JPS6016367B2 - Wet phosphoric acid manufacturing method - Google Patents
Wet phosphoric acid manufacturing methodInfo
- Publication number
- JPS6016367B2 JPS6016367B2 JP9795880A JP9795880A JPS6016367B2 JP S6016367 B2 JPS6016367 B2 JP S6016367B2 JP 9795880 A JP9795880 A JP 9795880A JP 9795880 A JP9795880 A JP 9795880A JP S6016367 B2 JPS6016367 B2 JP S6016367B2
- Authority
- JP
- Japan
- Prior art keywords
- sulfuric acid
- ore
- concentration
- phosphoric acid
- acid solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Description
【発明の詳細な説明】
本発明は湿式リン酸製造方法に関し、特にリン鉱石中に
不純物として含まれるマグネシウム分を除去して高品質
のリン酸を得る方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a wet method for producing phosphoric acid, and particularly to a method for obtaining high-quality phosphoric acid by removing magnesium contained as an impurity in phosphate rock.
本発明者らは、リン鉱石を硫酸で分解する場合の不純物
の挙動について研究を重ね、リン鉱石を濃度３０％以上
の硫酸溶液で洗浄すると、Ｍｇ、Ｎａ等を選択的に溶出
させることができるという知見を得、先に、こうして得
られた精製鉱石を通常の湿式リン酸製造用原料として用
いて、不純物の少ないリン酸を製造する方法を提案した
（侍開昭５６−母糊び号公報参照）。この方法では必然
的にリン鉱石の洗浄に用いた洗浄排液が生じるが、これ
は硫酸とリン鉱石に由来するＭｇ，Ｎａ等を多く含む。
ところで、本発明者らが測定したリン酸含有硫酸溶液中
へのＭ蚊の溶解度曲線によれば、図面に示すように、マ
グネシウム分は硫酸濃度５０〜７０％の間に溶解度の極
小点を持つ。The present inventors have repeatedly studied the behavior of impurities when phosphate rock is decomposed with sulfuric acid, and found that when phosphate rock is washed with a sulfuric acid solution with a concentration of 30% or more, Mg, Na, etc. can be selectively eluted. Based on this knowledge, we first proposed a method for producing phosphoric acid with few impurities by using the refined ore obtained in this way as a raw material for normal wet-process phosphoric acid production (Samurai Kaisho 56-Monoori No. Publication reference). This method inevitably generates cleaning waste liquid used for cleaning phosphate rock, which contains a large amount of sulfuric acid and Mg, Na, etc. derived from phosphate rock.
By the way, according to the solubility curve of the M mosquito in a sulfuric acid solution containing phosphoric acid measured by the present inventors, as shown in the drawing, the minimum point of solubility of the magnesium component is between 50% and 70% of the sulfuric acid concentration. .
この溶解度曲線は温度２５００、リン酸濃度Ｐ２０５と
して１０％の条件にて測定したものであるが、同一温度
であればリン酸濃度Ｐ２０５として５〜１５％の範囲内
ではたいして変化はない。本発明は、上記のような事象
、すなわち、硫酸溶液中へのＭｇ○の溶解度特性を利用
することにより完成せられたものである。This solubility curve was measured at a temperature of 2500 and a phosphoric acid concentration P205 of 10%, but there is no significant change within the range of 5 to 15% phosphoric acid concentration P205 at the same temperature. The present invention was completed by utilizing the above phenomenon, that is, the solubility characteristics of Mg○ in a sulfuric acid solution.
