CN111348671A - Method for purifying titanium gypsum - Google Patents
Method for purifying titanium gypsum Download PDFInfo
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- CN111348671A CN111348671A CN202010175830.3A CN202010175830A CN111348671A CN 111348671 A CN111348671 A CN 111348671A CN 202010175830 A CN202010175830 A CN 202010175830A CN 111348671 A CN111348671 A CN 111348671A
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- titanium gypsum
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- titanium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/468—Purification of calcium sulfates
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- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention belongs to the technical field of titanium gypsum recycling, and particularly relates to a method for purifying titanium gypsum. Aiming at the problems of high impurity content, high removal difficulty and difficult resource utilization of the existing titanium gypsum, the invention provides a method for purifying and purifying the titanium gypsum, which comprises the following steps: a. adding the leaching solution into the titanium gypsum, and uniformly stirring; b. reacting at room temperature for 30-45 min, performing suction filtration, adding clear water into the filter cake, soaking for 10min, and performing secondary suction filtration; c. and after secondary suction filtration, drying the filter cake to obtain the purified titanium gypsum. The method has the advantages of good effect of purifying the titanium gypsum, short flow, simple process, low energy consumption and suitability for popularization and application.
Description
Technical Field
The invention belongs to the technical field of titanium gypsum recycling, and particularly relates to a method for purifying titanium gypsum.
Background
A large amount of acid waste water is generated during the production of titanium dioxide by a sulfuric acid method, and the titanium gypsum is industrial waste residue which is generated by adding lime into the acid waste water for neutralization treatment and takes dihydrate gypsum as a main component. Compared with natural gypsum, the titanium gypsum has the advantages of large water content, large viscosity and higher impurities, and the main impurities are ferric oxide, ferric hydroxide and ferrous hydroxide, and also contain titanium, magnesium, manganese, barium and the like, and have certain radioactivity; at present, only a small amount of titanium gypsum is used as a composite cementing material additive, and a large amount of titanium gypsum is still directly stacked, so that a large amount of land resources are wasted, and environmental pollution is easily caused. Therefore, it is necessary to find a method for rapidly and simply reducing iron, manganese, aluminum, magnesium and the like in the titanium gypsum to improve the quality of the titanium gypsum, and a foundation is laid for realizing the large-scale and high-value production of the titanium gypsum in the next step.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the existing titanium gypsum has the problems of high impurity content, high removal difficulty and difficult resource utilization.
The technical scheme for solving the technical problems comprises the following steps: provides a method for purifying titanium gypsum. The method comprises the following steps:
a. adding the leaching solution into the titanium gypsum, and uniformly stirring;
b. reacting at room temperature for 30-45 min, performing suction filtration, adding clear water into the filter cake, soaking for 10min, and performing secondary suction filtration;
c. and after secondary suction filtration, drying the filter cake to obtain the purified titanium gypsum.
In the method for purifying and purifying the titanium gypsum, the titanium gypsum in the step a is orange powder obtained by drying and grinding waste residues generated by neutralizing titanium white wastewater.
Wherein, in the method for purifying and purifying the titanium gypsum, the particle size of the titanium gypsum in the step a is less than or equal to 0.125 mm.
Further, in the method for purifying and purifying titanium gypsum, the chemical components of the titanium gypsum in the step a include: in percent by weight, SO325～35％，CaO 20～30％，Fe2O310～20％，TiO21～2％，MnO 0.1～0.5％，MgO 1～2％，Al2O31～2％。
In the method for purifying and purifying the titanium gypsum, the leaching solution in the step a is at least one of citric acid, sulfuric acid, hydrochloric acid, acetic acid, boric acid, oxalic acid, sodium hydroxide, potassium hydroxide, ammonia water or ammonium sulfate aqueous solution.
Further, in the method for purifying and purifying the titanium gypsum, the concentration of the leaching solution in the step a is 10-30%.
In the method for purifying and purifying the titanium gypsum, the liquid-solid ratio of the leaching solution in the step a to the titanium gypsum is 3-5.
Wherein, in the method for purifying and purifying the titanium gypsum, the drying temperature in the step c is 210 ℃ and the time is 120 min.
The invention has the beneficial effects that:
the invention provides a method for purifying titanium gypsum, which is characterized in that the inventor screens the most suitable type and concentration of leaching solution through mass production tests, and performs purification and purification on the titanium gypsum by matching with suction filtration. The method has the advantages of good effect of purifying the titanium gypsum, short flow, simple process, low energy consumption and suitability for popularization and application.
Detailed Description
The invention provides a method for purifying titanium gypsum, which comprises the following steps:
a. adding the leaching solution into the titanium gypsum according to the liquid-solid ratio of 3-5, and stirring and uniformly mixing;
b. reacting at room temperature for 30-45 min, performing suction filtration, adding clear water into the filter cake, soaking for 10min, and performing secondary suction filtration;
c. and after secondary suction filtration, drying the filter cake to obtain the purified titanium gypsum.
