JPH0254731A - Separation of titanium - Google Patents

Abstract

PURPOSE:To separate and extract Ti ion in a sulfuric acid soln. contg. Ti and other metal ions as the sulfate complex or chloride complex by adding, if necessary, a specified chloride to the sulfuric acid soln. and then then bringing the soln. into contact with an oxygen-contg. org. solvent. CONSTITUTION:The sulfuric acid soln. contg. Ti ion and the ions of other metals is brought into countercurrent contact with an oxygen-contg. org. solvent selected from a group of esters, alcohols, amides, etc., in multiple stages to separate the Ti ion from other metal ions as the sulfate complex which is extracted and separated into the oxygen-contg. org. solvent. Alternatively, the chemical equivalent of at least one kind selected from a group of Na, Mg, K, Ca, and NH4 to the SO4 ion contained in the sulfuric acid soln. is added to the soln. as the chlorides, and the soln. is brought into countercurrent contact with the oxygen-contg. org. solvent to separate and extract the Ti ion into the org. solvent as the chloride complex. The Ti-contg. org. solvent is brought into contact with water to strip the Ti ion as the aq. soln. which is used as the raw material for Ti.

Description

[Detailed description of the invention] (Industrial application field) The present invention relates to a method for separating titanium.

[Prior art and problems to be solved by the invention] As a method for preparing titanium, a dry method is used in which titanium-containing raw materials heated to a high temperature are reacted with 2 gases to form titanium as shown in the following equation. There is a separation method that takes advantage of the high vapor pressure of chloride.

Ti-Fe+6CR2-* FeCl2+ Ti(
42↑FeO-TiO2+ 3G+ 8Cl□→ Fe
Cl2+ TiCL↑ + 3CO↑Produced TiC
L has a high vapor pressure of 760n+n+Hg at 136℃,
The difference in vapor pressure between chlorides of other metals that coexist is the separation factor.

If the content of other metals, such as Fe, in the raw material is large compared to Ti, the amount of Cl2 gas that combines with metals other than Ti will increase, reducing economic efficiency. There are limits to legal separation.

For this reason, when there is a large amount of other metals such as Fe compared to Ti, Ti is converted into slag at high temperatures in an electric furnace or blast furnace, separated from other metals, and then concentrated. Separation using the chlorine method has been adopted, but it has the disadvantage that such a concentration process is not economically viable in areas where electrical energy is high or fossil fuels are expensive.

As a wet separation method, there is a method using a solvent extraction technique. U.S. Pat. No. 3,057,010 discloses a method for selectively extracting Ti ions in a sulfuric acid solution by bringing them into contact with an organic solvent containing alkyl phosphoric acid in order to separate mainly Ti ions and Fe ions contained in the sulfuric acid solution. However, this method has the disadvantage that a large amount of Fe is co-extracted and a large amount of 5N to BN HCI is used to remove it, making it uneconomical.

US Pat. Nos. 3,795,727 and 31,049 SO disclose a method for separating Ti ions and Fe ions contained during chloride dissolution. Both methods extract the chloride complex of dissolved Fe, and the total HCffi in the target aqueous solution is extracted.
The concentration must be high, the extractants used must all have high solubility in aqueous solution, or the Ti
has many drawbacks, such as coexisting with impurity metal ions other than Fe, being unpurified, and requiring a further purification step.

It is used in the production of titanium oxide using the sulfuric acid method as one of the typical methods for separating Ti ions in an aqueous solution.

This method is applicable to cases containing a large amount of titanium, and simply dissolving ilmenite or anatase using concentrated sulfuric acid may result in a high Fe ion content.
After removing ions as iron sulfate crystals and reducing Fe ions as much as possible compared to Ti ions in the solution, K.
This method involves adding water to precipitate Ti ions as hydroxides, but it has the disadvantage that Ti ions cannot be completely removed and 5 to 8 g/l of Ti ions remain in the solution after precipitation.

