First, the determination of acid hydrolysis rate
Iron titanium ore by sulfuric acid decomposition after adding water leaching, where most of the transferee titanium solution be soluble titanium salts, and a small portion is not decomposed titanium sulfate is left in the residue. The percentage of soluble titanium in the total titanium of ilmenite is the acid hydrolysis rate. Therefore, to determine the acid hydrolysis rate, it is necessary to measure soluble titanium and insoluble titanium.
1. Determination of soluble titanium Sampling must be a turbid liquid with a uniform solid-liquid distribution representing the whole pot of leachate under agitation. When the test solution was uniformly stirred, 25 mL was weighed, filtered under reduced pressure, and the measuring cylinder and the funnel were washed with 10% sulfuric acid and the filter residue was washed until the washing liquid was added with 3% H 2 0 2 to test no color development. The filter residue was left for analysis in the next step. The filtrate was transferred to a 200 mL volumetric flask, diluted to the mark with water, and shaken to a titanium solution B for use.
Titanium was injected suction B20mL 500mL Erlenmeyer flask, add 20% 20mL sulfuric acid, 30mL of concentrated hydrochloric acid, aluminum sheets 2g, fitted with sealing pipe, plug plugged, the addition of saturated sodium bicarbonate solution in the liquid seal tube To about 2/3 of the volume of the vessel, heat it with a small fire in an electric furnace. Remove the heat source when it is vigorous. When the reaction is slow, continue to heat. Remove all the hydrogen from the solution. When the solution is clear, leave the heat source and cool it with running water. At room temperature, be sure to add saturated sodium bicarbonate solution at any time during the cooling process. After cooling, remove the liquid sealing tube, quickly pour some saturated sodium bicarbonate solution, and immediately titrate to 0. lmol/L ammonium sulphate standard solution to near colorless, add 40% ammonium thiocyanate indicator 2mL, continue Titrate to light brown for the end point.
2. Determination of insoluble titanium The filter residue and filter paper filtered by the above acid decomposing liquid are transferred together in a porcelain crucible, dried and ashed, and then cooled, and 6 g of potassium pyrosulfate is melted in a muffle furnace until it is transparent, and then immersed in cooling. In a beaker containing 80 mL of 10% sulfuric acid, slowly heating on an electric furnace until the melt is completely dissolved, remove the crucible, wash with water, transfer the solution to a 500 mL Erlenmeyer flask, add 25 mL of concentrated hydrochloric acid, and 1 g of aluminum sheet. Same as the above determination of titanium liquid B.
V o ---- draw the filtrate volume (pipette ml), mL;
c[NH 4 Fe(SO 4 ) 2 ]----the concentration of the substance of ferric ammonium sulfate, mol/L (may not be determined);
V 1 ---- titration filtrate consumption volume of ammonium ferric sulfate solution, ML;
V 2 ---- titration of filter residue consumption volume of ammonium ferric sulfate solution, mL;
The molar mass of 0.0799 titanium dioxide, kg / mol.
2. Determination of the content of titanium dioxide in titanium liquid
Pipette 10 mL of clarified titanium solution, transfer to a l00m1 volumetric flask, dilute to the mark with water, shake well, pipette 10 mL of the diluted solution, transfer to a 500 mL Erlenmeyer flask, add 20 mL of 20% sulfuric acid, 30 mL of concentrated hydrochloric acid, 2 g of aluminum flakes, the following steps were the same as the determination of Titanium B.
Wherein ÏTiO 2 - titanium dioxide mass concentration, g / L;
C[NH 4 Fe(S0 4 ) 2 ]----molar concentration of ammonium ferric sulfate solution, mol / L;
V----volume the volume of ammonium ferric sulfate solution, mL;
V 1 ---- volumetric flask volume, mL;
V 2 ---- take the volume of the diluted test solution, mL;
V 3 ---- take the volume of the original concentrated solution, mL;
0. 0799---- molar mass of titanium dioxide, kg / mol. [next]
3. Determination of the content of titanium dioxide in seed crystals (ortho-titanate)
The water-washed ortho-titanic acid is beaten and stirred evenly, and sampled under stirring. The slurry of about 0.5 g is accurately weighed in a 500 mL Erlenmeyer flask, 30 mL of concentrated hydrochloric acid is added, and the mixture is heated and dissolved until it is transparent. After cooling, 30 mL is added. % sulfuric acid, 1 g aluminum flakes, the following steps are the same as the determination of titanium liquid B.
c[NH 4 Fe(S04) 2 ]----the concentration of the substance of the ammonium ferric sulfate standard solution, mol / L;
V—volume the volume of the standard solution of ammonium ferric sulfate, mL;
M—the mass of the sample, g;
The molar mass of 0.0799 titanium dioxide, kg / mol.
Determination of Titanium Dioxide Content in Seed Solvents and Waste Acids
Under stirring, 5 mL of the seed sol was taken up, placed in a 500 mL Erlenmeyer flask, dissolved in 25 mL of 20% sulfuric acid, and then concentrated with 30 mL of hydrochloric acid and 2 g of aluminum sheet. The following procedure was the same as that of Titanium B.
Wherein ÏTiO 2 - titanium dioxide mass concentration, g / L;
c[NH 4 Fe(S0 4 ) 2 ]----the concentration of the substance of the ammonium ferric sulfate solution, mol / L;
V—volume the volume of the ammonium ferric sulfate solution, mL;
V1—take the sample volume, mL;
The molar mass of 0.0799 titanium dioxide, kg / mol.
Determination of titanium dioxide content in spent acid (hydrolysis mother liquor):
After the titanium liquid was hydrolyzed, it was filtered, and the filtrate (depleted acid) was placed in a 500 mL Erlenmeyer flask, 30 mL of concentrated hydrochloric acid was added, and the aluminum piece was 1.5 g. The following steps were the same as those of the titanium liquid B.
The determination of the total titanium content in the same seed solution was calculated.
5. Determination of ferrous sulfate content in titanium liquid
Titanium content measurement principle of ferrous sulfate solution as follows: a sample of ferrous sulfate in sulfuric acid medium, at a standard potassium permanganate titration, when ferrous sulfate is oxidized to all high-speed, high manganese excess of 1 drop The potassium acid solution makes the solution pale pink, which is the end point. Its reaction formula is as follows:
5Fe 2+ +MnO 4- +8H + ===5Fe 3+ +Mn 2+ +4H 2 O
Since the presence of trivalent titanium in the titanium liquid also consumes the potassium permanganate solution, the trivalent titanium should be deducted.
Pipette 10 mL of titanium solution into a 100 mL volumetric flask, dilute to the mark while shaking, and shake well.
Take 10 mL of the above test solution in a 250 mL Erlenmeyer flask, add 20 mL of 20% sulfuric acid, add [next]
V----the volume of potassium permanganate standard solution, mL;
c[(NH 4 ) 2 Fe(S0 4 ) 2 ]----the concentration of the substance of the ammonium ferric sulfate standard solution used for titrating the trivalent titanium, mol / L;
V 1 ---- titration of the volume of ammonium ferric sulfate solution consumed by trivalent titanium in the test solution, mL;
V 2 ---- volumetric flask volume, mL;
V 3 ---- take the volume of the diluted test solution, mL;
V 4 ---- take the volume of the original concentrated solution, mL;
The molar mass of 0.15185 ferrous sulfate, kg/mol.
Determination of the purity of ferrous sulfate (FeS0 4 ·7H 2 0)
Lmol/L Permanganic acid is dissolved in a 300 mL Erlenmeyer flask, and 50 mL of 5% sulfuric acid solution is added to dissolve it.
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