CN102515261A - Method for preparing grade-adjustable potassium fluotitanate through using high-silicon-titanium iron ore - Google Patents
Method for preparing grade-adjustable potassium fluotitanate through using high-silicon-titanium iron ore Download PDFInfo
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Abstract
The invention which belongs to a metallurgical technology concretely provides a method for preparing grade-adjustable potassium fluotitanate through using high-silicon-titanium iron ore. The method comprises three steps of leaching, silicon removal and potassium fluotitanate synthesis. According to the method, the iron ore with high contents of silicon and titanium is directly used as a raw material, the raw material can be directly used for production without preprocessing, and hydrofluoric acid can be directly used without refining; the impurity silicon is processed into high purity potassium fluosilicate, and potassium fluosilicate can be sold in the market and causes no wastes; and additionally, the potassium fluotitanate prepared through the method of the invention, which has the characteristics of adjustable grade and production cost saving, can satisfy demands of different clients.
Description
Technical field
The invention belongs to metallurgical technology, a kind of method for preparing the regulatable potassium fluotitanate of grade with the ferro-silico-titanium ore deposit specifically is provided.
Background technology
At present; Producing potassium fluotitanate raw materials used is ilmenite and hydrofluoric acid mostly; The topmost index of potassium fluotitanate is exactly the grade of potassium fluotitanate and the content of impurity silicon, and is therefore just very important as the index of the ilmenite of raw material and hydrofluoric acid, especially the silicone content in ilmenite and the hydrofluoric acid.The ilmenite of existing process using requires siliceously to be lower than 0.8%, and hydrofluoric acid need be made with extra care, and being that hydrofluoric acid is siliceous is lower than 0.5%, even has enterprise to require that hydrofluoric acid is siliceous to be lower than 0.3%, leach liquor direct production potassium fluotitanate.In view of existing potassium fluotitanate production technique desired raw material requires height, cause a large amount of siliceous high ilmenites can't be applied to produce high-purity potassium fluotitanate, waste is serious.In addition, the silicon in the existing raw material generally is to remove as impurity, it is not used, and also causes bigger waste.
In addition, potassium fluotitanate following grade arranged, different clients has different requirement to the grade of potassium fluotitanate, (National Standard GB/T22668-2008 " in, grade is divided into pet-1, pet-2), sees table 1.
Two kinds of grades of table 1 potassium titanate
But because the content of silicon has direct relation in the grade of potassium fluotitanate and production technique and the raw material, the potassium fluotitanate of every kind of grade all need be handled raw material and produce separately, and cost is high.
In view of the deficiency of above prior art, the method for developing a kind of new potassium fluotitanate has crucial meaning.
Summary of the invention
Weak point to prior art; The invention provides and a kind ofly prepare the method for the regulatable potassium fluotitanate of grade with the ferro-silico-titanium ore deposit, this method can use the high iron ore of silicon titanium content directly as raw material, and raw material does not need pre-treatment directly to be used for producing; Hydrofluoric acid need not made with extra care yet, and directly uses; And silicon impurity is treated to highly purified potassium silicofluoride, and potassium silicofluoride can be used for market sale, does not cause waste; In addition, prepare potassium fluotitanate through method of the present invention, the grade of potassium fluotitanate can be regulated and control, and saves production cost, and satisfies different clients' demand.
