TW528732B - Improved methods for leaching of ores - Google Patents
Improved methods for leaching of ores Download PDFInfo
- Publication number
- TW528732B TW528732B TW089104164A TW89104164A TW528732B TW 528732 B TW528732 B TW 528732B TW 089104164 A TW089104164 A TW 089104164A TW 89104164 A TW89104164 A TW 89104164A TW 528732 B TW528732 B TW 528732B
- Authority
- TW
- Taiwan
- Prior art keywords
- scope
- patent application
- item
- alkali metal
- group
- Prior art date
Links
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
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
528732 A7 B7 五、發明說明(1 ) 描述 瀝濾礦石之改良方法 前後對照相關申請案 此申請案宣稱1999年2月19曰入檔之申請日期暫定之申請 案 USSN60/120,820 的益處。 發明背景 鈷(Co)、鎳(Ni)、鈦(Ti)、銅(Cu)、鉬(Mo)、鉛(pb)、 鋅(Ζη)、金(Au)和銀(Ag)的氧化物是重要的無機物。已存 在各種可用於自發現礦石處回收這些化合物的方法。例如 ,經常利用壓熱器方法回收C〇、Ni和Ti氧化物。這些方法 是高成本和費力的。過去曾以氫氣酸方法瀝濾出M〇氧化物 。氰化物、硫代硫酸鹽和_化物被用於瀝濾A u和Ag金屬 和氧化物。可以硫酸瀝濾出CU、Zn和Pb。 金紅石(Ti〇2)是一種可用於許多目的之無機物。在其他 用途中,其是一種鈦金屬和顏料色素的來源。人工金紅石 一般被視爲任何自其他無機物,通常爲具有至少9〇% 丁丨〇2 之鈦鐵礦所製成的金紅石。高純度金紅石是99 9%+ Τι〇2。2 高純度的金紅石一般是具有商業價値的。 鈥鐵礦(FeTi〇3)最常在壓妖芎中获气备 U备干猎虱軋鉍進行鬲溫瀝濾以 轉化成人工金紅石。瀝濾溫度一般是藉於8〇〇至9〇〇t之間 。氣化鐵有時被用於這些壓熱器的歷渡作用中以增加低溫 時的反應速率。 Z_eWin等人(Β· Mlshr_GJ Kip〇r〇us 編著在:献的 草取和加工,無機物、金屬&材料協會⑽7),p22_128 ---.--------裝--------訂--------- (請先閱讀背面之注意事項再填寫本頁) -4- 528732 A7 B7 五、發明說明(2 頁發表在m至刚。CT,置於4至6當量濃度之氫氯酸中 將可仗獲自Sichuan省瓷器之鈦鐵礦溶解鐵(以)他們發 現反應速率是相對於初Fe2+濃度狀4倍。他們主張一種且 有=.97仟焦耳/莫耳之表觀活化能的表面反應_模型。 f貝用的熱壓器技術是高成纟、高保養費和耗能量。 Jin等人所揭示的方法包括使用大量氫氯酸,其是昂 貝的不液操作而且需要特殊不鏽鋼裝置。明確需要可用 於避遽礦石以獲得有價値之無機物之較有效率的方法。 氰化物是最常用於瀝濾金的瀝濾劑。每分子金盥兩分子 孔化物錯合。銅也與氰化物錯合,但其每個銅分子取4個氨 =物分子。銅在銅金礦的存在量經常在1/1〇至1%範圍。 至在這些礦石中的含量爲!至1 〇 ^ PPttl範圍。銅消耗這麼多 汛化物,其必須以氰化氫蒸餾,一 π „ 征吓貝且危險的操作方 法回收《。過去已提出先以硫酸避遽出銅的系統狄厚中 和此堆積物或批次物。然後利用氰化物避濾出金。當炊, 問題是中和的費用。在多積物操作中 、 屮和的憂慮。 ”,另外存在者不完全 =他礦石中,脈石或不要的無機物可能是酸的消耗者 岛有石灰石之岩石中的氧化銅是一例。 ^ 主要發明關於自礦石中歷濾出有價値 、錄(Ni)、鈥(Ti)、銅(Cu)、相 J#(C〇) 、Wu)和銀(Ag)新穎和高效率^0)。、紹(Pb)、辞(叫 衣發明的一個特點是關於自確石中回收鈥的方法。一個 訂 rV Uf η Μ 4 厂; 4 合 IV 社 γ, m 鮮(CNS)A4 規格(210 X l)97 公至7 528732 _____一 A7 B7 五、發明說明(3 ) 主要方法的具體實例是利用一種酸性溶液如硫酸自無機進 料中瀝滤出欽氧化欽。額外的改良和/或步驟可被併入該方 法中’其包括5例如研磨礦石、驗金屬鹵化物的添加,破 源的添加以及壓力和/或溫度的調整。在一個較佳具體實例 中,讓無機進料與酸和鹼金屬卣化物接觸以自進料中瀝濾 出鈥的乳化物。商業價値優於人工金紅石之高純度二氧化 鈦可利用主要發明方法製得。 本發明的另一個特點是關於自礦石中回收異於鈦的過渡 金屬。在一個具體實例中,本發明提供一種以酸性溶液瀝 滤進料以自無機進料回收鎳和鈷的方法。在—個例示具體 實例中,可利用硫酸和鹼金屬函化物的混合物自紅土礦中 瀝濾、出鉛和鎳。藉自碎金屬瀝濾出這些元素,此主要方法 也可用於回收鈷、鎳、鈷等。 此主要發明也關於在不同溶液中回收多金 物之方法。在一個具體實例中,礦石與酸性溶酸 接觸。然後收集固體殘留物並與鹼金屬卣化物和酸性溶液 接觸。在一個例示具體實例中,可使用此主要方法分別自 金和銀回收銅。初步在第—種酸性溶液回收鋼,然而在鹼 金屬ii化物和酸性溶液中回收金和銀。 周片簡述 圖1顯示自鈦鐵礦瀝濾出鈦和鐵的動力學。 圖2顯示連續進行四次一小時自鈦鐵礦出鈦和鐵的結果。 圖3顯示自鈦鐵礦瀝濾出鈦和鐵上的礦泥密度關係了 圖4顯示評估鹼金屬自化物⑺化^對硫酸瀝濾程序之作用 以張K t :¾用中關家標準(CNS)A4祕公^ (請先閱讀背面之注意事項再填寫本頁) _·* |裝--------訂---------^9— 財產^Ju工消赀合作社印製 -6- A7528732 A7 B7 V. Description of the invention (1) Description of the improved method of leaching ore Cross-reference related applications This application claims the benefits of the tentative application USSN60 / 120,820 which was filed on February 19, 1999. BACKGROUND OF THE INVENTION The oxides of cobalt (Co), nickel (Ni), titanium (Ti), copper (Cu), molybdenum (Mo), lead (pb), zinc (Zη), gold (Au), and silver (Ag) are Important inorganics. Various methods exist for recovering these compounds from where they were found. For example, autoclave methods are often used to recover Co, Ni and Ti oxides. These methods are costly and laborious. Mo oxides have been leached out in the past by the hydrogen acid method. Cyanide, thiosulfate, and sulfide are used to leach Au and Ag metals and oxides. CU, Zn, and Pb can be leached from sulfuric acid. Rutile (Ti02) is an inorganic substance that can be used for many purposes. Among other uses, it is a source of titanium metal and pigments. Artificial rutile is generally considered to be any rutile made from other inorganic materials, usually ilmenite with at least 90% butadiene. High-purity rutile is 99 9% + T2. 2 High-purity rutile is generally commercially available. “Iron ore (FeTi03) is most commonly obtained in the press, and is prepared by rolling bismuth with dry lice and leaching at high temperature to convert it into artificial rutile. The leaching temperature is generally borrowed between 800 and 900 t. Vaporized iron is sometimes used in these autoclaves to increase the reaction rate at low temperatures. Z_eWin et al. (B. Mlshr_GJ Kip〇r〇us, edited in: Herbal Extraction and Processing, Inorganic Materials, Metals & Materials Association 7), p22_128 ----------------------- ---- Order --------- (Please read the notes on the back before filling this page) -4- 732732 A7 B7 V. Description of the invention (2 pages published on m to Gang. CT, placed in Among 4 to 6 equivalents of hydrochloric acid, ilmenite dissolved in porcelain from Sichuan province can be used to dissolve the iron (in order). They found that the reaction rate is 4 times higher than the initial Fe2 + concentration. They advocate one and have = .97 The surface reaction model of the apparent activation energy of Joules / Moore. The autoclave technology used in f is high performance, high maintenance costs and energy consumption. The method disclosed by Jin et al. Includes the use of a large amount of hydrochloric acid, which It is Ampere's liquid-free operation and requires special stainless steel devices. There is a clear need for a more efficient method that can be used to avoid tritium ore to obtain valuable tritium inorganics. Cyanide is the most commonly used leaching agent for leaching gold. Gold per molecule Two molecules of pores are mismatched. Copper is also mismatched with cyanide, but each of its copper molecules takes 4 ammonia molecules. The deposit of copper in copper-gold ore The amount is often in the range of 1/10 to 1%. To the content in these ore is! To the range of 1 ^ PPttl. Copper consumes so many flooding compounds, it must be distilled with hydrogen cyanide, a π „scare shellfish and Hazardous operation method of recycling. In the past, it has been proposed that the system should first neutralize this deposit or batch with sulfuric acid to avoid the scouring of copper. Then use cyanide to avoid filtering out gold. When cooking, the problem is the cost of neutralization. Concerns and concerns in the operation of multiple deposits. ", The inexistence of other persons = other ore, gangue or unwanted minerals may be acid consumer copper island in limestone rock is an example. ^ Main The invention relates to novel and high-efficiency filtration of valuable rhenium, Ni (Ti), Cu (Cu), phase J # (C0), Wu) and silver (Ag) from ores. , Shao (Pb), Ci (A feature of the invention is about the method of recycling from self-confirmed stone. A rV Uf η M 4 plant; 4 Co IV company γ, m fresh (CNS) A4 specification (210 X l) 97 to 7 528732 _____ a A7 B7 V. Description of the invention (3) A specific example of the main method is the use of an acidic solution such as sulfuric acid to leach out oxooxine from an inorganic feed. Additional improvements and / or steps May be incorporated into the process' which includes 5 such as the addition of ground ore, metal halide addition, source addition, and adjustment of pressure and / or temperature. In a preferred embodiment, the inorganic feed is mixed with acid and Alkali metal halide is contacted to leach out the emulsified product from the feed. High-purity titanium dioxide, which has a commercial price that is better than artificial rutile, can be prepared by the main inventive method. Another feature of the present invention is the recovery of foreign materials from ore. Transition metal to titanium. In one specific example, the present invention provides a method for leaching feed with an acidic solution to recover nickel and cobalt from an inorganic feed. In one specific example, sulfuric acid and an alkali metal function can be used Compound The mixture is leached from laterite ore to produce lead and nickel. By leaching these elements from crushed metals, this main method can also be used to recover cobalt, nickel, cobalt, etc. This main invention also relates to the recovery of multiple gold objects in different solutions. Method. In a specific example, the ore is contacted with an acid soluble acid. The solid residue is then collected and contacted with an alkali metal halide and an acidic solution. In an exemplary embodiment, this main method can be used to recover copper from gold and silver, respectively. The steel was initially recovered in the first acidic solution, but gold and silver were recovered in alkali metal compounds and acidic solutions. Brief description of the weekly sheet Figure 1 shows the kinetics of leaching titanium and iron from ilmenite. Figure 2 shows The results of titanium and iron extraction from ilmenite were carried out four times an hour in a row. Figure 3 shows the relationship between the density of slime on leaching titanium and iron from ilmenite. The function of the leaching procedure is based on Zhang K t: ¾ using Zhongguanjia Standard (CNS) A4 Secret ^ (Please read the precautions on the back before filling in this page) _ · * | Installation -------- Order --------- ^ 9— Property ^ Printed by Ju 工 消 赀 赀 -6- A 7
,:τ·ίθ.&1;τ4^;:3:_τ-消货>作?i印 K 五、發明說明(4 ) 的實驗結果。 圖5顯示評估研磨礦石對回 丄、a 叹逯率 < 作用的實驗結果。 圖6顯示在硫酸瀝濾程序渦如a 、 實驗結果。 …,評估添加碳源之作用的 圖7顯示評估驗金屬自化物對硫酸避遽程序之作用 結果,其中硫酸瀝濾程序係γλ 貝…驗 斤保攸原紅土進料(紅土 _丨)中 出鎳。 您遽 圖8顯示評估鹼金屬鹵化物料云 奶對硫鉍瀝濾程序之作用的實 結果,其中硫酸瀝濾程序係從 、% 代你紅土進枓(紅土 - 1 )中廢 出鈷。 也 圖9顯示評估驗金屬自化物對硫酸避遽程序之作用的實ρ 結果,其中硫酸瀝濾、程序係、從第二種紅土進料(紅土 : 瀝濾出鎳。 γ 圖10顯示評估驗金屬自化物對硫m程序之作用的命 驗結裝,其中硫酸瀝濾程序係從第二種紅土進枓(紅土 屮瀝濾出鈷。 〜 營明細節揭示 此王要發明提供新穎材料和用於自礦石中回收無機物的 万法:本王要發明之瀝濾方法的重要部份是使用酸性溶液 在一個具體實例中,該酸是硫酸。瀝濾程序中所用的硫 :¾浪度可在從約2 0克/公升至約5〇〇克/公升之範圍。在—個 R仕4V體贫例中,硫酸的濃度範園是從約丨5〇克/公升至約 25()乞’公升。硫酸濃度最好是近2〇〇克/公升。 在主要發明的瀝濾方法中,除了利用硫酸性溶液之外本 : meg準(CNS)A‘丨規格(21U X 297 公釐) f請先閱讀背面之注音?事項再填寫本頁} >裝------ —訂------ 528732 A7 ----—__B7 五、發明說明(5 ) 王要發明的特佳具體實例係利用附加因素,其包括,例如 驗金屬卣化物的使用、研磨礦石、碳源的添加和/或程序進 行溫度的調整。 根據本主要發明,瀝濾程序的效率可在處理前藉研磨礦 石改善之。在一個較佳具體實例中,研磨此礦石使其可通 過2〇0網目之篩子。 在另一個具體實例中,可將鹼金屬鹽加入瀝濾溶液中以 改善回收率。該鹼金屬鹽可爲,例如一種鹼金屬卣化物、 鹼金屬術、鹼金屬硝酸鹽、鹼金屬亞硫酸鹽或鹼金屬亞硫 碳酸。金屬卣化物可爲,例如Naa、KC1、NaBr或KBr或這 些卣化物之一種或多種的混合物。金屬亞硫酸鹽可爲,例 如亞硫鉍鈉、偏亞硫酸氫鈉、亞硫酸氫鈉、二亞硫碳酸鈉 或其他驗金屬或亞硫酸銨、偏亞硫酸氫鹽、亞硫酸氫鹽或 二亞硫碳酸。一般熟諳此技之技術人員接受在此所揭示之 指導可容易地判斷這些可與特定酸性溶液結合之鹼金屬鹽 ’其中此酸性溶液係用於該程序之溶解步骤中。 本主要發明之另一個具體實例包括使用碳源以改善回收 率:該碳源是,例如石墨或活性碳。此材料來源可爲,例 如取自椰子殼或木頭。 因此在一個具體實例中,本發明可提供一種自含鈦和鐵 的供機進料回收鈦氧化物之方法,該方法包括下列步驟·· (a)在鹼金屬自化物的存在下,以酸性溶液瀝濾進料可溶 解出鈥和鐵; (b )選擇性地沈澱鈦氧化物和 乂 A 丐+ 0 g家標準(CNS)A4規格(210 X 297公爱) • · * ----.—.-----•裝--------訂---------^9. (請先閱讀背面之注意事項再填寫本頁) 528732 Λ7 五、發明說明(6 (C )回收鈦氧化物。 一般,鈦氧化物可爲二氧化鈥。 含鈦的無機進料一般是後重無機濃度產物。該進料將包 括鈦礦化物。一般此鈦礦化物的實例是鈦鐵礦(以们〇3) ' leucoxene、鈣鈦礦(CaTiOd和鈦磁鐵礦。 在另-個具體實例中,該進料包含一巨大鈦鐵礦濃縮物 。欲將其他含鈥典機進料材料納入本發明範圍内。 在另一個不同的具體實例中,本發明提供一種自含有鈦 鐵礦(FeTi〇3)之無機進料中回收人工金紅石(丁丨〇2)的方法, 該方法包括下列步驟: (a)在鹼金屬函化物的存在下,以酸性溶液瀝濾鈦鐵礦可 溶解出鈦和鐵; (b )選擇性地沈;殿鈥氧化物和 (c )回收鈦氧化物如Ti〇2。 在此方法之步驟(a)中,該酸性溶液最好包括硫酸。瀝濾 步驟中所用的硫酸濃度一般在從約2 〇克/公升至約5〇〇克/公 升之範圍内。在一個較佳具體實例,硫酸濃度是在從約1 50 怎/公升至約250克/公升之範圍内。硫酸濃度最好是約2〇〇 乞/公升。其他欲用於本發明步驟(a)之酸類包括,但不限 於一種鹵酸如氫氯酸或氫溴酸。所用的鹵酸滚度一般是在 W約丨50克/公升至約3 50克/公升的範圍内。 步驟(a ) —般是在驗金屬鹵化物的存在下進行,其中驗金 % :¾ t物相對於進料中鈦鐵礦的比例範圍是從約丨:1至2 :1 鹼倉屬鹵化物的比例最好是從約1 :丨至1 s ^。此 9 - ΊΛ; f票準(CNS)A-l 規烙(210 X 297 公釐) ----.---.-----·裝---- (請先閱讀背面之注意事項再填寫本頁) 訂--- 者丨 Α7 五、發明說明(7 ) 比例最好是約i 2 · t · 。通合的鹼金屬#化物包括,俨不限 ΤΓ:ΓΚΒγ或這些㈣之-種㈣的混合物 中ί::法中:可將驗金屬㈣直接加入瀝遽溶液 ^ 运入瀝濾落液之前,讓鹼金屬函化物與進料 二:Α例中,讓此進料在驗金屬i化物的存在下進行 煮〉辰前處理(即藉煮濃至適當乾度),因此在瀝濾之前,: 進枓被驗金屬卣化物所塗佈。視情況而定,先前的合併物 ’即在瀝遽〈前直接將驗金屬自化物加人進料中並混 金屬南化物與進料,可用於本主要方法。因此,例如i行 步驟(a)之前,-部料金屬自化物與進料混合並將一部份 驗金屬卣化物直接加入該歷滤溶液中。一般而言,一旦開 始溶解,步驟(a)和(b)可同時或個別進行。特佳爲同時自 避遽殘留物移出部份含有豐富内容物之溶液使避遽殘留物 產生沈澱。依此方法,可防止沈澱物塗佈在瀝濾殘留物上 ’因爲此塗佈可能會降低程序的效率。