CN110342561B - Method for efficiently removing iron from by-product gypsum of titanium dioxide by sulfuric acid process - Google Patents
Method for efficiently removing iron from by-product gypsum of titanium dioxide by sulfuric acid process Download PDFInfo
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- CN110342561B CN110342561B CN201910736957.5A CN201910736957A CN110342561B CN 110342561 B CN110342561 B CN 110342561B CN 201910736957 A CN201910736957 A CN 201910736957A CN 110342561 B CN110342561 B CN 110342561B
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- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/468—Purification of calcium sulfates
Abstract
The invention discloses a method for efficiently removing iron from a byproduct gypsum of titanium dioxide by a sulfuric acid method, which comprises the steps of weighing and proportioning, mixing and stirring, primary extraction, primary magnetic separation, secondary extraction, secondary magnetic separation, precipitation and filtration and the like, the method for removing iron adopts the double extraction effect of the P204 extractant and the acetone extractant, can extract and separate iron ions contained in the titanium gypsum mixed solution as completely as possible, and causes the phenomenon of incomplete extraction due to mutual adsorption of surface iron ions and other impurity particles in the titanium gypsum, meanwhile, the property components of other raw materials in the titanium gypsum can not be damaged, the high-efficiency and comprehensive iron removal effect is realized, meanwhile, magnetic separation treatment is carried out by adopting two times of different magnetic separation flow rates, the flow rate of iron ions generated after two times of extraction can be met, the operation purpose of double-layer magnetic separation is realized, and the comprehensiveness of the adsorption separation of the iron ions is improved to the maximum extent.
Description
Technical Field
The invention relates to the technical field of titanium gypsum iron removal methods, in particular to a method for efficiently removing iron from a titanium dioxide byproduct gypsum by a sulfuric acid method.
Background
When titanium gypsum is produced by adopting a sulfuric acid method, in order to treat acid wastewater, lime (or carbide slag) is added to neutralize a large amount of acid wastewater to generate waste slag which takes dihydrate gypsum as a main component, and the titanium gypsum produced by adopting the sulfuric acid method contains more ferrous sulfate, so that compared with the titanium gypsum produced by other methods, the content of iron ions in the titanium gypsum is very high, and the mechanical property of titanium gypsum blocks is reduced after the content of the iron ions in the titanium gypsum is increased, so that the iron ions in the titanium pigment produced by sulfuric acid method monk need to be removed.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for efficiently removing iron from gypsum as a byproduct of titanium dioxide by a sulfuric acid process.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for efficiently removing iron from a byproduct gypsum of titanium dioxide by a sulfuric acid method comprises the following preparation steps:
s1: weighing and proportioning, namely weighing sufficient raw materials such as titanium gypsum, P204, acetone, hydrochloric acid, purified water and the like independently, and weighing and classifying the raw materials one by one according to the using amount of the raw materials and the ratio of 1: 1;
s2: mixing and stirring, namely selecting hydrochloric acid, titanium gypsum and water purification raw materials, sequentially adding the hydrochloric acid, the titanium gypsum and the hydrochloric acid into a transparent glass container according to the sequence of water purification, titanium gypsum and hydrochloric acid, and stirring the added mixed solution by adopting a glass stirring rod in an anticlockwise rotating manner in the adding and pouring process;
s3: primary extraction, when the mixed solution is relatively static, pouring a P204 extractant into the mixed solution at a uniform speed along the same direction, so that the P204 extractant is in full contact with the mixed solution, and iron ions in the titanium gypsum in the mixed solution are extracted;
s4: performing primary magnetic separation, namely guiding the mixed solution after primary extraction out into magnetic separation equipment with parallel slideways, and performing magnetic adsorption on iron ions generated by extraction in the mixed solution by adjusting the magnetic adsorption force of the magnetic separation equipment to obtain primary magnetic separation liquid;
s5: secondary extraction, namely pouring the mixed solution subjected to primary magnetic separation into transparent glass containers with the same specification again, and pouring an acetone extracting agent into the mixed solution at a uniform speed along the same direction, so that the acetone extracting agent is in full contact with the mixed solution, and extracting the residual iron ions in the titanium gypsum in the mixed solution;
s6: performing secondary magnetic separation, namely guiding the mixed solution after secondary extraction into magnetic separation equipment with parallel slideways, and performing magnetic adsorption on iron ions generated by extraction in the mixed solution by adjusting the magnetic adsorption force of the magnetic separation equipment to obtain a secondary magnetic separation solution;
s7: and (2) precipitating and filtering, pouring the magnetic separation liquid after the second-stage magnetic adsorption into a transparent glass container with the same specification, arranging two layers of sieve plates with different filter hole sizes in the transparent glass container, carrying out double-layer filtering on the titanium gypsum solution after iron removal, and obtaining pure white titanium gypsum solution after a period of static precipitation.