In the method for purifying and purifying the titanium gypsum, the titanium gypsum in the step a is orange powder obtained by drying and grinding waste residues generated by neutralizing titanium white wastewater.
Wherein, in the method for purifying and purifying the titanium gypsum, the particle size of the titanium gypsum in the step a is less than or equal to 0.125 mm.
Further, in the method for purifying and purifying titanium gypsum, the chemical components of the titanium gypsum in the step a include: in percent by weight, SO325～35％，CaO 20～30％，Fe2O310～20％，TiO21～2％，MnO 0.1～0.5％，MgO 1～2％，Al2O31～2％。
In the method for purifying and purifying the titanium gypsum, the leaching solution in the step a is at least one of citric acid, sulfuric acid, hydrochloric acid, acetic acid, boric acid, oxalic acid, sodium hydroxide, potassium hydroxide, ammonia water or ammonium sulfate aqueous solution.
In the invention, the concentration of the leaching solution is too low, the impurity removal effect is poor, and the crystal form of the calcium sulfate is easily changed when the concentration of the leaching solution is too high (if higher than 35%). Therefore, in the method for purifying and purifying the titanium gypsum, the concentration of the leaching solution in the step a is 10-30%.
In order to economically and efficiently remove impurities, the liquid-solid ratio of the leaching solution in the step a to the titanium gypsum is 3-5 in the titanium gypsum purification method.
Wherein, in the method for purifying and purifying the titanium gypsum, the drying temperature in the step c is 210 ℃ and the time is 120 min.
The following examples are intended to illustrate specific embodiments of the present invention without limiting the scope of the invention to the examples.
The titanium gypsum composition used in the examples is shown in table 1.
TABLE 1 titanium Gypsum raw Material principal Components
| Composition (I) | SO3 | CaO | Fe2O3 | Al2O3 | MgO | MnO | TiO2 | SiO2 |
| Titanium gypsum raw material | 32.5 | 26.1 | 16.5 | 0.9 | 0.8 | 0.4 | 0.7 | 1.6 |
Example 1 purification of titanium Gypsum Using the method of the invention
Weighing 45ml of leaching solution, putting the leaching solution into a beaker, adding 15g of titanium gypsum while stirring, continuously stirring and reacting for 30min after the adding is finished, and quickly pouring the suspension in the beaker into a funnel for suction filtration after the reaction is finished; and after the filter cake is dried by pumping, stopping pumping filtration, pouring a certain amount of water into the filter cake, naturally soaking for 10min, starting a pumping filtration switch again to pump filter until no water drops, taking out the filter cake, and placing the filter cake in an oven for drying at 210 ℃. The main components of the purified titanium gypsum are shown in Table 2.
TABLE 2 purified titanium Gypsum Fibrosum major ingredient
| Composition (I) | SO3 | CaO | Fe2O3 | Al2O3 | MgO | MnO | TiO2 | SiO2 |
| Purified titanium gypsum | 39.5 | 34.3 | 1.6 | 0.21 | 0.12 | 0.10 | 0.70 | 1.4 |
Example 2 purification of titanium Gypsum Using the method of the invention
Weighing 60ml of leaching solution, adding 15g of titanium gypsum while stirring, continuously stirring and reacting for 30min after the adding is finished, and quickly pouring the suspension in the beaker into a funnel for suction filtration after the reaction is finished; and after the filter cake is dried by pumping, stopping pumping filtration, pouring a certain amount of water into the filter cake, naturally soaking for 10min, starting a pumping filtration switch again to pump filter until no water drops, taking out the filter cake, and placing the filter cake in an oven for drying at 210 ℃. The main components of the purified titanium gypsum are shown in Table 3.
TABLE 3 purified titanium Gypsum base
| Composition (I) | SO3 | CaO | Fe2O3 | Al2O3 | MgO | MnO | TiO2 | SiO2 |
| Purified titanium gypsum | 40.1 | 35.6 | 0.9 | 0.14 | 0.08 | 0.12 | 0.69 | 1.5 |
Example 3 purification of titanium Gypsum Using the method of the invention
Weighing 75ml of leaching solution, adding 15g of titanium gypsum while stirring, continuing stirring for reaction for 30min after the adding is finished, and quickly pouring the suspension in the beaker into a funnel for suction filtration after the reaction is finished; and after the filter cake is dried by pumping, stopping pumping filtration, pouring a certain amount of water into the filter cake, naturally soaking for 10min, starting a pumping filtration switch again to pump filter until no water drops, taking out the filter cake, and placing the filter cake in an oven for drying at 210 ℃. The main components of the purified titanium gypsum are shown in Table 4.
