CN113264552A - Preparation method of titanium-rich chloride material - Google Patents
Preparation method of titanium-rich chloride material Download PDFInfo
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- CN113264552A CN113264552A CN202110532074.XA CN202110532074A CN113264552A CN 113264552 A CN113264552 A CN 113264552A CN 202110532074 A CN202110532074 A CN 202110532074A CN 113264552 A CN113264552 A CN 113264552A
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- C01—INORGANIC CHEMISTRY
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- C01G23/00—Compounds of titanium
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- C01G23/047—Titanium dioxide
- C01G23/0475—Purification
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- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B7/00—Combinations of wet processes or apparatus with other processes or apparatus, e.g. for dressing ores or garbage
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
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Abstract
The invention discloses a preparation method of a chlorinated titanium-rich material, which comprises the following steps: s1, adding a flotation reagent into the crushed ore raw materials for flotation to obtain low-silicon titanium concentrate; s2, carrying out acid washing on the low-silicon titanium concentrate twice, and then filtering the acid-washed titanium concentrate to obtain acid-washed titanium concentrate; and S3, sequentially washing, drying, melting and crushing the titanium concentrate after acid washing to obtain the titanium-containing alloy. The advantages are that: 1) the method of the invention simplifies the whole work flow of the production of the titanium-rich chloride material, and simultaneously can ensure the smooth operation of the production of the titanium-rich chloride material, thereby reducing the production cost; 2) obviously reduces the impurity content of the titanium-rich chloride material and improves the product quality.
Description
Technical Field
The invention relates to a titanium dioxide production technology, in particular to a titanium dioxide production technology by a chlorination process.
Background
The primary products of the processed titanium ore are titanium concentrate and titanium-rich materials (high titanium slag and artificial rutile). The titanium-rich material generally refers to titanium slag or artificial rutile with the titanium dioxide content of not less than 75 percent, and is an important raw material for producing titanium dioxide and titanium sponge. More than 95 percent of titanium resources in China belong to primary vanadium titano-magnetite (mainly distributed in Panxi regions), and CaO, MgO and SiO of the ore2When the content of impurities is higher, the titanium concentrate is obtained by adopting the conventional mineral separation technology, and then the TiO in the titanium slag is smelted by using the titanium concentrate2The grade can only reach 70-77%, and the content of MgO + CaO reaches 8-10%, so that the catalyst cannot be used for boiling chlorination.
The existing preparation process of the titanium-rich chloride material is complex and has high energy consumption; meanwhile, only single acid washing treatment is carried out on the raw materials in the processing process, and the finished products after acid washing have poor quality and high impurity content.
Disclosure of Invention
The invention provides a preparation method of a titanium-rich chloride material, which aims to simplify the preparation process of the titanium-rich chloride material and reduce the impurity content of the titanium-rich chloride material product.
The technical scheme adopted by the invention is as follows: the preparation method of the chlorinated titanium-rich material comprises the following steps:
s1, adding a flotation reagent into the crushed ore raw materials for flotation to obtain low-silicon titanium concentrate;
s2, carrying out acid washing on the low-silicon titanium concentrate twice, and then filtering the acid-washed titanium concentrate to obtain acid-washed titanium concentrate;
and S3, sequentially washing, drying, melting and crushing the titanium concentrate after acid washing to obtain the titanium-containing alloy.
As a further improvement of the invention, the addition amount of the flotation reagent is as follows: 9-20 kg of the flotation reagent is added into each ton of ore raw materials.
As a further improvement of the invention, the flotation reagent comprises the following components in parts by weight: 2-9 parts of collecting agent, 1-8 parts of foaming agent, 1-7 parts of inhibitor and 0.3-0.5 part of regulator.
More preferably, the collector is selected from one or two of hydroximic acid and oleic acid; the foaming agent is composed of cresol pine oil and polylauryl diethanol amide according to the mass ratio of 1.5-1.8: 1; the inhibitor is water glass; the regulator is sodium hydroxide or sodium carbonate.
As a further improvement of the invention, in the step S2, the mass concentration of the hydrochloric acid used in the first acid washing is 35-40%, the mass concentration of the hydrochloric acid used in the second acid washing is 10-20%, and the mesh number of the screen used for filtering is 500-800 holes/square.
