CN115432739A - Recrystallization purification process of titanium dioxide byproduct ferrous sulfate - Google Patents
Recrystallization purification process of titanium dioxide byproduct ferrous sulfate Download PDFInfo
- Publication number
- CN115432739A CN115432739A CN202211290879.9A CN202211290879A CN115432739A CN 115432739 A CN115432739 A CN 115432739A CN 202211290879 A CN202211290879 A CN 202211290879A CN 115432739 A CN115432739 A CN 115432739A
- Authority
- CN
- China
- Prior art keywords
- ferrous sulfate
- titanium dioxide
- purification process
- recrystallization purification
- crystallization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a recrystallization purification process of a titanium dioxide byproduct ferrous sulfate, belonging to the technical field of ferrous sulfate impurity removal. The method comprises the following steps: 1) Adding deionized water into ferrous sulfate heptahydrate, heating to 65 ℃, stirring and dissolving to prepare saturated solution; 2) Filtering, removing solid-phase impurities, adjusting the pH value to 2 to obtain a clear solution, carrying out freeze crystallization on the obtained clear solution, controlling the temperature of the freeze crystallization at 5 ℃, carrying out freeze crystallization for 2-3 times to recrystallize dissolved ferrous sulfate out of the solution, carrying out vacuum filtration or filter pressing or filtering, and separating to obtain ferrous sulfate crystals; 3) And drying the ferrous sulfate crystals, and then sieving the dried ferrous sulfate by a 200-mesh sieve and a 700-mesh sieve respectively to obtain the sieved ferrous sulfate. The method can effectively remove impurities and purify the ferrous sulfate as a titanium white byproduct, and provides data reference for industrial application.
Description
Technical Field
The invention belongs to the technical field of ferrous sulfate impurity removal, relates to the technical field of purification of a titanium white byproduct ferrous sulfate, and particularly relates to a recrystallization purification process of the titanium white byproduct ferrous sulfate.
Background
Ferrous sulfate heptahydrate is a byproduct in the process of producing titanium dioxide by a sulfuric acid method, and widely exists in the fields of chemical industry, metallurgy and the like. As a large country for producing titanium dioxide in China, a large amount of by-product ferrous sulfate heptahydrate is produced every year, if the by-product ferrous sulfate heptahydrate is randomly stacked, the environment is polluted, resources are wasted, and meanwhile, the subsequent comprehensive utilization and material performance of the titanium dioxide by-product ferrous sulfate heptahydrate are influenced due to high impurity content and low purity of the titanium dioxide by-product ferrous sulfate heptahydrate, so that the titanium dioxide by-product ferrous sulfate heptahydrate is required to be producedPurifying the titanium white byproduct ferrous sulfate heptahydrate. The recrystallization method is an important separation and purification method, zhang Keyu and the like (2017) purify a titanium white byproduct ferrous sulfate by using a crystallization method, and the experimental method comprises the following steps: weighing a certain amount of raw material ferrous sulfate, placing the raw material ferrous sulfate in a beaker, adding deionized water in a corresponding proportion, heating to a certain temperature, cooling the solution to a certain temperature to fully crystallize the solute after the solute is completely dissolved, keeping for a certain time, and performing suction filtration and separation to obtain ferrous sulfate crystals. Repeating the steps to carry out crystallization and purification for many times. The crystallized product is dried in a forced air drying oven and is loaded to be tested. The result shows that the ferrous sulfate particles prepared by purification by the crystallization method have high crystallinity, good crystal grain appearance and low impurity content. Through the research on the influence of the crystallization temperature, the crystallization frequency and the pH value on the purification of ferrous sulfate crystals, the method finds that when the dissolution temperature is 60 ℃, the crystallization temperature is 10 ℃ and the pH value is 2, and 3 times of crystallization are adopted, impurities can be effectively removed, and the titanium white byproduct ferrous sulfate is purified. Yu Wang et al (2016) investigated the recrystallization of ferrous sulfate for its hydrothermal method of preparation of alpha-Fe 2 O 3 The influence of the particles, the research result shows that: the dissolution temperature is 64 ℃, the crystallization temperature is 10 ℃, and after 2 times of recrystallization, the mass fraction of impurities in the obtained product is less than 0.1 percent, but the method has the following problems: the crystallization temperature is too high, the impurity content of the purified ferrous sulfate serving as a titanium white byproduct is high, and the purification effect is poor.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a recrystallization purification process of a titanium dioxide by-product ferrous sulfate.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a recrystallization purification process of titanium dioxide byproduct ferrous sulfate comprises the following steps:
1) Adding deionized water in a corresponding proportion into ferrous sulfate heptahydrate, heating to 65-105 ℃, stirring and dissolving to prepare a saturated solution;
2) Filtering, removing solid phase impurities, adjusting pH value to 1-3 to obtain clear solution, performing freeze crystallization on the obtained clear solution, controlling the temperature of the freeze crystallization at 0-10 ℃, performing freeze crystallization for 2-3 times to recrystallize dissolved ferrous sulfate out of the solution, performing vacuum filtration or filter pressing or filtering, and separating to obtain ferrous sulfate crystals;
3) Drying the ferrous sulfate crystal obtained by separation in the step 2) to ensure that the free water content of the dried ferrous sulfate is less than or equal to 10-15%, and then sieving the dried ferrous sulfate by a 200-mesh sieve and a 700-mesh sieve respectively to obtain the sieved ferrous sulfate.
