CN111056573A - Continuous production method of crystalline ferric chloride - Google Patents
Continuous production method of crystalline ferric chloride Download PDFInfo
- Publication number
- CN111056573A CN111056573A CN201911300034.1A CN201911300034A CN111056573A CN 111056573 A CN111056573 A CN 111056573A CN 201911300034 A CN201911300034 A CN 201911300034A CN 111056573 A CN111056573 A CN 111056573A
- Authority
- CN
- China
- Prior art keywords
- concentrated solution
- crystallization kettle
- ferric chloride
- continuously
- stage 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
- C01G49/10—Halides
Abstract
The invention discloses a continuous production process of crystalline ferric chloride. The production process comprises the following steps: concentrating the low-concentration ferric chloride to 55-65% in an evaporation system; cooling the concentrated solution to 35-45 ℃ through a cooler, continuously transferring the concentrated solution into a first-stage crystallization kettle for cooling, and adding seed crystals into the first-stage crystallization kettle according to the proportion of adding 5-10 kg of crystalline ferric chloride into each cubic meter of the concentrated solution when the concentrated solution in the first-stage crystallization kettle is cooled to 25-35 ℃; the material added with the seed crystals is increased to 3-10% from the first-stage crystallization kettle and continuously transferred to the second-stage crystallization kettle, and then cooling and crystallization are continuously carried out; continuously transferring the concentrated solution with the crystal growing to 10-25% in the second-stage crystallization kettle into a third-stage crystallization kettle, and continuously cooling the concentrated solution in the third-stage crystallization kettle to reach the design proportion of 25-50% crystallization; and continuously transferring the concentrated solution reaching the designed crystallization ratio into an automatic centrifuge for continuous centrifugal separation to obtain granular crystallized ferric chloride products.
Description
Technical Field
The invention relates to the technical field of compound crystallization, in particular to a continuous production method of crystalline ferric chloride.
Background
Ferric chloride (ferric chloride),chemical formula (II)FeCl 3. Is a covalent compound. It is black brown crystal, has flake shape, melting point of 306 deg.C, boiling point of 315 deg.C, is easily soluble in water, and has strong effectWater absorptionIt can absorb moisture in air to deliquesce. Six FeCl3 are taken out from the aqueous solutionCrystal waterFor FeCl3 · 6H2O, ferric chloride hexahydrate is an orange-yellow crystal. Ferric chloride is of great importanceIron salts。
At present, the industrial production of solid ferric chloride in China is divided into anhydrous ferric chloride and ferric chloride hexahydrate, and the anhydrous ferric chloride is inconvenient to use due to caking in a product and large heat release of solution caused by the problems of a production process. The ferric chloride hexahydrate produced by the hanging bag centrifuge has low production quantity and high production cost due to the indirect nature of cooling crystallization and centrifugal separation operation, and influences the scale of industrial production and the popularization of the market.
Disclosure of Invention
The invention aims to solve the problem of low production in the existing intermittent production process of crystallized ferric chloride, and provides a production method for continuously cooling, crystallizing and continuously centrifuging a ferric chloride concentrated solution.
In order to solve the technical problems, the invention provides a continuous production method of crystalline ferric chloride, which comprises the following steps:
(1) concentrating the low-concentration ferric chloride into ferric chloride concentrated solution with concentration not lower than 55% in an evaporation system, and continuously evaporating and discharging;
(2) continuously cooling the ferric chloride concentrated solution to 35-45 ℃ through a cooler;
(3) continuously transferring the concentrated solution obtained in the step (2) into a first-stage crystallization kettle and continuously cooling to 25-35 ℃;
(4) during initial production, adding seed crystals into the concentrated solution obtained in the step (3) according to the proportion of 5-10 kg of crystalline ferric chloride seed crystals per cubic meter, and obtaining a concentrated solution with the crystal proportion of 3-10% in a first-stage crystallization kettle;
(5) continuously and stably transferring the concentrated solution obtained in the step (4) into a second-stage crystallization kettle, and continuously cooling to obtain a concentrated solution with a crystal proportion of 10-25% in the second-stage crystallization kettle;
(6) continuously and stably transferring the concentrated solution obtained in the step (5) into a third-stage crystallization kettle, and continuously cooling to obtain a concentrated solution with a crystal proportion of 25-50% in the third-stage crystallization kettle;
(7) and (4) continuously transferring the concentrated solution obtained in the step (6) into an automatic centrifuge for continuous centrifugal separation to obtain a crystallized ferric chloride product.
Preferably, in the step (1), the medium-low concentration ferric chloride is concentrated into 55-65% ferric chloride concentrated solution in an evaporation system.