For realizing above-mentioned purpose, technical scheme of the present invention is:
A kind ofly preparing the method for the regulatable potassium fluotitanate of grade with the ferro-silico-titanium ore deposit, is raw material with ilmenite and hydrofluoric acid, and the mass content of selecting silicon for use is 2%～3.5% ilmenite; Selecting mass concentration for use is 40%～45% hydrofluoric acid, and the mass content of silicon is 0.7%～1.2% in the hydrofluoric acid;
Concrete preparation process comprises the steps:
(1) leaches: above-mentioned ilmenite is joined in the above-mentioned hydrofluoric acid leach; The mole dosage of hydrofluoric acid be titanium and silicon total mole number in the ilmenite 1.08-1.12 doubly, reaction 0.5h-1.5h leaves standstill 2h～4h; Feed rate 0.4t/h～0.6t/h filters and obtains leach liquor; Moisturizing in the leaching process, rate of water make-up are separated out with the unsaturated crystallization of titanium in the leach liquor and are as the criterion, and control leach liquor content of titanium dioxide is 155g/L～170g/L;
(2) silica removal: analyze the silicone content of above-mentioned leach liquor,, add saturated Klorvess Liquid according to the silicone content of leach liquor; Wherein the mol ratio of silicon is 1.45-1.65 in Repone K and the leach liquor, and the reinforced time 1.5h～2.5h of control reacts 1h～2h then; Leave standstill 2h～4h after-filtration; Be purified liquid, filter residue is a potassium silicofluoride, and the mass content of potassium silicofluoride is 98.5%-99.0%;
(3) synthetic potassium fluotitanate: the 1.18-1.22 according to the mole number of titanium in the scavenging solution extraordinarily goes into saturated Klorvess Liquid; The reinforced time 1.5h～2.5h of control; 50 ℃-60 ℃ of temperature of reaction, reaction 1h～2h leaves standstill 3h～4h after-filtration; Through obtaining the potassium fluotitanate product after washing, the oven dry, the grade of potassium fluotitanate product is controlled according to the content of silicon in control (2) the step silica removal after liquid.
During said step (1) leached: the mole dosage of hydrofluoric acid was titanium and silicon total mole number 1.1 times in the ilmenite, reacts 1h, leaves standstill 2h, feed rate 0.6t/h.
In said step (2) silica removal: the mol ratio of silicon is 1.6 in Repone K and the leach liquor, the reinforced time 2h of control, and reaction 1h leaves standstill 2h.
In the synthetic potassium fluotitanate process of said step (3): extraordinarily go into saturated Klorvess Liquid according to 1.2 of the mole number of titanium in the scavenging solution, the reinforced time 2h of control, 55 ℃ of temperature of reaction, reaction 1h leaves standstill 3h.
Do further explanation and explanation in the face of the present invention down:
Step of the present invention (1) leaching process very exothermic elevates the temperature, and needs suitable moisturizing to ensure that the unsaturated crystallization of titanium is separated out in the leach liquor, analyzes titanium, the silicone content of leach liquor, control leach liquor content of titanium dioxide 155～170g/L.
In step of the present invention (2) the silica removal process, the content that can regulate silicon in the silica removal after liquid is controlled the grade of the finished product.The principle of silica removal process is; The solubility product of potassium silicofluoride is littler than potassium fluotitanate, utilizes chemical kinetics, and control adds time, the amount of Repone K; Potassium silicofluoride is precipitated than potassium fluotitanate more easily separates out; And the potassium silicofluoride titaniferous that is settled out is very low, thereby realizes separating of silicon and titanium, reaches the purpose that purifies silica removal.
Compared with prior art, advantage of the present invention is:
1) adaptability to raw material is strong, and the ilmenite that can adopt high silicon is the high-quality potassium fluotitanate of raw material production, reduce the waste of raw material, and potassium fluotitanate purity can reach more than 99.5%.
2) white residue that removes of silica removal process output is a potassium silicofluoride, and purity also reaches more than 98.5%, can be used as sub product and sells outward, has eliminated output solid slag contaminate environment.
3) grade of product potassium fluotitanate can be regulated and control as required, and regulation process is simple, can satisfy different clients' demand.
4) the preparation process of potassium fluotitanate of the present invention is simple, and is not high to ingredient requirement, simple to operate easy to control.
Description of drawings:
Fig. 1 is the concrete process flow sheet for preparing the method for the regulatable potassium fluotitanate of grade with the ferro-silico-titanium ore deposit of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention to be done further explanation and explanation, but the invention is not restricted to the scope of embodiment, percentage composition described in the embodiment all refers to the quality percentage composition.