(Means for Solving the Problem) This problem is solved by a method for extracting a titanium sulfate complex according to the present invention as set forth in claim 1, that is, a titanium sulfate complex containing mainly Ti ions and coexisting with one or more metal ions. A method of separating titanium by extracting Ti ions in the sulfuric acid solution by contacting the sulfuric acid solution K with an organic solvent consisting of one or more selected from the group of oxygen-containing organic solvents, and extracting Ti ions in the sulfuric acid solution. This problem is solved by a titanium separation method characterized by:

In addition, a sulfuric acid solution K mainly containing Ti ions and in which 1 f1 or more of iron-containing metal ions coexist;
After adding at least one Cl ion selected from the group of compounds of H, Na, Mg, Ca, and NH4 and Cl necessary for i ions to form a chloride complex, an oxygen-containing organic solvent is brought into contact. By this, T in the sulfuric acid solution
It is solved by extracting the i ion as a chloride complex.

Further, a sulfuric acid solution K mainly containing Ti ions and in which one or more metal ions including iron coexist, Na and M in chemical equivalents to the S04 ions contained in the sulfuric acid solution.
After adding at least one selected from the group of G, K, Ca, and NH4 in the form of a leaf compound, Ti ions in the solution are brought into contact with an oxygen-containing organic solvent in the form of a chloride complex. Extract. Next, by bringing a sulfuric acid solution containing mainly Ti ions into contact with the organic solvent containing extracted titanium, impurities including co-extracted iron chloride complexes are selectively transferred from the organic phase to the aqueous phase. The problem is solved by a titanium separation method characterized by the following. Unlike the hydrolysis method, which has conventionally been used to separate and purify Ti ions in an aqueous solution, in which water is added to a sulfuric acid solution containing a large amount of Ti ions to precipitate titanium, the present invention can reduce the titanium concentration. It can be used even at extremely low concentrations. Furthermore, Ti ions in the solution are extracted using an organic solvent containing alkyl phosphoric acid, and the co-extracted Fe
This is not a method in which ions are brought into contact with 5N~IiN)I(4) and transferred from an organic phase to an aqueous phase, and furthermore, Ti ions in a chloride solution are not separated by extracting a chloride complex of Fe ions. For example, it is emitted when manufacturing titanium oxide using the sulfuric acid method, which is produced around the world.

Contains a small amount of Ti ions, and also contains Fe, Mn, AM,
Si.

By directly bringing an oxygen-containing organic solvent into contact with a solution containing a large amount of various metal ions such as V, (:r), Ti ions in the solution are extracted as a sulfate complex, and other This method separates metal ions.

In addition, the amount of Cl necessary for Ti ions to form a chloride complex in a sulfuric acid solution containing a large amount of various metal ions along with Ti ions is calculated by calculating the amount of Cl necessary for Ti ions to form a chloride complex by H, Na, Mg, K, Ca, and N.
After adding at least one selected from the group of compounds of H and Cl, Ti ions in the sulfuric acid solution are extracted as a chloride complex by contacting with an oxygen-containing organic solvent and separated from other metals. This method is not limited to the sulfuric acid solution containing the target Ti ions.

(Function) In the present invention, regarding the sulfuric acid solution mainly containing Ti ions, there are no restrictions on the concentration of Ti ions, coexisting metal ions, or free S04 concentration, and any solution can serve as the starting material.

That is, it contains Ti ions and has 1 fi or 2 f! By bringing an oxygen-containing organic solvent into contact with a sulfuric acid solution in which the above coexist, Ti ions in the sulfuric acid solution are separated from other metals by extracting them as a complex into an organic phase, as shown in the following formula, for example. Can be done.

Ti0SO4+Org -Ti0SO4・OrgThe above equation only shows an example of an extraction reaction, and it varies depending on the SO in the aqueous solution, its concentration (see Figure 5), the concentration and type of coexisting metal ions, and the extractant used. It should be understood that the type of incarnation of Ti that is extracted also changes depending on the following.

In addition, sulfuric acid solution K containing Ti ions and coexisting with metal ions of 1 fi or more including iron, T contained in the solution
The amount of CI required for the i ion to form chloride is expressed as H,N
a, Mg, Ca, K or N) After adding at least one selected from the group of compounds of Cl and chlorine,
Ti in the solution is removed by contacting with an oxygen-containing organic solvent.
Extract the ions as chloride complexes.

