CN114105186A - Pyrogenic separation method of chloride - Google Patents

Pyrogenic separation method of chloride Download PDF

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Publication number
CN114105186A
CN114105186A CN202110804373.4A CN202110804373A CN114105186A CN 114105186 A CN114105186 A CN 114105186A CN 202110804373 A CN202110804373 A CN 202110804373A CN 114105186 A CN114105186 A CN 114105186A
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chloride
zinc
separation
ammonium chloride
zinc chloride
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甘渭佳
甘国昕
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G9/00—Compounds of zinc
    • C01G9/04—Halides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/16—Halides of ammonium
    • C01C1/164—Ammonium chloride
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00—Halides of sodium, potassium or alkali metals in general
    • C01D3/04—Chlorides
    • C01D3/08—Preparation by working up natural or industrial salt mixtures or siliceous minerals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/20—Obtaining zinc otherwise than by distilling
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B19/00—Obtaining zinc or zinc oxide
    • C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001—Dry processes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention discloses a pyrogenic separation method of chloride, which comprises the following steps: the method comprises the following steps: putting a material containing ammonium chloride, zinc chloride, potassium chloride and sodium chloride into a rotary kiln, heating, wherein the heating temperature is higher than the boiling point of the ammonium chloride but lower than the boiling point of the zinc chloride, volatilizing the ammonium chloride in the material to form smoke, and cooling and collecting the ammonium chloride in the smoke; step two: continuously heating the solid calcined in the step one, wherein the heating temperature is higher than the boiling point of zinc chloride but lower than the boiling point of potassium chloride, volatilizing the zinc chloride in the material to form smoke, and cooling and collecting the zinc chloride in the smoke; step three: and D, conveying the solid calcined in the step two to a potassium chloride and sodium chloride wet separation system to separate potassium chloride, sodium chloride and other components in the solid. The pyrogenic separation method of the chloride aims to solve the problems of high production cost and incomplete separation of the chloride in the existing industrial byproduct by wet separation.