,: τ · ίθ. &1; τ4 ^ ;: 3: _τ-Consumption > made as i K. V. Experimental results of invention description (4). Figure 5 shows the results of experiments to evaluate the effect of ground ore on the recovery rate and a sigh rate. Figure 6 shows the results of experiments such as a in the sulfuric acid leaching program. …, To evaluate the effect of adding a carbon source. Figure 7 shows the results of evaluating the effect of metal autochemicals on the sulfuric acid avoidance procedure. The sulfuric acid leaching procedure is γλ... nickel. Figure 8 shows the results of evaluating the effect of alkali metal halide milk cloud on the bismuth sulfide leaching process, in which the sulfuric acid leaching process wastes cobalt from the red clay feed (red clay-1). Fig. 9 also shows the actual results of the evaluation of the effect of the autogenous compounds on the sulfuric acid avoidance procedure, in which sulfuric acid leaching, the program system, and the feed from a second laterite (laterite: leaching out nickel.) Fig. 10 shows the evaluation test Determining the effect of metal autogenous compounds on the sulfur m program, in which the sulfuric acid leaching program is imported from the second type of laterite (the laterite is leached out of cobalt.) Yingming revealed the details of this invention to provide new materials and applications. Ways to recover inorganic matter from ore: An important part of the leaching method that the king wants to invent is to use an acidic solution. In a specific example, the acid is sulfuric acid. The sulfur used in the leaching process: In the range from about 20 g / L to about 500 g / L. In a case of R 4V body poverty, the concentration range of sulfuric acid is from about 50 g / L to about 25 g) Liter. The sulfuric acid concentration is preferably nearly 200 g / liter. In the leaching method of the main invention, in addition to the use of a sulfuric acid solution: meg standard (CNS) A '丨 specifications (21U X 297 mm) f Please read the Zhuyin on the back? Matters before filling out this page} > Install ------ —Order ------ 52 8732 A7 ----__ B7 V. Description of the invention (5) The specific example of Wang Yao's invention is the use of additional factors, including, for example, the use of metal test compounds, grinding ore, the addition of carbon sources and / or procedures The temperature is adjusted. According to the main invention, the efficiency of the leaching process can be improved by grinding the ore before processing. In a preferred embodiment, the ore is ground so that it can pass through a 200 mesh screen. In another In a specific example, an alkali metal salt may be added to the leaching solution to improve the recovery rate. The alkali metal salt may be, for example, an alkali metal halide, alkali metal, alkali metal nitrate, alkali metal sulfite, or alkali metal. Sulfuric acid. The metal halide may be, for example, Naa, KC1, NaBr, or KBr or a mixture of one or more of these halide. The metal sulfite may be, for example, sodium bismuth sulfite, sodium metabisulfite, sulfurous acid Sodium bicarbonate, sodium disulfite, or other metals or ammonium sulfite, metabisulfite, bisulfite, or dithionite. Those skilled in the art will accept the guidance disclosed here It is easy to judge these alkali metal salts that can be combined with a specific acidic solution, wherein the acidic solution is used in the dissolution step of the procedure. Another specific example of the main invention includes the use of a carbon source to improve the recovery rate: the carbon source is , Such as graphite or activated carbon. This material source can be, for example, from coconut shell or wood. Therefore, in a specific example, the present invention can provide a method for recovering titanium oxide from a machine feed containing titanium and iron, The method includes the following steps: (a) in the presence of an alkali metal compound, leaching the feed with an acidic solution to dissolve the iron and iron; (b) selectively precipitating titanium oxide and 乂 A + + 0 g Home Standard (CNS) A4 Specification (210 X 297 Public Love) • · * ----.—.----- • Equipment -------- Order --------- ^ 9. (Please read the notes on the back before filling out this page) 528732 Λ7 V. Description of the invention (6 (C) Recovery of titanium oxide. Generally, titanium oxide can be dioxide. Titanium-containing inorganic feeds are generally post heavy inorganic concentration products. The feed will include titanium mineralization. Examples of such ilmenite are generally ilmenite (Lecoxene), leucoxene, perovskite (CaTiOd and ilmenite. In another specific example, the feed contains a huge ilmenite concentrate It is intended to include other materials containing the machine into the scope of the present invention. In another different specific example, the present invention provides a method for recovering artificial rutile from an inorganic feed containing ilmenite (FeTi03) ( Ding 〇2) method, the method includes the following steps: (a) leaching ilmenite in an acidic solution in the presence of an alkali metal function to dissolve titanium and iron; (b) selectively sinking; “Oxide and (c) recover titanium oxide such as Ti02. In step (a) of this method, the acidic solution preferably includes sulfuric acid. The sulfuric acid concentration used in the leaching step is generally from about 20 g / Liters to a range of about 500 g / L. In a preferred embodiment, the sulfuric acid concentration is in the range of from about 150 g / L to about 250 g / L. The sulfuric acid concentration is preferably about 200. Beg / liter. Other acids to be used in step (a) of the present invention include, but are not limited to, a halogen Acids such as hydrochloric acid or hydrobromic acid. The halogen acid used generally has a roll in the range of about 50 g / liter to about 3 50 g / liter. Step (a) is generally performed on metal halides. The test is performed in the presence of gold, wherein the ratio of the gold test% to the ilmenite in the feed is from about 丨: 1 to 2: 1. The ratio of the alkali halide is preferably from about 1: 1 to 1 s ^. This 9-ΊΛ; f ticket standard (CNS) Al gauge (210 X 297 mm) ----.---.----- · install ---- (Please read the first Note: Please fill in this page again) Order --- A7 V. Description of the invention (7) The ratio is preferably about i 2 · t ·. Common alkali metal compounds include, without limitation ΤΓ: ΓΚΒγ or these ㈣ Zhi: In the mixture of ㈣: Method: You can directly add the metal test rhenium to the leaching solution ^ Before transporting the leaching liquid, let the alkali metal halide and feed two: In the case of A, let this feed Boil in the presence of the test metal compound> Pre-treatment (ie, by boiling to a proper dryness), so before leaching: Apply the test metal compound and, as the case may be, the previous The combination 'i.e. Adding the metallographic test compound to the feed and mixing the metal south compound and the feed can be used in this main method. Therefore, for example, before step (a) of line i,-the partial metal selfcide is mixed with the feed and The test metal halide is directly added to the calendar filtration solution. Generally, once dissolution begins, steps (a) and (b) can be performed simultaneously or individually. It is particularly preferred to remove the radon residue at the same time with rich content The solution of the substance causes precipitation of the sludge avoidance residue. In this way, the precipitation can be prevented from being coated on the leaching residue 'because this coating may reduce the efficiency of the process.
在一個具體實例中,沈澱步驟(b)可藉溫度和/或溶液pH 之調整而調節之。一般,步驟(昀是在從約8(rc至約]2〇χ 的溫度範圍下進行,較佳係在從約9 〇至約丨t vc的範圍下 進忭。在一個較佳具體實例中,步驟(a)的操作溫度是約 100X:。 在一個具體實例中,步骤(a)之瀝濾溶液的固體含量高達 約6 0重量%。瀝濾溶液的固體含量最好是從約1 〇 %至約 40% . 將該進料磨成細微粒子以幫助更快速地進行瀝濾。在一 -10 Η七H S家標準(CNS)A4規格(210 X 297公爱) * . 一 裝--------訂--------- (請先閱讀背面之注意事項再填寫本頁) 528732 A7 B7 -ιι 作 Η t*fj ί-· 五、發明說明(8 個較佳具體實例中,讓該進料進行精細研磨。研磨後,進 料中大部份的粒子最好可通過7 5微米篩子。 /見情況而定,在此主要方法中供應一種碳源。該碳源可 :任商業可取碳源之形態,其包括,例如活性態、煤、 焦炭、、木炭或石墨。較佳碳源爲獲自椰子殼的活=碳。碳 目對於進料(如鈦鐵礦)的比例一般介於約〇 〇1 : 1至1 : 1之 間0 根據本發明方法可在或高於—大氣壓下進行。使用高壓 、時,進行本發明方法之典型高壓和溫度是在從約丨巴至約 ^巴的範圍内。壓力最好是在從約!巴至約5巴的範圍内。 *王要方法中所用的溫度範園是從約100X:至約235Χ:。溫 k 圍最好是從約10(TC至約1 50X:。 ^驟U)所製得的避遽殘留物一步㉟行避遽以溶解 酸2分中未溶解的鐵和/或鈦。此進一步瀝濾可利用新鮮的 4 4名液來完成。在一個可替換的具體實例中,可使用遞 〜廢次或新鮮酸性溶液和瀝濾廢液之合併物。 0在=個具體實例中,該主要方法之㈣(a)可在亞鐵和 • 1冰^的存在下冗成以促進鐵礦化物的溶解。亞鐵離子 k存在於再循環程序工廠溶液中。 丨=想要,可利用標準技術如沈澱技術自瀝濾劑溶液中除 =,目的是自任何程序溶液中除去可溶性鐵。溶劑萃 ! ^人換、可逆滲透或其他技術也可用於除去可溶性鐵。 5 (例的瀝濾時間一般相當長,其範圍普遍在從约 上:、〕丨2〇小時内。瀝濾時間最好是從約6〇至約1〇〇小時。 (請先閱讀背面之注意事項再填寫本頁) * t _ 裝--------訂---------In a specific example, the precipitation step (b) can be adjusted by adjusting the temperature and / or the pH of the solution. In general, the step (进行) is performed at a temperature ranging from about 8 (rc to about) 2χ, preferably at a temperature ranging from about 90 to about vc. In a preferred embodiment, The operating temperature of step (a) is about 100X: In a specific example, the solids content of the leaching solution in step (a) is up to about 60% by weight. The solids content of the leaching solution is preferably from about 100%. % To about 40%. Grind the feed into fine particles to help leaching more quickly. In a -10 ΗHS home standard (CNS) A4 specification (210 X 297 public love) *. One pack- ------ Order --------- (Please read the notes on the back before filling this page) 528732 A7 B7 -ι Zuo t * fj ί- · V. Description of the invention (8 In a preferred embodiment, the feed is finely ground. After grinding, most of the particles in the feed can preferably pass through a 75 micron sieve. / As the case may be, a carbon source is supplied in this main method. Carbon source: Any commercially available form of carbon source, including, for example, active form, coal, coke, charcoal, or graphite. The preferred carbon source is living carbon obtained from coconut shell. Carbon The ratio to the feed (such as ilmenite) is generally between about 0.001: 1 to 1: 1. 0 The method according to the present invention can be carried out at or above-atmospheric pressure. When using high pressure, the method of the present invention is carried out. The typical high pressure and temperature are in the range from about 丨 bar to about ^ bar. The pressure is preferably in the range from about! Bar to about 5bar. * The temperature range used in Wang Yao's method is from about 100X : To about 235 × :. The temperature k range is preferably from about 10 (TC to about 150X: ^ step U). The avoidance residue prepared in one step avoids dissolution to dissolve undissolved iron in 2 points of acid. And / or titanium. This further leaching can be done with fresh 44 fluids. In an alternative specific example, a combination of waste or fresh acidic solution and leaching waste can be used. 0 在In a specific example, (a) of the main method can be redundant in the presence of ferrous iron and 1 ice ^ to promote the dissolution of iron minerals. Ferrous ions k are present in the recycling process plant solution. 丨= If desired, it can be removed from the leaching solution using standard techniques such as precipitation techniques = for the purpose of removal from any process solution Soluble iron. Solvent extraction! Human replacement, reversible osmosis, or other techniques can also be used to remove soluble iron. 5 (Leaching time is generally quite long, and its range is generally from about :,] to 20 hours. Leach The filtering time is preferably from about 60 to about 100 hours. (Please read the precautions on the back before filling in this page) * t _ equipment -------- order -------- -
11 - (CNS)A4 CMC χ 297 公釐) 528732 A7 B7 五、發明說明(9 ) 但是,此操作條件遠比慣用壓熱器技術溫和,故具有節省 大量資本和操作成本之優點。硫酸和鹼金屬自化物比上面 Zoumei Jin等人所提之程序中所用的氫氣酸易操作。 在另一個不同的具體實例中,本發明提供一種自含鈦和 鐵之無機進料回收鈥的方法,該方法包括下列步驟: (a )在驗金屬卣化物和活性碳來源的存在下,以酸性溶液 瀝濾進料溶解出鈇和鐵; (b )選擇性地沈澱鈦氧化物和 (c)自瀝濾殘留物中回收鈥氧化物。 在另一個不同的具體實例中,本發明提供一種自含鈦鐵 礦(FeTi〇3)之無機進料回收鈦的方法,該方法包括下列步 驟: / (a)在鹼金屬自化物和活性碳來源的存在下,藉酸性溶液 避遽鈥鐵礦以溶解出鈦鐵礦中的鈦和鐵; (b )選擇性地沈澱鈦氧化物和 (c )自避濾殘留物中回收鈦氧化物。 在另-個不同的具體實例中,本發明提供一種自含鈦鐵 礦(FeTi〇3)之無機進料回收鈦氧化物的方法,該方法包 T列步驟: '、匕 在從約\0至120乇的溫度範圍和鹼金屬_化物的存在 下,以Sa性落液瀝濾鈦鐵礦,其中瀝瀘溶液包冬高 約60重量%之固體以產生_種含有鐵和欽離;: 濾劑溶液: (b )自瀝濾劑溶液中的鈦分離出鐵:和11-(CNS) A4 CMC χ 297 mm) 528732 A7 B7 V. Description of the invention (9) However, this operating condition is much milder than the conventional autoclave technology, so it has the advantage of saving a lot of capital and operating costs. Sulfuric acid and alkali metal compounds are easier to handle than the hydrogen acids used in the procedure mentioned by Zoumei Jin et al. In another different embodiment, the present invention provides a method for recovering an inorganic feed containing titanium and iron, which method comprises the following steps: (a) in the presence of a metal halide and an activated carbon source, to The acid solution leaching feed dissolves rhenium and iron; (b) selectively precipitates titanium oxide and (c) recovers the oxide from the leaching residue. In another different specific example, the present invention provides a method for recovering titanium from an inorganic feed containing ilmenite (FeTi〇3), the method includes the following steps: (a) in an alkali metal autogenate and activated carbon In the presence of the source, the acid solution was used to avoid the iron ore to dissolve the titanium and iron in the ilmenite; (b) selectively precipitate titanium oxide and (c) recover the titanium oxide from the filtering residue. In another different specific example, the present invention provides a method for recovering titanium oxide from an inorganic feed containing ilmenite (FeTi〇3). The method includes steps T: Leaching ilmenite with Sa-like liquid in the temperature range to 120 ° F and the presence of alkali metal compounds, where the leach solution contains about 60% by weight of solids in winter to produce iron species and iron; Filter solution: (b) Separating iron from titanium in the leaching solution: and
^纸弘、< 用中ra 0家標準(CNS)A4規k (210 X^ Paper Hong, < Chinese Standard 0 (CNS) A4 Regulation (210 X