In addition, a sulfuric acid solution K mainly containing Ti ions and coexisting with one or more metal ions including iron, Na, Mg, and the like in chemical equivalents to the SO4 ions contained in the solution.
At least one selected from the group of K, Ca and NH4
After adding the species in the form of a chlorine-containing compound, by contacting with an oxygen-containing organic solvent, Ti ions are extracted into the organic phase as a chloride complex, as shown in the following equation.

Ti0SO, + 2N)I4CL)-Org→TiO1
2・Org + (NH4)2SO4TiO5O4+
2Kf4+ Org = Ti0CUz ・Org + K2S04Ti
O5O4+ MgCl, +Org -TiOCR, -Org + Mg5O, tTiOS
O4+ CaCl1! , + Org-* Ti0C
L・Org + Ca5L added Na, K
, N) I, , When there are many chlorine compounds with Ca or Mg, various metal ions coexisting with Ti also form a chloride complex.

Fe2 (SO4)3 + 6NaCl+ 20rg
= 2FeCl3・Org+ 3Na2SO4FeSO
4+ 2KCLl+Org 4 Fe (42・Org+ 2S04 Yamata 2 (S0
4) 3 + 6NH4CR+ Org→2AuCl
3+ Org + 3(NH4) Since the extraction and distribution ratio of Fe2'' ion chloride is smaller than that of 2SO4Ti ion, it is preferable to adjust the chloride so that it exists as Fe'' ion.

The FeCl and FeC sentences extracted together with Ti are T
Contacting a sulfuric acid solution containing i ions, or a compound of Na and Cl, a compound of Na and SO4, a compound of Ni and C
M compound, K and SO4 compound, Mg and CI compound, Mg and SO4 compound, N) Cl and Cl compound, N
Impurities other than Tl in the organic phase are selectively back-extracted from the organic phase to the aqueous phase by contacting with an aqueous solution containing one or more selected from the group of compounds of H4 and SO, and compounds of Ti and C9. Therefore, Ti is manufactured in front of the vehicle.

(TiOCl, ・Org + FeCLJrg) +
Ti0SO4-+ TiOCl2-Org+ Ti0
5O4・Org+ FeCls(Ti0CUz・Org
+ FeCUz・Org) + Ti05O4-TiO(
4zJrg+ Ti05O,,・Org+ FeCL(
TiOflJ2zJrg+ Fe(4s・Org)+
Ti0CL-* 2TiOCl2z・Org+ Fe
Cl1゜(TiOCll!2Jrg+ FeCuzJr
g) + Na2SO4 + Ti0(42→ 2TiOC
Also 2・Org+ FeCl2+ Na25O4(TiO
CL ・Org+ZnClzJrg)+ (NH4)2
SO4+ Ti0SO4-+ Ti0C,O2・Org
+ Ti0SO4・Org+ ZnCuz+ (NH4
)2SO4 Titanium chloride complexes and sulfuric acid complexes extracted into oxygen-containing organic solvents can be extracted by replacing the organic solvent with Na5Oa or (NH4
) T by contacting with 2sO4-containing liquid or water.
The i ions, Cl ions, Ti ions, and S04 ions move to the aqueous phase as shown in the following equation, and the organic solvent is regenerated.

Ti0SO4'Org + water → Org + Ti05O4
TiOCR2・Org Jusui = Org + TioCf
fiz There are various methods for recovering titanium, which is an optional step of the present invention, and the product can be freely selected from titanium oxide, titanium hydroxide, and titanium alkoxide, taking into account the application position of the present invention.

Ti0C transferred to the aqueous phase extracted from the oxygen-containing organic solvent
Titanium oxide and TiO5O4 are neutralized with an alkali to obtain a hydroxide, which can be fired to produce titanium oxide.

TiO5O4+2NaOH-”Ti0(OH)z↓+N
a25O4TiOCl2-1-Ca (OH) 2 →
After extracting the sulfuric acid complex or chloride complex of TiO(OH) 2↓+CaC9zTi ions, the aqueous solution contains SO.
Because they often contain large amounts of 4 ions, they cannot be discharged directly into rivers.