1, preparation process is following:
(1) leach: ilmenite is joined in the hydrofluoric acid leaches, the mole dosage of hydrofluoric acid be titanium and silicon total mole number in the ilmenite 1.08-1.12 doubly, reaction 0.5h-1.5h leaves standstill 2h～4h, feed rate 0.4t/h～0.6t/h, filtration obtains leach liquor; Moisturizing in the leaching process, rate of water make-up are separated out with the unsaturated crystallization of titanium in the leach liquor and are as the criterion, and control leach liquor content of titanium dioxide is 155g/L～170g/L;
(2) silica removal: analyze the silicone content of above-mentioned leach liquor,, add saturated Klorvess Liquid according to the silicone content of leach liquor; Wherein the mol ratio of silicon is 1.45-1.65 in Repone K and the leach liquor, and the reinforced time 1.5h～2.5h of control reacts 1h～2h then; Leave standstill 2h～4h after-filtration; Be purified liquid, filter residue is a potassium silicofluoride, and the mass content of potassium silicofluoride is 98.5%-99.0%;
(3) synthetic potassium fluotitanate: the 1.18-1.22 according to the mole number of titanium in the scavenging solution extraordinarily goes into saturated Klorvess Liquid; The reinforced time 1.5h～2.5h of control; 50 ℃-60 ℃ of temperature of reaction, reaction 1h～2h leaves standstill 3h～4h after-filtration; Through obtaining the potassium fluotitanate product after washing, the oven dry, the grade of potassium fluotitanate product is controlled according to the content of silicon in control (2) the step silica removal after liquid.
2, the concrete control condition that leaches is following:
(1) leach: the 15.t ilmenite, contain titanium oxide 50%, siliceous 2.3%, 2.5h adds;
Hydrofluoric acid: 40%, 2.8m
3, (being 1.1 times of mole number of silicon);
Water: 1.4m
3
Reaction 1h leaves standstill 2h, filters
1. leach liquor 4.5m
3, contain titanium oxide 167.3g/L, silicon-dioxide 9.32g/L.
(2) leach: the 15.t ilmenite, contain titanium oxide 50%, siliceous 2.3%, 2.5h adds;
Hydrofluoric acid: 40%, 2.75m3, (being 1.08 times of mole number of silicon);
Water: 1.3m
3
Reaction 1h leaves standstill 2h, filters
2. leach liquor 4.3m
3, contain titanium oxide 174.4g/L, silica 1 0.43g/L.
(3) leach: the 15.t ilmenite, contain titanium oxide 50%, siliceous 2.3%, 2.5h adds
Hydrofluoric acid: 40%, 2.85m
3, (being 1.12 times of mole number of silicon)
Water: 1.5m
3
Reaction 1h leaves standstill 2h, filters
3. leach liquor 4.6m
3, contain titanium oxide 164.3g/L, silicon-dioxide 8.87g/L.
(4) leach: the 15.t ilmenite, contain titanium oxide 50%, siliceous 2.3%, 2.5h adds
Hydrofluoric acid: 40%, 2.8m
3, (being 1.1 times of mole number of silicon)
Water: 1.5m
3
Reaction 1h leaves standstill 2h, filters
4. leach liquor 4.5m3 contains titanium oxide 168.5g/L, silicon-dioxide 9.41g/L.
For the stability of production batch, will be 1. 2. 3. 4. leach liquor be added to a container for storing liquid, leave standstill 24h after, get the liquid analysis and contain titanium oxide 169.45g/L, silicon-dioxide 9.63g/L.
3, produce first grade:
Embodiment 1:
Purify silica removal: with 3m
3The mixing leach liquor in add the Klorvess Liquid 0.44m3 (theoretical value 1.6 times) of concentration 259g/L, joining day 1.8h leaves standstill 3h, filters;
Output: scavenging solution 3.52m
3, contain titanium oxide 141.21g/L, contain silica 1 .12g/L,
Potassium silicofluoride: 92.03kg, purity 98.7%;
Crystallization: this scavenging solution 3.52m
3The Klorvess Liquid 4.35m that adds concentration 259g/L
3(theoretical value 1.2 times), joining day 2h leaves standstill 3h, filters;
Output: potassium fluotitanate: 1441kg, purity 99.7%, dioxide-containing silica 0.101% (Si0.05%).