* I 麵 ------------裝--------訂--------- (請先閱讀背面之注意事項再填寫本頁) 528732 A7 B7 五、發明說明(10 ) (c)回收已分離的欽如Ti02。 如上所述’曾觀察到將鈥保留在溶液中遠比使其如殘留 物般沈澱更可進一步提高以純產物形式回收鈥的希望。大 部分鈦殘留之處,其他可在鈦鐵礦無機物如鉻鐵礦:石灰 、氧化鎂、氧化矽、錳、氧化鋁、釩、噚酸鹽和錐附近找 到的物質也可隨未溶解的鐵保留在殘留物中。此物質的存 在像要稀釋可自殘留物回收之鈦的純度。 視遞濾、溶液中的金屬含量而定,在此具體實例中,一般 步驟(a)的反應時間可高達約!小時。步驟(a)的反應時間^ 好高達約半小時。特佳爲反應時間是在從約5至約15分鐘 範圍内。在近此段反應時間中可見到鈦的溶解度達到高峰。 …視情況而定,可重複上述步驟(a)以溶解步驟(a)後所獲 计 < 殘留物中未瀝濾、0勺鈥’以獲得漸增至最大的鈇溶解度 。重複步驟U)時,可使用新鮮的酸性溶液和鹼金屬南化物 ,在—個具體實例中,步驟(a)可包括—個對流瀝濾環路。 …在此具體實例中,在一個或多個重複連續進行瀝濾的步 I中可以虱氣§'《補充鉍性落液以協助提高鈦溶解度的特性。 個不同的具體實例中,明提供一種自含鈦和 戏足無機進料回收鈦的方法,該方法包括下列步驟: )苁進料物貝與d敝落液或一種酸·鹼金屬画化物溶液 裕觸一段足以落化鈦但不足以使鈦沈澱之時間: (b )迸擇性地沈澱鈦氧化物:和 (c) W收鈦氧化物。 ⑽中所用的函酸可爲,例如氫氣酸或氫溴酸所用 (請先閱讀背面之注意事項再填寫本頁) I裝 訂i — 者· 13- 528732 Λ7 __B7 五、發明說明(11) 鹵酸之濃度範圍是從約150至約350克/公升酸。 可在連續瀝濾操作中回收任何此具體實例之瀝濾殘留物 中所沈澱的鈦。 在另一個不同的具體實例中,本發明提供_種自含有精 細研磨過的鈦鐵礦(FeTi〇3)之進料回收鈦的方法,該方法 包括下列步驟: (a) 在約100X:的溫度下和選自包含NaC1、Kci*k汾之鹼 金屬卣化物與活性碳來源的存在下,以包含硫酸之酸 性落液瀝濾鈦破礦高達約半小時以製造一種含有鐵和 鈦離子之瀝濾劑溶液,鹼金屬自化物相對於進料中之 欽鐵礦的比例是約1 . 2 : ;活性碳相對於進料中之 欽鐵礦的比例是約0·01 : 1,該瀝濾溶液的固體含量 係向達約6 0重量% ; (b) 重複步驟(&); (c )自避濾殘留物中分離出至少部份含有豐富内容物之溶 液: (d)自含有豐富内容物之溶液中選擇性地沈澱出鈦氧化物 : 和 (e )回收已分離的鈦氧化物如Ti〇2。 。在一個特佳的具體實例中,本發明提供自具有鐵和鈦之 蒸機進料歷濾鐵和鈦的多重階段方法,該方法包括下列步 .骤: (a )瓖進料物質與一種酸-鹼金屬函化物溶液接觸一段足 以溶化鈦但不足以使鈦沈澱之時間: -14 - 7*’票準(C\TS)A4 規格(210 X 297 公餐1 ''----- —.—*-----·裝-------丨訂·--------- (請先閱讀背面之注意事項再填寫本頁) 528732 ________ 五、發明說明(12 ) (b )自避濾水溶液中分離出泥漿; (c) 孩泥漿與新鮮的瀝濾水溶液接觸並重複步驟(&)和(b) 直到瀝濾出所有經濟上可行的鈦;和 (d) 在不同步驟中,藉沈澱、溶劑萃取或其他方式自該瀝 濾溶液中選擇性地回收鈦和鐵。 步骤(a)的條件可包含約】%至約6 〇 %之固體,以重量/重 量爲基準。一般固體百分比是在從約10%至40%範圍内。 了私居固體磨成細微粒子以背助遞;慮,一般可使該進料 通過7 3微米的篩子。最普遍使用的酸是疏酸。該酸的濃度 範圍是從約2 0至約300克/公升酸。最常使用的酸濃度範圍 是從約150至230克/公升。 孩鹼金屬齒化物可爲任何鹼金屬_化物。該鹼金屬鹵化 物最好是NaCl、κα、NaBr或KBr。鹼金屬_化物的濃度範 圍可從50克/公升至約400克/公升。鹼金屬鹵化物的濃度最 好是約100至約200克/公升: 以在約室溫下進行遞:;慮爲取普遍。在一大氣壓下,該溫 介於約4 0 °C和約1丨〇 C之間°避濾'溫度最好是介於約 g 0 C和約1 〇5°C之間。一大氣壓下所進行的瀝濾一般是在一 % ®濾容器中完成,該容器具有冷凝器以限制瀝滤溶液中 ;’γ凌生之自酸的損失。當鈦再度開始沈澱在瀝濾進枓物質 上之前,佬可能使其達到最高濃度。此濃度一般輕微高於4 1汰/公升溶液。完成此落斿的瀝遽時間將視各種前述參數 6〈,泣通常在從約1 〇分鐘至1小時之範圍内。 々:¾ (b)中分離固體-液體的方法可爲任何可在相當短的 -15- ___ ________ 〔.卜ΐ 糾(CXS)A-U、297 公望) ' ^ ' --------^---------^9. (請先閱讀背面之注意事項再填寫本頁) 528732 tif 4: Ϋ ii 社 f 口 ti Λ7 五、發明說明(13 ) 時間内自瀝濾水溶液完全分離出固體的方法。這些包括如 旋風器、過濾器、離心機、磁力分離器和澄清器等方法。 此名卓不欲排除任何未提及的方法。 在步驟(C )中新鮮瀝濾水溶液可自鈦含量已降低或減少的 瀝濾水溶液。應控制此水溶液的鐵含量使瀝濾期間無任何 鐵化合物發生沈澱。 可 可藉任何對特定工廠而言是最經濟的方法自步驟㈧丨之 濾水溶液中將鈦完全或部份去除。可使用的方法包括,作 不限於以放入晶種、pH調整、結晶、溶劑萃取和離子交= 使其沈澱。 在回收鈦之前或之後,可以相似方式於一步驟中回 。可在不同階段以不同產物形式回收鈦和鐵。可以鈦矂: 最普遍的是τω2形態回收鈥。鐵最普遍地是回收鐵鹽:二 化亞鐵或硫酸亞鐵形態的鐵。 a 氣 除了鈦和鐵瀝濾之外,本發明也關於自礦石、土壤、淳 縮物、礦渣或殘留物中回收其他無機物如鎳、鈷、鋼、= 、鉛、鋅、金或銀的方法。在一個具體實例中,提供—種 自含鎳、鈷和鐵之無機進料中溶解出鎳和鈷的方法,該方 法包括以酸性溶液瀝濾進料以溶解進料中的鎳、鈷和^万 在另-個具體實例中,可將驗金屬鹽加入㈣溶液以二善 回收率。鹼金屬鹽可爲,例如鹼金屬卣化物、鹼金屬亞 酸鹽、鹼金屬硝酸鹽、鹼金屬亞硫酸鹽或鹼金屬亞^碜酸 。該金屬i化物可爲,例如NaCl、κα、NaBi^KBr::S 或多種這些金屬ί化物的混合物。該金屬亞硫酸鹽可爲, 16- (請先閱讀背面之注音?事項再填寫本頁> * * |裝--------訂------ m F3 3 家標準(CKS)A4^f^(2i〇x~ 公釐) 528732 A7 五、發明說明(14 例如亞硫酸鈉、偏亞硫酸氫鈉、亞硫酸氫鈉、二亞硫碳酸 鈉或其他鹼金屬或銨的亞硫酸鹽、偏亞硫酸氫鹽、亞二^ 氫鹽或二亞硫碳酸。一般熟諳此技之技術人員接受在此所 揭示之指導可容易地判斷這些可與特定酸性溶液結合之^ 金屬鹽,其中此酸性溶液係用於該程序之溶解步驟;。在 個具體實例中,在以沈澱、溶劑萃取或其他方式萃取 金屬之前,本發明方法在或高於周溫下和在或高於一 壓下進行。 、又乱 ”有/、趣的金屬是鎳和姑之處,含鎳和録的無機進料一般 瑕後因粉碎和增稠產物而受益。一種典型鎳和鈷礦化物的 貧^是紅土礦。或者,該進料可能包含大量的紅土濃縮物。 一個本發明方法之具體實例提供自含有紅土之無機進料 ^回收線和姑的方法,該方法包括以既定沈澱、溶劑萃取 或其他万式萃取鎳和鈷之前,於不超過約15〇。(:的溫度和正* I side ------------ install -------- order --------- (Please read the precautions on the back before filling this page) 528732 A7 B7 V. Description of the invention (10) (c) Recovery of separated Chiron Ti02. As described above, 'it has been observed that the retention of "in solution is much more promising than the fact that it precipitates like a residue". Where most of the titanium remains, other substances found near ilmenite inorganics such as chromite: lime, magnesia, silica, manganese, alumina, vanadium, osmates and cones can also be found with undissolved iron Remain in residue. The presence of this substance is like the purity of titanium that can be recovered from the residue by diluting it. Depending on the filtration and metal content in the solution, in this specific example, the reaction time of the general step (a) can be as high as about! hour. The reaction time in step (a) is preferably up to about half an hour. Particularly preferably, the reaction time is in a range from about 5 to about 15 minutes. It can be seen that the solubility of titanium reaches a peak in this reaction time. … Depending on the situation, the above step (a) can be repeated to dissolve the residue obtained after the step (a) < unleached in the residue, 0 scoop 'to increase the solubility to a maximum. When step U) is repeated, a fresh acid solution and an alkali metal south compound may be used. In a specific example, step (a) may include a convection leaching loop. … In this specific example, lice may be leached in one or more of the steps of repeating the leaching step § '<supplemental bismuth drip to help improve the solubility of titanium. In different specific examples, a method for recovering titanium from an inorganic feed containing titanium and pedicure inorganic feedstock is provided. The method includes the following steps:) 苁 feed material and d 敝 liquid or an acid · alkali metal paint solution For a period of time sufficient to precipitate titanium but not enough to precipitate titanium: (b) Selectively precipitate titanium oxide: and (c) W to collect titanium oxide. The funic acid used in ⑽ can be, for example, used for hydrogen acid or hydrobromic acid (please read the precautions on the back before filling this page) I Binding i — 13 · 528732 Λ7 __B7 V. Description of the invention (11) Halic acid The concentration range is from about 150 to about 350 grams per liter of acid. The titanium precipitated from the leaching residue of any of this specific example can be recovered in a continuous leaching operation. In another different specific example, the present invention provides a method for recovering titanium from a feed containing finely ground ilmenite (FeTi〇3), the method comprising the following steps: (a) at about 100X: At a temperature and in the presence of an alkali metal halide selected from the group consisting of NaC1, Kci * k and fen, and activated carbon sources, the ore is leached with an acidic falling solution containing sulfuric acid for about half an hour to produce an iron and titanium ion-containing compound. Leachant solution, the ratio of alkali metal self-product to the iron ore in the feed is about 1.2:; the ratio of activated carbon to the iron ore in the feed is about 0.01: 1, the leaching The solids content of the filtration solution is up to about 60% by weight; (b) the steps are repeated (&); (c) the solution containing at least part of the rich content is separated from the filtering residue: (d) self-contained The titanium oxide is selectively precipitated from the rich solution: and (e) the separated titanium oxide such as Ti02 is recovered. . In a particularly preferred embodiment, the present invention provides a multi-stage process for filtering iron and titanium from a steamer with iron and titanium, the method comprising the following steps: (a) 瓖 feed material and an acid- Alkali metal halide solution contacted for a period of time sufficient to dissolve titanium but not enough to precipitate titanium: -14-7 * 'Ticket (C \ TS) A4 Specification (210 X 297 Meal 1' '----- —. — * ----- · Installation ------- 丨 Order · --------- (Please read the notes on the back before filling out this page) 528732 ________ V. Description of the invention (12) (b) separating the mud from the leaching solution; (c) contacting the mud with fresh leaching solution and repeating steps (&) and (b) until all economically viable titanium is leached; and (d) In different steps, titanium and iron are selectively recovered from the leaching solution by precipitation, solvent extraction, or other means. The conditions of step (a) may include about]% to about 60% solids at a weight / weight As a benchmark. Generally the percentage of solids is in the range from about 10% to 40%. Private solids are ground into fine particles for back-up delivery; considering that the feed can generally be passed through 7 3 micron Sieves. The most commonly used acid is sparse acid. The concentration of this acid ranges from about 20 to about 300 g / liter of acid. The most commonly used acid concentration ranges from about 150 to 230 g / liter of acid. The dentate can be any alkali metal halide. The alkali metal halide is preferably NaCl, κα, NaBr or KBr. The concentration of the alkali metal halide can range from 50 g / L to about 400 g / L. Alkali metal halide The concentration is preferably about 100 to about 200 grams per liter: to be transferred at about room temperature: it is considered to be generally accepted. At atmospheric pressure, the temperature is between about 40 ° C and about 1 ° C. The temperature of the “avoidance filter” is preferably between about g 0 C and about 105 ° C. The leaching at atmospheric pressure is generally performed in a% filter vessel, which has a condenser to Limit the leaching solution; 'γ Lingsheng's loss of self-acid. When titanium begins to precipitate again on the leached material, it may reach its highest concentration. This concentration is generally slightly higher than 4 1 T / L solution The completion time for this drop will depend on a variety of the aforementioned parameters 6 <, usually from about 10 minutes to 1 hour 々: ¾ (b) The method for separating solid-liquid can be any -15- ___________ [. Ϊ́ ΐ (CXS) AU, 297 public expectations) '^' ----- --- ^ --------- ^ 9. (Please read the notes on the back before filling out this page) 528732 tif 4: Ϋ ii 社 社 口 ti Λ7 V. Description of the invention (13) Method for completely separating solids by leaching the aqueous solution. These include methods such as cyclones, filters, centrifuges, magnetic separators and clarifiers. The name Zhuo does not want to exclude any methods not mentioned. The freshly leached aqueous solution in step (C) can be obtained from the leached aqueous solution whose titanium content has been reduced or reduced. The iron content of this aqueous solution should be controlled so that no iron compounds precipitate during leaching. Cocoa can completely or partially remove titanium from the filtered aqueous solution of step ㈧ by any method that is the most economical for a particular plant. Methods that can be used include, but are not limited to, seeding, pH adjustment, crystallization, solvent extraction, and ion exchange = precipitation. Before or after the titanium is recovered, it can be returned in a similar manner in one step. Titanium and iron can be recovered as different products at different stages. Can Titanium: The most common is τω2 morphological recovery. Iron is most commonly the recovered iron salt: iron in the form of ferrous dioxide or ferrous sulfate. In addition to titanium and iron leaching, the present invention also relates to a method for recovering other inorganic materials such as nickel, cobalt, steel, copper, lead, zinc, gold or silver from ore, soil, shrinkage, slag or residue. . In a specific example, a method is provided for dissolving nickel and cobalt from an inorganic feed containing nickel, cobalt, and iron, the method comprising leaching the feed with an acidic solution to dissolve the nickel, cobalt, and cobalt in the feed In another specific example, a metal test salt can be added to the rhenium solution to achieve a secondary recovery rate. The alkali metal salt may be, for example, an alkali metal halide, an alkali metal sulfite, an alkali metal nitrate, an alkali metal sulfite, or an alkali metal sulfite. The metal compound may be, for example, NaCl, κα, NaBi ^ KBr :: S, or a mixture of a plurality of these metal compounds. The metal sulfite can be, 16- (Please read the note on the back? Matters before filling out this page> * * | install -------- order ------ m F3 3 home standards ( CKS) A4 ^ f ^ (2i〇x ~ mm) 528732 A7 V. Description of the invention (14 For example, sodium sulfite, sodium metabisulfite, sodium bisulfite, sodium disulfite, or other alkali metal or ammonium sulfite Salts, metabisulfites, dihydrogen salts, or dithiocarbonates. Those skilled in the art can easily determine these metal salts that can be combined with specific acidic solutions by receiving the guidance disclosed herein, of which This acidic solution is used in the dissolution step of the procedure; in a specific example, the method of the present invention is at or above ambient temperature and at or above a pressure before the metal is precipitated, solvent-extracted, or otherwise extracted. It ’s messy. The interesting metal is nickel and its origins. Inorganic feeds containing nickel and nickel generally benefit from crushed and thickened products. A typical nickel and cobalt mineral is poor. Laterite. Alternatively, the feed may contain a large amount of laterite concentrate. A practical example of the method of the invention The example provides a method for recovering a line and an inorganic feed from a laterite-containing inorganic feed. The method includes not exceeding about 150 ° C (: temperature and positive temperature) before extracting nickel and cobalt with a predetermined precipitation, solvent extraction, or other methods.