Preferably, the step (2) comprises continuously cooling the ferric chloride concentrated solution to 35-45 ℃ by a graphite heat exchanger taking cooling inlet water as a cold medium and not higher than 20 ℃.
Preferably, in the step (3), the concentrated solution is continuously transferred to a first-stage crystallization kettle and is continuously cooled to 25-35 ℃, and the first crystallization kettle is an enamel kettle with jacket cooling water.
Preferably, in the step (5), the concentrated solution obtained in the step (4) is continuously and stably transferred to a second-stage crystallization kettle by a pump and is continuously cooled, the discharging speed of the first-stage crystallization kettle is equivalent to the feeding speed, and the concentrated solution with the crystal proportion of 10-25% is obtained in the second-stage crystallization kettle.
Preferably, in the step (6), the concentrated solution obtained in the step (5) is continuously and stably transferred to a third-stage crystallization kettle by a pump and is continuously cooled, the discharging speed of the second-stage crystallization kettle is equivalent to the feeding speed, and the concentrated solution with the crystal proportion of 25-50% is obtained in the third-stage crystallization kettle.
The continuous production method has the advantages of simple operation mode, stable production process and stable product quality, is suitable for large-batch industrial production, and can obviously improve the productivity of the crystallized ferric chloride.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to specific embodiments.
Example 1
1. And (3) feeding 29% ferric chloride into an evaporation system at the speed of 2t/h for concentration, and discharging when the concentration reaches 58% with the discharging speed of 1 t/h.
2. The evaporated concentrated solution is cooled by a graphite heat exchanger, the cooling water is fed into the graphite heat exchanger for 20 ℃, and the concentrated solution is discharged for 35 ℃.
3. And (3) opening the jacket of the first-stage crystallization kettle, introducing the concentrated solution passing through the graphite heat exchanger into the first-stage crystallization kettle, and continuously cooling to 26 ℃.
4. Adding crystalline ferric chloride seed crystals into the first-stage crystallization kettle in batches, wherein 5kg of crystalline ferric chloride seed crystals are added into each cubic meter of the first-stage crystallization kettle, and the crystallization proportion accounts for 10% of the total amount of the concentrated solution when the crystallization kettle is nearly full.
5. And (3) continuously cooling and crystallizing the material transferred from the first-stage crystallization kettle to the second-stage crystallization kettle, wherein the cooling water is introduced at 20 ℃, and the crystal reaches 25% of the total amount of the concentrated solution.
6. And (4) continuously cooling and crystallizing the material transferred from the second-stage crystallization kettle to the third-stage crystallization kettle, cooling and feeding water to 20 ℃, wherein the crystal amount reaches 45% of the total amount of the concentrated solution.
7. And (3) transferring the concentrated solution with the crystal amount reaching 45% into an automatic centrifuge by using a pump for centrifugal separation to produce a granular crystalline ferric chloride product, wherein the ferric chloride content is 59.5%, and the yield is 0.45 t/h.
Example 2
1. And (3) feeding 30% ferric chloride into an evaporation system at a speed of 4t/h for concentration, and discharging when the concentration reaches 60% at a discharge speed of 2 t/h.
2. The evaporated concentrated solution is cooled by a graphite heat exchanger, the cooling water is fed into the graphite heat exchanger for 20 ℃, and the concentrated solution is discharged for 38 ℃.
3. And (3) opening the jacket of the first-stage crystallization kettle, allowing the concentrated solution passing through the graphite heat exchanger to enter the first-stage crystallization kettle, and continuously cooling to 30 ℃.
4. Adding 8kg of crystallized ferric chloride crystals into the first-stage crystallization kettle in batches, wherein when the crystallization kettle is close to the full kettle, the crystallization proportion accounts for 8% of the total amount of the concentrated solution.
5. And (3) continuously cooling and crystallizing the material transferred from the first-stage crystallization kettle to the second-stage crystallization kettle, cooling and feeding water to 20 ℃, wherein the crystal amount reaches 20% of the total amount of the concentrated solution.
6. And (4) continuing cooling and crystallizing the material transferred from the second-stage crystallization kettle to the third-stage crystallization kettle, cooling and feeding water to 20 ℃, wherein the crystal amount reaches 40% of the total amount of the concentrated solution.
7. And (3) transferring the concentrated solution with the crystal amount of 40% into an automatic centrifuge by using a pump for centrifugal separation to produce a granular crystalline ferric chloride product, wherein the ferric chloride content is 59.2%, and the yield is 0.8 t/h.
Example 3
1. And (3) feeding 30% ferric chloride into an evaporation system at the speed of 6t/h for concentration, and discharging when the concentration reaches 64% at the discharging speed of 2.8 t/h.