Embodiment 2:
Purify silica removal: with 3m
3The mixing leach liquor in add the Klorvess Liquid 0.45m of concentration 259g/L
3(theoretical value 1.65 times), joining day 1.9h leaves standstill 2.83h, filters,
Output: scavenging solution 3.56m
3, contain titanium oxide 140.79g/L, contain silicon-dioxide 0.88g/L, potassium silicofluoride: 93.44kg, purity 99.0%;
Crystallization: this scavenging solution 3.56m
3The Klorvess Liquid 4.25m that adds concentration 259g/L
3(theoretical value 1.18 times), joining day 2.2h leaves standstill 3.5h, filters;
Output: potassium fluotitanate: 1438.85kg, purity 99.8%, dioxide-containing silica 0.09% (Si0.042%).
4, produce seconds:
Embodiment 3:
Purify silica removal: with 3m
3The mixing leach liquor in add the Klorvess Liquid 0.39m of concentration 259g/L
3(theoretical value 1.4 times), joining day 1.6h leaves standstill 3h, filters,
Output: scavenging solution 3.44m
3, contain titanium oxide 146.81g/L, contain silica 1 .82g/L, potassium silicofluoride: 84.08kg, purity 98.6%;
Crystallization: this scavenging solution 3.44m
3The Klorvess Liquid 4.35m that adds concentration 259g/L
3(theoretical value 1.2 times), joining day 2.1h leaves standstill 3h, filters;
Output: potassium fluotitanate: 1466.44kg, purity 98.6%, dioxide-containing silica 0.42% (Si0.20%).
Embodiment 4:
Purify silica removal: with 3m
3The mixing leach liquor in add the Klorvess Liquid 0.42m of concentration 259g/L
3(theoretical value 1.5 times), joining day 1.8h leaves standstill 3h, filters,
Output: scavenging solution 3.5m
3, contain titanium oxide 144.25g/L, contain silica 1 .42g/L, potassium silicofluoride: 88.93kg, purity 98.9%;
Crystallization: this scavenging solution 3.5m
3The Klorvess Liquid 4.28m that adds concentration 259g/L
3(theoretical value 1.18 times), joining day 2.2h leaves standstill 3h, filters;
Output: potassium fluotitanate: 1464.05kg, purity 98.8%, dioxide-containing silica 0.32% (Si0.14%).
Claims (4)
1. one kind prepares the method for the regulatable potassium fluotitanate of grade with the ferro-silico-titanium ore deposit, is raw material with ilmenite and hydrofluoric acid, it is characterized in that the mass content of selecting silicon for use is 2%～3.5% ilmenite; Selecting mass concentration for use is 40%～45% hydrofluoric acid, and the mass content of silicon is 0.7%～1.2% in the hydrofluoric acid;
Concrete preparation process comprises the steps:
(1) leaches: above-mentioned ilmenite is joined in the above-mentioned hydrofluoric acid leach; The mole dosage of hydrofluoric acid be titanium and silicon total mole number in the ilmenite 1.08-1.12 doubly, reaction 0.5h-1.5h leaves standstill 2h～4h; Feed rate 0.4t/h～0.6t/h filters and obtains leach liquor; Moisturizing in the leaching process, rate of water make-up are separated out with the unsaturated crystallization of titanium in the leach liquor and are as the criterion, and control leach liquor content of titanium dioxide is 155g/L～170g/L;
(2) silica removal: analyze the silicone content of above-mentioned leach liquor,, add saturated Klorvess Liquid according to the silicone content of leach liquor; Wherein the mol ratio of silicon is 1.45-1.65 in Repone K and the leach liquor, and the reinforced time 1.5h～2.5h of control reacts 1h～2h then; Leave standstill 2h～4h after-filtration; Be purified liquid, filter residue is a potassium silicofluoride, and the mass content of potassium silicofluoride is 98.5%-99.0%;
(3) synthetic potassium fluotitanate: the 1.18-1.22 according to the mole number of titanium in the scavenging solution extraordinarily goes into saturated Klorvess Liquid; The reinforced time 1.5h～2.5h of control; 50 ℃-60 ℃ of temperature of reaction, reaction 1h～2h leaves standstill 3h～4h after-filtration; Through obtaining the potassium fluotitanate product after washing, the oven dry, the grade of potassium fluotitanate product is controlled according to the content of silicon in control (2) the step silica removal after liquid.