常硬、T ,,在鹼金屬鹵化物的存在下以一種酸性溶液歷滤 、11 土以;容化紅土中的鎳和鈷及鐵的步驟c 、δ(性芯液最好包括疏酸。瀝濾步驟中所用的硫酸濃度 ^在從約2 0克/公升至約500克/公升範圍内。在一個較佳 …·」·只例中,硫酸的濃度在從約1 50克/公升至約250克/公 广園内。最好,硫酸的濃度在約2〇0克/公升。其他欲 1 1衣發明中之酸類包括_酸,例如氫氣酸或氫溴酸。所用 U J :11酸之澴度一般在從約5 0至約350克/公升酸的範圍内。 ,1, : · 、 〜’法一般是在鹼金屬鹵化物的存在下進行,其中鹼金 d化物相對於進料中紅土的比例範圍是從約0 05 : 1至約 -17- ΪΓΪ準(CNS)A4規格⑵0 X 297公釐) (請先閱讀背面之注意事項再填寫本頁} 裝--------訂------ S, 528732 A7 五、發明說明(15 ) 4 : 1。此比例最好是約〇」:】和最佳爲約〇 2 : ι。 在任何已描述的本發明具體實例中,其包括這些關於自 無機進料中瀝遽欽和非钦過渡金屬元素的方法,可直接將 驗金屬鹽加入瀝遽溶液中。或者,在導入歷遽溶液之前, 先使驗金屬鹽與進料合併。在此例中,讓進料在驗金屬鹽 的存在下進行—種煮濃的前處理(即煮濃至近乾),因此使 该進料表面在瀝濾之前已被鹼金屬鹽所塗佈。在另一個可 交替的具體實例中,可將鹼金屬鹽溶液噴在紅土礦堆上並 使其蒸發。另外可採用先前組合物。換言之,在溶化之前 先將一部份驗金屬鹽與進料ί昆合,再將—部份驗金屬鹽直 接加入瀝濾溶液中。特佳爲同時自瀝濾殘留物移出部份含 有丘3内谷物之溶液使鎳和鈷與瀝濾殘留物分離。 此方法一般是在從約8 0 至約12 0 X:的溫度範圍下進行。 該溫度最好在從約9(TC至約11〇。〇的範園内。一個典型可用 於本發明之操作溫度是約1 〇〇。0。 此主要方法之瀝濾、溶液的固體含量最好高達約6 0重量% 歷I洛液的固體含量最好是從約〗〇 %至約4 〇 % d 將該進料磨成細微粒子以幫助更快速地進行瀝濾。最好 ··’&孩進料進行精細研磨。進料中大部份的粒子最好可通過 7)微米篩子。一般,進料中至少75%粒子體積可使其通過 7 5微米篩子孔洞。 根據本發明方法可在或高於一大氣壓下進行。使用高壓 力時’可完成本發明方法之典型的高壓和溫度是在從約1巴 至約3 0巴範圍内。最好,壓力是在從約1巴至約5巴的範圍 -18- :·、义乂 :¾叩屮1¾ η家標準(CNSW規格(210 X 297 公釐) 裝--------訂--- (請先閱讀背面之注意事項再填寫本頁) 528732 Λ7 B7 五、發明說明(16 ) η 内和溫度範圍是從約10(TC至約235。(:。較佳係在從約ι〇〇χ 至約150°C的範圍内。在本發明具體實例中所描述的方法不 會與已知壓熱器技術相衝突,本發明包括鹼金屬齒化物與 硫酸合併使用,然而壓熱器技術則利用純酸或含氨溶液自 紅土進料礦石中瀝濾鎳和鈷。 本方法所製得的瀝濾殘留物可進—步進行瀝濾以溶解殘 留物中未溶解的鐵和/或鎳。此進—步瀝遽可利用新鮮的酸 性溶液來完成。在一個可替換的具體實例中,此方法中可 使用瀝遽廢液或新鮮酸性溶液和瀝遽廢液之合併物。 而且,此方法可在亞鐵和/或鐵離子的存在下完成以促進 鐵礦化物㈣解。離子一般存在於再循❹序工薇溶 液中。 視瀝濾溶液中的金屬含量而定,典型此具體實例之方法 所需反應時間可高達約M、時。該反應時間最好高達約 時特佳爲反應時間是在從約15分鐘至約3小時範圍内。 在近此段反應時間内,彳見到鎳和鉛的溶解度達到高峰。 7般熟諳此技者可變化避遽時間以避濾較少損害部份故和 4回收率4不想要的物種如廷或鐵。 αΓ重段上述万法以溶解殘留物中未經㈣的n姑,以 Γ讓增至最大的鎳和鈷溶解度。重複此方法時,可使用 行鮮的酸性溶液和驗金屬南化物。在—個具體實射,該 y法可包括一個對流瀝濾環路。 U㈣實例中’在-個或多個重複連續進行㈣的步 w h乂錢Μ无酸性溶液以協助提高鈦溶解度的特性。 -19- ΐ ❻準(CNS)A·丨規格(210、297 公餐)— (請先閱讀背面之注音?事項再填寫本頁) 一裝---- · n n ϋ 兮口 s, 528732 一Λ> A7 五、發明說明(17 ) 在另一個本發明具體實例中,可使用金 :一種水性泥裝或在與硫酸接觸之前,先將其,在= 質中並使其蒸發。 耳在進枓物 當與硫酸接觸時,讓所得泥浆遞滤一段短時 川分鐘),但最好約5分鐘或更短。錢 奸氏= :進行鉛的回收。此急速避遽方法係利用避據的;:;: 、鐵等。 履其中该洛液只包含少量的鎳、錳 =以金屬㈣和切之混合物避濾急速歷遽後之剩 余歹w物-段較長的時間以溶解錄和任何殘留的鉛。 在另-個具體實例中,可藉金屬商化物鹽類和硫酸之處 可^ 慮超^金屑和其他回收的金屬合金。金屬自化物鹽 ς 的濃度將視特定碎屑混合物而定。此具體實例可 彳用於選擇性地將特定金屬或所有金屬㈣人溶液中。此 具體實例也可用於自放射性碎片中溶解此類金屬如鎳的放 射性核甘。可將氧或其他氧化性氣體如氣加入㈣ 化該金屬。 “對於一些包含多價過渡金屬如高氧化態c〇和Μη物種之 供機物的氧化物礦石而言,鹼金屬由化物可被以硫爲基質 的還原化合物取代。例如,亞硫酸納、偏亞繞酸氣鈉、亞 极酸氫納、二亞硫碳酸鈉或其他鹼金屬或按的亞硫酸鹽、 ^亞嵘酸氫鹽、亞硫酸氫鹽或二亞硫碳酸可用於取代鹼金 免由化物。這些以硫爲基質的還原化合物將可幫助過渡金 免的還原,藉硫酸打開礦石以攻擊之。經濟上有興趣的金 20. < ’:.5⑴屮阀因家標準(CNS)A4規恪(210 X 297公釐) — — — — — — — —— — I — ·1111111 « — — — — — — I— (請先閱讀背面之注意事項再填寫本頁) 528732Normally hard, T, filtered in an acidic solution in the presence of an alkali metal halide, 11 soil; steps c, δ of accommodating nickel and cobalt and iron in laterite (the core solution preferably includes sparse acid. The concentration of sulfuric acid used in the leaching step is in the range of from about 20 g / L to about 500 g / L. In a preferred ... "" example, the concentration of sulfuric acid is from about 150 g / L to About 250 g / gongyuan. Preferably, the sulfuric acid concentration is about 2000 g / l. Other acids in the invention include acid, such as hydrogen acid or hydrobromic acid. UJ: 11 acid used The degree of alkalinity is generally in the range from about 50 to about 350 grams per liter of acid. The method is generally carried out in the presence of an alkali metal halide, wherein the alkali gold d compound is relative to the feed. The ratio of laterite ranges from about 0 05: 1 to about -17- ΪΓΪ 准 (CNS) A4 size⑵0 X 297 mm) (Please read the precautions on the back before filling out this page} Pack ------- -Order ------ S, 528732 A7 V. Description of the invention (15) 4: 1. This ratio is preferably about 0 ":] and most preferably about 02: ι. In any of the inventions that have been described specific In the example, it includes these methods on the transition metal elements of leaching and non-ching from the inorganic feed, and the metal test salt can be directly added to the leaching solution. Alternatively, the metal test salt can be made before introducing the rhenium solution. Combined with the feed. In this example, let the feed be performed in the presence of metal salts-a kind of pre-cooking (ie, boiled to near dry), so that the surface of the feed has been alkali metal before leaching Coated with salt. In another alternative embodiment, an alkali metal salt solution can be sprayed on the laterite ore heap and allowed to evaporate. Alternatively, the previous composition can be used. In other words, a portion of the solution is tested before dissolution. The metal salt is mixed with the feed, and then-part of the test metal salt is directly added to the leaching solution. It is particularly good to remove a part of the solution containing the grain in the hill 3 from the leaching residue at the same time, so that nickel and cobalt are leached. Separation of residues. This method is generally carried out at a temperature ranging from about 80 to about 120 ° C. The temperature is preferably in a range from about 9 ° C to about 11.0 °. A typical can be used in the present The operating temperature of the invention is about 100. 0. This main The leaching and solids content of the solution is preferably as high as about 60% by weight. The solids content of Lilo solution is preferably from about 0% to about 40%. D The feed is ground into fine particles to help more quickly. Leaching in place. It is best to finely grind the feed. Most of the particles in the feed are best passed through a 7) micron sieve. Generally, at least 75% of the particle volume in the feed can pass it through. 7 5 micron sieve holes. The method according to the invention can be carried out at or above atmospheric pressure. Typical pressures and temperatures that can be used to complete the method of the invention when using high pressures are in the range from about 1 bar to about 30 bar. Preferably, the pressure is in the range from about 1 bar to about 5 bar. -18-: ·, meaning: ¾ 叩 屮 1¾ η house standard (CNSW specification (210 X 297 mm) installed ------- -Order --- (Please read the notes on the back before filling out this page) 528732 Λ7 B7 V. Description of the invention (16) The temperature range of η is from about 10 (TC to about 235). (:. It is preferably in the range from about ιιχχ to about 150 ° C. The method described in the specific example of the present invention does not conflict with known autoclave technology, and the present invention includes alkali metal teeth Compounds are used in combination with sulfuric acid, but autoclave technology uses pure acid or ammonia-containing solutions to leaching nickel and cobalt from laterite feed ore. The leaching residue produced by this method can be further leached to dissolve Undissolved iron and / or nickel in the residue. This further step can be accomplished using fresh acidic solutions. In an alternative embodiment, the method can use leachate waste or fresh acidic solutions and Combination of leachate waste liquid. Furthermore, this method can be completed in the presence of ferrous and / or iron ions to promote the disintegration of iron minerals. The ions are generally present in the re-sequencing solution. Visual leaching solution Depending on the metal content in the reaction, the reaction time required for a typical method of this specific example can be as high as about M hours. The reaction time is preferably as high as about hours, and most preferably the reaction time is in the range from about 15 minutes to about 3 hours. In the near reaction time, see The solubility of nickel and lead has reached a peak. Generally, the skilled person can change the avoidance time to avoid less damage to the filter, and the recovery rate is 4 and the unwanted species such as tin or iron. The non-condensed n in the residue is increased to maximize the solubility of nickel and cobalt with Γ. When repeating this method, a fresh acid solution and a metal southern compound can be used. In a specific shot, the y method A convection leaching loop can be included. In the U㈣ example, one or more repetitive steps are performed in succession. The non-acidic solution helps to improve the solubility of titanium. -19- ΐ ❻ 准 (CNS) A · 丨 Specifications (210, 297 meals) — (Please read the phonetic on the back? Matters before filling out this page) One pack ---- · nn ϋ 口, 528732 Λ > A7 V. Description of the invention (17) In another specific embodiment of the present invention, gold can be used: an aqueous clay pack or before contacting with sulfuric acid, it is placed in a substance and allowed to evaporate. When the ear feed is in contact with sulfuric acid, let the obtained The mud is filtered for a short period of time), but preferably about 5 minutes or less. Money traitor =: Recycling of lead. This rapid avoidance method is based on avoidance;:;, iron, etc. This solution contains only a small amount of nickel and manganese = a mixture of metal and cuts to avoid filtration; the remaining residue after a rapid history; a long period of time to dissolve and remove any residual lead. In another specific example, metal ions and sulfuric acid can be used to take into account gold scrap and other recovered metal alloys. The concentration of the metal autoclave salt will depend on the specific debris mixture. This specific example can be used to selectively incorporate a specific metal or all metals into a solution. This specific example can also be used for radioactive ribosol dissolving such metals such as nickel from radioactive debris. Oxygen or other oxidizing gases, such as gas, can be added to the metal for hydration. "For some oxide ores containing multivalent transition metals such as the donors of the highly oxidized co and Mn species, the alkali metal ions can be replaced by sulfur-based reducing compounds. For example, sodium sulfite, Sodium sulfite, sodium bisulfite, sodium disulfite, or other alkali metals or sulfites, hydrogen sulfite, hydrogen sulfite, or disulfite carbonate can be used to replace alkali gold From sulfur compounds, these sulfur-based reducing compounds will help reduce the reduction of transitional gold, and open the ore by sulfuric acid to attack it. Economically interested gold 20. < ': .5 ⑴ 屮 Valve family standard (CNS) A4 (210 X 297 mm) — — — — — — — — — — — 1111111 «— — — — — — I— (Please read the notes on the back before filling out this page) 528732
A7 ________β7 五、發明說明(18 ) 屬不茜要疋已原的金屬。驗金屬靖酸鹽或亞确酸鹽可與 硫酸一起使用以瀝濾大部分金屬。這些技術可用於從硫化 物礦物或從碎屑、殘留物、礦渣、濃縮物或土壤中瀝濾出 金屬。 在另一個具體實例中,經少部份改良之利用金屬自化物 鹽類的方法可將硫酸用於目前存在的逆流傾析(CCD)環路 中。此種具體實例將利用新鮮進料物質以達到中和溶液至 足將鐵保留在溶液中之p Η。在完成液體-固體分離之後, 可在黏合劑的存在下進一步中和所得的瀝濾水溶液,使鐵 以氫氧化物形式沈澱。然後可部份乾燥鐵沈澱物並將其製 成圓球狀以製造生鐵進料儲備溶液。 液體-固體分離方法可爲任何可在相當短的時間内自瀝滹 水溶液中完全分離出固體的方法。這些包括如旋風器、過 濾器、離心機、磁力分離器和澄清器等方法。 藉對特定工廠而言是最經濟的方法可自避遽水溶液中將 坟或鈷完全或邵份去除。可使用的方法包括,但不限於以 故入晶種、pH調整、結晶、溶劑萃取和離子交換而使其沈 物的方法。具經濟價値之A機你 获錢物種經常與可消耗用於瀝 其之化學試劑的物種有關。有眭 %呼即使Ά耗物種疋具有經 馉位的,也會使整個瀝滹狻ώ 丁 ^、十, ^ 、 -又成不經濟的。此叙晋過的實A7 ________ β7 V. Description of the invention (18) It belongs to the original metal which does not need to be destroyed. Metallic acid salts or hypochlorites can be used with sulfuric acid to leach most metals. These techniques can be used to leach metals from sulfide minerals or from debris, residues, slag, concentrates, or soil. In another specific example, a slightly modified method using metal autologous salts can use sulfuric acid in a countercurrent decantation (CCD) loop that currently exists. This specific example will utilize fresh feed material to achieve a neutralization solution sufficient to retain iron in the solution. After the liquid-solid separation is completed, the resulting leached aqueous solution can be further neutralized in the presence of a binder to cause iron to precipitate as a hydroxide. The iron precipitate can then be partially dried and made into a sphere shape to make a pig iron feed stock solution. The liquid-solid separation method can be any method which can completely separate solids from the aqueous solution of bitumen in a relatively short time. These include methods such as cyclones, filters, centrifuges, magnetic separators and clarifiers. The most economical method for a particular plant is to remove graves or cobalt completely or shame from the tritium solution. Methods that can be used include, but are not limited to, seeding by precipitation, pH adjustment, crystallization, solvent extraction, and ion exchange. Economically priced A machines are often associated with species that can consume chemicals used to drain them. It is said that even if the consumption of species has a position in the economy, it will make the entire market 、, ,, ^,--uneconomical. This reality
