CN108910938B - Method for jointly producing zinc sulfate monohydrate and zinc sulfate heptahydrate - Google Patents
Method for jointly producing zinc sulfate monohydrate and zinc sulfate heptahydrate Download PDFInfo
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- CN108910938B CN108910938B CN201810671021.4A CN201810671021A CN108910938B CN 108910938 B CN108910938 B CN 108910938B CN 201810671021 A CN201810671021 A CN 201810671021A CN 108910938 B CN108910938 B CN 108910938B
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Abstract
The invention discloses a method for jointly producing zinc sulfate monohydrate and zinc sulfate heptahydrate. The existing method for preparing zinc sulfate has high production cost; the process is complex and tedious; needs evaporative crystallization, and has large equipment investment and high energy consumption. The method comprises the following steps: extracting the zinc-containing solution to obtain a loaded organic phase, carrying out back extraction on the loaded organic phase to obtain a zinc sulfate solution, removing oil from the zinc sulfate solution, dividing the zinc sulfate solution into two parts, continuously adding sulfuric acid into one part, controlling the stirring speed and the aging time to separate out zinc sulfate monohydrate crystals, filtering, washing and drying to obtain a high-purity zinc sulfate monohydrate product; and preparing heptahydrate zinc sulfate by concentrating and crystallizing the other part of the heptahydrate zinc sulfate, removing part of the obtained heptahydrate zinc sulfate to prepare a saturated zinc sulfate solution for washing the monohydrate zinc sulfate, and drying the other part of the obtained heptahydrate zinc sulfate to obtain a finished product of the heptahydrate zinc sulfate. The invention has the advantages of lower production cost, simpler and more convenient process flow, less investment and the like.
Description
Technical Field
The invention relates to a preparation process of zinc sulfate, in particular to a method for jointly producing zinc sulfate monohydrate and zinc sulfate heptahydrate by leaching, extracting, back-extracting and other processes aiming at zinc-containing materials.
Background
At present, the process for preparing zinc sulfate at home and abroad can roughly comprise the following steps: the production process comprises the following steps of acid dissolution, impurity removal, evaporative crystallization, drying and the like, and has the following problems in the production process: firstly, a large amount of zinc powder is needed in the impurity removal process, so that the production cost is high; secondly, iron and ferrous iron obtained in the leaching process are oxidized to remove iron, and the process is complex and tedious; thirdly, evaporation crystallization is needed to obtain the zinc sulfate monohydrate, so that the equipment investment is large and the energy consumption is high.
Therefore, it is necessary to develop a new process with simpler production process, shorter flow and lower cost to carry out the combined production of the zinc sulfate monohydrate and the zinc sulfate heptahydrate, and replace the prior art.
Disclosure of Invention
The invention aims to overcome the defects in the existing production process of the zinc sulfate monohydrate and provide a combined production method of the zinc sulfate monohydrate and the zinc sulfate heptahydrate, which has the advantages of short flow, low cost and low investment.