Further, in the step 1), the solid-to-liquid ratio of the ferrous sulfate heptahydrate to the deionized water is 1:3.
further, in the step 1), heating to 65 ℃, stirring and dissolving to prepare a saturated solution.
Further, in the step 2), the temperature of the frozen crystals is controlled at 5 ℃, and the time of the frozen crystals is controlled at 2h.
Further, in the step 3), the free water content of the dried ferrous sulfate is less than or equal to 10%.
Further, in the step 3), the impurity removal rate of the screened ferrous sulfate is not lower than 99%.
Compared with the prior art, the invention has the beneficial effects that:
(1) The method can effectively remove impurities and purify the ferrous sulfate as a titanium white byproduct, and provides data reference for industrial application.
(2) The recrystallization method has mature process, simple and reliable equipment, and the purification effect can adjust the recrystallization times according to the requirements of products.
(3) The filtered ferrous sulfate solution can be utilized, and zero emission is realized really.
Detailed Description
The invention is further described with reference to specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Modifications or substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and scope of the invention. In the following examples, unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
The ferrous sulfate heptahydrate in the following examples was obtained from Jiangsu Yuxing science and technology, inc.
Example 1
A recrystallization purification process of titanium dioxide byproduct ferrous sulfate comprises the following steps:
1) Adding ferrous sulfate heptahydrate into a mixture with a solid-liquid ratio of 1:3, heating the deionized water to 65 ℃, stirring and dissolving to prepare a saturated solution;
2) Filtering, removing solid-phase impurities, adjusting the pH value to 2 to obtain a clear solution, performing freeze crystallization on the obtained clear solution, controlling the temperature of the freeze crystallization to be 5 ℃, performing freeze crystallization for 2 times to recrystallize dissolved ferrous sulfate out of the solution, performing vacuum filtration or filter pressing or filtering, and separating to obtain ferrous sulfate crystals;
3) Drying the ferrous sulfate crystal obtained by separation in the step 2) to ensure that the free water content of the dried ferrous sulfate is less than or equal to 10-15%, and then sieving the dried ferrous sulfate by a 200-mesh sieve and a 700-mesh sieve respectively to obtain the sieved ferrous sulfate.
Example 2
A recrystallization purification process of titanium dioxide byproduct ferrous sulfate comprises the following steps:
1) Adding ferrous sulfate heptahydrate into a mixture with a solid-liquid ratio of 1:3, heating the deionized water to 100 ℃, stirring and dissolving to prepare a saturated solution;
2) Filtering, removing solid-phase impurities, adjusting the pH value to 2 to obtain a clear solution, performing freeze crystallization on the obtained clear solution, controlling the temperature of the freeze crystallization to be 5 ℃, performing freeze crystallization for 2 times to recrystallize dissolved ferrous sulfate out of the solution, performing vacuum filtration or filter pressing or filtering, and separating to obtain ferrous sulfate crystals;
3) Drying the ferrous sulfate crystal obtained by separation in the step 2) to ensure that the free water content of the dried ferrous sulfate is less than or equal to 10-15%, and then sieving the dried ferrous sulfate by a 200-mesh sieve and a 700-mesh sieve respectively to obtain the sieved ferrous sulfate.
Example 3
A recrystallization purification process of titanium dioxide byproduct ferrous sulfate comprises the following steps:
1) Adding ferrous sulfate heptahydrate into a mixture with a solid-liquid ratio of 1:3, heating the deionized water to 65 ℃, stirring and dissolving to prepare a saturated solution;
2) Filtering, removing solid-phase impurities, adjusting the pH value to 2 to obtain a clear solution, performing freeze crystallization on the obtained clear solution, controlling the temperature of the freeze crystallization to be 0 ℃, performing freeze crystallization for 2 times to recrystallize dissolved ferrous sulfate out of the solution, performing vacuum filtration or filter pressing or filtering, and separating to obtain ferrous sulfate crystals;
3) Drying the ferrous sulfate crystal obtained by separation in the step 2) to ensure that the free water content of the dried ferrous sulfate is less than or equal to 10-15%, and then sieving the dried ferrous sulfate by a 200-mesh sieve and a 700-mesh sieve respectively to obtain the sieved ferrous sulfate.