tv A Κ列實例將説明實施本發明 之程序。這些實例不構成限 528732 A7 B7 IU 4 五、發明說明(19 ) 制。除非另外指示,否則所有百分比是以重量爲基準而且 所有溶劑混合物比例是以體積爲基準。 i例1 -自鈦鐵礦瀝濾出鈦和鐵 自鈦鐵礦瀝濾出鈦和鐵的動力實驗顯示兩者先被瀝濾出 ’然後鈦沈澱並減緩鐵的瀝濾速度。以100克被磨成_2〇〇網 目的鈦鐵礦進行實驗。以1000克濃度爲200克/公升(克/公升 )之硫酸和120克/公升NaCl溶液進行這些試驗。加入1〇〇克 活性碳並將溶液加熱至1 〇〇°C。在9 6小時的瀝濾過程中監測 F e和T i的濃度。結果表示於圖1中。該結果表示出一種τ i 先被避濾至水溶液中,接著氫氧化,然後沈澱的機制。當 此機制發生時’其減緩瀝濾、鐵的速度。在1小時内出現被避 濾出來的T i。 在一個不同但相似的實驗中,1〇〇克之鈦鐵礦量在l〇crc 下於1公升由200克/公升ΗΑ〇4·120克/公升鹼金屬鹵化物所 形成的溶液中避濾、7 2小時,其中鈥鐵礦的主要分析含量爲 34.0% Fe和27.0% Ti而且其粒徑可使全部粒子都通過一個 75微米的篩子。100克之活性碳量也存在於此瀝濾溶液中。 定期監測此瀝濾水溶液中的T i和F e含量。實驗結果則表示 於表1中。鈥被溶解接著可見到其沈殿。最後分析5 7.4克 殘留物顯示其只包含0.67% Fe和46.6% Ti。因此98.9%的 錢已被萃取至落液中’而9 9.7 %的鈥仍保留在殘留物中。該 實驗指示由於T i的初溶解度,因此τ i和F e兩者可藉重複短 期;歷,慮作用從欽鐵礦中理想地被萃取出。 .—-—.-----狀衣--------訂·--------. (請先閱讀背面之注意事項再填寫本頁) -二、 ϋ· 社 22 t :¾丨丨]小3 Η家標準(CNS)Al規恪(210 X 297公餐) A7The TV AK example will illustrate the procedure for implementing the present invention. These examples do not constitute a limitation. 528732 A7 B7 IU 4 V. Description of Invention (19). Unless otherwise indicated, all percentages are by weight and all solvent mixture ratios are by volume. Example 1-Leaching of titanium and iron from ilmenite Dynamic experiments of leaching titanium and iron from ilmenite show that both are leached first 'and then titanium precipitates and slows down the leaching rate of iron. The experiment was performed with 100 g of ilmenite that was ground to 200 mesh. These tests were performed with 1000 g of 200 g / L (g / L) sulfuric acid and 120 g / L of NaCl solution. 100 g of activated carbon was added and the solution was heated to 100 ° C. The concentrations of F e and T i were monitored during a 96-hour leaching process. The results are shown in Fig. 1. The results show a mechanism in which τ i is first filtered into an aqueous solution, then oxidized, and then precipitated. When this mechanism occurs' it slows down the rate of leaching, iron. The filtered T i appeared within 1 hour. In a different but similar experiment, 100 grams of ilmenite was filtered under 10 crc in 1 liter of a solution of 200 g / liter of ΗΑ04.120 g / liter of alkali metal halide, For 72 hours, the main analytical content of iron ore is 34.0% Fe and 27.0% Ti and its particle size allows all particles to pass through a 75 micron sieve. An amount of 100 grams of activated carbon is also present in the leaching solution. The T i and Fe content in this leaching solution are monitored regularly. The experimental results are shown in Table 1. “It was dissolved and then you can see its Shen Dian. A final analysis of 5 7.4 g of residue showed that it contained only 0.67% Fe and 46.6% Ti. So 98.9% of the money has been extracted into the liquid 'while 99.7%' remains in the residue. This experiment indicates that due to the initial solubility of T i, both τ i and F e can be repeated for a short period of time; calendar effects are ideally extracted from the iron ore. .—-—.----- Zhang Yi -------- Order · --------. (Please read the notes on the back before filling this page)-二 、 ϋ · 社22 t: ¾ 丨 丨] Small 3 Family Standard (CNS) Al Regulations (210 X 297 Meals) A7
528732 五、發明說明(2Q ) 表1 自鈦鐵礦丨 __— 時間 毫克/公升 體積 克 ^^一 累積 _1 克 ______ 累積 小時 公升 萃取 Fe Ti L·--- 1 5600 3720 0.720 _ 4.03 1 1 Q OAO ——--- ο 9. 2 5650 3700 0.720 _4.07 ΔΌ〇 ---- 1 Λ 0 4 5950 3810 0.720 _ 4.28 Ί 1 1 ZOO — 1 Λ A 6 6010 3880 0.720 4 --1^,1 2/4 1 IAS-- 1 π 0 一―12 6220 3830 0.720 4.48 -LoA 1 /1 A 2/9 —"V 一 1 n q _ 24 16900 1410 0.720 」2·17 卜 1 W Ζ /〇 1 ΠΟ ι u.y.—一 A S _^8_ 35000 212 0.720 25.20 -—^/. 1 7A N 1 .Uz Π 1 ς --- 1 1 _72__ 38200 121 0.720 27.50 -/ v) J / QA Λ U. 1 J Α Α〇 1 ------ i 1 37600 90 0.720 27.07 一 ^4丨4 QO Q U.UV π Α/ΐ 1 〇 液 1 5000 20 1.000 5.00 14 7 vJ. UC) 〇 09 ι · ---- 〇 1__ 375 1 0.990 0.37 — 1 兮 /_ _1.1 yJ. \JJL 0.00 _ " 1 __^ 自欽鐵礦連% 1小時避滤出欽和鐵 利用實例1的數據以發展一種新的鈦鐵礦瀝濾程序:該柱 Y d括瀝濾鈦鐵礦約1小時或更短時間,然後使其與新鲜瀝 怎液接觸。在此方法中,鐵和鈦一起被瀝濾出來。以利 ⑴朽9 6 -小時試驗中相同的條件測試之。四次連續一小時在 ⑴同的確石樣品中瀝濾的結果表示於圖2中。如所見,在备 ’近等量的鐵和欽被瀝濾、出。一般熟諳此技之技術 欠U接殳在此所描述之指導可決定適當的試劑濃度、溫度 •23- 3 Υίΐ準TCNSMI uiO X公¥)— —*—,-----裝--------訂---------. (請先閱讀背面之注意事頊再填寫本頁) 528732 A7 B7 ιΑ*、 * Μ 4 4 w ϋ 丄 y\ ii lL ffJ i.j 步驟2 步骤3 步骤4 步骤5 五、發明說明(21 、礦石粒徑,不論是否包括碳和其形態(如活性碳或石墨) 或適合特定礦石之大氣壓力(一般<3大氣壓)。藉短瀝濾時 間以Τι〇2形態分離T i,接著沈澱Ti〇2的技術也可適用於其 他瀝濾系統如氫氣酸瀝濾系統。 下面兩實驗進一步説明以多階段方式自鈦鐵礦中瀝濾出 鈥和鐵的方法: 實驗A包括將裝有一種60克鹼金屬鹵化物、i〇〇*h2S〇4 和350克HA所形成的瀝濾溶液的錐形瓶在攪拌加熱板上加 熱至100°C,並將5 〇克減至7 5微米粒徑的鈦鐵礦加入其中 以獲得9 %泥漿密度。 實驗B包括將裝有一種6〇克鹼金屬鹵化物、1〇〇克h2s〇4 和3 50克所形成的瀝濾溶液的錐形瓶在攪拌加熱板上加 熱至1 00°C,並將1 〇〇克_ 7 5微米粒徑的鈦鐵礦加入其中以獲 得丨6 %泥装密度。 該鈥鐵礦的主要分析含量爲3 〇 %鈦和3 4 %鐵。 將下列程序步驟分別應用在實驗A和實驗B中: 步驟1 將冷凝器放在裝有前述溶液和鈦鐵礦進料之泥漿 的錐形瓶上: 以磁石攪拌器激烈攪拌該泥漿約3 〇分鐘並將溫 度保持在100°C : 將該錐形瓶和内容物在室溫水槽中冷卻幾分鐘; 將錐形瓶溶液傾倒入離心管中並在4,〇〇〇 rpm下離 心5分鐘; 將離心管中的水溶液倒入樣品瓶中並與固體分離 24- ---.---Κ-----裝·-------訂·-------- (請先閱讀背面之注意事項再填寫本頁) 528732 A7 B7 五、發明說明(22 ) ,測量體積和重量並保留之以進一步測試包括分 析使用; 步驟6 种量離心管中剩餘固體重,然後以5 10克新鮮瀝: 濾溶液清洗之並將其倒回步驟4後錐形瓶中剩餘 殘留物裏;528732 V. Description of the invention (2Q) Table 1 From Ilmenite 丨 __— time mg / litre volume g ^^ one accumulation_1 g ______ Cumulative hour liter extraction Fe Ti L · --- 1 5600 3720 0.720 _ 4.03 1 1 Q OAO ——--- ο 9. 2 5650 3700 0.720 _4.07 ΔΌ〇 ---- 1 Λ 0 4 5950 3810 0.720 _ 4.28 Ί 1 1 ZOO — 1 Λ A 6 6010 3880 0.720 4 --1 ^, 1 2/4 1 IAS-- 1 π 0-12 6220 3830 0.720 4.48 -LoA 1/1 A 2/9 — " V-1 nq _ 24 16900 1410 0.720 `` 2 · 17 bu 1 W ZZ / 〇1 ΠΟ ι uy—One AS _ ^ 8_ 35000 212 0.720 25.20 --- ^ /. 1 7A N 1 .Uz Π 1 ς --- 1 1 _72__ 38200 121 0.720 27.50-/ v) J / QA Λ U. 1 J Α Α〇1 ------ i 1 37600 90 0.720 27.07 1 ^ 4 丨 4 QO Q U.UV π Α / ΐ 1 〇Liquid 1 5000 20 1.000 5.00 14 7 vJ. UC) 〇09 ι ·- --- 〇1__ 375 1 0.990 0.37 — 1 Xi / _ _1.1 yJ. \ JJL 0.00 _ " 1 __ ^ Since the Qin iron ore company% 1 hour to avoid filtering out the data of Qin He iron use case 1 to develop a New Ilmenite Leaching Procedure: The column Y d includes leaching ilmenite for about 1 hour or less Between, then allowed to drain how the fresh liquid contact. In this method, iron and titanium are leached together. Eli was tested under the same conditions in the 9 6-hour test. The results of leaching from different samples of Quercus for four consecutive hours for one hour are shown in Figure 2. As you can see, nearly equal amounts of iron and Chin in the preparation were leached and extracted. The techniques generally familiar with this technique are not sufficient. The instructions described here can determine the appropriate reagent concentration and temperature. 23- 3 Υ ΐquasi-TCNSMI uiO X public ¥) — — * —, ----- install --- ----- Order ---------. (Please read the notes on the back before filling this page) 528732 A7 B7 ιΑ *, * Μ 4 4 w ϋ 丄 y \ ii l ffJ ij steps 2 Step 3 Step 4 Step 5 V. Description of the invention (21, ore particle size, whether or not including carbon and its form (such as activated carbon or graphite) or atmospheric pressure suitable for a specific ore (generally < 3 atmospheres). By short drain The technology of separating T i in the form of T2, followed by precipitation Ti02 can also be applied to other leaching systems such as hydrogen acid leaching system. The following two experiments further illustrate the leaching from ilmenite in a multi-stage manner. Â € ¢ Method of iron: Experiment A consisted of heating an Erlenmeyer flask containing a leaching solution of 60 g of an alkali metal halide, 100 × h2S04 and 350 g of HA on a stirring hot plate to 100 ° C, and 50 grams of ilmenite reduced to 75 micron particle size was added to obtain 9% mud density. Experiment B consisted of loading 60 grams of The conical flask of the leaching solution formed by the alkali metal halide, 100 g of h2s04 and 3 50 g was heated to 100 ° C on a stirring hot plate, and the particle size of 1000 g-7 5 microns Ilmenite was added to obtain 6% mud density. The main analytical contents of this iron ore are 30% titanium and 34% iron. The following procedure steps were applied in Experiment A and Experiment B, respectively: Step 1 Place the condenser on a conical flask containing the aforementioned solution and the slurry of the ilmenite feed: Vigorously stir the slurry with a magnetic stirrer for about 30 minutes and keep the temperature at 100 ° C: Place the conical flask and The contents were cooled in a room temperature water tank for several minutes; the conical flask solution was poured into a centrifuge tube and centrifuged at 4,000 rpm for 5 minutes; the aqueous solution in the centrifuge tube was poured into a sample bottle and separated from the solids 24 ----.--- Κ ----- installation ------- order --------- (Please read the precautions on the back before filling out this page) 528732 A7 B7 5 2. Description of the invention (22), measuring the volume and weight and retaining it for further testing including analysis and use; Step 6: The amount of solids remaining in the centrifuge tube is measured, and then fresh with 5 10 g : The washing solution was filtered and poured back to step 4 after the remaining residue in an Erlenmeyer flask;
步驟7 攪拌重新組成的泥漿並將泥漿溫度升高至100°C 女% 8 重複步驟1至步驟7在内以繼續進行此程序,其 總共7次,因此等於總瀝濾時間爲4小時: 步驟9 每次重複步驟5所收集的離心後水溶液個別微採 樣並分析其欽和鐵含量; …展0進行计算以測定固體和水溶液中的鈥和鐵含量並 比較其個別鈥鐵礦礦石進料的元素分析値: V 1 1將步驟9進行微採樣之後,個別剩餘的水溶液合 ^ 併於燒瓶中並微採樣和分析其鈦和鐵含量: 丨2可藉對任何特定工廠而言是最經濟的方法自瀝遽 水溶液中將鈦完全或部份去除。可使用的方法包 括’但不限於藉放入晶種、p H調整、結晶、溶 ^ 釗萃取和離子交換使其沈澱。 R驗結果表示於表2和圖3中。對 ' ^ ^ 4 ^ ' 對1兩種固體百分比而言 、丈、.々寺ϊ的鈦在各步驟中被萃取出來。 11 ;_____,-----^-------I -------- (請先閱讀背面之注意事項再填寫本頁) _ 11 (CNS)Al (:>ι〇 x :>97 528732 A7 B7 五、發明說明(23 ) ί? /、 作 社 印 表2自鈦鐵礦瀝濾出鈦和鐵之泥漿密度關係 9%固體,< 以重量/1 t量爲基準 克/公升 Fe Ti 歷滤 時間 Fe Ti 體積 克 累積 克 累積 小時 公升 萃取 萃取 1 0.5 6.32 3.96 0.400 2.53 14.8% 1.58 10.6 2 0.5 3.97 3.32 0.423 1.68 24.7 1.40 19.9 3 0.5 3.14 2.88 0.412 1.29 32.3 1.19 27.8 4 0.5 2.15 2.18 0.410 0.88 37.4 0.89 33.8 5 0.5 1.77 1.85 0.415 0.73 41.7 0.77 38.9 6 0.5 1.71 1.81 0.412 0.70 45.9 0.75 43.9 7 0.5 1.50 1.75 0.412 0.62 49.5 0.72 48.7 8 0.5 1.34 1.61 0.417 0.56 52.8 0.67 53.2 9 0.5 1.44 1.69 0.410 0.59 56.2 0.69 57.8 10 0.5 1.06 1.28 0.415 0.44 58.8 0.53 61.3 11 0.5 0.90 1.18 0.409 0.37 61.0 0.48 64.5 清洗液1 0.00 0.00 0.390 0.00 61.0 0.00 64.6 12 0.5 1.03 1.040 0.403 0.42 63.4 0.42 67.3 13 0.5 0.91 0.960 0.415 0.38 65.6 0.40 70.0 14 0.5 0.86 0.93 0.410 0.35 67.7 0.38 72.5 15 0.5 0.85 0.89 0.412 0.35 69.8 0.37 75.0 16 0.5 0.77 0.75 0.420 0.32 71.7 0.32 77.1 17 0.5 0.63 0.64 0.415 0.26 73.2 0.27 78.9 18 0.5 0.65 71.0% 0.402 0.26 74.7 0.29 80.8 -26- (請先閱讀背面之注意事項再填寫本頁) .:S 中円ΡΓ幻票準(CNS)A4規格(210 X 1)97公釐) 528732 A7 _B7 五、發明說明(24 ) 19 0.5 0.58 0.65 0.415 0.24 76.1 0.27 82.6 20 0.5 0.52 0.6 0.412 0.21 77.4 0.25 84.2 21 0.5 0.53 0.58 0.415 0.22 78.7 0.24 85.8 22 0.5 0.48 0.53 0.417 0.20 79.9 0.22 87.3 23 0.5 0.41 0.48 0.413 0.17 80.8 0.20 88.6 清洗液2 0.002 0.0024 0.540 0.00 80.9 0.00 88.6 24 0.5 0.37 0.43 0.410 0.15 81.7 0.18 89.8 清洗液3 0.0023 0.0019 0.590 0.00 81.7 0.00 89.8 16%固體, 以重量/重量爲基準 克/公升 Fe Ti 遞:〉慮 時間 Fe Ti 體積 克 累積 克 累積 小時 公升 萃取 萃取 0.25 7.07 4.00 0.010 0.07 0.2 0.04 0.1 1 0.50 8.16 4.52 0.380 3.10 9.3 1.72 5.9 0.25 4.77 4.63 0.010 0.05 9.4 0.05 6.0 2 0.50 5.78 5.44 0.402 2.32 16.3 2.19 1 j. J j 0.50 4.74 4.54 0.418 1.98 22.1 1.90 19.6 4 0.50 4.16 4.13 0.419 1.74 27.2 1.73 25.4 ί 1 丨 5 0.50 3.62 3.63 0.418 1.51 31.6 1.52 30.5 6 0.50 3.30 3.27 0.425 1.40 35.7 1.39 35.1 :义洗液1 0.05 0.04 0.511 0.03 35.8 0.02 35.2 7 0.50 2.54 2.65 0.408 1.04 38.8 1.08 38.8 S 0.50 2.08 2.41 0.417 0.87 41.4 1.00 42.1 ,:/Γ洗液2 0.50 0.08 0.09 0.450 0.04 41.5 0.04 42.3 (請先閱讀背面之注意事項再填寫本頁) -27-;i:漯準(CNSM.丨規济(21() X 297公坌) 528732 A7 五、發明說明(25 -驗金屬鹵化物的影& 、進订評估驗金屬卣化物對根據主要發明方法利用硫酸自 礦石中回收鐵之影響的實驗。該結果表示於圖4中。在此例 中,所用的鹽是濃度爲〇 〇/〇、5 0/〇、j 5 %和2 5 % (重量/重量) 之NaCl。這些試驗是利用濃度爲2〇〇克/公升的硫酸溶液, 在100 C和無活化碳的存在下,於未經研磨的礦石上完成。 鹽的添加加速反應速率。但是,大約15至2〇%鹽(15〇至2〇〇 克/公升)NaC1變成反生產的。實際所瀝濾出鐵的總百分比 自達到1 5% NaCl後下降。 在一個不同但相似的實驗以進一步説明鹼金屬鹵化物對 自鈦鐵礦中瀝濾出鐵的影響中,1〇〇克鈦鐵礦進料樣品在 1 〇〇 C F以200克硫酸、700克水和不同鹼金屬鹵化物量瀝濾 “】時邊驗金屬鹵化物的量是0、50、150和250克,其 代表〇、5、】5和2 5 %(重量/重量)鹼金屬鹵化物溶液。可 說察到鐵的瀝濾速率。該結果表示於表3中。