Description

Pyrogenic separation method of chloride
Technical Field
The invention relates to the technical field of industrial waste recycling, in particular to a pyrogenic separation method of chloride.
Background
The smelting process of the nonferrous industry can generate byproducts simultaneously containing soluble salts such as zinc chloride, ammonium chloride, sodium chloride, potassium chloride and the like with certain components, the chlorides are respectively separated by a wet method at present, the soluble salts such as the zinc chloride, the ammonium chloride, the sodium chloride, the potassium chloride and the like are similar in properties in the solution, the chlorides are difficult to be completely separated by the wet method, the components are difficult to be completely separated, the components are required to be converted for many times, the production cost is high, the industrial-grade (battery-grade) zinc chloride cannot be produced, only products with lower purity can be obtained, the actual income is lower, and therefore, most of the byproducts containing the chlorides are finally treated as industrial waste materials and are difficult to be better utilized.
Disclosure of Invention
The invention discloses a pyrogenic separation method of chloride, aiming at the problems of high production cost and incomplete separation of the chloride in the existing industrial byproduct by wet separation.
The invention discloses a pyrogenic separation method of chloride, which comprises the following steps:
the method comprises the following steps: putting a material containing ammonium chloride, zinc chloride, potassium chloride and sodium chloride into a rotary kiln, heating, wherein the heating temperature is higher than the boiling point of the ammonium chloride but lower than the boiling point of the zinc chloride, volatilizing the ammonium chloride in the material to form smoke, and cooling and collecting the ammonium chloride in the smoke;
step two: continuously heating the solid calcined in the step one, wherein the heating temperature is higher than the boiling point of zinc chloride but lower than the boiling point of potassium chloride, volatilizing the zinc chloride in the material to form smoke, and cooling and collecting the zinc chloride in the smoke;
step three: and D, conveying the solid calcined in the step two to a potassium chloride and sodium chloride wet separation system to separate potassium chloride, sodium chloride and other components in the solid.
Furthermore, in the first step, one or more modes of cooling gravity settling, water spraying dust removal and purification and wet electrostatic dust removal are adopted to recover the crude ammonium chloride product.
Further, in the first step, the recovered crude ammonium chloride is dissolved by a wet method, crystallized and concentrated to obtain high-purity ammonium chloride.
Further, in the first step, the heating temperature is 500-700 ℃.
Furthermore, in the second step, one or more modes of cooling gravity settling, water spraying dust removal and purification and wet electrostatic dust removal are adopted to recover the crude zinc chloride product.
Furthermore, In the second step, the recovered zinc chloride crude product is dissolved by a wet method, crystallized and concentrated to obtain high-purity zinc chloride, and valuable elements of Ag, Pb, In, Bi, Sn, Sb, Cd and Au are separated and recovered from the solution.
Further, in the second step, the heating temperature is 800-.
Further, in the third step, the other components in the solid include one or more of zinc oxide, lead oxide and aluminum oxide.
Further, before the first step, the material to be treated is heated at the temperature of over 1450 ℃ to separate ammonium chloride, zinc chloride, potassium chloride and sodium chloride from the material, and the smoke is cooled to collect the smoke and obtain the material containing the ammonium chloride, the zinc chloride, the potassium chloride and the sodium chloride.
Compared with the existing wet separation method, the method has the following beneficial effects:
1. the method has the advantages that the temperature, the material quantity and the kiln speed of a high-temperature section in the rotary kiln are controlled to effectively separate the volatile ammonium chloride (boiling point 520 degrees) zinc chloride (boiling point 732 degrees) and the non-volatile sodium chloride (boiling point 1465 degrees) potassium chloride (boiling point 1420 degrees) respectively, so that the separation effect which cannot be achieved by a wet method is achieved, the production cost is greatly reduced, qualified products can be produced respectively by the wet method, and the economic benefit maximization is realized;
2, the intermediate products separated by adopting the pyrogenic process are all solid, so that technical parameters of the wet process are well adjusted and optimized, and the energy cost is greatly reduced;
3, further improving the separation method, improving the process level, making the use of certain materials impossible, and improving the resource level of the materials;
4, the method is environment-friendly, and all indexes can reach the standard and even exceed the emission standard.
Detailed Description
The invention discloses a pyrogenic separation method of chloride, which combines a pyrogenic process and a wet process, does not need to change conversion components, and respectively produces corresponding qualified industrial products from all components in materials with lower production cost. .
The technical solutions of the present invention will be described clearly and completely below, and it is obvious that the description is only a part of the embodiments of the present invention, not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention discloses a pyrogenic separation method of chloride, which comprises the following steps:
the method comprises the following steps: putting a material containing ammonium chloride, zinc chloride, potassium chloride and sodium chloride into a rotary kiln, heating, wherein the heating temperature is higher than the boiling point of the ammonium chloride but lower than the boiling point of the zinc chloride, volatilizing the ammonium chloride in the material to form smoke, and cooling and collecting the ammonium chloride in the smoke;