Therefore, the technical scheme adopted by the invention is as follows: a method for the co-production of zinc sulfate monohydrate and zinc sulfate heptahydrate comprising the steps of:
1) preparation of Zinc sulfate solution
a) Leaching and filtering the zinc material to prepare a zinc-containing leaching solution;
b) mixing the zinc-containing leachate with an extractant for extraction to obtain an organic phase loaded with zinc ions, washing the organic phase, and then adopting 1.5-4mol/L H2SO4Carrying out back extraction on the back extraction solution to obtain zinc sulfate pregnant solution;
c) c, the raffinate after the zinc extraction in the step b) enters the next working procedure to extract other metals;
d) b), air floatation and activated carbon oil removal are carried out on the zinc sulfate rich solution obtained in the step b), and zinc sulfate preparation front solution is obtained;
2) preparation of zinc sulfate monohydrate
e) Pumping a part of zinc sulfate preparation front liquid obtained in the step d) into a zinc sulfate monohydrate crystallization kettle, and starting stirring;
f) raising the temperature of the zinc sulfate monohydrate preparation precursor liquid in the crystallization kettle to 45-90 ℃;
g) after the temperature of the step f) is reached, adding sulfuric acid into the crystallization kettle, and increasing the concentration of the sulfuric acid in the solution to 200-600 g/L;
h) after the addition of the sulfuric acid is finished, the heat preservation and the aging are carried out for 1 to 5 hours, and the zinc sulfate monohydrate is continuously crystallized and separated out;
i) after the heat preservation is finished, carrying out centrifugal filtration on the slurry containing the zinc sulfate monohydrate at the temperature of 45-90 ℃ to obtain a zinc sulfate monohydrate semi-finished product and a crystallization mother liquor;
j) washing the semi-finished product of the zinc sulfate monohydrate obtained in the step i) by using a zinc sulfate solution to obtain zinc sulfate monohydrate (wet base) and a washing solution;
k) returning the washing liquid obtained in the step j) to the step e), and pumping the washing liquid and the zinc sulfate preparation front liquid into a zinc sulfate monohydrate crystallization kettle;
l) drying the zinc sulfate monohydrate (wet basis) obtained in the step j) to obtain a finished zinc sulfate monohydrate product;
3) preparation of zinc sulfate heptahydrate
m) pumping the other part of zinc sulfate preparation front solution obtained in the step d) into a multi-effect zinc sulfate heptahydrate evaporation crystallizer, carrying out evaporation crystallization, and carrying out centrifugal filtration to obtain zinc sulfate heptahydrate and mother solution;
n) preparing a part of zinc sulfate heptahydrate obtained in the step m) with another part of zinc sulfate preparation front solution obtained in the step d) to obtain a saturated zinc sulfate solution, wherein the saturated zinc sulfate solution is used for washing zinc sulfate monohydrate;
and o) drying the other part of the zinc sulfate heptahydrate obtained in the step m) to obtain a finished product of the zinc sulfate heptahydrate.
The finished product of the zinc sulfate monohydrate obtained by the invention meets the national class I product standard requirements of industrial zinc sulfate.
Preferably, the method further comprises the steps of:
p) mixing the crystallization mother liquor obtained in the step i) with the mother liquor obtained in the step m), and after adding sulfuric acid and pure water, forming zinc strip front liquor to return to the step b) to be used as strip liquor in subsequent production.
Preferably, in step a), the composition form of zinc in the leachate is one or more of zinc chloride, zinc sulfate and zinc dichlorodiammine.
Preferably, in the step b), the adopted extracting agent is P204, P507 or C272, and the zinc-containing rich solution of zinc sulfate is 150-250 g/L.
Preferably, in the step d), the oil content of the zinc sulfate preparation pre-liquid is controlled to be less than 10 ppm.
Preferably, in the step e), the stirring speed of the crystallization kettle is controlled to be 30-200 r/min.
Preferably, in the step g), the concentration of sulfuric acid in the crystallization process of the zinc sulfate monohydrate is controlled to be 200-600 g/L.
Preferably, in step j), the semi-finished zinc sulfate monohydrate is washed with a saturated zinc sulfate solution to reduce the dissolution of zinc sulfate.
Preferably, in step j), the washing temperature of the zinc sulfate monohydrate semifinished product is controlled between 45 and 90 ℃ to reduce the formation of no other crystalline products.
Preferably, in step l), the drying equipment of the zinc sulfate monohydrate is selected from a rotary kiln, a belt dryer, a disc dryer, a rake dryer or a box dryer.
The invention produces the zinc sulfate monohydrate, is carried on according to the equilibrium principle of solubility product of zinc sulfate in aqueous solution, because zinc sulfate is under certain temperature, the solubility in water is certain, the solubility product of zinc ion and sulfate ion is also certain, through adding sulfuric acid to solution, increase the sulfate ion concentration in the solution, thus break the actual equilibrium of zinc ion, sulfate ion, at this moment, control certain temperature, zinc ion will combine with sulfate ion to form zinc sulfate monohydrate crystal to separate out from solution.
