pH of this solution was adjusted to 8.0 to 9.0 by adding aqueous ammonia, and then an ammonium salt was added, and the mixture was cooled and stirred to precipitate ammonium metavanadate into crystals, which was recovered. Characteristic vanadium recovery method. 7) The ammonium salt is one or two of ammonium chloride, ammonium sulfate, and ammonium nitrate.
7. The method for recovering vanadium according to claim 6, which is a mixture of more than one species.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61144792A JPS632810A (en) | 1986-06-23 | 1986-06-23 | Method for recovering vanadium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61144792A JPS632810A (en) | 1986-06-23 | 1986-06-23 | Method for recovering vanadium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS632810A true JPS632810A (en) | 1988-01-07 |
Family
ID=15370560
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61144792A Pending JPS632810A (en) | 1986-06-23 | 1986-06-23 | Method for recovering vanadium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS632810A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103088207A (en) * | 2013-01-02 | 2013-05-08 | 河北钢铁股份有限公司承德分公司 | Efficient vanadium extraction method by performing alkali roasting on vanadium mineral |
| CN109207745A (en) * | 2017-07-07 | 2019-01-15 | 中国科学院过程工程研究所 | A method of it leaches from ammonium oxalate containing separation ammonium metavanadate in vanadium raw materials roasting clinker solution |
| CN112267028A (en) * | 2020-12-24 | 2021-01-26 | 矿冶科技集团有限公司 | Method for extracting vanadium and chromium from vanadium slag and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60166228A (en) * | 1984-01-25 | 1985-08-29 | ゲー・エフ・エー、ゲゼルシヤフト、フユール、エレクトロメタルルギー、ミツト、ベシユレンクテル、ハフツング | Manufacture of vanadium compound from vanadium-containing residue |
-
1986
- 1986-06-23 JP JP61144792A patent/JPS632810A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60166228A (en) * | 1984-01-25 | 1985-08-29 | ゲー・エフ・エー、ゲゼルシヤフト、フユール、エレクトロメタルルギー、ミツト、ベシユレンクテル、ハフツング | Manufacture of vanadium compound from vanadium-containing residue |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103088207A (en) * | 2013-01-02 | 2013-05-08 | 河北钢铁股份有限公司承德分公司 | Efficient vanadium extraction method by performing alkali roasting on vanadium mineral |
| CN103088207B (en) * | 2013-01-02 | 2015-02-25 | 河北钢铁股份有限公司承德分公司 | Efficient vanadium extraction method by performing alkali roasting on vanadium mineral |
| CN109207745A (en) * | 2017-07-07 | 2019-01-15 | 中国科学院过程工程研究所 | A method of it leaches from ammonium oxalate containing separation ammonium metavanadate in vanadium raw materials roasting clinker solution |
| CN112267028A (en) * | 2020-12-24 | 2021-01-26 | 矿冶科技集团有限公司 | Method for extracting vanadium and chromium from vanadium slag and application thereof |
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