Step 7 Stir the reconstituted mud and raise the mud temperature to 100 ° C Female% 8 Repeat steps 1 to 7 to continue this process, which totals 7 times, so it equals a total leaching time of 4 hours: Step 9 Repeat the micro-samples of the centrifuged aqueous solution collected in step 5 each time and analyze the content of iron and iron; Calculate the calculation to determine the “and iron content in the solid and aqueous solution and compare the individual” iron ore feed Elemental analysis 値: V 1 1 After micro-sampling in step 9, individual remaining aqueous solutions are combined in a flask and micro-sampling and analysis of its titanium and iron content: 丨 2 can be the most economical for any specific plant Method Titanium is completely or partially removed from the aqueous solution of bitumen. Useful methods include, but are not limited to, precipitation by seeding, pH adjustment, crystallization, solvent extraction, and ion exchange. The R test results are shown in Table 2 and Figure 3. For '^ ^ 4 ^' For 1 two solid percentages, titanium, 丈, 々 temple ϊ titanium was extracted in each step. 11 _____, ----- ^ ------- I -------- (Please read the precautions on the back before filling this page) _ 11 (CNS) Al (: > ι 〇x: > 97 528732 A7 B7 V. Description of the invention (23) ί / / Printed by Sakusha 2 Leaching from the ilmenite The density relationship between titanium and iron is 9% solids, < by weight / 1 t The amount is based on grams per liter of Fe Ti. Filtration time Fe Ti Volume grams Cumulative grams Cumulative hours Liter Extraction and extraction 1 0.5 6.32 3.96 0.400 2.53 14.8% 1.58 10.6 2 0.5 3.97 3.32 0.423 1.68 24.7 1.40 19.9 3 0.5 3.14 2.88 0.412 1.29 32.3 1.19 27.8 4 0.5 2.15 2.18 0.410 0.88 37.4 0.89 33.8 5 0.5 1.77 1.85 0.415 0.73 41.7 0.77 38.9 6 0.5 1.71 1.81 0.412 0.70 45.9 0.75 43.9 7 0.5 1.50 1.75 0.412 0.62 49.5 0.72 48.7 8 0.5 1.34 1.61 0.417 0.56 52.8 0.67 53.2 9 0.5 1.44 1.69 0.410 0.59 56.2 0.69 57.8 10 0.5 1.06 1.28 0.415 0.44 58.8 0.53 61.3 11 0.5 0.90 1.18 0.409 0.37 61.0 0.48 64.5 Cleaning solution 1 0.00 0.00 0.390 0.00 61.0 0.00 64.6 12 0.5 1.03 1.040 0.403 0.42 63.4 0.42 67.3 13 0.5 0.91 0.960 0.415 0.38 65.6 0.40 7 0.0 14 0.5 0.86 0.93 0.410 0.35 67.7 0.38 72.5 15 0.5 0.85 0.89 0.412 0.35 69.8 0.37 75.0 16 0.5 0.77 0.75 0.420 0.32 71.7 0.32 77.1 17 0.5 0.63 0.64 0.415 0.26 73.2 0.27 78.9 18 0.5 0.65 71.0% 0.402 0.26 74.7 0.29 80.8 -26- (Please read the notes on the back before filling this page).: S in 円 ΡΓ magic ticket standard (CNS) A4 specification (210 X 1) 97 mm) 528732 A7 _B7 V. Description of the invention (24) 19 0.5 0.58 0.65 0.415 0.24 76.1 0.27 82.6 20 0.5 0.52 0.6 0.412 0.21 77.4 0.25 84.2 21 0.5 0.53 0.58 0.415 0.22 78.7 0.24 85.8 22 0.5 0.48 0.53 0.417 0.20 79.9 0.22 87.3 23 0.5 0.41 0.48 0.413 0.17 80.8 0.20 88.6 Cleaning solution 2 0.002 0.0024 0.540 0.00 80.9 0.00 88.6 24 0.5 0.37 0.43 0.410 0.15 81.7 0.18 89.8 Washing liquid 3 0.0023 0.0019 0.590 0.00 81.7 0.00 89.8 16% solids, based on weight / weight g / litre Fe Ti Re:> time to consider Fe Ti volume gram cumulative gram cumulative hour cumulative hour liter extraction Extraction 0.25 7.07 4.00 0.010 0.07 0.2 0.04 0.1 1 0.50 8.16 4.52 0.380 3.10 9.3 1.72 5.9 0.25 4.77 4. 63 0.010 0.05 9.4 0.05 6.0 2 0.50 5.78 5.44 0.402 2.32 16.3 2.19 1 j. J j 0.50 4.74 4.54 0.418 1.98 22.1 1.90 19.6 4 0.50 4.16 4.13 0.419 1.74 27.2 1.73 25.4 ί 1 丨 5 0.50 3.62 3.63 0.418 1.51 31.6 1.52 30.5 6 0.50 3.30 3.27 0.425 1.40 35.7 1.39 35.1: meaning lotion 1 0.05 0.04 0.511 0.03 35.8 0.02 35.2 7 0.50 2.54 2.65 0.408 1.04 38.8 1.08 38.8 S 0.50 2.08 2.41 0.417 0.87 41.4 1.00 42.1,: / Γ lotion 2 0.50 0.08 0.09 0.450 0.04 41.5 0.04 42.3 (Please read the precautions on the back before filling this page) -27-; i: 漯 standard (CNSM. 丨 Regulations (21 () X 297) 坌) 528732 A7 V. Description of the invention (25-Metal halide inspection The effect of metal oxide & order evaluation experiments on the effect of metal halide on the recovery of iron from ore using sulfuric acid according to the main invention method. The results are shown in FIG. 4. In this example, the salts used were NaCl at concentrations of 0/0, 50/0, j5%, and 25% (weight / weight). These tests were performed on a non-milled ore using a sulfuric acid solution at a concentration of 200 g / L in the presence of 100 C and no activated carbon. The addition of salt accelerated the reaction rate. However, approximately 15 to 20% salt (150 to 2000 g / L) NaC1 becomes counterproductive. The total percentage of actually leached iron has decreased since reaching 15% NaCl. In a different but similar experiment to further illustrate the effect of alkali metal halides on leaching of iron from ilmenite, a sample of 100 g of ilmenite feedstock at 1000 CF with 200 g sulfuric acid, 700 g The amount of water and different alkali metal halides leached "], the amount of metal halides tested was 0, 50, 150, and 250 grams, which represent 0, 5, 5 and 25% (weight / weight) alkali metal halides. Solution. It can be said that the leaching rate of iron was observed. The results are shown in Table 3.
in----*-----•裝--------訂 (請先閱讀背面之注意事項再填寫本頁C 4 ii· -fi ~ ~ ------------------ 士 3驗金屬鱼丄匕物對硫酸瀝濾程序的影響 !驗金屬鹵也物 __ ,間,小時 Fe毫克/公升 體積,公升 —-~~---- 86 0.700 J 990 0.700 6 1460 0.700 Fe萃取 0.06 0.69 1.02 累積 0.2% 2.0% 3.0% -28 528732 A7 _B7 五、發明說明(26 ) 12 3000 0.700 2.10 6.2% 24 4000 0.700 2.80 8.2% 36 6100 0.700 4.27 12.6% 48 10200 0.700 7.14 21.0% 60 14600 0.700 10.22 30.1% 72 20700 0.720 14.90 46.5% 清洗液1 860 1.020 0.88 清洗液2 28 0.990 0.03 5%鹼金屬_化物 時間,小時 Fe毫克/公升 體積, 公升 Fe萃取 克 累積 0 100 0.700 0.07 0.2% j 1110 0.700 0.78 2.4% 6 1860 0.700 1.30 4.0% 12 3500 0.700 2.45 7.6% 24 4700 0.700 3.29 10.2% 36 6500 0.700 4.55 14.1% 4S i 10100 0.700 7.07 21.8% 60 18600 0.700 13.02 40.2% 72 21700 0.790 17.14 56.5% :?「洗液1 1100 1.000 1.10 :?「洗液2 34 1.000 0.03 :15%¾ [1 化物 丨時叫,小時 Fe毫克/公升 體積, 公升 Fe萃取 (請先閱讀背面之注意事項再填寫本頁) -29- 準(CNS)Al 公f ) 528732 A7B7 五、發明說明(27 ) rV /Μ 么、 社 卬 1 j 克 累積 0 189 0.700 0.13 0.4% 3 1910 0.700 1.34 4.3% 6 2500 0.700 1.75 5.7% 12 4400 0.700 3.08 10.0% 24 5600 0.700 3.92 12.8% 36 7900 0.700 5.53 18.0% 48 12300 0.700 8.61 28.0% 60 18200 0.700 12.74 41.4% 72 25300 0.720 18.22 63.9% 清洗液1 1350 1.020 1.38 清洗液2 61 0.990 0.06 25%鹼金屬_化物 時間,小時 Fe毫克/公升 體積,公升 Fe萃取 克 累積 0 250 0.700 0.18 0.5% j 2600 0.700 1.82 5.2% 6 4200 0.700 2.94 8.4% 12 9800 0.700 6.86 19.7% 24 11700 0.700 8.19 23.5% 36 14500 0.700 10.15 29.1% 48 17300 0.700 12.11 34.7% 60 18900 0.700 13.23 37.9% 72 18700 0.720 13.46 47.9% -30- 叫+ 家標準蜆恪(210 X 297公堃) —.—*-----裝--------訂--------- (請先閱讀背面之注意事項再填寫本頁) ☆ 528732 Α7 Β7 五、發明說明(28 ) 清洗液1 2960 1.020 3.02 清洗液2 230 0.990 0.23 實例4-磨碎礦石的影響 根據本主要發明,可利用磨碎礦石增加自鈦鐵礦瀝濾出 鐵的反應速率。這表示於圖5和表4中。兩試驗皆是利用100 克鈥鐵礦量置於1公升由200克/公升硫酸和〗50克/公升驗金 屬鹵化物所形成的溶液中並加熱至100X:。在相同鈦鐵礦進 料的兩個樣品中進行試驗。一個實驗使用粗鈦鐵礦(1 〇〇°/〇 留在7 5微米篩子上),另一個實驗利用細鈦鐵礦(1 00%通過 7 5微米篩子)。激烈攪拌該泥漿約7 2小時並定期監測鐵的 濃度。碎礦石(粒徑較小的樣品)的瀝濾動力學一直比未經 研磨的礦石(粒徑較粗的樣品)快速。在5至2 5小時期間, 礦石的動力學此兩試驗是相似的。 長4進料硫酸瀝濾程序的影響結果 ί 仗鐵碼 --------— !時叫 :小時 Fe 毫克/公升 體積 公升— Fe萃取 克 累積 〇 189 0.700 0.13 0.4% 3 1910 0.700 1.34 4.3% h 2500 0.700 1.75 5.7% 1: 4400 0.700 3.08 10.0% /- ii μ - 31 - (CNS)AI (^10 χ -97 —.—.-----裝--------訂·-------- (請先閱讀背面之注意事項再填寫本頁) 528732 A7 B7 五、發明說明(29 ) 24 5600 0.700 3.92 12.8% 36 7900 0.700 5.53 18.0% 48 12300 0.700 8.61 28.0% 60 18200 0.700 12.74 41.4% 72 25300 0.720 18.22 59..3% 清洗液1 1350 1.020 1.38 清洗液2 61 0.990 0.06 細鈇鐵礦 時間 Fe 體積 Fe萃取 小時 毫克/公升 公升 克 累積 0 2300 0.700 1.61 4.8% j 5000 0.700 3.50 10.5% 6 5100 0.700 3.57 10.7% 12 5400 0.700 3.78 11.3% 24 6600 0.700 4.55 13.6% 48 20000 0.700 14.00 42.0% 60 24000 0.700 16.80 50.4% 72 29300 0.815 23.88 76.3% 清洗液1 1550 0.995 1.54 清洗液2 44 1.000 0.04 (請先閱讀背面之注意事項再填寫本頁) 實例5 -碳源的添力口 活性碳或石墨形式之碳源的加入可加速瀝濾反應的動力 么、 社 印 32- 準(CNS)A!規格(210 X 297公釐) ^8732 A7 B7 ----- 五、發明說明(30 ) 學。碳相對於所使用礦石比爲1 : 2和1 : 1。在i0(rc下以 120克/公升鹽和200克/公升硫酸所完成的試驗結聚是表示 於表6中。最節省成本之碳相對於礦石的比例將视最終避滤 條件而定。熟諳此技者接受目前所揭示之益處可指出對於 特定程序而言適當的碳相對於痛石之比例。 在一個説明碳源的添加對自鈦鐵礦瀝濾出鐵以留下Ti〇2 ;辰縮液殘留物之影響的不同但相似實驗中,相對於上述實 驗中所使用的120克/公升鹽類,則使用15〇克/公升之鹼金 屬鹵化物溶液。該實驗使用具有可使1〇〇0/〇粒子通過7 5微米 篩子之粒徑的鈦鐵礦。將不同量的椰子殼活性碳放在各容 器中。相同地,依上述實驗評估碳相對於樣品的比例。對 万、〇 1 2和1 · 1之碳對樣品比,其碳量分別爲〇、5 0和 7克/激烈攪拌泥漿約72小時並定期監測鐵的濃度,該結 果表:於表5中。碳對進料物質比爲1 :丨之瀝濾條件些微 優於其他兩個條件的動力學。 酸;歷!加入碳的結果 A啖源 |時叫(小時) Fe(毫克/公 升) 體積 (公升) Fe萃取 克 ____ 0 3000 0.700 2.10 5700 0.700 3.00 5900 0.700 4.13 累精 6〇% 11.5% 1.9% ) (請先閱讀背面之注意事項再填寫本頁) 裝--------訂--- 舞 -33- 528732in ---- * ----- • Equipment -------- Order (Please read the notes on the back before filling in this page C 4 ii · -fi ~ ~ -------- ---------- The effect of Shi 3 metal fish mackerel test on sulfuric acid leaching process! Metal halide test __, sometimes, hour Fe mg / liter volume, liter --- ~~- -86 0.700 J 990 0.700 6 1460 0.700 Fe extraction 0.06 0.69 1.02 Cumulative 0.2% 2.0% 3.0% -28 528732 A7 _B7 V. Description of the invention (26) 12 3000 0.700 2.10 6.2% 24 4000 0.700 2.80 8.2% 36 6100 0.700 4.27 12.6% 48 10200 0.700 7.14 21.0% 60 14600 0.700 10.22 30.1% 72 20700 0.720 14.90 46.5% Cleaning solution 1 860 1.020 0.88 Cleaning solution 2 28 0.990 0.03 5% Alkali metal compound time, hour Fe mg / liter volume, liter Fe extraction Gram accumulation 0 100 0.700 0.07 0.2% j 1110 0.700 0.78 2.4% 6 1860 0.700 1.30 4.0% 12 3500 0.700 2.45 7.6% 24 4700 0.700 3.29 10.2% 36 6500 0.700 4.55 14.1% 4S i 10100 0.700 7.07 21.8% 60 18600 0.700 13.02 40.2 % 72 21700 0.790 17.14 56.5%:? `` Washing liquid 1 1100 1.000 1.10:? '' Washing liquid 2 34 1.000 0 .03: 15% ¾ [1 compound called, hour Fe mg / liter volume, liter Fe extraction (please read the precautions on the back before filling this page) -29- quasi (CNS) Al male) 528732 A7B7 5 、 Explanation of invention (27) rV / M ?, 1 gram cumulative 0 189 0.700 0.13 0.4% 3 1910 0.700 1.34 4.3% 6 2500 0.700 1.75 5.7% 12 4400 0.700 3.08 10.0% 24 5600 0.700 3.92 12.8% 36 7900 0.700 5.53 18.0% 48 12300 0.700 8.61 28.0% 60 18200 0.700 12.74 41.4% 72 25300 0.720 18.22 63.9% Cleaning liquid 1 1350 1.020 1.38 Cleaning liquid 2 61 0.990 0.06 25% Alkali metal compound time, hour Fe mg / liter volume, liter Fe Cumulative extraction gram 0 250 0.700 0.18 0.5% j 2600 0.700 1.82 5.2% 6 4200 0.700 2.94 8.4% 12 9800 0.700 6.86 19.7% 24 11700 0.700 8.19 23.5% 36 14500 0.700 10.15 29.1% 48 17300 0.700 12.11 34.7% 60 18900 0.700 13.23 37.9 % 72 18700 0.720 13.46 47.9% -30- Call + Home Standard (210 X 297 Gong) —. — * ----- Installation -------- Order -------- -(Please read the notes on the back before filling this page) ☆ 528732 Α7 Β7 V. Description of the invention (28) Cleaning liquid 1 2960 1.020 3.02 Cleaning liquid 2 230 0.990 0.23 Example 4-Impact of ground ore According to the main invention, ground ore can be used to increase the reaction of leaching iron from ilmenite rate. This is shown in Figure 5 and Table 4. In both tests, 100 g of iron ore was placed in a 1 liter solution of 200 g / L sulfuric acid and 50 g / L metal halide and heated to 100X :. Tests were performed on two samples of the same ilmenite feed. One experiment used coarse ilmenite (100 ° / 〇 left on a 75 micron sieve), and another experiment used fine ilmenite (100% through a 75 micron sieve). The slurry was stirred vigorously for about 72 hours and the iron concentration was monitored regularly. The leaching kinetics of crushed ore (smaller particle size samples) has been faster than unground ore (larger particle size samples). The kinetics of the ore during 5 to 25 hours were similar between the two tests. The effect of the sulphuric acid leaching program for long 4 feeds ί The iron code --------! When called: Hour Fe mg / L volume liters — Fe extraction gram accumulation 0189 0.700 0.13 0.4% 3 1910 0.700 1.34 4.3% h 2500 0.700 1.75 5.7% 1: 4400 0.700 3.08 10.0% /-ii μ-31-(CNS) AI (^ 10 χ -97 —.—.----- installation -------- Order · -------- (Please read the notes on the back before filling this page) 528732 A7 B7 V. Description of the invention (29) 24 5600 0.700 3.92 12.8% 36 7900 0.700 5.53 18.0% 48 12300 0.700 8.61 28.0 % 60 18200 0.700 12.74 41.4% 72 25300 0.720 18.22 59..3% Cleaning liquid 1 1350 1.020 1.38 Cleaning liquid 2 61 0.990 0.06 Fine iron ore time Fe Volume Fe extraction hours mg / L liter Cumulative 0 2300 0.700 1.61 4.8% j 5000 0.700 3.50 10.5% 6 5100 0.700 3.57 10.7% 12 5400 0.700 3.78 11.3% 24 6600 0.700 4.55 13.6% 48 20000 0.700 14.00 42.0% 60 24000 0.700 16.80 50.4% 72 29 300 0.815 23.88 76.3% Cleaning liquid 1 1550 0.995 1.54 Cleaning liquid 2 44 1.000 0.04 (Please read the notes on the back before filling in this ) Example 5-Is the addition of carbon source activated carbon or graphite in the form of carbon source can accelerate the leaching reaction power, press 32-standard (CNS) A! Specifications (210 X 297 mm) ^ 8732 A7 B7 ----- V. Description of the invention (30) Science. The ratio of carbon to the ore used is 1: 2 and 1: 1. It is completed at 120 g / L of salt and 200 g / L of sulfuric acid at i0 (rc). The experimental agglomeration is shown in Table 6. The ratio of the most cost-effective carbon to ore will depend on the final filtration conditions. Those skilled in the art accepting the benefits currently revealed can point to the appropriate carbon for a particular procedure. Relative to the pain stone ratio. In a different but similar experiment illustrating the effect of the addition of a carbon source on the leaching of iron from ilmenite to leave Ti02; chin shrinkage residues, relative to the 120 g / L salt used in the above experiment For example, an alkali metal halide solution of 15 g / liter is used. This experiment uses ilmenite with a particle size that allows 1000/0 particles to pass through a 75 micron sieve. Place different amounts of coconut shell activated carbon in each container. Similarly, the ratio of carbon to sample was evaluated according to the experiments described above. For the carbon-to-sample ratios of 10,000, 012, and 1.1, the carbon content was 〇, 50, and 7 g / rigidly stirring the mud for about 72 hours and the iron concentration was regularly monitored. The result table is shown in Table 5. . The leaching conditions with a carbon to feed material ratio of 1: 丨 are slightly better than the other two conditions. Acid; calendar! Results of adding carbon A 啖 source | when called (hours) Fe (mg / liter) volume (liters) Fe extraction grams ____ 0 3000 0.700 2.10 5700 0.700 3.00 5900 0.700 4.13 Accumulated refined 60% 11.5% 1.9 %) (Please read the precautions on the back before filling out this page) Loading -------- Order --- Mai-33- 528732