Preferably, after the hydrochloric acid and the titanium gypsum are mixed, stirred and dissolved in the step S2, the calcium sulfate will uniformly sink and precipitate, wherein the stirring duration of the glass stirring rod is 5-8min, and the stirring speed is 20-30 min/rad.
Preferably, the pouring direction of the P204 extractant in step S3 is counterclockwise, wherein the continuous temperature of the primary extraction is 25-28 ℃, the ratio of the P204 to the mixed liquor is 2:1, the volume fraction of the mixed liquor is 30%, and the equilibrium time is 45 min.
Preferably, the flow width of the mixed liquid poured out in the step S4 is 35-40cm, the liquid level height is 2-3cm, wherein the magnetic separation device adopts a comb magnetic separator, the single-machine flow rate is controlled to be 120L/min-850L/min, and the continuous separation time is controlled to be 3-5 min.
Preferably, the pouring direction of the acetone extractant in the step S5 is clockwise, the temperature of the secondary extraction is controlled at normal temperature, a glass stirring rod is used for continuously stirring along the clockwise direction, wherein the ratio of the acetone extractant to the mixed solution is 3:1, and the stirring duration is controlled to be 5-7 min.
Preferably, the flow width of the mixed liquid poured out in the step S6 is 15-20cm, the liquid level height is 1-2cm, wherein the magnetic separation equipment adopts a comb magnetic separator, the flow rate of a single machine is controlled to be 500L/min-1500L/min, and the continuous separation time is controlled to be 3-5 min.
Preferably, in the step S7, the diameter of the filter hole of the upper sieve plate is 3mm, the diameter of the filter hole of the lower sieve plate is 2mm, and the settling time is controlled to be 30-45 min.
Advantageous effects
The invention provides a method for efficiently removing iron from a byproduct gypsum of titanium dioxide by a sulfuric acid method. The method has the following beneficial effects:
(1): the method for removing the iron adopts the double extraction effect of the P204 extractant and the acetone extractant, can extract and separate iron ions contained in the titanium gypsum mixed solution as comprehensively as possible, can cause the phenomenon of incomplete extraction due to mutual adsorption of surface iron ions and other impurity particles in the titanium gypsum, can not damage the property components of other raw materials in the titanium gypsum, and realizes the efficient and comprehensive iron removal effect.
(2): the iron removing method adopts two magnetic separation steps, the mixed liquid after two times of extraction can be respectively subjected to independent magnetic separation operation, the phenomenon that the speed and the effect of secondary extraction are influenced due to the fact that the mixed liquid containing iron ions after primary extraction is mixed with each other is avoided, meanwhile, the flow of the two times of magnetic separation is different in size, the flow of iron ions generated after two times of extraction can be met, and accordingly the comprehensiveness of adsorption separation of the iron ions is improved to the maximum extent.
Drawings
FIG. 1 is a schematic flow diagram of a method for efficiently removing iron from gypsum as a byproduct in titanium dioxide production by a sulfuric acid process.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1, a method for efficiently removing iron from a byproduct gypsum of titanium dioxide by a sulfuric acid process, comprises the following preparation steps:
s1: weighing and proportioning, namely weighing sufficient raw materials such as titanium gypsum, P204, acetone, hydrochloric acid, purified water and the like independently, and weighing and classifying the raw materials one by one according to the using amount of the raw materials and the ratio of 1: 1;
s2: mixing and stirring, namely selecting hydrochloric acid, titanium gypsum and water purification raw materials, sequentially adding the hydrochloric acid, the titanium gypsum and the hydrochloric acid into a transparent glass container according to the sequence of water purification, titanium gypsum and hydrochloric acid, and stirring the added mixed solution by adopting a glass stirring rod in an anticlockwise rotating manner in the adding and pouring process;
s3: primary extraction, when the mixed solution is relatively static, pouring a P204 extractant into the mixed solution at a uniform speed along the same direction, so that the P204 extractant is in full contact with the mixed solution, and iron ions in the titanium gypsum in the mixed solution are extracted;
s4: performing primary magnetic separation, namely guiding the mixed solution after primary extraction out into magnetic separation equipment with parallel slideways, and performing magnetic adsorption on iron ions generated by extraction in the mixed solution by adjusting the magnetic adsorption force of the magnetic separation equipment to obtain primary magnetic separation liquid;
s5: secondary extraction, namely pouring the mixed solution subjected to primary magnetic separation into transparent glass containers with the same specification again, and pouring an acetone extracting agent into the mixed solution at a uniform speed along the same direction, so that the acetone extracting agent is in full contact with the mixed solution, and extracting the residual iron ions in the titanium gypsum in the mixed solution;
s6: performing secondary magnetic separation, namely guiding the mixed solution after secondary extraction into magnetic separation equipment with parallel slideways, and performing magnetic adsorption on iron ions generated by extraction in the mixed solution by adjusting the magnetic adsorption force of the magnetic separation equipment to obtain a secondary magnetic separation solution;
s7: and (2) precipitating and filtering, pouring the magnetic separation liquid after the second-stage magnetic adsorption into a transparent glass container with the same specification, arranging two layers of sieve plates with different filter hole sizes in the transparent glass container, carrying out double-layer filtering on the titanium gypsum solution after iron removal, and obtaining pure white titanium gypsum solution after a period of static precipitation.