In the process of producing the zinc sulfate monohydrate, since the addition amount of the sulfuric acid (the concentration of the solution sulfuric acid is as high as 200-600g/L) is higher than the amount required by the total precipitation of the actual zinc ions (the concentration of the zinc ions is 150-250g/L) in the solution, if the zinc sulfate monohydrate is produced singly by the method, two situations occur: firstly, a large amount of acid exists in the mother solution of the zinc sulfate monohydrate, and the acid-containing solution enters a stripping section, so that the pregnant solution (namely the zinc sulfate pregnant solution) after zinc stripping has high acid content, therefore, the pregnant solution cannot be used for preparing the washing solution, and a zinc sulfate monohydrate product is required to be used for preparing the saturated solution, which leads to high production cost of qualified zinc sulfate monohydrate. Secondly, the acid-containing liquid enters a back extraction section, and rich liquid after zinc back extraction is free from acid through back extraction control, so that the rich liquid needs more sulfuric acid to separate out zinc sulfate monohydrate, and the acid-containing liquid is expanded continuously.
The invention produces the zinc sulfate heptahydrate while producing the zinc sulfate monohydrate. The acid expanded during the production of zinc sulfate monohydrate is balanced in the way of producing zinc sulfate heptahydrate. Firstly, a large amount of sulfuric acid and industrial water are needed for producing zinc sulfate heptahydrate, and the excessive sulfuric acid can be well utilized in the process of producing the zinc sulfate monohydrate; and secondly, by producing the zinc sulfate heptahydrate, the mother liquor of the zinc sulfate heptahydrate and the mother liquor of the zinc sulfate monohydrate are prepared, so that the acid concentration in the solution before back extraction is reduced, the back extraction pregnant solution (namely the zinc sulfate pregnant solution) is neutral, a part of the back extraction pregnant solution can be opened to prepare the zinc sulfate, and the zinc sulfate can be used as a washing solution, so that the cost for producing the zinc sulfate monohydrate is greatly reduced.
Compared with the traditional method, the production method of the zinc sulfate monohydrate has the advantages that firstly, a plurality of purification processes of the solution are omitted; secondly, the crystallization process of the zinc sulfate monohydrate does not need an evaporation concentration process, so that the investment is saved and the production cost of the zinc monohydrate is greatly reduced; in addition, the by-product of zinc sulfate heptahydrate can be continuously produced in the process of producing the zinc sulfate monohydrate, the production cost of the zinc sulfate monohydrate and the zinc sulfate heptahydrate can be further reduced, and the competitiveness of the product can be improved.
The invention jointly produces the zinc sulfate monohydrate and the zinc sulfate heptahydrate, can solve the problems of acid expansion, water expansion and the like generated in the process of producing the zinc sulfate monohydrate by matching products, and can not generate other secondary pollution.
Therefore, compared with the existing single evaporative crystallization and drying method, the method has the advantages of investment saving, short flow, energy consumption saving, low operation cost and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is further described with reference to the drawings and the detailed description.
The embodiment provides a method for jointly producing zinc sulfate monohydrate and zinc sulfate heptahydrate, and the process flow chart is shown in figure 1.