step two: continuously heating the solid calcined in the step one, wherein the heating temperature is higher than the boiling point of zinc chloride but lower than the boiling point of potassium chloride, volatilizing the zinc chloride in the material to form smoke, and cooling and collecting the zinc chloride in the smoke;
step three: and D, conveying the solid calcined in the step two to a potassium chloride and sodium chloride wet separation system to separate potassium chloride, sodium chloride and other components in the solid.
Ammonium chloride, zinc chloride, potassium chloride, sodium chloride in the material adopt the fire method to combine wet process can effectively separate and can corresponding qualified product of output by basic equivalent, need not throw into other industrial chemicals for the separation except purifying the edulcoration and change into another kind of material and separate.
In some embodiments of the present invention, in the first step, the crude ammonium chloride is recovered by one or more of cooling gravity settling, water spraying dust removal purification, and wet electrostatic dust removal.
Under the condition that the temperature reduces, ammonium chloride in the smog can be separated out with graininess solid state thing, take place to subside under the effect of gravity, some ammonium chloride particulate matters can be carried the flow by the air current because the particle size undersize, at this moment, can further retrieve the ammonium chloride in the smog through the mode of water spraying dust removal purification and wet process electrostatic precipitator, improve recovery efficiency, avoid the pollution of tail gas, wherein the granule of ammonium chloride is less, and easily dissolve in water, its most can be collected by the mode of water spraying dust removal purification and wet process electrostatic precipitator.
In some embodiments of the present invention, in the first step, the recovered crude ammonium chloride is subjected to wet dissolution, crystallized and concentrated to obtain high-purity ammonium chloride.
As some impurities inevitably remain in the recovered crude ammonium chloride and the content of the impurities is relatively low, the crude ammonium chloride can be further purified by concentration and crystallization to obtain ammonium chloride with higher purity.
In some embodiments of the present invention, in the first step, the heating temperature is 500-.
In some embodiments of the present invention, in the second step, the crude zinc chloride is recovered by one or more of cooling gravity settling, water spraying dust removal purification, and wet electrostatic dust removal.
Under the condition that the temperature reduces, zinc chloride in the smog can be appeared with graininess solid-state thing, subsides under the effect of gravity, and partial zinc chloride particulate matter can be carried the flow by the air current because the particle size undersize, and at this moment, can further retrieve the zinc chloride in the smog through the mode of water spraying dust removal purification and wet process electrostatic precipitator, improves recovery efficiency, avoids the pollution of tail gas, and wherein the granule of zinc chloride is great, and most accessible cooling gravity subsides's mode is collected.
In some embodiments of the invention, In the second step, the recovered crude zinc chloride is dissolved by a wet method, crystallized and concentrated to obtain high-purity zinc chloride, and valuable elements of Ag, Pb, In, Bi, Sn, Sb, Cd, and Au are separated and recovered from the solution.
As the chlorides of Ag, Pb, In, Bi, Sn, Sb, Cd and Au have close boiling points with zinc chloride, crude zinc chloride is mixed In the process of pyrogenic separation, and meanwhile, the industrial-grade zinc chloride has higher requirement on the purity of the zinc chloride, so that the industrial-grade zinc chloride is favorably obtained by further wet purification.
In some embodiments of the present invention, the heating temperature in the second step is 800-.
In some embodiments of the present invention, in the third step, the other components in the solid include one or more of zinc oxide, lead oxide and aluminum oxide.
The metal oxide has a high boiling point and is finally left in the solid after the pyrogenic process, and potassium chloride and sodium chloride can be separated from the metal oxide by means of wet processing.
In another embodiment of the invention, before the first step, the material to be treated is heated at a temperature above 1450 ℃ to separate ammonium chloride, zinc chloride, potassium chloride and sodium chloride from the material, and the smoke is cooled to collect the material containing ammonium chloride, zinc chloride, potassium chloride and sodium chloride.
Ammonium chloride, zinc chloride, potassium chloride and sodium chloride are separated independently at a higher temperature, so that volatile components and nonvolatile components can be completely separated, and the subsequent separation operation is simplified.
The invention is illustrated by the following specific examples:
example 1:
the embodiment provides a plurality of test samples, all test samples 1, 2 and 3 are respectively taken from chlorination blocks produced by different secondary zinc oxide desorption F, CI, each temperature test is obtained by heating the sample from room temperature to 200 ℃ to dry moisture, then continuously heating to the required temperature and calcining at the constant temperature for 30min, the slag rate test is completed in a muffle furnace, and the flue gas receiving test is completed in a tubular electric furnace and a flue gas receiving device.
Wherein, the quantitative test of the zinc chloride adopts EDTA titration method, AAS method or icp method to detect;
the quantitative test of ammonium chloride is detection by NaOH titration;
the quantitative test of potassium chloride and sodium chloride is AAS method or icp method.
ND means no or below the detection limit of the method.
The test results obtained are shown in tables 1, 2 and 3 (the following percentage units are all mass percent):
TABLE 1
Figure BDA0003164453090000051
Figure BDA0003164453090000061
Figure BDA0003164453090000071
TABLE 2
Figure BDA0003164453090000072
Figure BDA0003164453090000081
TABLE 3
Figure BDA0003164453090000091
Figure BDA0003164453090000101
From the above test results, it can be seen that various chlorides can be effectively separated by the pyrogenic separation method.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.