As a further improvement of the invention, the acid leaching temperature of the two acid pickling processes in the step S2 is 130-180 ℃, the pressure during acid leaching is 0.1-0.5 Mpa, and the acid leaching time is 3-8 h.
As a further improvement of the invention, the temperature in the furnace when melting in the step S3 is 1500-1800 ℃, and the melting time is 0.5-1 h.
The invention also discloses a titanium-rich chloride material, which is prepared by the preparation method of the titanium-rich chloride material.
The invention has the beneficial effects that: 1) the method of the invention simplifies the whole work flow of the production of the titanium-rich chloride material, and simultaneously can ensure the smooth operation of the production of the titanium-rich chloride material, thereby reducing the production cost; 2) obviously reduces the impurity content of the titanium-rich chloride material and improves the product quality.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples.
The first embodiment is as follows:
the chlorinated titanium-rich material is produced according to the following steps:
s1, adding a flotation reagent into the crushed ore raw materials for flotation, wherein the mass of the flotation reagent added into each ton of the ore raw materials is 15 kg; the flotation reagent comprises the following components in parts by weight: 9 parts of collecting agent, 3 parts of foaming agent, 4 parts of inhibitor and 0.4 part of regulator; the collecting agent is formed by mixing hydroximic acid and oleic acid according to the mass ratio of 1:0.3, the foaming agent is formed by cresol pine oil and polylauryl diethanol amine according to the mass ratio of 1.5:1, the inhibitor is water glass, and the regulator is sodium hydroxide. And obtaining the low-silicon titanium concentrate after the flotation is finished.
S2, carrying out acid pickling on the low-silicon titanium concentrate twice, wherein the mass concentration of hydrochloric acid used in the first acid pickling is 40%, the mass concentration of hydrochloric acid used in the second acid pickling is 20%, the acid pickling temperature in the two acid pickling processes is 150 ℃, the pressure in the acid pickling process is 0.4Mpa, and the acid pickling time is 6 h. (ii) a The titanium concentrate after acid washing was then filtered using a screen having a mesh number of 600 holes/square. And obtaining the titanium concentrate after acid washing. In the step, impurity ratio detection is respectively carried out on the materials after the first pickling and the materials after the second pickling, and the results are shown in table 1.
S3, washing, drying and melting the titanium concentrate after acid washing in sequence, and when melting, firstly heating the temperature in the melting furnace to 1500 ℃, and then continuously raising the temperature in the melting furnace, wherein the temperature change range is as follows: 1500-1800 ℃, then keeping the temperature in the interval for 0.8h, naturally cooling the melted material to room temperature, then crushing the material to obtain the titanium-rich chloride material, and carrying out component detection on the obtained titanium-rich chloride material, wherein the result is shown in table 2.
Example two:
the chlorinated titanium-rich material is produced according to the following steps:
s1, adding a flotation reagent into the crushed ore raw materials (the same batch as the first batch in the example) for flotation, wherein the mass of the flotation reagent added into each ton of the ore raw materials is 12 kg; the flotation reagent comprises the following components in parts by weight: 7 parts of collecting agent, 5 parts of foaming agent, 5 parts of inhibitor and 0.5 part of regulator; the collecting agent is formed by mixing hydroximic acid and oleic acid according to the mass ratio of 1:0.3, the foaming agent is formed by cresol pine oil and polylauryl diethanol amine according to the mass ratio of 1.8:1, the inhibitor is water glass, and the regulator is sodium hydroxide. And obtaining the low-silicon titanium concentrate after the flotation is finished.
S2, carrying out acid pickling on the low-silicon titanium concentrate twice, wherein the mass concentration of hydrochloric acid used in the first acid pickling is 40%, the mass concentration of hydrochloric acid used in the second acid pickling is 20%, the acid pickling temperature in the two acid pickling processes is 150 ℃, the pressure in the acid pickling process is 0.5Mpa, and the acid pickling time is 5 h. (ii) a The titanium concentrate after acid washing was then filtered using a screen having a mesh number of 600 holes/square. And obtaining the titanium concentrate after acid washing. In the step, impurity ratio detection is respectively carried out on the materials after the first pickling and the materials after the second pickling, and the results are shown in table 1.