2. The evaporated concentrated solution is cooled by a graphite heat exchanger, the cooling water is fed into the graphite heat exchanger for 20 ℃, and the concentrated solution is discharged for 45 ℃.
3. And (3) opening the jacket of the first-stage crystallization kettle, allowing the concentrated solution passing through the graphite heat exchanger to enter the first-stage crystallization kettle, and continuously cooling to 35 ℃.
4. Adding crystalline ferric chloride seed crystals into the first-stage crystallization kettle in batches, wherein 10kg of crystalline ferric chloride seed crystals are added into each cubic meter of the first-stage crystallization kettle, and the crystallization proportion accounts for 8 percent of the total amount of the concentrated solution when the crystallization kettle is nearly full.
5. And (3) continuously cooling and crystallizing the material transferred from the first-stage crystallization kettle to the second-stage crystallization kettle, wherein the cooling water is introduced at 20 ℃, and the crystal reaches 18 percent of the total amount of the concentrated solution.
6. And (4) continuing cooling and crystallizing the material transferred from the second-stage crystallization kettle to the third-stage crystallization kettle, cooling and feeding water to 20 ℃, wherein the crystal reaches 35% of the total amount of the concentrated solution.
7. And (3) transferring the concentrated solution with the crystal amount of 35% into an automatic centrifuge by using a pump for centrifugal separation to produce granular crystalline ferric chloride products, wherein the ferric chloride content is 63.5%, and the yield is 0.95 t/h.
Example 4
1. And (3) feeding 32% ferric chloride into an evaporation system at the speed of 6t/h for concentration, and discharging when the concentration reaches 60% at the discharging speed of 3.2 t/h.
2. The evaporated concentrated solution is cooled by a graphite heat exchanger, the cooling water is fed into the graphite heat exchanger for 18 ℃, and the concentrated solution is discharged for 40 ℃.
3. And (3) opening the jacket of the first-stage crystallization kettle, introducing the concentrated solution passing through the graphite heat exchanger into the first-stage crystallization kettle, and continuously cooling to 32 ℃.
4. Adding crystalline ferric chloride seed crystals into the first-stage crystallization kettle in batches, wherein 5kg of crystalline ferric chloride seed crystals are added into each cubic meter of the first-stage crystallization kettle, and the crystallization proportion accounts for 3% of the total amount of the concentrated solution when the crystallization kettle is nearly full.
5. And (3) continuously cooling and crystallizing the material transferred from the first-stage crystallization kettle to the second-stage crystallization kettle, wherein the cooling water is fed at 18 ℃, and the crystal reaches 10% of the total amount of the concentrated solution.
6. And (4) continuing cooling and crystallizing the material transferred from the second-stage crystallization kettle to the third-stage crystallization kettle, wherein the cooling water is fed into the second-stage crystallization kettle for 18 ℃, and the crystal reaches 25 percent of the total amount of the concentrated solution.
7. And (3) transferring the concentrated solution with the crystal amount of 25% into an automatic centrifuge by using a pump for centrifugal separation to produce granular crystalline ferric chloride products, wherein the ferric chloride content is 60.1%, and the yield is 0.7 t/h.
Example 5
1. And (3) feeding 32% ferric chloride into an evaporation system at the speed of 8t/h for concentration, and discharging when the concentration reaches 56% at the discharge speed of 4.6 t/h.
2. The evaporated concentrated solution is cooled by a graphite heat exchanger, the cooling water is fed into the graphite heat exchanger for 12 ℃, and the concentrated solution is discharged for 35 ℃.
3. And (3) opening the jacket of the first-stage crystallization kettle, allowing the concentrated solution passing through the graphite heat exchanger to enter the first-stage crystallization kettle, and continuously cooling to 25 ℃.
4. Adding crystalline ferric chloride seed crystals into the first-stage crystallization kettle in batches, wherein 10kg of crystalline ferric chloride seed crystals are added into each cubic meter of the first-stage crystallization kettle, and the crystallization proportion accounts for 10% of the total amount of the concentrated solution when the crystallization kettle is nearly full.
5. And (3) continuously cooling and crystallizing the material transferred from the first-stage crystallization kettle to the second-stage crystallization kettle, wherein the cooling water inlet temperature is 12 ℃, and the crystal amount reaches 25% of the total amount of the concentrated solution.
6. And (4) continuing cooling and crystallizing the material transferred from the second-stage crystallization kettle to the third-stage crystallization kettle, wherein the cooling water is fed into the second-stage crystallization kettle for 12 ℃, and the crystal reaches 50% of the total amount of the concentrated solution.