Claims (9)

1. A pyrogenic separation method of chloride is characterized by comprising the following steps:
the method comprises the following steps: putting a material containing ammonium chloride, zinc chloride, potassium chloride and sodium chloride into a rotary kiln, heating, wherein the heating temperature is higher than the boiling point of the ammonium chloride but lower than the boiling point of the zinc chloride, volatilizing the ammonium chloride in the material to form smoke, and cooling and collecting the ammonium chloride in the smoke;
step two: continuously heating the solid calcined in the step one, wherein the heating temperature is higher than the boiling point of zinc chloride but lower than the boiling point of potassium chloride, volatilizing the zinc chloride in the material to form smoke, and cooling and collecting the zinc chloride in the smoke;
step three: and D, conveying the solid calcined in the step two to a potassium chloride and sodium chloride wet separation system to separate potassium chloride, sodium chloride and other components in the solid.
2. The pyrogenic separation method of chloride according to claim 1, wherein in step one, one or more of cooling gravity settling, water spray dust removal purification, and wet electrostatic dust removal are used in combination to recover the crude ammonium chloride.
3. The method for separating the chlorides by the pyrogenic process according to claim 2, wherein in the first step, the recovered crude ammonium chloride is dissolved by a wet method, crystallized and concentrated to obtain the high-purity ammonium chloride.
4. The method as claimed in claim 1, wherein the heating temperature in the first step is 500-700 ℃.
5. The pyrogenic separation method of chloride according to claim 1, wherein in step two, one or more of cooling gravity settling, water spray dust removal purification, and wet electrostatic dust removal are used in combination to recover the crude zinc chloride.
6. The pyro-separation method of chlorides according to claim 5, wherein In the second step, the recovered crude zinc chloride is dissolved by a wet method, crystallized and concentrated to obtain high-purity zinc chloride, and valuable elements of Ag, Pb, In, Bi, Sn, Sb, Cd and Au are separated and recovered from the solution.
7. The method for the pyrometallurgical separation of chlorides as claimed in claim 1, wherein the heating temperature in the second step is 800-.
8. The method for the pyrometallurgical separation of chlorides according to claim 1, wherein in the third step, the other components in the solid include one or more of zinc oxide, lead oxide and aluminum oxide.
9. A method for the pyrogenic separation of chlorides according to claim 1, wherein, prior to step one, the material to be treated is heated at a temperature above 1450 ℃ to separate ammonium chloride, zinc chloride, potassium chloride, and sodium chloride from the material, and the cooled fumes are collected to obtain a material containing ammonium chloride, zinc chloride, potassium chloride, and sodium chloride.
CN202110804373.4A 2021-07-15 2021-07-15 Pyrogenic separation method of chloride Pending CN114105186A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5846290A (en) * 1996-02-21 1998-12-08 Metals Recycling Technologies Corp. Method for the recovery of group IA salts during the treatment of industrial process waste streams
CN1561401A (en) * 2001-10-03 2005-01-05 优米科尔公司 Chloride melt process for the separation and recovery of zinc
CN105753029A (en) * 2016-05-19 2016-07-13 东北大学 Method for preparing anhydrous aluminum chloride by performing microwave chlorination on bauxite
CN106319234A (en) * 2016-08-23 2017-01-11 魏清松 Method for recovering zinc, aluminum, ferrum and lead in galvanizing slag

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5846290A (en) * 1996-02-21 1998-12-08 Metals Recycling Technologies Corp. Method for the recovery of group IA salts during the treatment of industrial process waste streams
CN1561401A (en) * 2001-10-03 2005-01-05 优米科尔公司 Chloride melt process for the separation and recovery of zinc
CN105753029A (en) * 2016-05-19 2016-07-13 东北大学 Method for preparing anhydrous aluminum chloride by performing microwave chlorination on bauxite
CN106319234A (en) * 2016-08-23 2017-01-11 魏清松 Method for recovering zinc, aluminum, ferrum and lead in galvanizing slag

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