Therefore, free HxSOa contained in the raffinate of Ti ions
and after adding at least one selected from the group of chlorine-containing compounds of Na, K, Mg, Ca, and NH4 to the sulfuric acid-containing solution, with respect to the total of SO4 ions combined with Fe ions, The Fe ions in the sulfuric acid solution are Fe
``If it is an ion, add an oxidizing agent or add an electrostatic μ-dialysis method to convert Fe ion to Fe' ion, and then contact it with oxygen-containing organic solvent B to convert it into an aqueous solution. Fe ions are extracted as a chloride complex.

Fe2 (SO4) 3 +6NaC + Org-2
FeC! 13' Org + 3Na2SO4Fe
2(SO4)3 + 6NH4Cl+ Org= 2
FeCl3・Org + 3 (NH4)2S04F
e2(SO4) 3 + 3Mg[:L+ Org-2
FeCl3・Org + 3Mg5O4FeS04
+ 2KGf+ Org ”FeCfh・Org +2s04FeS04 +
CaCl2 + Org-h FFeCl2Jr
+Ca5O*The Fe chloride complex extracted into the organic phase is not limited to the chemical species in the above formula, but varies depending on the amount and type of total H2SO, total)1c4 and coexisting metal ions in the aqueous solution. I hope you understand that.

The oxygen-containing organic solvents A and B used in the present invention are selected from the following group:

(a) Group of esters 1lI RIO-P-OR3RIO-P-R3 0R2QR2 II IfR
IO-P-R3 and R, -P-R3R2R2 In the formula, R1, R2, and R3 represent various alkyl groups and aryl groups, and those having 4 to Cl carbon atoms are used. Moreover, each alkyl group and aryl group are R+ = R2= R
3, those in which R1=R2≠R0, R, ToR, and ≠R3 have different alkyl groups and aryl groups, and those in which they are mixed with alkyl/aryl groups are also used.

(b) Alcohol group Various (n-secondary and tertiary) alcohols having 4 to 18 carbon atoms (c) Amide group R-C-N) I2 R-N-C-CI (
31II ORoo R-N-C-CH2-C-N-R 11l1l R'0 0R" In the formula, R, R', and R" represent an alkyl group and an aryl group, and those having 2 to 18 carbon atoms can be used. .

There are also R=R' or Rf-R' and mixtures of alkyl and aryl groups.

The petroleum hydrocarbon used for diluting the organic solvent in the present invention is an aromatic hydrocarbon, an aliphatic hydrocarbon, or a mixture thereof. Miscellaneous hydrocarbon mixtures such as kerosene are also commonly used.

The compound containing Na and Ci used in the present invention is typified by rock salt (NalQ), and is not limited by purity, and NaCl0 can also be used.

Of course, seawater and industrial waste can also be used.

Compounds containing Ca and Cl, compounds containing Na and SO4,
Compounds containing NH4 and R, compounds of NH4 and SO4, K
Although large amounts of compounds containing chlorine and Cl are discharged as industrial waste, they can be used regardless of their purity.

In the present invention, compounds containing Mg and SOa, and compounds containing Mg and SOa can also be used regardless of their purity.

Embodiments of the present invention will be described in more detail below based on the drawings, but it should be understood that the present invention is not limited thereto.

The flow sheet of FIG. 1 is a diagram showing the basic type of operation of the present invention, in which a sulfuric acid solution A containing mainly Ti ions and in which one or more metals coexist is guided to an extraction step, where an oxygen-containing organic solvent One or two types selected from the group f41! By contacting with the organic solvent (1) consisting of the above, Ti ions in the sulfuric acid solution are extracted as a sulfate complex and separated from other coexisting metals. The titanium sulfuric acid complex transferred to the organic phase is extracted with NaSO3 or (NH4) in back extraction step C.
By contacting with a 2SO4-containing liquid or water (1), Ti ions and S04 ions in the organic phase are back-extracted into the aqueous solution, and the oxygen-containing organic solvent (2) is regenerated.

Titanium hydroxide can be produced by diluting or adding an alkali to the solution containing back-extracted Ti ions and S04 ions.