7. And (3) transferring the concentrated solution with the crystal amount of 50% into an automatic centrifuge by using a pump for centrifugal separation to produce a granular crystalline ferric chloride product, wherein the ferric chloride content is 59.1%, and the yield is 2.1 t/h.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (6)
1. A continuous production method of crystalline ferric chloride is characterized by comprising the following steps:
(1) concentrating the low-concentration ferric chloride into ferric chloride concentrated solution with concentration not lower than 55% in an evaporation system, and continuously evaporating and discharging;
(2) continuously cooling the ferric chloride concentrated solution to 35-45 ℃ through a cooler;
(3) continuously transferring the concentrated solution obtained in the step (2) into a first-stage crystallization kettle and continuously cooling to 25-35 ℃;
(4) during initial production, adding seed crystals into the concentrated solution obtained in the step (3) according to the proportion of 5-10 kg of crystalline ferric chloride seed crystals per cubic meter, and obtaining a concentrated solution with the crystal proportion of 3-10% in a first-stage crystallization kettle;
(5) continuously and stably transferring the concentrated solution obtained in the step (4) into a second-stage crystallization kettle, and continuously cooling to obtain a concentrated solution with a crystal proportion of 10-25% in the second-stage crystallization kettle;
(6) continuously and stably transferring the concentrated solution obtained in the step (5) into a third-stage crystallization kettle, and continuously cooling to obtain a concentrated solution with a crystal proportion of 25-50% in the third-stage crystallization kettle;
(7) and (4) continuously transferring the concentrated solution obtained in the step (6) into an automatic centrifuge for continuous centrifugal separation to obtain a crystallized ferric chloride product.
2. A continuous process for the production of crystalline ferric chloride as claimed in claim 1, wherein: and (1) concentrating the medium-low concentration ferric chloride into 55-65% ferric chloride concentrated solution in an evaporation system.
3. A continuous process for the production of crystalline ferric chloride as claimed in claim 1, wherein: and (2) continuously cooling the ferric chloride concentrated solution to 35-45 ℃ through a graphite heat exchanger taking cooling inlet water at the temperature of not higher than 20 ℃ as a cooling medium.
4. A continuous process for the production of crystalline ferric chloride as claimed in claim 1, wherein: and (3) continuously transferring the concentrated solution to a first-stage crystallization kettle and continuously cooling to 25-35 ℃, wherein the first crystallization kettle is an enamel kettle with jacket cooling water.
5. A continuous process for the production of crystalline ferric chloride as claimed in claim 1, wherein: and (5) continuously and stably transferring the concentrated solution obtained in the step (4) to a second-stage crystallization kettle by using a pump, and continuously cooling, wherein the discharging speed of the first-stage crystallization kettle is equivalent to the feeding speed, and the concentrated solution with the crystal proportion of 10-25% is obtained in the second-stage crystallization kettle.
6. A continuous process for the production of crystalline ferric chloride as claimed in claim 1, wherein: and (6) continuously and stably transferring the concentrated solution obtained in the step (5) to a third-stage crystallization kettle by using a pump, and continuously cooling, wherein the discharging speed of the second-stage crystallization kettle is equivalent to the feeding speed, and the concentrated solution with the crystal proportion of 25-50% is obtained in the third-stage crystallization kettle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911300034.1A CN111056573A (en) | 2019-12-16 | 2019-12-16 | Continuous production method of crystalline ferric chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911300034.1A CN111056573A (en) | 2019-12-16 | 2019-12-16 | Continuous production method of crystalline ferric chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111056573A true CN111056573A (en) | 2020-04-24 |
Family
ID=70301892
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911300034.1A Pending CN111056573A (en) | 2019-12-16 | 2019-12-16 | Continuous production method of crystalline ferric chloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111056573A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113476885A (en) * | 2021-07-08 | 2021-10-08 | 斯瑞尔环境科技股份有限公司 | Method for continuously producing iron salt crystals |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2855495Y (en) * | 2005-11-16 | 2007-01-10 | 南京师范大学 | Multi-stage segamental continuous crystallizer |
| CN102553291A (en) * | 2012-02-29 | 2012-07-11 | 中粮生物化学（安徽）股份有限公司 | Cooling crystallization method |
| CN102643169A (en) * | 2012-04-25 | 2012-08-22 | 北京化工大学 | Method for purifying resorcinol by means of continuous crystallization |
| CN102701290A (en) * | 2012-06-19 | 2012-10-03 | 惠州市斯瑞尔环境化工有限公司 | Method for preparing blocky ferric trichloride |
| CN103183390A (en) * | 2013-04-19 | 2013-07-03 | 绵阳天明磷化工有限公司 | Production process of high purity ferric trichloride |
| CN106745321A (en) * | 2016-12-27 | 2017-05-31 | 唐山市斯瑞尔化工有限公司 | The production method of graininess Iron(III) chloride hexahydrate |
| CN110451582A (en) * | 2019-08-09 | 2019-11-15 | 斯瑞尔环境科技股份有限公司 | A kind of ferric trichloride quantity-produced method |
-
2019
- 2019-12-16 CN CN201911300034.1A patent/CN111056573A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2855495Y (en) * | 2005-11-16 | 2007-01-10 | 南京师范大学 | Multi-stage segamental continuous crystallizer |
| CN102553291A (en) * | 2012-02-29 | 2012-07-11 | 中粮生物化学（安徽）股份有限公司 | Cooling crystallization method |
| CN102643169A (en) * | 2012-04-25 | 2012-08-22 | 北京化工大学 | Method for purifying resorcinol by means of continuous crystallization |
| CN102701290A (en) * | 2012-06-19 | 2012-10-03 | 惠州市斯瑞尔环境化工有限公司 | Method for preparing blocky ferric trichloride |
| CN103183390A (en) * | 2013-04-19 | 2013-07-03 | 绵阳天明磷化工有限公司 | Production process of high purity ferric trichloride |
| CN106745321A (en) * | 2016-12-27 | 2017-05-31 | 唐山市斯瑞尔化工有限公司 | The production method of graininess Iron(III) chloride hexahydrate |
| CN110451582A (en) * | 2019-08-09 | 2019-11-15 | 斯瑞尔环境科技股份有限公司 | A kind of ferric trichloride quantity-produced method |
Non-Patent Citations (1)
| Title |
|---|
| 陈冠荣等: "《化工百科全书》", 30 September 1994, 化学工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113476885A (en) * | 2021-07-08 | 2021-10-08 | 斯瑞尔环境科技股份有限公司 | Method for continuously producing iron salt crystals |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102701290B (en) | Method for preparing blocky ferric trichloride | |
| WO2018113478A1 (en) | Method for producing lithium hydroxide monohydrate using lithium carbonate as raw material | |
| CN102992957B (en) | Solvent-out crystallization method of erythritol | |
| CN1312030C (en) | Method for purifying wet-process phosphoric acid by crystallization | |
| CN105236439B (en) | A kind of bulky grain boric acid and its continuous coo1ing recrystallization preparation technology and device | |
| CN106629784B (en) | A kind of technique of adding halogen method production rice-shaped crystallization potassium nitrate | |
| CN111056573A (en) | Continuous production method of crystalline ferric chloride | |
| CN103496715A (en) | Method for producing industrial grade superior ammonium sulfate through coked coarse ammonium sulfate dilution crystallization | |
| CN110683563B (en) | LiPF6 production process and production system | |
| CN103466664A (en) | Fully-automatic production line type potassium nitrate recovering process | |
| CN101269804B (en) | Method for producing high-purity phosphoric acid crystal | |
| CN106987608B (en) | Dynamic crystallization method of calcium gluconate | |
| US3005684A (en) | Process for making ammonium bifluoride | |
| CN115557980B (en) | Synthesis and purification process of sodium bisoxalato | |
| CN112552167A (en) | Preparation method of calcium gluconate | |
| CN107673946A (en) | The method that continuity method isomerization produces durol | |
| CN102126756B (en) | Method for producing industrial grade ammonium paramolybdate | |
| CN103265072A (en) | Method for crystallizing zirconium oxychloride | |
| CN106349057A (en) | Treatment process for deferrization purification of sodium citrate mother liquor | |
| CN108609635A (en) | A kind of method prepared by potassium nitrate | |
| CN101987747A (en) | Preparation method of reagent-grade ammonium molybdate | |
| CN103569980A (en) | Production method of solid phosphoric acid | |
| CN112939032A (en) | Method for preparing potassium nitrate by nitric acid method | |
| CN109437300B (en) | Method for preparing high-purity sodium metavanadate by solid-phase method | |
| CN208413873U (en) | A kind of device producing sodium bicarbonate |
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 | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Ding Decai Inventor after: Zhou Xiaojiang Inventor after: Chen Xiaozhe Inventor after: Zhu Hao Inventor after: Wang Quanyong Inventor after: Cao Yongfei Inventor before: Ding Decai Inventor before: Zhou Xiaojiang Inventor before: Chen Xiaozhe Inventor before: Zhu Hao Inventor before: Wang Quanyong Inventor before: Cao Yongfei |
|
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200424 |