Example 1
Leaching the material containing zinc 40% with hydrochloric acid, filtering, controlling pH of the leachate at 3.0-5.0 to obtain zinc chloride leachate, mixing the leachate with P204 extractant, extracting to obtain organic phase loaded with zinc ions, washing the organic phase, and performing 1.5-4mol/L H2SO4The back extraction solution (mother liquor obtained after the zinc sulfate monohydrate and the zinc sulfate heptahydrate are produced by the subsequent process, sulfuric acid and water are added for configuration, and the obtained pre-back extraction solution is returned to be used as the back extraction solution) is subjected to back extraction to obtain zinc sulfate pregnant solution containing zinc of 180 g/L. After the zinc sulfate pregnant solution is subjected to active carbon deoiling, zinc sulfate preparation front solution with oil content less than 10ppm is obtained. Will be provided withPumping a part of zinc sulfate preparation pre-solution into a crystallization kettle, starting stirring, controlling the stirring speed at 50r/min, simultaneously heating the solution in the kettle to 50-60 ℃ through jacket steam, then adding sulfuric acid into the crystallization kettle, controlling the concentration of the sulfuric acid to be about 600g/L, preserving heat and aging for 2h to obtain zinc sulfate monohydrate, centrifugally filtering slurry containing the zinc sulfate monohydrate, controlling the temperature to be 50-60 ℃, washing the obtained zinc sulfate monohydrate semi-finished product at the temperature of 45-60 ℃ by using a saturated zinc sulfate solution to obtain zinc sulfate monohydrate (wet basis), and drying in a box type dryer to obtain the zinc sulfate monohydrate finished product. And pumping the other part of zinc sulfate before preparation to triple effect evaporation, producing zinc sulfate heptahydrate through evaporation and cooling crystallization, drying and selling one part of the obtained zinc sulfate heptahydrate, and preparing the other part of zinc sulfate heptahydrate and the other part of zinc sulfate before preparation at the temperature of 45-60 ℃ to obtain a saturated zinc sulfate solution, wherein the solution is used for washing the semi-finished zinc sulfate monohydrate.
Example 2
Leaching zinc-25% material with sulfuric acid, filtering, controlling pH of leachate at 3.0-5.0 to obtain zinc sulfate leachate, mixing the leachate with P204 extractant, extracting to obtain organic phase loaded with zinc ions, washing the organic phase, and performing 1.5-4mol/L H2SO4The back extraction solution (mother liquor obtained after the zinc sulfate monohydrate and the zinc sulfate heptahydrate are produced by the subsequent process, sulfuric acid and water are added for configuration, and the obtained pre-back extraction solution is returned to be used as the back extraction solution) is subjected to back extraction to obtain zinc sulfate pregnant solution containing zinc of 200 g/L. After the zinc sulfate pregnant solution is subjected to active carbon deoiling, zinc sulfate preparation front solution with oil content less than 10ppm is obtained. Pumping a part of the zinc sulfate preparation precursor solution into a crystallization kettle, starting stirring, controlling the stirring speed at 50r/min, simultaneously heating the solution in the kettle to 50-70 ℃ through jacket steam, then adding sulfuric acid into the crystallization kettle, controlling the concentration of the sulfuric acid to be about 500g/L, preserving heat and aging for 3h to obtain zinc sulfate monohydrate, centrifugally filtering the slurry containing the zinc sulfate monohydrate, controlling the temperature to be 50-70 ℃, washing the obtained zinc sulfate monohydrate semi-finished product at the temperature of 50-70 ℃ by using a saturated zinc sulfate solution to obtain the zinc sulfate monohydrate (wet zinc sulfate)And) drying by adopting a disc type dryer to obtain a finished product of the zinc sulfate monohydrate. And pumping the other part of the zinc sulfate preparation pre-solution to triple effect evaporation, producing zinc sulfate heptahydrate through evaporation and cooling crystallization, drying and selling one part of the obtained zinc sulfate heptahydrate, and preparing the other part of the zinc sulfate heptahydrate and the other part of the zinc sulfate preparation pre-solution at the temperature of 45-60 ℃ to obtain a saturated zinc sulfate solution, wherein the saturated zinc sulfate solution is used for washing a zinc sulfate monohydrate semi-finished product.
The foregoing embodiments have described some of the details of the present invention, but are not to be construed as limiting the invention, and those skilled in the art may make variations, modifications, substitutions and alterations herein without departing from the principles and spirit of the invention.