なお、この明細書において、リン酸濃度ｐ公。換算値に
て示す。また％はすべて重量％である。本発明による温
式ＩＪン酸製造方法は、リン鉱石を濃度３０％〜６０％
の範囲の硫酸溶液で常温ないしその付近で洗浄してリン
分の溶出を極力抑えて鉱石中に不純物として含まれるマ
グネシウム分を選択的に溶出させる工程と、精製鉱石と
洗液を分離する工程と、分離した洗液の硫酸濃度が５０
〜７０％の範囲になるように洗液に濃硫酸を添加して、
硫酸マグネシウムを主体とした沈殿を析出させる工程と
、析出した固形物と硫酸溶液を分離する工程と、分離し
た硫酸溶液を前記精製鉱石の分離用硫酸として用いるか
、あるいは前記リン鉱石洗浄用硫酸として用いる工程と
を含むものである。リン鉱石洗浄用の硫酸溶液の濃度が
３０〜６０％の範囲に限定されかつ硫酸溶液の温度が常
温ないしその付近に限定される理由は、濃度が３０％以
下または６０％以上でありかつ温度が常温ないしその付
近より高い場合には、リン鉱石中のリン分の溶出を抑え
てマグネシウム分を選択的に溶出させることができない
からである。常温ないしその付近とは１０〜２５ｑＣ程
度の温度であり、好ましくは約２０００である。分離し
た洗液の硫酸濃度が５０〜７０％の範囲に限定される理
由は、濃度５０％以下または７０％以上の場合、添付図
面から明らかなように、マグネシウム分の溶解度が大き
すぎてマグネシウムの沈澱物を析出させることができな
いからである。In addition, in this specification, phosphoric acid concentration p public. Shown as converted value. All percentages are by weight. The hot IJ acid production method according to the present invention uses phosphate rock with a concentration of 30% to 60%.
A step in which the ore is washed with a sulfuric acid solution at or around room temperature to minimize the elution of phosphorus and selectively elute the magnesium contained in the ore as an impurity, and a step in which the purified ore and the washing liquid are separated. , the sulfuric acid concentration of the separated washing liquid is 50
Add concentrated sulfuric acid to the washing solution to a range of ~70%,
A step of precipitating a precipitate mainly composed of magnesium sulfate, a step of separating the precipitated solids and a sulfuric acid solution, and using the separated sulfuric acid solution as sulfuric acid for separating the refined ore or as sulfuric acid for cleaning the phosphate ore. The method includes a step of using the method. The reason why the concentration of the sulfuric acid solution for phosphate rock cleaning is limited to a range of 30 to 60% and the temperature of the sulfuric acid solution is limited to room temperature or around it is that the concentration is 30% or less or 60% or more and the temperature is This is because if the temperature is higher than room temperature or around room temperature, it is not possible to suppress the elution of the phosphorus component in the phosphate rock and selectively elute the magnesium component. Room temperature or its vicinity is a temperature of about 10 to 25 qC, preferably about 2000 qC. The reason why the sulfuric acid concentration of the separated washing liquid is limited to a range of 50 to 70% is that when the concentration is less than 50% or more than 70%, the solubility of magnesium is too high, as is clear from the attached drawings. This is because a precipitate cannot be separated out.
つぎに本発明の実施例を挙げる。Next, examples of the present invention will be described.
実施例 ・
５０％硫酸水溶液１２００ｋ９を温度２０００に保持し
、これに表１に示す組成を有するリン鉱石の粉末１００
０ｋ９を加えた。Example - 50% sulfuric acid aqueous solution 1200K9 was maintained at a temperature of 2000C, and phosphate rock powder 100 having the composition shown in Table 1 was added to it.
Added 0k9.
表 １
混合物を１時間境詩芋して鉱石を洗浄し、鉱石中の不純
物を硫酸水溶液中に溶出させた。Table 1 The mixture was boiled for 1 hour to wash the ore, and impurities in the ore were eluted into an aqueous sulfuric acid solution.
生じたスラリーを、プラスチック製炉布を内袋した炉過
器で炉遇し、精製鉱石１０７０ｋ９と洗浄１１３０ｋ９
を得た。これらの組成を表２に示す。− ２
この洗液に斑％硫酸１００３ｋ９を加え、硫酸濃度を６
５％に調整した。The resulting slurry was passed through a furnace lined with plastic furnace cloth, and refined ore 1070k9 and washed 1130k9
I got it. Their compositions are shown in Table 2. -2 Add % sulfuric acid 1003k9 to this washing solution to bring the sulfuric acid concentration to 6.