S3, washing, drying and melting the titanium concentrate after acid washing in sequence, and when melting, firstly heating the temperature in the melting furnace to 1500 ℃, and then continuously raising the temperature in the melting furnace, wherein the temperature change range is as follows: 1500-1800 ℃, then keeping the temperature in the interval for 0.6h, naturally cooling the melted material to room temperature, then crushing the material to obtain the titanium-rich chloride material, and carrying out component detection on the obtained titanium-rich chloride material, wherein the result is shown in table 2.
Comparative example one:
this comparative example is a comparative example to example one, designed according to the same procedures and conditions as example one, except that: the foaming agent is cresol pine oil. The method comprises the following specific steps:
s1, adding a flotation reagent into the crushed ore raw materials (the same batch as the first batch in the example) for flotation, wherein the mass of the flotation reagent added into each ton of the ore raw materials is 15 kg; the flotation reagent comprises the following components in parts by weight: 9 parts of collecting agent, 3 parts of foaming agent, 4 parts of inhibitor and 0.4 part of regulator; the collecting agent is formed by mixing hydroximic acid and oleic acid according to the mass ratio of 1:0.3, the foaming agent is cresol pine oil, the inhibitor is water glass, and the regulator is sodium hydroxide. And obtaining the low-silicon titanium concentrate after the flotation is finished.
S2, carrying out acid pickling on the low-silicon titanium concentrate twice, wherein the mass concentration of hydrochloric acid used in the first acid pickling is 40%, the mass concentration of hydrochloric acid used in the second acid pickling is 20%, the acid pickling temperature in the two acid pickling processes is 150 ℃, the pressure in the acid pickling process is 0.4Mpa, and the acid pickling time is 6 h. (ii) a The titanium concentrate after acid washing was then filtered using a screen having a mesh number of 600 holes/square. And obtaining the titanium concentrate after acid washing.
S3, washing, drying and melting the titanium concentrate after acid washing in sequence, and when melting, firstly heating the temperature in the melting furnace to 1500 ℃, and then continuously raising the temperature in the melting furnace, wherein the temperature change range is as follows: 1500-1800 ℃, then keeping the temperature in the interval for 0.8h, naturally cooling the melted material to room temperature, then crushing the material to obtain the titanium-rich chloride material, and carrying out component detection on the obtained titanium-rich chloride material, wherein the result is shown in table 2.
Comparative example two:
this comparative example is a comparative example to example one, designed according to the same procedures and conditions as example one, except that: the foaming agent is polylauryl diethanol amide. The method comprises the following specific steps:
s1, adding a flotation reagent into the crushed ore raw materials (the same batch as the first batch in the example) for flotation, wherein the mass of the flotation reagent added into each ton of the ore raw materials is 15 kg; the flotation reagent comprises the following components in parts by weight: 9 parts of collecting agent, 3 parts of foaming agent, 4 parts of inhibitor and 0.4 part of regulator; the collecting agent is formed by mixing hydroximic acid and oleic acid according to the mass ratio of 1:0.3, the foaming agent is polylauryl diethanol amine, the inhibitor is water glass, and the regulator is sodium hydroxide. And obtaining the low-silicon titanium concentrate after the flotation is finished.
S2, carrying out acid pickling on the low-silicon titanium concentrate twice, wherein the mass concentration of hydrochloric acid used in the first acid pickling is 40%, the mass concentration of hydrochloric acid used in the second acid pickling is 20%, the acid pickling temperature in the two acid pickling processes is 150 ℃, the pressure in the acid pickling process is 0.4Mpa, and the acid pickling time is 6 h. (ii) a The titanium concentrate after acid washing was then filtered using a screen having a mesh number of 600 holes/square. And obtaining the titanium concentrate after acid washing.
S3, washing, drying and melting the titanium concentrate after acid washing in sequence, and when melting, firstly heating the temperature in the melting furnace to 1500 ℃, and then continuously raising the temperature in the melting furnace, wherein the temperature change range is as follows: 1500-1800 ℃, then keeping the temperature in the interval for 0.8h, naturally cooling the melted material to room temperature, then crushing the material to obtain the titanium-rich chloride material, and carrying out component detection on the obtained titanium-rich chloride material, wherein the result is shown in table 2.