And step S2, after the hydrochloric acid and the titanium gypsum are mixed, stirred and dissolved, the calcium sulfate can uniformly sink and precipitate, and the mixed solution after the hydrochloric acid is dissolved can be subjected to a pre-separation and clarification operation by utilizing the sinking principle of the calcium sulfate, so that the subsequent extraction treatment of the mixed solution is facilitated, wherein the stirring duration of the glass stirring rod is 5-8min, and the stirring speed is 20-30 min/rad.
In the step S3, the pouring direction of the P204 extractant is in the counterclockwise direction, wherein the continuous temperature of primary extraction is 25-28 ℃, the ratio of the P204 to the mixed solution is 2:1, the volume fraction of the mixed solution is 30%, and the balance time is 45min, so that the P204 extractant can be in full contact with the mixed solution, and the extraction rate of the P204 extractant on iron ions in the mixed solution is greatly accelerated.
The flow width of the mixed liquid poured out in the step S4 is 35-40cm, the liquid level height is 2-3cm, wherein, the magnetic separation equipment adopts a comb magnetic separator, the single machine flow is controlled to be 120L/min-850L/min, and the continuous separation time is controlled to be 3-5 min.
In the step S5, the pouring direction of the acetone extractant is clockwise, the temperature of the secondary extraction is controlled at normal temperature, a glass stirring rod is adopted to continuously stir along the clockwise direction, wherein the ratio of the acetone extractant to the mixed solution is 3:1, and the stirring duration is controlled to be 5-7 min.
The flow width of the mixed liquid poured out in the step S6 is 15-20cm, the liquid level height is 1-2cm, wherein the magnetic separation equipment adopts a comb magnetic separator, the single-machine flow rate is controlled to be 500L/min-1500L/min, the continuous separation time is controlled to be 3-5min, the magnetic separator technology is a technology for separating different magnetic substances by means of the action of a magnetic field force, and can generate large and obvious adsorption force on the extracted iron ions, so that the iron ions can be adsorbed and separated by magnetic separation, and the magnetic separation effect on the iron ions in the mixed liquid is achieved.
In the step S7, the diameter of the filter hole of the upper-layer sieve plate is 3mm, the diameter of the filter hole of the lower-layer sieve plate is 2mm, the precipitation time is controlled to be 30-45min, the mixed liquid obtained after two times of magnetic separation can be subjected to the effect of twice filtration, and particle impurities in the mixed liquid are removed as far as possible, so that clean pure white liquid is obtained.