2. according to the said a kind of method for preparing the regulatable potassium fluotitanate of grade with the ferro-silico-titanium ore deposit of claim 1; It is characterized in that during said step (1) leached: the mole dosage of hydrofluoric acid was titanium and silicon total mole number 1.1 times in the ilmenite, reacts 1h; Leave standstill 2h, feed rate 0.6t/h.
3. a kind ofly prepare the method for the regulatable potassium fluotitanate of grade according to claim 1 is said, it is characterized in that in said step (2) silica removal: the mol ratio of silicon is 1.6 in Repone K and the leach liquor with the ferro-silico-titanium ore deposit, the reinforced time 2h of control, reaction 1h leaves standstill 2h.
4. according to the said a kind of method for preparing the regulatable potassium fluotitanate of grade with the ferro-silico-titanium ore deposit of claim 1; It is characterized in that; In the synthetic potassium fluotitanate process of said step (3): extraordinarily go into saturated Klorvess Liquid, the reinforced time 2h of control, 55 ℃ of temperature of reaction according to 1.2 of the mole number of titanium in the scavenging solution; Reaction 1h leaves standstill 3h.
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Cited By (5)
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| CN102897829A (en) * | 2012-10-26 | 2013-01-30 | 福建省漳平市九鼎氟化工有限公司 | Process for producing potassium fluotitanate by environment-friendly treating fluorine-contained and potassium-contained waste |
| CN103789559A (en) * | 2014-02-26 | 2014-05-14 | 广西冶金研究院 | Titanium separation method in scandium oxide purification process |
| CN104386740A (en) * | 2014-11-21 | 2015-03-04 | 湖南有色湘乡氟化学有限公司 | Preparation method of high-purity calcium hydrofluotitanate |
| CN105174269A (en) * | 2015-09-14 | 2015-12-23 | 福建省漳平市九鼎氟化工有限公司 | Process for recycling potassium fluosilicate in process of potassium fluotitanate production |
| CN117509715A (en) * | 2023-10-31 | 2024-02-06 | 衡阳市东氟新材料股份有限公司 | Continuous production process of potassium fluotitanate |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102897829A (en) * | 2012-10-26 | 2013-01-30 | 福建省漳平市九鼎氟化工有限公司 | Process for producing potassium fluotitanate by environment-friendly treating fluorine-contained and potassium-contained waste |
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| CN104386740A (en) * | 2014-11-21 | 2015-03-04 | 湖南有色湘乡氟化学有限公司 | Preparation method of high-purity calcium hydrofluotitanate |
| CN104386740B (en) * | 2014-11-21 | 2016-04-06 | 湖南有色湘乡氟化学有限公司 | A kind of preparation method of high-purity fluorine calcium titanate |
| CN105174269A (en) * | 2015-09-14 | 2015-12-23 | 福建省漳平市九鼎氟化工有限公司 | Process for recycling potassium fluosilicate in process of potassium fluotitanate production |
| CN105174269B (en) * | 2015-09-14 | 2017-07-28 | 福建省漳平市九鼎氟化工有限公司 | A kind of technique that potassium fluosilicate is reclaimed in potassium fluotitanate production process |
| CN117509715A (en) * | 2023-10-31 | 2024-02-06 | 衡阳市东氟新材料股份有限公司 | Continuous production process of potassium fluotitanate |
| CN117509715B (en) * | 2023-10-31 | 2024-05-03 | 衡阳市东氟新材料股份有限公司 | Continuous production process of potassium fluotitanate |
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Application publication date: 20120627 |