Example 4
A recrystallization purification process of titanium dioxide byproduct ferrous sulfate comprises the following steps:
1) Adding deionized water into ferrous sulfate heptahydrate at a solid-to-liquid ratio of 1:3, heating to 65 ℃, and stirring for dissolving to prepare a saturated solution;
2) Filtering, removing solid-phase impurities, adjusting the pH value to 2 to obtain a clear solution, performing freeze crystallization on the obtained clear solution, controlling the temperature of the freeze crystallization to be 10 ℃, performing freeze crystallization for 2 times to recrystallize dissolved ferrous sulfate out of the solution, performing vacuum filtration or filter pressing or filtering, and separating to obtain ferrous sulfate crystals;
3) Drying the ferrous sulfate crystal obtained by separation in the step 2) to ensure that the free water content of the dried ferrous sulfate is less than or equal to 10-15%, and then sieving the dried ferrous sulfate by a 200-mesh sieve and a 700-mesh sieve respectively to obtain the sieved ferrous sulfate.
Comparative example
1) Adding deionized water into ferrous sulfate heptahydrate at a solid-to-liquid ratio of 1:3, heating to 65 ℃, stirring and dissolving to prepare saturated solution;
2) And cooling the saturated solution to 10 ℃, carrying out 2 times of freezing crystallization to recrystallize the dissolved ferrous sulfate out of the solution, carrying out vacuum filtration or filter pressing or filtration, and separating to obtain ferrous sulfate crystals.
The quality of the recrystallized product of each example is shown in table 1 below:
TABLE 1
| Mn | Mg | Ca | Al | Si | |
| Raw material | 648 | 3641 | 91 | 123 | 348 |
| Example 1 | 71 | 139 | 10 | 7 | 15 |
| Example 2 | 375 | 1585 | 46 | 52 | 83 |
| Example 3 | 222 | 621 | 26 | 27 | 83 |
| Example 4 | 130 | 247 | 14 | 11 | 41 |
| Comparative example 1 | 396 | 1675 | 56 | 61 | 95 |
Claims (6)
1. A recrystallization purification process of titanium dioxide byproduct ferrous sulfate is characterized by comprising the following steps:
1) Adding deionized water in a corresponding proportion into ferrous sulfate heptahydrate, heating to 65-105 ℃, stirring and dissolving to prepare a saturated solution;
2) Filtering, removing solid phase impurities, adjusting pH value to 1-3 to obtain clear solution, performing freeze crystallization on the obtained clear solution, controlling the temperature of the freeze crystallization at 0-10 ℃, performing freeze crystallization for 2-3 times to recrystallize dissolved ferrous sulfate out of the solution, performing vacuum filtration or filter pressing or filtering, and separating to obtain ferrous sulfate crystals;
3) Drying the ferrous sulfate crystal obtained by separation in the step 2) to ensure that the free water content of the dried ferrous sulfate is less than or equal to 10-15%, and then sieving the dried ferrous sulfate by a 200-mesh sieve and a 700-mesh sieve respectively to obtain the sieved ferrous sulfate.
2. The recrystallization purification process of the titanium dioxide byproduct ferrous sulfate according to claim 1, wherein in the step 1), the solid-to-liquid ratio of the ferrous sulfate heptahydrate to the deionized water is 1:3.
3. The recrystallization purification process of the titanium dioxide byproduct ferrous sulfate according to claim 1, characterized in that in the step 1), the temperature is heated to 65 ℃, and the saturated solution is prepared by stirring and dissolving.
4. The recrystallization purification process of the titanium dioxide by-product ferrous sulfate as claimed in claim 1, wherein in the step 2), the temperature of the frozen crystallization is controlled at 5 ℃, and the time of each frozen crystallization is controlled at 2h.
5. The recrystallization purification process of the titanium dioxide byproduct ferrous sulfate according to claim 1, wherein in the step 3), the free water content of the dried ferrous sulfate is less than or equal to 10%.