It was adjusted to 5%.
この液を温度２５つ０にて３時間櫨拝し、析出した沈殿
を炉別した。こうして淀液２０６４ｋｇと析出固形物斑
ｋ９を得た。これらの分析値を表３に示す。表 ３
この炉液を前記精製鉱石の分解用硫酸として用いた。This liquid was stirred at a temperature of 25°C for 3 hours, and the deposited precipitate was filtered out. In this way, 2064 kg of stagnation liquid and precipitated solid matter k9 were obtained. These analytical values are shown in Table 3. Table 3 This furnace liquid was used as sulfuric acid for decomposing the refined ore.
またこの炉液の一部を濃度調整した後、前記リン鉱石洗
浄用硫酸として用いた。なお、上記析出固形物はＭｇＳ
０４をＭｇとして５．２ｋ９（リン鉱石中のＭｇ分の約
５３％に相当）含み、その他ＣａＳ０４、硫酸等を含む
ので、これを系外に取出して水で可溶分を再溶解し、不
溶性のＣａＳ０４を炉別し、過剰の硫酸分をＭ奴によっ
て中和すれば副生品として硫酸マグネシウムを得ること
もできる。Further, after adjusting the concentration of a part of this furnace liquid, it was used as the sulfuric acid for washing the phosphate rock. In addition, the above-mentioned precipitated solid matter is MgS
It contains 5.2k9 (corresponding to about 53% of the Mg content in phosphate rock) as Mg, and also contains CaS04, sulfuric acid, etc., so this is taken out of the system, the soluble content is redissolved with water, and the insoluble content is dissolved. By furnace-separating the CaS04 and neutralizing the excess sulfuric acid with M, magnesium sulfate can be obtained as a by-product.
本発明は以上のとおり構成されているので、リン鉱石に
由釆するマグネシウム分を効率よく除去して高品質のリ
ン酸を製造することができるとともに、洗浄後の硫酸溶
液を有効に再使用することができる。Since the present invention is configured as described above, it is possible to efficiently remove the magnesium content in phosphate rock to produce high-quality phosphoric acid, and it is also possible to effectively reuse the sulfuric acid solution after washing. be able to.
また除去マグネシウムを硫酸マグネシウムに転換して高
価値創生品として得ることもできる。Also, the removed magnesium can be converted into magnesium sulfate to obtain a high value creation product.
図面は硫酸に対するＭｇ０の溶解度曲線である。 The figure shows the solubility curve of Mg0 in sulfuric acid.