TABLE 4 purified titanium Gypsum Fibrosum major ingredient
| Composition (I) | SO3 | CaO | Fe2O3 | Al2O3 | MgO | MnO | TiO2 | SiO2 |
| Purified titanium gypsum | 41.1 | 36.3 | 0.7 | 0.10 | 0.07 | 0.12 | 0.65 | 1.3 |
Example 4 purification of titanium Gypsum Using the method of the invention
Weighing 45ml of leaching solution, putting the leaching solution into a beaker, adding 15g of titanium gypsum while stirring, continuing stirring to react for 45min after the addition is finished, and quickly pouring the suspension in the beaker into a funnel for suction filtration after the reaction is finished; and after the filter cake is dried by pumping, stopping pumping filtration, pouring a certain amount of water into the filter cake, naturally soaking for 10min, starting a pumping filtration switch again to pump filter until no water drops, taking out the filter cake, and placing the filter cake in an oven for drying at 210 ℃. The main components of the purified titanium gypsum are shown in Table 5.
TABLE 5 purified titanium Gypsum Fibrosum major component
| Composition (I) | SO3 | CaO | Fe2O3 | Al2O3 | MgO | MnO | TiO2 | SiO2 |
| Purified titanium gypsum | 39.7 | 35.2 | 1.4 | 0.08 | 0.09 | 0.11 | 0.64 | 1.4 |
Example 5 purification of titanium Gypsum Using the method of the invention
Adding 45ml of leaching solution into a beaker, adding 15g of titanium gypsum while stirring, continuously stirring and reacting for 30min after the adding is finished, and quickly pouring the suspension in the beaker into a funnel for suction filtration after the reaction is finished; and after the filter cake is dried by pumping, stopping pumping filtration, pouring a certain amount of water into the filter cake, naturally soaking for 10min, starting a pumping filtration switch again to pump filter until no water drops, taking out the filter cake, and placing the filter cake in an oven for drying at 210 ℃. The main components of the purified titanium gypsum are shown in Table 6.
TABLE 6 purified titanium Gypsum Fibrosum major component
| Composition (I) | SO3 | CaO | Fe2O3 | Al2O3 | MgO | MnO | TiO2 | SiO2 |
| Purified titanium gypsum | 39.5 | 34.3 | 1.6 | 0.24 | 0.31 | 0.15 | 0.70 | 1.4 |
Claims (8)
1. The method for purifying and purifying the titanium gypsum is characterized by comprising the following steps:
a. adding the leaching solution into the titanium gypsum, and uniformly stirring;
b. reacting at room temperature for 30-45 min, performing suction filtration, adding clear water into the filter cake, soaking for 10min, and performing secondary suction filtration;
c. and after secondary suction filtration, drying the filter cake to obtain the purified titanium gypsum.
2. The method for purifying titanium gypsum according to claim 1, wherein: the titanium gypsum in the step a is orange powder obtained by drying and grinding waste residues generated by neutralizing titanium white wastewater.
3. The method for purifying titanium gypsum according to claim 1, wherein: the particle size of the titanium gypsum in the step a is less than or equal to 0.125 mm.
4. The method for purifying titanium gypsum according to claim 1, wherein: the titanium gypsum in the step a comprises the following chemical components: in percent by weight, SO325～35％，CaO 20～30％，Fe2O310～20％，TiO21～2％，MnO 0.1～0.5％，MgO 1～2％，Al2O31～2％。
5. The method for purifying titanium gypsum according to claim 1, wherein: the leaching solution in the step a is at least one of citric acid, sulfuric acid, hydrochloric acid, acetic acid, boric acid, oxalic acid, sodium hydroxide, potassium hydroxide, ammonia water or ammonium sulfate aqueous solution.
6. The method for purifying titanium gypsum according to claim 1, wherein: the concentration of the leaching solution in the step a is 10-30%.
7. The method for purifying titanium gypsum according to claim 1, wherein: the liquid-solid ratio of the leaching solution in the step a to the titanium gypsum is 3-5.
8. The method for purifying titanium gypsum according to claim 1, wherein: and c, drying at 210 ℃ for 120 min.
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| CN202010175830.3A CN111348671A (en) | 2020-03-13 | 2020-03-13 | Method for purifying titanium gypsum |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109161971A (en) * | 2018-10-11 | 2019-01-08 | 西昌学院 | A method of calcium sulfate crystal whiskers are prepared by titanium gypsum |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109161971A (en) * | 2018-10-11 | 2019-01-08 | 西昌学院 | A method of calcium sulfate crystal whiskers are prepared by titanium gypsum |
Non-Patent Citations (1)
| Title |
|---|
| 蒋美雪: ""钛石膏除杂制备硫酸钙晶须与酸浸液处理研究"", 《中国优秀硕士论文全文数据库》 * |
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