7 7 A B ¥ ·. 7 :ΐ fi- 五、發明說明(31 ) 12 6200 0.700 4.34 12.5% 24 14500 0.700 10.15 29.1% 48 25000 0.700 17.50 50.3% 60 27000 0.700 18.90 54.3% 72 36500 0.740 27.01 83.6% 清洗液1 2060 0.995 2.05 清洗液2 60 1.010 0.06 1 : 2碳:欽鐵礦 時間(小時) Fe 體積 Fe萃取 毫克/公升 公升 克 累積 0 4100 0.700 2.87 8.4% j 8200 0.700 5.74 16.7% 6 11100 0.700 7.77 22.6% 12 12300 0.700 8.61 25.1% 24 20200 0.700 14.14 41.2% 48 24000 0.700 16.80 49.9% 60 27000 0.700 18.90 55.1% 72 39300 0.695 27.31 89.3% 清洗液1 3240 0.980 3.18 清洗液2 150 1.000 0.15 1 : 1碳:鈦鐵礦 时間(小時) Fe 體積 Fe萃取 毫克/公升 公升 -34- (請先閱讀背面之注意事項再填寫本頁) 义1 :ί…+円闷家標準(CNS)/V丨規恪(210 x 297公t ) 528732 A7 B7 五 、發明說明(32 ) 克 累積 0 4800 0.700 3.36 10.0% 3 8000 0.700 5.60 16.7% 6 10100 0.700 7.07 21.1% 12 14500 0.700 10.15 30.3% 24 24000 0.700 16.80 50.2% 48 27000 0.700 16.90 56.4% 60 31000 0.700 21.70 64.8% 72 45400 0.550 24.97 93.5% 清洗液1 6040 0.990 5.98 355 0.990 0.35 .—^ —.-----.— (請先閱讀背面之注意事項再填寫本頁) 訂--· 以硫酸-鹵化物-碳系統自紅土礦中瀝濾銅史錄 此礦石的主要分析含量爲2.36% Co、1.26% Ni、1丨.〇〇〇/。Fe 、1 ().8()% Μη。先以200克溶於650克水的NaCl處理loo克磨 八、2〇〇網目4礦石的樣品。在加熱板上蒸掉水份以此程 十炊逑模擬一種鹽溶液噴礦石堆的情形並使其自然基掉。 4沒此礦石-鹽固體在200克硫酸於700克水所形成的溶液中 T;成泥漿。在一個攪拌加熱板上將攪拌的泥漿加熱至1 、$浚加入1 00克+ 6 5網目、椰子殼、活性碳。利用在* 6和2 4小時時所採集的水溶液進行4 8小時測試。該結果 乂七於長6中。鈷的萃取最好是在第一個小時内完成鈷可 ‘一”…匕々,液的離子強度F沈殿而且無法被回收直到清洗於 …、w其;S解。’除了省略NaCl,在相同條件下瀝濾礦石約 準(CNS):U 規$ (1MU、公望) -35- ^/32 ,r> 社 A7 B7 五、發明說明(33 ) 120小時之後,Co回收率是63.9%和Ni回收率58·2% 表6自紅土礦瀝 亀萃取出來的百分比 時間(小時) Co Ni Fe j Μη 1 81.5% 67.5% 18.8% i 63.4% 2 81.5% 78.2% 25.5% —---- 71.0% 4 81.5% 85.5% 31.5% 71.0% 6 81.5% 84.8% 36.0% 72.6% 24 85.0% 87.5% 54.8% 73.3% 48 81.5% 86.2% 67.5% 71.0% 清洗液1 13.1% 12.9% 18.5% 11.5% 清洗液2 5.4% 0.6% 2.2% 0.4% 最終水溶液: 100.0% 99.6% 88.2% 82.9% 例 7 -鹼金屬_鹵化物瀝濾鎳和鈷的影響^ 在兩個100克紅石-1進料樣品中進行實驗,其中該樣品包 會具有使近80%通過75微米網目之粒徑的1〇%鎳和〇丨〇/。 yti : 在第一個實驗中,於100X:下以200克硫酸 驗金屬I#化物瀝濾1 〇〇克樣品。 在第二個實驗中,於100X:下以2〇〇克硫酸 克給金屬(I化物(氯化鈉)瀝濾100克樣品。 、800克水和矣 800兄水和2⑽ --------*-----·裝--------丨訂P-------- (請先閱讀背面之注意事項再填寫本頁) dwwra雜準(cns)a、i 規恪⑺〇x 297 公 -36- 528732 A7 B7 五、發明說明(34 ) 各實驗共進行6小時並在0.25、0.5、} Q、 2.0 6 · 0小時時採集溶液。該結果表示於表7和固7 4·0和最後 鈷而言,利用齒化物之第二個實驗明顯二# 8。對鎳和 ,特別是鈷。 出較佳的結果 表7自紅土-1遞:滤出鍊和姑 無驗金屬函化物7 7 AB ¥ .. 7: ΐ fi- V. Invention description (31) 12 6200 0.700 4.34 12.5% 24 14500 0.700 10.15 29.1% 48 25000 0.700 17.50 50.3% 60 27000 0.700 18.90 54.3% 72 36500 0.740 27.01 83.6% Cleaning liquid 1 2060 0.995 2.05 Cleaning solution 2 60 1.010 0.06 1: 2 Carbon: Qinite time (hours) Fe Volume Fe extraction mg / L liter Cumulative 0 4100 0.700 2.87 8.4% j 8200 0.700 5.74 16.7% 6 11100 0.700 7.77 22.6% 12 12300 0.700 8.61 25.1% 24 20200 0.700 14.14 41.2% 48 24000 0.700 16.80 49.9% 60 27000 0.700 18.90 55.1% 72 39 300 0.695 27.31 89.3% Cleaning liquid 1 3240 0.980 3.18 Cleaning liquid 2 150 1.000 0.15 1: 1 Carbon: Ilmenite Time (hours) Fe Volume Fe Extraction mg / L / L -34- (Please read the precautions on the back before filling out this page) Meaning 1: ί… + 円 不 家家 标 (CNS) / V 丨 Regulations (210 x 297g t) 528732 A7 B7 V. Description of the invention (32) Gram accumulation 0 4800 0.700 3.36 10.0% 3 8000 0.700 5.60 16.7% 6 10100 0.700 7.07 21.1% 12 14500 0.700 10.15 30.3% 24 24000 0.70 0 16.80 50.2% 48 27000 0.700 16.90 56.4% 60 31000 0.700 21.70 64.8% 72 45400 0.550 24.97 93.5% Cleaning liquid 1 6040 0.990 5.98 355 0.990 0.35 .— ^ —.-----.— (Please read the notes on the back first Please fill in this page for further details) Order-· The history of leaching copper from laterite ore with sulfuric acid-halide-carbon system records the main analytical content of this ore is 2.36% Co, 1.26% Ni, 1 丨 .00 //. Fe, 1 (). 8 ()% Mn. A 200 g sample of ore mesh 4 was treated with 200 g of NaCl dissolved in 650 g of water. The process of steaming off the water on the hot plate in this process simulates a situation in which a salt solution sprays the ore pile and causes it to naturally fall off. 4 This ore-salt solid was dissolved in a solution of 200 g of sulfuric acid in 700 g of water; into a slurry. Heat the stirred mud to 1 on a stirring hot plate, add 100 g + 6 5 mesh, coconut shell, activated carbon. A 48 hour test was performed using the aqueous solution collected at * 6 and 24 hours. The result is 27 in Chang 6. The extraction of cobalt is best completed within the first hour. Cobalt can be 'a' ... dagger, liquid ionic strength F Shen Dian and can not be recovered until washed in ..., W; S solution. ' Under the conditions of leaching of ore (CNS): U regulation $ (1MU, Gongwang) -35- ^ / 32, r > News Agency A7 B7 V. Description of the invention (33) After 120 hours, the Co recovery rate is 63.9% and Ni Recovery rate 58.2% Table 6 Percent time extracted from laterite ore bitumen (hours) Co Ni Fe j Μη 1 81.5% 67.5% 18.8% i 63.4% 2 81.5% 78.2% 25.5% —---- 71.0% 4 81.5% 85.5% 31.5% 71.0% 6 81.5% 84.8% 36.0% 72.6% 24 85.0% 87.5% 54.8% 73.3% 48 81.5% 86.2% 67.5% 71.0% Cleaning liquid 1 13.1% 12.9% 18.5% 11.5% Cleaning liquid 2 5.4% 0.6% 2.2% 0.4% Final aqueous solution: 100.0% 99.6% 88.2% 82.9% Example 7-Effect of alkali metal_halide leaching of nickel and cobalt ^ Experiments were performed in two 100 g samples of redstone-1 feed, The sample package will have 10% nickel and 〇 丨 〇 / that pass nearly 80% of the particle size through a 75 micron mesh. Yti: In the first experiment, at 100X: 200 g sulfuric acid The test metal I # compound leached a 100 g sample. In a second experiment, 100 g of the metal (I compound (sodium chloride) was leached to 100 g sample at 100X: 200 g of sulfuric acid. 800 g Water and 矣 800 brother water and 2⑽ -------- * ----- · install -------- 丨 P -------- (Please read the note on the back first Please fill in this page again for details) dwwra miscellaneous standards (cns) a, i regulations 0x 297 public -36- 528732 A7 B7 V. Description of the invention (34) Each experiment was performed for 6 hours in total, 0.25, 0.5,} Q, The solution was collected at 2.0 6 · 0 hours. The results are shown in Table 7 and solid 7 4 · 0 and the last cobalt, the second experiment using the dentate was obviously two # 8. For nickel and, especially cobalt. The best results are shown in Table 7.
0.5 380.0 30.0 0.010 0.010 2.40 3.80 21.3% 33.7% 0.20 20.3% 0.30 30.5% 550.0 39.0 0.010 5.50 48.8% 0.39 39.6% 740.0 53.0 0.010 7.40 65.8% 0.53 53.8% 820.0 64.0 0.010 8.20 72.7% 0.64 65.0% 丨6小時PLS:义洗液1 1060.0 75.0 0.780 826.80 94.0% 58.50 78.2% , 裝--------訂---------· f靖先閱讀背面之;tt!咅?事項再填寫本頁) 116.0 40.0 0.670 77.72 26.80 12.0 1.3 0.700 8.40 0.91 tv *、 、一 包分給金'屬1¾化物 Ni Co ':、時 〈δ克/公升 體積 公升 毫克 累積萃 取量 毫克 累積萃 取量 Ni Co -37- w»732 A7 B7 五、 發明說明(35 0.25 741.7 100.0 0.010 7.42 69.4% 1.00 97.7% 0.5 867.2 958.4 1026.9 1049.7 100.0 100.0 100.0 100.0 0.010 0.010 0.010 0.010 8.67 9.58 10.27 10.50 81.2% 89.7% 96.1% 98.3% 1.00 97.7% 1.00 97.7% 1.00 97.7% 1.00 97.7%0.5 380.0 30.0 0.010 0.010 2.40 3.80 21.3% 33.7% 0.20 20.3% 0.30 30.5% 550.0 39.0 0.010 5.50 48.8% 0.39 39.6% 740.0 53.0 0.010 7.40 65.8% 0.53 53.8% 820.0 64.0 0.010 8.20 72.7% 0.64 65.0% 丨 6 hours PLS: meaning Lotion 1 1060.0 75.0 0.780 826.80 94.0% 58.50 78.2%, install -------- order --------- f Jing first read the back; tt! 咅? Please fill in this page again) 116.0 40.0 0.670 77.72 26.80 12.0 1.3 0.700 8.40 0.91 tv *,, One pack of gold 'is a compound of Nitrile Ni Co':, hour <δ g / liter volume liter milligram cumulative extraction amount milligram cumulative extraction amount Ni Co -37- w »732 A7 B7 V. Description of the invention (35 0.25 741.7 100.0 0.010 7.42 69.4% 1.00 97.7% 0.5 867.2 958.4 1026.9 1049.7 100.0 100.0 100.0 100.0 0.010 0.010 0.010 0.010 0.010 8.67 9.58 10.27 10.50 81.2% 89.7% 96.1% 98.3 % 1.00 97.7% 1.00 97.7% 1.00 97.7% 1.00 97.7%
6小時PLS 清洗液1 凊洗液2 1050.0 103.8 60.5 100.0 10.0 5.7 0.765 0.670 0.590 803.25 69.57 35.68 98.3% 76.50 97.7% 6.70 3.36 复土[8 -驗金屬鹵化物對自紅土 _ 2中瀝濾出鎳和鈷的影響 在兩種100克包含具有使近8 0%通過75微米網目之粒徑的 1 . 1 %鎳和0 · 1 %鈷之紅石_ 2進料樣品中進行實驗。 在第一個實驗中,於10(TC下以200克硫酸、8⑽克水和無 驗金屬鹵化物瀝濾100克樣品。 ‘在第二個實驗中,於10(rc下以2〇〇克硫酸、8〇〇克水和2⑼ 兄驗金屬鹵化物(氣化鈉)瀝濾1 00克樣品。 表實驗共進行6小時並在0.25、0.5、!·〇、2.0、4.〇和最後 :0 I時時扣集;谷;夜。該結果表示於表8和圖9和丨。對鎳 而言,鹼金屬1^化物(氣化鈉)試驗明顯表現出較佳的 h ’特別是關於達到完全(1GQ%)溶解的速度。 濾出鎳和鈷 至图化物6 hours PLS cleaning solution 1 凊 washing solution 2 1050.0 103.8 60.5 100.0 10.0 5.7 0.765 0.670 0.590 803.25 69.57 35.68 98.3% 76.50 97.7% 6.70 3.36 Compound [8-Test metal halide pair leaching nickel and cobalt from laterite_ 2 The effects were tested in two 100-gram samples of 1.1% nickel and 0.1% cobalt redstone-2 with a particle size that passed nearly 80% through a 75 micron mesh. In the first experiment, a 100-gram sample was leached at 10 ° C with 200 g of sulfuric acid, 8 g of water, and a non-test metal halide. 'In a second experiment, 200 g Sulfuric acid, 800 g of water, and 2 g of metal halide (sodium gaseous solution) were leached for a sample of 100 g. Table experiments were performed for a total of 6 hours and at 0.25, 0.5,! · 〇, 2.0, 4.0 and finally: 0 I hourly buckle set; valley; night. The results are shown in Table 8 and Figures 9 and 丨. For nickel, the alkali metal 1 ^ compound (sodium gasification) test clearly shows better h ', especially with respect to Achieve complete (1GQ%) dissolution rate. Filter out nickel and cobalt to the pattern