Claims (1)
温ないしその付近で洗浄してリン分の溶出を極力加えて
鉱石中に不純物として含まれるマグネシウム分を選択的
に溶出させる工程と、精製鉱石と洗液を分離する工程と
、分離した洗液の硫酸濃度が５０〜７０％の範囲になる
ように洗液に濃硫酸を添加して、硫酸マグネシウムを主
体とした沈殿を析出させる工程と、析出した固形物と硫
酸溶液を分離する工程と、分離した硫酸溶液を前記精製
鉱石の分解用硫酸として用いるか、あるいは前記リン鉱
石洗浄用硫酸として用いる工程とを含む湿式リン酸製造
方法。1. A step of washing phosphate ore with a sulfuric acid solution having a concentration of 30 to 60% at or around room temperature to elute phosphorus as much as possible to selectively elute magnesium contained as an impurity in the ore, and purification. A step of separating the ore from the washing liquid, and a step of adding concentrated sulfuric acid to the washing liquid so that the sulfuric acid concentration of the separated washing liquid is in the range of 50 to 70% to precipitate a precipitate mainly composed of magnesium sulfate. A wet method for producing phosphoric acid, comprising the steps of separating precipitated solid matter and a sulfuric acid solution, and using the separated sulfuric acid solution as sulfuric acid for decomposing the refined ore or as sulfuric acid for cleaning the phosphate ore.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9795880A JPS6016367B2 (en) | 1980-07-16 | 1980-07-16 | Wet phosphoric acid manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9795880A JPS6016367B2 (en) | 1980-07-16 | 1980-07-16 | Wet phosphoric acid manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5722107A JPS5722107A (en) | 1982-02-05 |
| JPS6016367B2 true JPS6016367B2 (en) | 1985-04-25 |
Family
ID=14206170
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9795880A Expired JPS6016367B2 (en) | 1980-07-16 | 1980-07-16 | Wet phosphoric acid manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6016367B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6353759A (en) * | 1986-08-22 | 1988-03-08 | Hitachi Vlsi Eng Corp | Memory device |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61150346U (en) * | 1985-03-08 | 1986-09-17 | ||
| CN103539170B (en) * | 2013-11-06 | 2014-12-10 | 吴杰 | Method for producing magnesium sulfate and industrial-grade monoammonium phosphate by using tail solution from refining of wet process phosphoric acid by solvent extraction method |
-
1980
- 1980-07-16 JP JP9795880A patent/JPS6016367B2/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6353759A (en) * | 1986-08-22 | 1988-03-08 | Hitachi Vlsi Eng Corp | Memory device |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5722107A (en) | 1982-02-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3420622A (en) | Process for obtaining fluorine compounds from digestion solutions of crude phosphates with nitric acid or hydrochloric acid | |
| US4299804A (en) | Removal of magnesium and aluminum impurities from wet process phosphoric acid | |
| CN104058378A (en) | Method for producing monoammonium phosphate and magnesium ammonium phosphate by using wet concentrated phosphoric acid residues | |
| CA1043075A (en) | Processes for the manufacture of feed-grade dicalcium phosphate and phosphoric acid | |
| CN105600763A (en) | Method for producing industrial monoammonium phosphate through fluoride salt purification method | |
| US4088738A (en) | Process for producing phosphoric acid using mixed acid feed and a dicalcium phosphate intermediate | |
| JPS6016367B2 (en) | Wet phosphoric acid manufacturing method | |
| US4556548A (en) | Process for purifying wet-processed phosphoric acid | |
| CN100999312A (en) | Coproduction method of potassium dihydrogen phosphate, sulfur base composite fertilizer and aluminium polychloride | |
| US3563699A (en) | Process for the preparation of very pure cryolite from sodium fluosilicate and ammonia | |
| US3416887A (en) | Method of manufacturing wet process phosphoric acid | |
| US3151938A (en) | Phosphatic materials and methods for the production thereof | |
| US3663168A (en) | Method of producing concentrated phosphoric acid | |
| CN110451513B (en) | Method for preparing large-particle industrial urea phosphate product by wet-process phosphoric acid continuous reaction crystallization | |
| JPS59116111A (en) | Purification of wet process phosphoric acid | |
| CN102869609B (en) | Preparation KNO 3polyhalite IMI method | |
| US20070166217A1 (en) | Method for producing strong base phosphates | |
| US2767046A (en) | Method of solubilizing and recovering | |
| WO2004076348A1 (en) | A process for the manufacture of feed grade dicalcium phosphate | |
| WO2005087661A1 (en) | A cyclic process for the continuous production of dicalcium phosphate | |
| US4005175A (en) | Process for the joint production of sodium tripolyphosphate and titanium dioxide | |
| CN111115595B (en) | Method for purifying raffinate acid | |
| CN109179617B (en) | Phosphorus removing agent and preparation method and use method thereof | |
| DE2208049C3 (en) | Process for the production of phosphoric acid by the wet process with the production of a gypsum suitable for further processing | |
| RU2172358C2 (en) | Method of processing manganese-containing materials |