The flow sheet of FIG. 2 is basically the same as that of FIG. 1, except that the extracted species of Ti ions is extracted with a chloride complex. A sulfuric acid-containing solution A containing mainly Ti ions and coexisting with one or more metal ions including Fe ions is led to a chlorination step, and the Ti ions contained in the sulfuric acid solution are necessary to form a chloride complex. The amount of Cl, H, Na, K
.

One or two selected from the group of Mg, Ca and NH.
After adding at least one species in the form of a chlorine-containing compound (2), in the extraction step, the Ti ions in the sulfuric acid solution are extracted into the organic solvent (2) as a chloride complex by contacting with an oxygen-containing organic solvent (2). , separate from other coexisting metal ions. Next, organic solvent ① is led to washing step F, where Ti05O4
Sulfuric acid solution containing or Na and ci, Na and SO4, old (4 and Cl1, NH4 and S04, Mg and Cl, Mg
and SO4, N1 (4 and Cl, NH4 and S04 and Ti0
Water containing one or more selected from the group of CUz?
By contacting with &■, impurity ions other than Ti ions and SO4 ions or Ti ions and Cl ions are selectively back-extracted from the organic solvent ■ into an aqueous solution, and then brought into contact with water ■ in back extraction step B. This is a titanium separation method in which Ti ions are back-extracted into an aqueous phase to obtain a back-extraction liquid containing Ti ions and saliva ions, and an organic solvent is regenerated.

The flow sheet of FIG. 3 is basically the same as that of FIG. The sulfuric acid complex of Ti extracted into the organic solvent is brought into contact with water (2), and the Ti ions obtained by back extraction to the aqueous phase are transferred to S04.
A solution containing ions? r! A portion where Ti is recovered as hydroxide G by adding alkali or water to i and D was included. The difference also includes the method of neutralizing the Ti ion extraction residue (sulfuric acid solution containing mainly Fe ions).

That is, the Ti ion raffinate is led to the chlorination and oxidation step H,
The free SO4 ions contained in the raffinate are combined with Fe to form equivalent chemical equivalents of Na and NO to the sample of SO4 ions.
After adding at least one fffi selected from the group of chlorine compounds of 4, K, Ca and Mg, the mixture is led to a step J of extracting the chloride complex of Fe, and is brought into contact with an oxygen-containing organic solvent (2). Neutralized liquid N is obtained by extracting Fe ions in the sulfuric acid solution as a chloride complex.

On the other hand, the Fe ions and Cl ions extracted from the organic phase are brought into contact with water (1) in a back extraction step, and are back extracted into an aqueous solution to obtain an iron chloride-containing solution M, while the organic solvent (2) is regenerated. In the chlorination and oxidation step H, NO3 such as HNO3, NH4NO3, 11aNO3, etc. is used as a softening agent.
If a substance containing F is used in the extraction step J,
In addition to e-ions and Cl-ions, HNO3 is also extracted. H
I am co-extracting NO3! ll solvent is )lNO3
In the cleaning step K for selectively removing Na, Cl, Mg
By contacting with an aqueous solution containing one or more selected from the group of compounds of ci, K, NH4, CM, and Fe and Cl, HNO3 in the organic phase is transferred to the aqueous solution and recovered. .

The aqueous solution containing HNO, is recycled to the chlorination and oxidation steps to remove the contained substances, such as Na(4 and HNO3).
is reused.

The flow sheet of FIG. 4 is basically the same as that of FIG. Impurities may remain in the organic solvent that exits Step C of back-extracting the Ti chloride complex. For example, Sin,'-
There are ions, etc. Optional step P to remove these impurities and step Q to solidify and remove the impurities back-extracted into the aqueous solution.
The only difference is in the parts including. The optional neutralization treatment of the raffinate obtained by extracting Ti is the same as that shown in FIG. 3.

The flow sheet in Figure 4 shows that the amounts of Na, K, Mg, Cu, and NH4 compounds with chlorine added during the chlorination step greatly exceeded the amount necessary to form a Ti chloride complex. The flow sheet shown in FIG. 4 does not change even when it is added.

〔Example〕

The present invention will be explained below with reference to Examples.

Example (1) The following synthetic solution was prepared and an extraction test for a Ti sulfuric acid complex was conducted.

Table 1 Extraction stock solution of Ti05O4 Unit: g/l For the extraction experiment, a separatory funnel was used and a continuous contact test was conducted.