6. The recrystallization purification process of the titanium dioxide byproduct ferrous sulfate according to claim 1, wherein in the step 3), the impurity removal rate of the sieved ferrous sulfate is not lower than 99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211290879.9A CN115432739A (en) | 2022-10-20 | 2022-10-20 | Recrystallization purification process of titanium dioxide byproduct ferrous sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211290879.9A CN115432739A (en) | 2022-10-20 | 2022-10-20 | Recrystallization purification process of titanium dioxide byproduct ferrous sulfate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115432739A true CN115432739A (en) | 2022-12-06 |
Family
ID=84252175
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211290879.9A Pending CN115432739A (en) | 2022-10-20 | 2022-10-20 | Recrystallization purification process of titanium dioxide byproduct ferrous sulfate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115432739A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649588A (en) * | 2012-04-18 | 2012-08-29 | 四川大学 | Method for producing iron oxide red by using ferrous sulfate as titanium dioxide byproduct |
| CN105366736A (en) * | 2015-11-11 | 2016-03-02 | 何定 | Titanium white by-product copperas dehydration and drying method |
| US20200157696A1 (en) * | 2017-02-24 | 2020-05-21 | Vanadiumcorp Resources Inc. | Metallurgical And Chemical Processes For Recovering Vanadium And Iron Values From Vanadiferous Titanomagnetite And Vanadiferous Feedstocks |
| CN111847527A (en) * | 2020-08-11 | 2020-10-30 | 攀枝花学院 | Method for deeply purifying titanium white copperas |
-
2022
- 2022-10-20 CN CN202211290879.9A patent/CN115432739A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102649588A (en) * | 2012-04-18 | 2012-08-29 | 四川大学 | Method for producing iron oxide red by using ferrous sulfate as titanium dioxide byproduct |
| CN105366736A (en) * | 2015-11-11 | 2016-03-02 | 何定 | Titanium white by-product copperas dehydration and drying method |
| US20200157696A1 (en) * | 2017-02-24 | 2020-05-21 | Vanadiumcorp Resources Inc. | Metallurgical And Chemical Processes For Recovering Vanadium And Iron Values From Vanadiferous Titanomagnetite And Vanadiferous Feedstocks |
| CN111847527A (en) * | 2020-08-11 | 2020-10-30 | 攀枝花学院 | Method for deeply purifying titanium white copperas |
Non-Patent Citations (1)
| Title |
|---|
| 张克宇: "钛白副产硫酸亚铁制备电池级草酸亚铁的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》, pages 016 - 167 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112142081B (en) | Method for preparing battery-grade lithium carbonate by using lepidolite | |
| CN110950363A (en) | Production process of battery-grade lithium hydroxide monohydrate by applying novel combined calcium removal | |
| CN107473241B (en) | Preparation method of solid cyanamide | |
| CN110642886B (en) | Continuous production method of amino trimethylene phosphonic acid crystal | |
| CN113929148B (en) | Preparation method of superfine high-purity ammonium rhenate for rhenium powder reduction | |
| CN114890889A (en) | Purification method of electronic-grade citric acid | |
| CN112279279B (en) | Preparation method of battery grade lithium hydroxide monohydrate | |
| CN115432739A (en) | Recrystallization purification process of titanium dioxide byproduct ferrous sulfate | |
| CN110642887B (en) | Continuous production method of hydroxyethylidene diphosphonic acid crystal | |
| CN112679560A (en) | Kasugamycin crystallization process | |
| CN113735142A (en) | Method for preparing lithium sulfate monohydrate by using spodumene | |
| CN114573055A (en) | Preparation and application method of liquid nickel sulfate seed crystal | |
| CN114162841A (en) | Comprehensive treatment method for graphene oxide waste acid | |
| CN113277560A (en) | Preparation method of potassium fluoroniobate crystal | |
| CN113024383A (en) | Preparation method of high-purity p-nitrochlorobenzene | |
| KR20170036231A (en) | Purifying method of dodecanedioic acid | |
| CN117003262B (en) | Process for purifying sodium hexafluorophosphate by complex recrystallization | |
| CN114082216A (en) | Efficient evaporation crystallization method of calcium formate | |
| CN115893456B (en) | Flash evaporation crystallization method of lepidolite lithium extraction concentrated sodium potassium sulfate solution | |
| CN114804132B (en) | Sepiolite nanocrystallization treatment method | |
| CN110384195B (en) | Rice bran fresh-keeping method | |
| CN115849455A (en) | Preparation method of high-purity ferric hydroxide | |
| CN117446869A (en) | Ammonium rhenate purification method | |
| CN114478400A (en) | Crystallization method of azoxystrobin | |
| CN116514156A (en) | Electronic grade ceric ammonium nitrate crystallization purification method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |