CN112850797A - Production method of ultrapure ferric trichloride - Google Patents
Production method of ultrapure ferric trichloride Download PDFInfo
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- CN112850797A CN112850797A CN202011157602.XA CN202011157602A CN112850797A CN 112850797 A CN112850797 A CN 112850797A CN 202011157602 A CN202011157602 A CN 202011157602A CN 112850797 A CN112850797 A CN 112850797A
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- ferric trichloride
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- ferrous chloride
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- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 title claims abstract description 77
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 32
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 107
- 229960002089 ferrous chloride Drugs 0.000 claims abstract description 44
- 229910052742 iron Inorganic materials 0.000 claims abstract description 44
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 28
- 230000003647 oxidation Effects 0.000 claims abstract description 19
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims description 11
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- -1 electromagnet Chemical compound 0.000 claims description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical class [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 25
- 239000002994 raw material Substances 0.000 abstract description 6
- 238000005530 etching Methods 0.000 abstract description 5
- 239000003651 drinking water Substances 0.000 abstract description 4
- 235000020188 drinking water Nutrition 0.000 abstract description 4
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 3
- 239000000543 intermediate Substances 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 15
- 238000002156 mixing Methods 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 229910001385 heavy metal Inorganic materials 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000010309 melting process Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 229940032296 ferric chloride Drugs 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 159000000014 iron salts Chemical class 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003883 substance clean up Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a production method of ultrapure ferric trichloride, which comprises the steps of adding iron-containing chloride into elementary iron for reaction, filtering to obtain ferrous chloride, and oxidizing the ferrous chloride into ferric trichloride; reacting ferric trichloride with elementary iron, filtering to obtain an ultra-pure ferrous chloride solution, and oxidizing to obtain ultra-pure ferric trichloride; if the obtained ultrapure ferric trichloride can not meet the requirements, the processes of iron melting and oxidation can be repeated for many times, so that the product meets the specific requirements. The invention has the advantages of economic and easily obtained production raw materials, simple process, less equipment investment and high production safety. The ferric trichloride produced by the process has the advantages of low acidity, low impurity, high content and the like, and can be applied to the fields of drinking water treatment, medical intermediates, analysis and test, precision etching and the like.
Description
Technical Field
The invention relates to the technical field of compound purification, in particular to a production method of ultrapure ferric trichloride.
Background
Ferric chloride is an important iron salt, mainly used for metal etching, sewage treatment, printing and dyeing roller engraving, electronic industry circuit boards, building industry for preparing concrete, inorganic industry for manufacturing other iron salts and ink, dye industry for preparing oxidant when dyeing with landfills, organic industry for preparing catalyst, oxidant and chlorinating agent, etc.
The ferric trichloride with high purity requirement is mainly applied to the fields of drinking water treatment, medical intermediates, analysis and test, precision etching and the like. Different countries and industries respectively put forward different index requirements according to different requirements on the purity of ferric trichloride. The conventional method for producing high-purity ferric trichloride by using hydrochloric acid synthesized by high-purity iron processing industry has the defects of extremely high production cost, tiny profit, great potential safety hazard due to the generation of a large amount of flammable and combustible hydrogen and limitation on the actual production application of the process.
CN 110002509A discloses a ferric trichloride crystal and a preparation method and application thereof. The invention utilizes the extraction characteristic of the ferric extractant on the ferric iron to achieve the purpose of purification, has better purification effect, but can ensure the extraction unicity of the ferric extractant on the iron element only by strictly controlling the acidity, otherwise, the content of various heavy metal impurities in the ferric trichloride is higher, and the dilute acid is needed during back extraction, thus easily causing the over-standard acidity in the ferric trichloride product.
CN 103183390A discloses a production process of high-purity ferric trichloride. The method takes industrial-grade anhydrous ferric trichloride as a raw material, dissolves the raw material in water, controls the concentration to be within 55-58%, cools and crystallizes to separate out ferric trichloride crystals, wherein the content of lead, sodium and cadmium elements is below 20ppm, and the content of copper, manganese and nickel elements is within 50ppm, so that the method can only meet the requirement of the electronic industry, and is far away from the requirement that many indexes of ultra-pure ferric trichloride are lower than 1 ppm.
CN 110902727A discloses a production process of a pharmaceutical grade ferric trichloride crystal. The invention improves the purity of the product by optimizing the raw materials and combining the recrystallized ferrous chloride and the crystallized ferric chloride. The ferric trichloride crystal obtained by the process has high purity, can stably reach the standard of pharmaceutical grade ferric trichloride at home and abroad, and also can reach a reagent grade ferric trichloride crystal with relatively low purity requirement, but has relatively high production cost due to high purity requirement.
The method for increasing the concentration of ferric trichloride mainly comprises four processes of evaporation concentration, addition of anhydrous or hexahydrate ferric trichloride and addition of solid ferrous chloride, and then oxidation of the added solid ferrous chloride into ferric trichloride. When the product requires low acidity, ferric trichloride is easily hydrolyzed into ferric hydroxide when the concentration is increased by an evaporation concentration process, so that the quality and the use of the product are influenced; the method of adding solid ferrous chloride for concentration is adopted, because the solid ferrous chloride is easily oxidized into ferric trichloride, when the ferric trichloride is dissolved in a low-acidity solution, the ferric trichloride is hydrolyzed, and the hydrolysate cannot be effectively removed in a filter pressing process; impurities are introduced when sodium chlorate or hydrogen peroxide is added to reduce acidity.
There are two common methods for reducing heavy metal impurities in solution systems: adding a sulfide to form an insoluble metal sulfide, and adding a basic substance such as sodium hydroxide or aqueous ammonia to precipitate a metal hydroxide. Both methods introduce impurities into the system solution, which is not beneficial to the purification of the product.
Ferric trichloride used in the fields of drinking water treatment, medical intermediates, analytical tests, precision etching and the like all require low acidity and high purity, so that a production method of low-cost, low-acidity, high-purity and high-concentration ferric trichloride needs to be developed to meet the requirement of the market on high-end ferric trichloride.
Disclosure of Invention
The invention aims to produce low-acidity ferric trichloride by using iron-containing chloride as a raw material, improve the concentration and purity of the ferric trichloride, provide a safe, economic and efficient production process, and enable product indexes to meet the requirements of drinking water grade, pharmaceutical grade, reagent grade or precise etching agents.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a production method of ultrapure ferric trichloride comprises the following steps:
s1, adding the iron-containing chloride liquid into the elementary iron for reaction, and filtering to obtain a ferrous chloride solution;
s2, oxidizing the ferrous chloride solution into ferric chloride solution;
s3, adding elementary substance iron into the ferric trichloride solution for reaction, and filtering to obtain an ultra-pure ferrous chloride solution;
s4 oxidizes the ultrapure ferrous chloride solution into an ultrapure ferric trichloride solution.
Further, in step S1, the iron-containing chloride may be one of ferrous chloride, ferric chloride, ferrous chloride and a mixture of ferric chloride;the substance containing simple substance iron can be sheet iron, ring iron, electromagnet, iron powder, oxide skin, etc. The more excessive elementary iron, the finer the particles, the larger the contact area and the higher the solution temperature, and Fe3+The faster the reaction with Fe, the faster and more thorough the reaction between hydrochloric acid and Fe, and the faster and more thorough the replacement reaction between heavy metal impurities and elemental iron, so the excess iron powder is preferably used to improve the production efficiency, the amount of the added iron powder is 10-200% of the mass of the solution, but the excessive iron powder increases the difficulty of the subsequent filter pressing, and the added elemental iron is comprehensively considered to be 30-50% of the mass of the solution. Meanwhile, the reaction time is prolonged, so that impurity metals and simple substance iron can be subjected to displacement reaction, and the content of the impurity heavy metals is further reduced. The technical means is beneficial to improving the iron content in the solution, reducing the acidity to be below 0.2 percent and reducing most of toxic impurity metals to be below 1ppm, the acidity in the ferrous chloride is generally less than 3 percent, only a small amount of hydrogen is generated, which is about 10 percent of that of the industrial hydrochloric acid, and the potential safety hazard in the production is greatly eliminated, and four effects are achieved at a stroke.
Further, the oxidation manner in step S2 may be a plurality of oxidation manners such as oxygen oxidation, air oxidation, ozone oxidation, sodium chlorate oxidation, hydrogen peroxide oxidation, and the like, and most preferably chlorine oxidation with the least introduced impurities.
Further, in step S3, the main purpose of the iron-melting process is to increase the total iron content of the solution, which can quickly increase the iron content from 9% -15% to 14-22%, and reduce the acidity and impurity metals again.
The method for improving the concentration in the iron melting process is simple, high in production efficiency and low in cost, and can finish the concentration process within 10-30 min, which is incomparable with the evaporation concentration process.
The temperature is preferably kept at 40-100 ℃ during iron melting to ensure a high reaction rate. The optimal reaction time is 1-12 h, if the reaction time is too short, heavy metals are not completely removed, if the reaction time is too long, the solution surface is easily oxidized into ferric trichloride, and hydrolysis occurs under the condition of low acidity, so that the product is precipitated, the difficulty of subsequent filter pressing is increased, and the iron content is reduced. In the process of continuously reducing the acidity, the impurity heavy metal begins to be hydrolyzed, precipitated and replaced into a simple substance to separate out a solution system, so that the aim of removing the impurity is fulfilled. The single process skillfully utilizes two impurity removing principles, does not introduce new impurities, and can remove impurity metals more thoroughly so as to ensure the purity of products.
In addition, ferrous chloride and simple substance iron with low impurity content are preferably selected according to the index requirement of the product, so that the iron melting times can be effectively reduced, the production efficiency is improved, and the production cost is reduced. When the iron powder is used, the iron powder is required to be prevented from being accumulated together in a stirring mode, the stirring speed is preferably the stirring speed, all the iron powder can be stirred, the iron powder is fully contacted with the solution, and if the iron powder is elementary substance iron with large volume such as sheet iron or ring iron, the solute transfer rate can be increased in a solution circulation mode.
Further, in step S4, chlorine gas oxidation is preferably performed to reduce the content of impurities in the product.
In summary, when the product requires low acidity, it is better to increase the concentration and purity of the product by the iron-melting process.
The invention has the following beneficial effects:
1. the raw materials are economical and easy to obtain, the purification method is simple to operate, the concentration is improved, the acidity is reduced, the impurities are removed in one step, and the technical effect is good.
2. Only a small amount of hydrogen is generated, and the safety risk of production is greatly reduced.
3. The equipment investment is low, the product quality is high, and high economic value is generated.
4. When the product requires low acidity, the concentration of ferric trichloride can be effectively improved without introducing impurities, which is a technical effect that other processes cannot achieve.
5. No new impurities are introduced in the impurity removing process, so that the purity of the product is further improved.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments.
Example 1
A production method of ultrapure ferric trichloride is characterized by comprising the following steps:
S11kg of ferrous chloride liquid A0Adding 0.3kg of reduced iron powder, reacting for 5h at normal temperature at the rotating speed of a stirrer of 200r/min, and filtering to obtain a ferrous chloride solution A1；
S2 mixing the ferrous chloride solution A1Oxidizing into ferric trichloride solution A;
s3 adding 0.3kg of reduced iron powder into the ferric trichloride solution A, stirring at the speed of 200r/min, reacting for 1h without heating, and filtering to obtain ultrapure ferrous chloride solution B1；
S4 mixing the super-pure ferrous chloride solution B1Oxidized into ultrapure ferric trichloride solution B.
The experimental data are shown in the following table.
Example 2
A production method of ultrapure ferric trichloride is characterized by comprising the following steps:
s1 mixing ferrous chloride liquid A1 kg0Adding 0.3kg of reduced iron powder, stirring at 200r/min, reacting in water bath at 60 deg.C for 2h, and filtering to obtain ferrous chloride solution C1；
S2 mixing ferrous chloride solution C1Oxidizing into ferric trichloride solution C;
s3 adding 0.3kg of reduced iron powder into the ferric trichloride solution C, stirring at 200r/min, reacting in water bath at 60 deg.C for 1h, and filtering to obtain ultrapure ferrous chloride solution D1；
S4 mixing the ultrapure ferrous chloride solution D1Oxidized into ultrapure ferric trichloride solution D.
The experimental data are shown in the following table.
Example 3
A production method of ultrapure ferric trichloride is characterized by comprising the following steps:
s1 is to1kg of ferrous chloride liquid A0Adding 0.5kg of reduced iron powder, stirring at 200r/min, reacting in water bath at 90 deg.C for 1h, and filtering to obtain ferrous chloride solution E1；
S2 mixing the ferrous chloride solution E1Oxidizing into ferric trichloride E;
s3 adding 0.5kg of reduced iron powder into the ferric trichloride solution E, stirring at 200r/min, reacting in water bath at 90 ℃ for 1h, and filtering to obtain ultrapure ferrous chloride solution F1；
S4 preparing ultra-pure ferrous chloride solution F1Oxidized into ultrapure ferric trichloride solution F.
The experimental data are shown in the following table.
Example 4
A production method of ultrapure ferric trichloride is characterized by comprising the following steps:
s1 mixing ferrous chloride liquid 0.5kg and ferric chloride solution 0.5kg to obtain B0Adding 1.5kg of iron flakes, heating the solution to 105-110 ℃ at the rotating speed of a stirrer of 100r/min for reacting for 2h, and filtering to obtain a ferrous chloride solution G1；
S2 mixing ferrous chloride solution G1Oxidizing into ferric trichloride solution G;
s3 adding 2kg of ring iron into the ferric trichloride solution G, stirring at 150r/min, reacting in water bath at 30 ℃ for 1H, and filtering to obtain ultrapure ferrous chloride solution H1；
S4 mixing the ultrapure ferrous chloride solution H1Oxidized into ultrapure ferric trichloride solution H.
S5 adding 0.03kg of ring iron into the ultrapure ferric chloride solution H, reacting in a water bath at 90 ℃ for 0.5H at the rotating speed of a stirrer of 150r/min, and filtering to obtain the ultrapure ferrous chloride solution I1；
S6 preparing ultra-pure ferrous chloride solution I1Oxidized into ultrapure ferric trichloride solution I.
The experimental data are shown in the following table.
The experimental data of examples 1-4 show that: the method can meet the index requirements of different ferric trichloride contents and impurity metals by flexibly changing the conditions of the addition amount of the simple substance iron, the reaction temperature, the iron melting times and the like so as to meet different market requirements.
In the invention, the simple substance iron has rich sources and can be iron-containing leftover materials discarded by various units. The metal impurities which can be removed at one time are nearly 20, and the metal of various impurities can be reduced to below 1ppm, thus meeting the requirements of various high-purity ferric trichloride. Simple process equipment, relatively low cost, safe production and operation and popularization value.
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 (10)
1. A production method of ultrapure ferric trichloride is characterized by comprising the following steps:
s1, adding the iron-containing chloride liquid into the elementary iron for reaction, and filtering to obtain a ferrous chloride solution;
s2, oxidizing the ferrous chloride solution into ferric chloride solution;
s3, adding elementary substance iron into the ferric trichloride solution for reaction, and filtering to obtain an ultra-pure ferrous chloride solution;
s4 oxidizes the ultrapure ferrous chloride solution into an ultrapure ferric trichloride solution.
2. The method of claim 1, wherein the iron-containing chloride in step S1 is one of ferrous chloride, ferric chloride, a mixture of ferrous chloride and ferric chloride.
3. The method of claim 1, wherein the elemental iron in step S1 is one or more selected from the group consisting of sheet iron, ring iron, electromagnet, iron powder, and oxide skin.
4. The method for producing ultrapure ferric trichloride of claim 1 wherein said oxidation in steps S2, S4 is one or more combinations of oxygen oxidation, air oxidation, ozone oxidation, sodium chlorate oxidation, hydrogen peroxide oxidation and chlorine oxidation.
5. The method of claim 4, wherein the step S2 or S4 is carried out by chlorine oxidation.
6. The method for producing ultrapure iron trichloride according to claim 1 wherein the amount of elemental iron added in steps S1, S3 is 10% to 200% by weight of the solution.
7. The method of claim 6, wherein the amount of elemental iron added in steps S1 and S3 is 30-50% by weight of the solution.
8. The method for producing ultrapure ferric trichloride according to claim 1, wherein the reaction temperature in steps S1 and S3 is 30-110 ℃ and the reaction time is 1-12 hours.
9. The method for producing ultrapure iron trichloride according to claim 8, wherein the reaction temperature in steps S1 and S3 is 60 to 90 ℃.
10. The method for producing ultrapure iron trichloride of claim 1 wherein in step S4, if the ultrapure iron trichloride solution fails to meet the specification requirements of the product, steps S3 and S4 are repeated a plurality of times to meet the specification of the product.
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| CN114014372A (en) * | 2021-11-26 | 2022-02-08 | 吉林省益能科技有限公司 | Preparation process of ferric trichloride solution |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62192588A (en) * | 1986-02-19 | 1987-08-24 | Toagosei Chem Ind Co Ltd | Removing method for chromium and nickel contained in iron chloride aqueous solution |
| JPH05255869A (en) * | 1992-03-10 | 1993-10-05 | Toagosei Chem Ind Co Ltd | Method for removing nickel in aqueous nickel-containing iron chloride solution |
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| CN111018192A (en) * | 2019-12-30 | 2020-04-17 | 斯瑞尔环境科技股份有限公司 | Method for preparing high-purity ferrous iron by using heavy metal ions in ferrous solution precipitated by sodium sulfide solid |
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| JPS62192588A (en) * | 1986-02-19 | 1987-08-24 | Toagosei Chem Ind Co Ltd | Removing method for chromium and nickel contained in iron chloride aqueous solution |
| JPH05255869A (en) * | 1992-03-10 | 1993-10-05 | Toagosei Chem Ind Co Ltd | Method for removing nickel in aqueous nickel-containing iron chloride solution |
| JPH0692643A (en) * | 1992-09-14 | 1994-04-05 | Daiso Co Ltd | Production of ferric chloride solution |
| KR960010531A (en) * | 1994-09-15 | 1996-04-20 | 김만제 | Method for preparing ferric chloride aqueous solution |
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| 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 |
| CN111018192A (en) * | 2019-12-30 | 2020-04-17 | 斯瑞尔环境科技股份有限公司 | Method for preparing high-purity ferrous iron by using heavy metal ions in ferrous solution precipitated by sodium sulfide solid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114014372A (en) * | 2021-11-26 | 2022-02-08 | 吉林省益能科技有限公司 | Preparation process of ferric trichloride solution |
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