TABLE 1 Pickling materials impurity ratio
| The impurity ratio after the first acid washing | The impurity ratio after the second acid washing | |
| Example one | 0.08％ | 0.02％ |
| Example two | 0.10％ | 0.02％ |
TABLE 2 table of the test results of the components of the titanium-rich chloride material
| TiO2％ | CaO％ | MgO％ | SiO2％ | |
| Example one | 98.54 | 0.08 | 0.61 | 0.77 |
| Example two | 98.37 | 0.07 | 0.84 | 0.73 |
| Comparative example 1 | 95.14 | 0.13 | 2.20 | 2.53 |
| Comparative example No. two | 93.40 | 0.16 | 2.89 | 3.55 |
As can be seen from Table 1, the impurity ratios of the materials after the second acid washing in the first and second examples are both obviously lower than the impurity ratio of the materials after the first acid washing, which indicates that the quality and purity of the materials after acid washing and filtering can be improved and the impurity content in the acid-washed materials can be greatly reduced by adopting two acid washing in the acid washing stage.
As can be seen from the detection results of the components of the titanium-rich chloride material product in the first embodiment, the first comparative embodiment and the second comparative embodiment of the table 2, under the condition that the use amounts of the foaming agents are completely the same, the foaming agent compounded by cresol pine oil and polylauryl diethanol amide can be adopted to obviously reduce the impurity content of the titanium-rich chloride material product, and the effect of the foaming agent is obviously better than the effect of the two components when the two components are used independently.
Claims (11)
1. The preparation method of the chlorinated titanium-rich material comprises the following steps:
s1, adding a flotation reagent into the crushed ore raw materials for flotation to obtain low-silicon titanium concentrate;
s2, carrying out acid washing on the low-silicon titanium concentrate twice, and then filtering the acid-washed titanium concentrate to obtain acid-washed titanium concentrate;
and S3, sequentially washing, drying, melting and crushing the titanium concentrate after acid washing to obtain the titanium-containing alloy.
2. The method for preparing the titanium-rich chloride material according to claim 1, wherein the method comprises the following steps: the addition amount of the flotation reagent is as follows: 9-20 kg of the flotation reagent is added into each ton of ore raw materials.
3. The method for preparing the titanium-rich chloride material according to claim 1, wherein the method comprises the following steps: the flotation reagent comprises the following components in parts by weight: 2-9 parts of collecting agent, 1-8 parts of foaming agent, 1-7 parts of inhibitor and 0.3-0.5 part of regulator.
4. The method for preparing the titanium-rich chloride material according to claim 3, wherein the method comprises the following steps: the collector is selected from one or two of hydroximic acid and oleic acid.
5. The method for preparing the titanium-rich chloride material according to claim 3, wherein the method comprises the following steps: the foaming agent is composed of cresol pine oil and polylauryl diethanol amide according to the mass ratio of 1.5-1.8: 1.
6. The method for preparing the titanium-rich chloride material according to claim 3, wherein the method comprises the following steps: the inhibitor is water glass.
7. The method for preparing the titanium-rich chloride material according to claim 3, wherein the method comprises the following steps: the regulator is sodium hydroxide or sodium carbonate.
8. The method for preparing the titanium-rich chloride material according to claim 1, wherein the method comprises the following steps: in the step S2, the mass concentration of the hydrochloric acid used in the first acid washing is 35-40%, the mass concentration of the hydrochloric acid used in the second acid washing is 10-20%, and the mesh number of the screen used for filtering is 500-800 holes/square.
9. The method for preparing the titanium-rich chloride material according to claim 1, wherein the method comprises the following steps: in the step S2, the acid leaching temperature in the two acid pickling processes is 130-180 ℃, the pressure during acid leaching is 0.1-0.5 Mpa, and the acid leaching time is 3-8 h.
10. The method for preparing the titanium-rich chloride material according to claim 1, wherein the method comprises the following steps: in the step S3, the temperature in the melting furnace is 1500-1800 ℃ and the melting time is 0.5-1 h.
11. The titanium-rich chloride material prepared by the method for preparing the titanium-rich chloride material according to any one of claims 1 to 10.
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