TOPO (tri-octyl phosphine oxide) dissolved in kerosene was used. The results obtained are shown in Table 2.

Number of extraction stages 4 stages countercurrent contact C = Q, 5/1.0 Contact time 5 minutes Table 2 Raffinate Unit g/lTi extraction distribution ratio was 2.0 or more, which confirmed that the extraction was extremely good. Ta. Further, an extraction test was conducted by diluting the stock solution shown in Table 1 twice, and the same extraction distribution ratio was obtained.

It was also confirmed that when the number of carbon atoms in the alkyl group of the extractant changed from 4.5° to 6.8, the extraction and distribution ratio of various coexisting metal ions changed.

The back extraction test was conducted using water under the following conditions. The results are shown in Table 3. Note that this is a value obtained by dissolving precipitated Ti after back extraction.

The same extraction conditions were used. The results are shown in Table 4.

As seen above, all but K and St ions were almost completely back-extracted. Regarding residual St ions, after TL back-extraction, N
a OHXN a 2 CO3, NH4F, (NH4
)2SO4, NI(4)+(:03 and Na, So
It was confirmed that it could be completely removed by contacting with the liquid containing No. 4.

Example (2) After adding NaCl to the stock solution in Table 1, an extraction test was performed. The extraction conditions were the same as the previous extraction, followed by washing and removing Fe ions and Zu ions co-extracted with Ti ions. Tested.

Cleaning liquid: H2SO4200g/λ Ti 4.1g/u
The containing liquid was used.

The washing conditions are as follows.

Use the organic solvents listed in Table 4.

0/A = 571 Countercurrent 6-stage contact Contact time 5 minutes Temperature constant 45°C The results are shown in Table 5.

Table 5 Impurity cleaning test unit g/fL TiOCj! 2. Back Extraction Test Using the organic solvents shown in Table 5, a back extraction test was conducted for the extracted Ti chloride complex.

All conditions for back extraction were the same as those for back extraction of Ti sulfate. The results are shown in Table 6.

Extraction of Fe chloride complex The concentration was adjusted by adding equivalent chemical equivalents of NaCf1 and iron powder to the SO4 ions contained in the raffinate in Table 4, and HNO3 was used as the oxidizing agent for Fe ions. Pre-extraction solutions shown in Table 7 were prepared and tested.

The organic solvent used was an alkyl phosphine oxide (a mixture of alkyl groups having 4.6 and 8 carbon atoms) diluted with an aromatic hydrocarbon. The extraction conditions are as follows.

0/A=2.0/1.0 8-stage countercurrent contact contact time 5
Temperature per minute: 25°C to 40°C 100g/liter of Sl remaining in the organic phase
(N)+4) After contacting once with a solution containing 40 g/It of 2CO3 at a ratio of 0/A-1/1, the organic phase was analyzed and the residual St was found to have decreased to 0.3 g/J2.

As shown in Table 7, the raffinate has been largely neutralized.
When cooled to 30° C. or lower, Na25o4·l0H20 precipitated.

HNO3 scrubbing test The organic solvents shown in Table 7 were used, and the cleaning solution was FeCl3.
An aqueous solution containing NaCf and NaCf was used.

The scrubbing conditions are as follows.

0/A = 8/1 6 Countercurrent contact Contact time 5 minutes Temperature 25-30°C The results are shown in Table 8.

As can be seen by comparing the organic phases in Tables 7 and 8, K and HNO3, which had been co-extracted into the organic phase, were completely back-extracted into the aqueous solution.

The organic solvent containing only Fe ions and Cl ions was easily back-extracted to the aqueous solution side by contacting with water.