In the description herein, references to the description of "one embodiment," "an example," "a specific example," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. A method for efficiently removing iron from a sulfuric acid method titanium dioxide byproduct gypsum is characterized by comprising the following preparation steps:
s1: weighing and proportioning, namely weighing sufficient titanium gypsum, P204, acetone, hydrochloric acid and water purification raw materials respectively and independently, and weighing and classifying the raw materials one by one according to the using amount of each raw material and the proportion of 1: 1;
s2: mixing and stirring, namely selecting hydrochloric acid, titanium gypsum and water purification raw materials, sequentially adding the hydrochloric acid, the titanium gypsum and the hydrochloric acid into a transparent glass container according to the sequence of water purification, titanium gypsum and hydrochloric acid, and stirring the added mixed solution by adopting a glass stirring rod in an anticlockwise rotating manner in the adding and pouring process;
s3: primary extraction, when the mixed solution is relatively static, pouring a P204 extractant into the mixed solution at a uniform speed along the same direction, so that the P204 extractant is in full contact with the mixed solution, and iron ions in the titanium gypsum in the mixed solution are extracted;
s4: performing primary magnetic separation, namely guiding the mixed solution after primary extraction out into magnetic separation equipment with parallel slideways, and performing magnetic adsorption on iron ions generated by extraction in the mixed solution by adjusting the magnetic adsorption force of the magnetic separation equipment to obtain primary magnetic separation liquid;
s5: secondary extraction, namely pouring the mixed solution subjected to primary magnetic separation into transparent glass containers with the same specification again, and pouring an acetone extracting agent into the mixed solution at a uniform speed along the same direction, so that the acetone extracting agent is in full contact with the mixed solution, and extracting the residual iron ions in the titanium gypsum in the mixed solution;
s6: performing secondary magnetic separation, namely guiding the mixed solution after secondary extraction into magnetic separation equipment with parallel slideways, and performing magnetic adsorption on iron ions generated by extraction in the mixed solution by adjusting the magnetic adsorption force of the magnetic separation equipment to obtain a secondary magnetic separation solution;
s7: precipitating and filtering, pouring the magnetic separation liquid after the secondary magnetic adsorption into a transparent glass container with the same specification, arranging two layers of sieve plates with different filter hole sizes in the transparent glass container, carrying out double-layer filtering on the titanium gypsum solution after iron removal, and obtaining pure white titanium gypsum solution after a period of static precipitation;
in the step S3, the pouring direction of the P204 extractant is anticlockwise, wherein the continuous temperature of primary extraction is 25-28 ℃, the ratio of the P204 to the mixed solution is 2:1, the volume fraction of the mixed solution is 30%, and the balance time is 45 min;
the flow width of the mixed liquid led out in the step S4 is 35-40cm, the liquid level height is 2-3cm, wherein, the magnetic separation equipment adopts a comb magnetic separator, the flow rate of a single machine is controlled to be 120L/min-850L/min, and the continuous separation time is controlled to be 3-5 min;
the flow width of the mixed liquid led out in the step S6 is 15-20cm, the liquid level height is 1-2cm, wherein, the magnetic separation equipment adopts a comb magnetic separator, the flow rate of a single machine is controlled to be 500L/min-1500L/min, and the continuous separation time is controlled to be 3-5 min.
2. The method for efficiently removing iron from the gypsum as a byproduct in the production of titanium dioxide by sulfuric acid process according to claim 1, wherein calcium sulfate is uniformly precipitated after the hydrochloric acid and the titanium gypsum are mixed, stirred and dissolved in the step S2, wherein the stirring duration of the glass stirring rod is 5-8min, and the stirring speed is 20-30 min/rad.
3. The method for efficiently removing iron from the gypsum as a byproduct in the production of titanium dioxide by a sulfuric acid process according to claim 1, wherein the pouring direction of the acetone extractant in the step S5 is clockwise, the temperature of the secondary extraction is controlled at normal temperature, a glass stirring rod is used for continuously stirring along the clockwise direction, the ratio of the acetone extractant to the mixed solution is 3:1, and the stirring duration is controlled to be 5-7 min.
4. The method for efficiently removing iron from the gypsum as a byproduct in the production of titanium dioxide by the sulfuric acid process according to claim 1, wherein in the step S7, the diameter of the filter holes of the upper sieve plate is 3mm, the diameter of the filter holes of the lower sieve plate is 2mm, and the settling time is controlled to be 30-45 min.
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Citations (3)
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| JPH06115933A (en) * | 1992-10-02 | 1994-04-26 | Chiyoda Corp | Production of white gypsum |
| CN105502464A (en) * | 2015-12-15 | 2016-04-20 | 合肥学院 | Separation and removal technology of iron element in titanium gypsum |
| CN109734341A (en) * | 2019-03-13 | 2019-05-10 | 西南科技大学 | A kind of method that ardealite physical chemistry brightened and prepared cementitious material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06115933A (en) * | 1992-10-02 | 1994-04-26 | Chiyoda Corp | Production of white gypsum |
| CN105502464A (en) * | 2015-12-15 | 2016-04-20 | 合肥学院 | Separation and removal technology of iron element in titanium gypsum |
| CN109734341A (en) * | 2019-03-13 | 2019-05-10 | 西南科技大学 | A kind of method that ardealite physical chemistry brightened and prepared cementitious material |
Non-Patent Citations (2)
| Title |
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| 硫酸法钛白石膏的纯化工艺研究;朱静平等;《西昌学院学报·自然科学版》;20120630;第26卷(第2期);第67-69页 * |
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