二)97公呈) - ---*---------^^裝--------訂--- (請先閱讀背面之注意事項再填寫本頁) -38· 528732 7 7 Λ Β 五、發明說明(36 ) ☆ 時間 毫克/公升 體積 毫克 累積萃 毫克 累積萃 小時 公升 取量 取量 Ni Co 0.25 738.9 45.0 0.010 7.39 60.0% 0.45 51.6% 0.5 915.3 54.0 0.010 9.15 74.3% 0.54 61.9% 1 1036.6 65.0 0.010 10.37 84.2% 0.65 74.5% 2 1113.8 80.0 0.010 11.14 90.4% 0.80 91.7% 4 1146.9 80.0 0.010 11.47 93.1% 0.80 91.7% 6小時PLS 1180.0 85.0 0.725 855.50 95.8% 61.63 97.4% 清洗液1 264.7 21.0 0.530 140.28 11.13 清洗液2 51.8 4.1 0.695 36.02 2.85 包含驗金屬卣化物 Ni Co 時間 毫克/公升 體積 毫克 累積萃 毫克 累積萃 小時 公升 取量 取量 Ni Co !〇.25 906.5 80.0 0.010 9.07 76.4% 0.80 88.9% 0.5 1054.1 90.0 0.010 10.54 88.8% 0.90 100.0% 1 1149.0 90.0 0.010 11.49 96.8% 0.90 100.0% 1159.5 90.0 0.010 11.60 97.7% 0.90 100.0% 4 1170.0 90.0 0.010 11.70 98.6% 0.90 100.0% 〇']'時IIS 1 170.0 90.0 0.750 877.50 98.6% 67.50 100.0% :n:ti 177.1 13.0 0.800 141.67 10.40 4洗液2 25.3 2.1 0.795 9.07 1.67 (請先閱讀背面之注意事項再填寫本頁) -39- 糸^準(C\S)A4 少)7 公t ) ilf ίί 社 A7 五、發明說明(37 ) 上面兩個實驗説明自兩種不同的鎳-鈷紅石樣品瀝濾出 和鈷的結果。 下列程序步驟被分別用於各紅石樣品: 步驟1將冷凝器放在裝有前述溶液和紅石進料之泥漿的 錐形瓶上; β 步驟2測試期間以磁石攪拌器激烈攪拌該泥漿並將溫度 保持在l〇〇°C ; ^ 步驟3此試驗是在預定時間如1 5分鐘、3 〇分鐘等利用定 量管從錐形瓶中吸取1 〇毫升熱泥漿至離心管中以 冗成採樣,然後在4,000 rpm下離心5分鐘: 步驟4將經一段時間離心過的瀝濾溶液移至— 以供曰後分析; 中 女.¾ 5利用1 〇毫升組成瀝濾溶液清洗離心過的殘留物並 倒回錐形瓶中,然而在加熱板上於100X;下繼續授 拌錐形瓶内容物: /^4 6 4 .¾中終了時(6小時)’將錐形瓶的内容物倒入兩 個離心管中,另外利用極少量蒸餾水清洗出任何 錐形瓶内緣所剩餘的殘留物,然後離心之: 步骤7將兩離心管中經過離心的内容物(含量豐富的瀝廣 浴液-P L· S )倒入量筒中並使其冷卻; 步驟8然後讀取PLS溶液的體積,將近2 0毫升移至試管 中並分析其鎳和鈷含量,· g 步驟9進行計算以測定水溶液中的鎳和鈷含量並比較其 個別紅土礦進料的元素分析値: -40- 円网家標準丨規络(210x297公坌) —;--·*---*-----^^裝--------訂·-- (請先閱讀背面之注音?事項再填寫本頁} Φ -! n n n . 528732 五、發明說明(38 步驟1 〇可藉對任何特定工廠而言是最經濟的方法自歷遽 水/奋液中將鎳和鈷完全或部份去除。可使用的方 法包括,但不限於藉放入晶種、pH調整或結晶; ’谷劑萃取和元素金屬電解冶金法;和離子交換使 金屬鹽類沈澱。 复土] 9 -瀝濾、銀 此貫例顯tf自銅精緻燃燒工廠的殘渣瀝濾銀。此試驗是 在100C下以200克/公升硫酸和2〇〇克/公升NaC1*進行。5〇 克& ;查樣品是在500毫升溶液中瀝濾、。該瀝遽進行* 8小時。 該結果表示於表9中。 C請先閱讀背面之注意事項再填寫本頁} 裝 青製殘渣中瀝;慮銀約4 8小時的結果 樣品 主要Ag含量,ppm 水溶液中的Ag含量 回收率°/〇 '—____ ,ppm 14.75 18 80 58.9 59 —-----—— 65 Ppm二每百萬分之一B) 97 public presentation)---- * --------- ^^ equipment -------- order --- (Please read the precautions on the back before filling this page) -38 · 528732 7 7 Λ Β V. Description of the invention (36) ☆ Time mg / litre Volume mg Cumulative extraction Milligram Cumulative extraction Hour Liter Measured Ni Co 0.25 738.9 45.0 0.010 7.39 60.0% 0.45 51.6% 0.5 915.3 54.0 0.010 9.15 74.3% 0.54 61.9% 1 1036.6 65.0 0.010 10.37 84.2% 0.65 74.5% 2 1113.8 80.0 0.010 11.14 90.4% 0.80 91.7% 4 1146.9 80.0 0.010 11.47 93.1% 0.80 91.7% 6 hours PLS 1180.0 85.0 0.725 855.50 95.8% 61.63 97.4% Cleaning solution 1 264.7 21.0 0.530 140.28 11.13 Cleaning solution 2 51.8 4.1 0.695 36.02 2.85 Contains metal test compounds Ni Co Time mg / L volume mg Cumulative extraction mg Cumulative extraction Hour Liter Measured amount Ni Co! 0.25 256.5 80.0 0.010 9.07 76.4% 0.80 88.9% 0.5 1054.1 90.0 0.010 10.54 88.8% 0.90 100.0% 1 1149.0 90.0 0.010 11.49 96.8% 0.90 100.0% 1159.5 90.0 0.010 11.60 97.7% 0.90 100.0% 4 1170.0 90.0 0.010 11.70 98.6% 0.90 100.0% 〇 ']' IIS 1 170.0 90.0 0.750 877.50 98.6% 67.50 100.0%: n: ti 177.1 13.0 0.800 141.67 10.40 4 Washing liquid 2 25.3 2.1 0.795 9.07 1.67 (Please read the precautions on the back before filling this page) -39- 糸 ^ 糸 (C \ S) A4 less) 7 male t) ilf ί community A7 V. Description of the invention (37) The above two experiments illustrate the results of leaching and cobalt from two different nickel-cobalt redstone samples. The following procedure steps were used for each redstone sample: Step 1 Place the condenser on the conical flask containing the aforementioned solution and the slurry of the redstone feed; β Step 2 During the test, stir the slurry vigorously with a magnetic stirrer and bring the temperature Keep at 100 ° C; ^ Step 3 This test is to take 10 ml of hot mud from the Erlenmeyer flask in a centrifuge tube at a predetermined time such as 15 minutes, 30 minutes, etc. to the centrifuge tube for redundant sampling, and then Centrifuge at 4,000 rpm for 5 minutes: Step 4 Move the leached solution that has been centrifuged for a period of time to — for post-mortem analysis; maiden. ¾ 5 Use 10 ml of leaching solution to wash the centrifuged residue and pour it Return to the Erlenmeyer flask, but continue to incubate the Erlenmeyer flask contents on a hot plate at 100X: / ^ 4 6 4 .¾ At the end of the middle (6 hours) 'Pour the Erlenmeyer flask contents into two In the centrifuge tube, use a very small amount of distilled water to wash out the remaining residue on the inner edge of any conical flask, and then centrifuge it: Step 7 Centrifuge the contents of the two centrifuge tubes (rich Liguang bath-PL · S) Pour into the graduated cylinder and let it cool; step 8 Then read the volume of the PLS solution, transfer nearly 20 ml to the test tube and analyze its nickel and cobalt content, g Step 9 Perform calculations to determine the nickel and cobalt content in the aqueous solution and compare the elements of its individual laterite ore feed Analysis: -40- 标准 Internet standards 丨 profile (210x297 public address) —; --- * --- * ----- ^^ install -------- order --- (please Read the phonetic on the back? Matters and then fill out this page} Φ-! Nnn. 528732 V. Description of the invention (38 Step 1 〇 You can use the most economical method for any specific factory And cobalt are completely or partially removed. Methods that can be used include, but are not limited to, seeding, pH adjustment or crystallization; 'grain extraction and elemental metal electrolytic metallurgy; and ion exchange to precipitate metal salts. ] 9-Leaching, silver This example shows tf leaching silver from the residue of a copper refinery combustion plant. This test was performed at 100C with 200 g / L sulfuric acid and 200 g / L NaC1 *. 50 g & Check the sample is leached in a 500 ml solution. The leaching is performed for * 8 hours. The results are shown in Table 9. C Please read the note on the back first Please fill in this page again after filling out the matter.} Fill the green residue; take about 4 to 8 hours to consider the results. The main Ag content in the sample, the Ag content recovery rate in ppm aqueous solution ° / 〇 '—____, ppm 14.75 18 80 58.9 59 —- -------- 65 Ppm 2 per million
———訂P 0 -瀝濾鉬 好主要含有0.070% Μ 〇級的鉬氧化物礦樣品磨成-200網 ::並以1 00克/公升硫酸和1 00克/公升氯化鈉所形成的溶液 々::包之並在室溫下中榄拌4 8小時。此瀝濾可回收樣品中 N 〇 >) 倜取自相同礦石之未經研磨的礦石樣品過篩以選 41 - ,i.:C準(CNS)A_!規烙(」丨()x上厂公望) rYn.,,·:: r -Η4 Α :!;1-.,11.货->作钍印公 528732 A7 ___B7___ 五、發明說明(39 ) 擇-18,850+833微米(-3/4英吋+20網目)部份的粒子。將此 部份放在管柱中,以0·05加俞/分鐘·平方英吸的速度將相 同100克/公升硫酸和100克/公升氯化納所形成的溶液用於 該礦石中達5 6天。連續再循環此瀝遽溶液。此瀝濾、流程可 獲得8 2 %鉬回收率。 复例1 1 -兩階段瀝濾不同金屬以形成兩種瀝攄水溶液 在一個攪拌槽中於室溫下以100克/公升硫酸瀝濾被磨成· 200網目尺寸之氧化物銅礦樣品,其中該樣品的主要包含 〇· 91 % Cu、2· 0克/噸A u和2 · 4克/噸A g。然後過濾出固體殘 留物,將其置於另一個容器内並在室溫下以5 0克/公升溴化 鉀溶液瀝濾3 0小時並以足量的硫酸(6毫升)並伴隨攪拌將 P Η調整至1 · 〇。此結果表示於表1 〇中。 表1 0階段的回收百分比 瀝瀘階段 Cu Au Ag i〇〇g/i h2so, 71 0 0 ivBr-H2S04 28 100 100 •1,_ q·人住从匕4田心<日彳 J 登1¾ S泛濃 和溫度以在第一階段達到完全回收銅,但在第二階段仍 保持fei佳的A u和A g回收率。也可容易地變化此主要方 以適合礦石堆瀝濾。 战、瞭解在此所描述的實例和具體實例只爲了説明在其 示下將可提供熟諳此技者在此申請案之精神和範圍以及 '付申請專利範圍内所包含的各種改良和變化。 七円卜以標準(CN^Tl^T^ X 297公望) (請先閱讀背面之注意事項再填寫本頁) 裝-------:—訂 -42---—— Order P 0-Leached molybdenum mainly contains 0.070% Mo grade molybdenum oxide ore sample milled into -200 mesh :: and formed with 100 g / L sulfuric acid and 100 g / L sodium chloride Solution 々 :: Cover and mix for 4 8 hours at room temperature. This leaching recoverable sample N 〇>) 未经 Unmilled ore samples taken from the same ore are sieved to select 41-, i.:C 准 (CNS) A_! Chang Gongwang) rYn. ,, ::: r -Η4 Α:!; 1-., 11. Goods- > Zuo Yin Gong 528732 A7 ___B7___ V. Description of Invention (39) Select -18,850 + 833 microns (-3 / 4 inch + 20 mesh) particles. This part was placed in a column, and the same solution of 100 g / L of sulfuric acid and 100 g / L of sodium chloride was used in the ore at a rate of 0.05 05 g / min · sq. day. This bitumen solution was continuously recycled. This leaching process can achieve 82% molybdenum recovery. Repeat Example 1 1-Two-stage leaching of different metals to form two leachate aqueous solutions. Milled to a 200 mesh oxide copper ore sample in a stirred tank at 100 g / l sulfuric acid leaching at room temperature, where The sample mainly contained 0.91% Cu, 2.0 g / ton Au and 2.4 g / ton Ag. The solid residue was then filtered off, placed in another container and leached at room temperature with a 50 g / L potassium bromide solution for 30 hours and with a sufficient amount of sulfuric acid (6 ml) with stirring. Η is adjusted to 1 · 〇. The results are shown in Table 10. Table 1 Recovery percentage at stage 0 Cu Au Ag i〇〇g / i h2so, 71 0 0 ivBr-H2S04 28 100 100 • 1, _ q · Personal living from dagger 4 Tianxin & Sundial J Deng 1¾ S enrichment and temperature to achieve full copper recovery in the first stage, but still maintain good Fe and Au recovery in the second stage. This principal can also be easily changed to suit ore heap leaching. It is to be understood that the examples and specific examples described herein are provided only to illustrate that they will provide those skilled in the art with the spirit and scope of this application, as well as the various improvements and changes included in the scope of the patent application. Seven 円 bu standard (CN ^ Tl ^ T ^ X 297) (Please read the precautions on the back before filling out this page) Pack -------:-order -42-
Claims (1)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AUPQ2706A AUPQ270699A0 (en) | 1999-09-08 | 1999-09-08 | Improvements in or relating to methods for leaching titanium ores |
AUPQ4144A AUPQ414499A0 (en) | 1999-11-18 | 1999-11-18 | Improvements in orrelating to methods for leaching nickel and cobalt ores |
Publications (1)
Publication Number | Publication Date |
---|---|
TW528732B true TW528732B (en) | 2003-04-21 |
Family
ID=28455346
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
TW089104164A TW528732B (en) | 1999-09-08 | 2000-03-08 | Improved methods for leaching of ores |
Country Status (1)
Country | Link |
---|---|
TW (1) | TW528732B (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7922788B2 (en) | 2007-09-18 | 2011-04-12 | Barrick Gold Corporation | Process for recovering gold and silver from refractory ores |
US8262770B2 (en) | 2007-09-18 | 2012-09-11 | Barrick Gold Corporation | Process for controlling acid in sulfide pressure oxidation processes |
US8262768B2 (en) | 2007-09-17 | 2012-09-11 | Barrick Gold Corporation | Method to improve recovery of gold from double refractory gold ores |
TWI564094B (en) * | 2012-08-22 | 2017-01-01 | 吉田英夫 | Decontamination method and system for soil and the like |
-
2000
- 2000-03-08 TW TW089104164A patent/TW528732B/en not_active IP Right Cessation
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8262768B2 (en) | 2007-09-17 | 2012-09-11 | Barrick Gold Corporation | Method to improve recovery of gold from double refractory gold ores |
US7922788B2 (en) | 2007-09-18 | 2011-04-12 | Barrick Gold Corporation | Process for recovering gold and silver from refractory ores |
US8262770B2 (en) | 2007-09-18 | 2012-09-11 | Barrick Gold Corporation | Process for controlling acid in sulfide pressure oxidation processes |
TWI564094B (en) * | 2012-08-22 | 2017-01-01 | 吉田英夫 | Decontamination method and system for soil and the like |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US6471743B1 (en) | Methods for leaching of ores | |
Tripathy et al. | A pyro-hydrometallurgical process for the recovery of alumina from waste aluminium dross | |
CN109112304A (en) | It is a kind of to extract expensive, low-priced, rare element hydrometallurgical process method | |
Ma et al. | Pilot-scale plant study on the innovative nitric acid pressure leaching technology for laterite ores | |
KR101248200B1 (en) | Process for enhanced acid leaching of laterite ores | |
McDonald et al. | Pressure oxidation leaching of chalcopyrite. Part I. Comparison of high and low temperature reaction kinetics and products | |
Kim et al. | Selective recovery of Cr from stainless steel slag by alkaline roasting followed by water leaching | |
Pagnanelli et al. | Leaching of low-grade manganese ores by using nitric acid and glucose: optimization of the operating conditions | |
US20090241731A1 (en) | System and method for extracting base metal values from oxide ores | |
CN101356292A (en) | Combined leaching process | |
EP1880029A1 (en) | An improved process for heap leaching of nickeliferous oxidic ores | |
Huang et al. | pH-Controlled precipitation of cobalt and molybdenum from industrial waste effluents of a cobalt electrodeposition process | |
RU2567414C2 (en) | Method of extraction of metals and metal compounds from produced ore and other sources of metal-bearing raw materials | |
Peng et al. | Recovery of chromium by calcium-roasting, sodium-roasting, acidic leaching, alkaline leaching and sub-molten technology: a review | |
CN101978080A (en) | Process for atmospheric leaching of laterite ores using hypersaline leach solution | |
KR20110055385A (en) | Process for leaching from laterite using impact-grinding effect | |
Hu et al. | A clean metallurgical process for vanadium precipitation from chromium-containing vanadate solution | |
TW528732B (en) | Improved methods for leaching of ores | |
CN105755283B (en) | The method of valuable metal in villaumite Selectively leaching lateritic nickel ore | |
CN105110300A (en) | Method for extracting manganese and sulfur from composite manganese mine containing manganese sulfide | |
CN101864523B (en) | Clean production process for processing low-grade laterite-nickel ore by sodium hydroxide alkali fusion method | |
Jia et al. | Behavior of metals in discard nickel smelter slag upon reacting with sulfuric acid | |
JPS58126937A (en) | Recovery of metal valuable matters from mat | |
Cam et al. | Iron removal from bauxite by oxalic acid and further Al extraction by high-pressure alkali leaching | |
Altansukh et al. | Recovery of nickel and cobalt from a low grade laterite ore |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
GD4A | Issue of patent certificate for granted invention patent | ||
MM4A | Annulment or lapse of patent due to non-payment of fees |