[Brief explanation of the drawing]

FIG. 1 is a flow sheet showing the basic method of the operation of the present invention, and FIG. 2 is a flow sheet showing the basic method for extracting contained titanium as a chloride complex. Figure 3 is exactly the same as Figure 1, but includes neutralization treatment after removing Ti ions, and Figure 4 is the same as Figure 2.
Although it is exactly the same as the figure, it incorporates the removal of impurity ions remaining in the organic solvent after the back extraction of Ti ions, and the neutralization of the Ti ion raffinate is the same as in Figure 3. be. FIG. 5 is a graph showing the relationship between H2SO4 concentration and TiSO4 extraction amount. B...Ti sulfuric acid complex or chloride complex extraction process C...Ti back extraction process E...Ti chlorination process F...Cleaning process for impurities extracted together with Ti ions G... Hydroxide of Ti H...Chlorination and oxidation process of Fe J...Chloride complex extraction process of Fe K...Washing process of INO (extracted with Fe ions)...Reverse extraction of Fe Step ■...Oxygen-containing organic solvent B ■...Alkali or diluting water ■...Water N...Fe raffinate solution (neutralized liquid) P...Removal of impurities co-extracted with Ti Process Q...
Impurity filtration step R... Impurity ■... Oxygen-containing organic solvent A ■... NaSO3 or (NH4) 2SO4-containing liquid or wood base 4 compound groups Na, Mg, K, NH4 and Ti
Figure 1 and Figure 2

Claims (1)

[Scope of Claims] 1. An organic solvent consisting of one or more selected from the group of oxygen-containing organic solvents is added to a sulfuric acid solution containing mainly Ti ions and in which one or more metal ions coexist. A method for separating titanium, characterized in that Ti ions in the sulfuric acid solution are extracted as a sulfate complex by contacting with a solvent. 2. A sulfuric acid solution that mainly contains Ti ions and in which one or more metal ions including iron coexists is added to a solution containing Ti in the solution.
The amount of Cl required for the ions to form a chloride complex is expressed as H,
After adding at least one selected from the group of compounds containing Na, Mg, K, Ca, and NH_4 and chlorine, T in the sulfuric acid solution is removed by contacting with an oxygen-containing organic solvent.
A titanium separation method characterized by extracting i-ions as a chloride complex. 3. Adding chemical equivalents of Na, Mg,
At least one selected from the group of K, Ca and NH_4
After adding the species in the form of a compound of Cl, the Ti ions in the sulfuric acid solution are extracted in the form of chloride complexes by contacting with an oxygen-containing organic solvent, and then the titanium is extracted and mainly added to the containing organic solvent. A titanium separation method characterized in that co-extracted impurities such as iron chloride complexes are selectively transferred from an organic phase to an aqueous phase by contacting with a sulfuric acid solution containing Ti ions. 4. A sulfuric acid solution containing mainly Ti ions and coexisting with one or more types of metal ions including iron is
The amount of Cl required for the ions to form a chloride complex is expressed as H
, Na, Mg, K, Ca, and NH_4, and then contact with oxygen-containing organic solvent A to transform Ti in the sulfuric acid solution into a chloride complex. A step of extracting Ti as
Organic solvent A containing ions and Cl ions is converted into NaSO_
4 or (NH_4)_2SO_4 content or a first step of back-extracting Ti and Cl ions in the organic phase into the aqueous phase and regenerating the organic solvent A by contacting with water;
In the raffinate of the process, a compound containing chlorine of Na, K, Mg, Ca and NH_4 in a chemical equivalent amount to the sum of free SO_4 ions and SO_4 ions bound to iron contained in the raffinate is added. After adding at least one selected from the group, extracting Fe ions in the aqueous solution as a chloride complex by contacting with an oxygen-containing organic solvent B, and then an organic solvent containing Fe ions and Cl ions. A method for separating titanium, comprising a second step of bringing B into contact with water to back-extract Fe ions and Cl ions in the organic phase into an aqueous phase and regenerating the organic solvent B. 5 In order to selectively remove impurities extracted together with titanium chloride complexes or sulfate complexes, Na and Cl compounds, Na and SO_4 compounds, Mg and Cl compounds, Mg
and SO_4 compound, K and Cl compound, K and SO_4
compound, NH_4 and Cl compound, NH_4 and SO_
Impurities other than Ti ions and Cl ions in the organic solvent are selectively transferred to the aqueous phase by contacting with an aqueous solution containing one or more selected from the group of compounds of 4 and Ti and Cl compounds. 4. The method for separating titanium according to claim 1, comprising back extraction. 6. The method for separating titanium according to claim 2, wherein the compound of Na and Cl to be added is rock salt.