Claims (10)
1. A method for jointly producing zinc sulfate monohydrate and zinc sulfate heptahydrate, which is characterized by comprising the following steps:
1) preparation of Zinc sulfate solution
a) Leaching and filtering the zinc material to prepare a zinc-containing leaching solution;
b) mixing the zinc-containing leachate with an extractant for extraction to obtain an organic phase loaded with zinc ions, washing the organic phase, and then adopting 1.5-4mol/L H2SO4Carrying out back extraction on the back extraction solution to obtain zinc sulfate pregnant solution;
c) c, the raffinate after the zinc extraction in the step b) enters the next working procedure to extract other metals;
d) b), air floatation and activated carbon oil removal are carried out on the zinc sulfate rich solution obtained in the step b), and zinc sulfate preparation front solution is obtained;
2) preparation of zinc sulfate monohydrate
e) Pumping a part of zinc sulfate preparation front liquid obtained in the step d) into a zinc sulfate monohydrate crystallization kettle, and starting stirring;
f) raising the temperature of the zinc sulfate monohydrate preparation precursor liquid in the crystallization kettle to 45-90 ℃;
g) after the temperature of the step f) is reached, adding sulfuric acid into the crystallization kettle, and increasing the concentration of the sulfuric acid in the solution to 200-600 g/L;
h) after the addition of the sulfuric acid is finished, the heat preservation and the aging are carried out for 1 to 5 hours, and the zinc sulfate monohydrate is continuously crystallized and separated out;
i) after the heat preservation is finished, carrying out centrifugal filtration on the slurry containing the zinc sulfate monohydrate at the temperature of 45-90 ℃ to obtain a zinc sulfate monohydrate semi-finished product and a crystallization mother liquor;
j) washing the semi-finished product of the zinc sulfate monohydrate obtained in the step i) by using a zinc sulfate solution to obtain the zinc sulfate monohydrate and a washing solution;
k) returning the washing liquid obtained in the step j) to the step e), and pumping the washing liquid and the zinc sulfate preparation front liquid into a zinc sulfate monohydrate crystallization kettle;
l) drying the zinc sulfate monohydrate obtained in the step j) to obtain a finished zinc sulfate monohydrate product;
3) preparation of zinc sulfate heptahydrate
m) pumping the other part of zinc sulfate preparation front solution obtained in the step d) into a multi-effect zinc sulfate heptahydrate evaporation crystallizer, carrying out evaporation crystallization, and carrying out centrifugal filtration to obtain zinc sulfate heptahydrate and mother solution;
n) preparing a part of zinc sulfate heptahydrate obtained in the step m) with another part of zinc sulfate preparation front solution obtained in the step d) to obtain a saturated zinc sulfate solution, wherein the saturated zinc sulfate solution is used for washing zinc sulfate monohydrate;
and o) drying the other part of the zinc sulfate heptahydrate obtained in the step m) to obtain a finished product of the zinc sulfate heptahydrate.
2. The method of claim 1, further comprising the steps of:
p) mixing the crystallization mother liquor obtained in the step i) with the mother liquor obtained in the step m), and after adding sulfuric acid and pure water, forming zinc strip front liquor to return to the step b) to be used as strip liquor in subsequent production.
3. The method according to claim 1 or 2, wherein in step a), the zinc in the leachate is in the form of one or more of zinc chloride, zinc sulfate and zinc dichlorodiammine.
4. The method as claimed in claim 1 or 2, wherein in step b), the extractant used is P204, P507 or C272, and the zinc-rich zinc solution contains zinc of 150-250 g/L.
5. The method as claimed in claim 1 or 2, characterized in that in step d), the oil content of the zinc sulfate preparation pre-liquor is controlled to be less than 10 ppm.
6. The method as claimed in claim 1 or 2, characterized in that in step e), the stirring speed of the crystallization kettle is controlled to be 30-200 r/min.
7. The method as claimed in claim 1 or 2, wherein in step g), the concentration of sulfuric acid in the crystallization process of zinc sulfate monohydrate is controlled to be 200-600 g/L.
8. The method according to claim 1 or 2, characterized in that in step j) the semi-finished zinc sulphate monohydrate is washed with a saturated zinc sulphate solution.
9. The method according to claim 1 or 2, wherein in step j) the washing temperature of the zinc sulphate monohydrate semifinished product is controlled between 45 and 90 ℃.
10. The method as claimed in claim 1 or 2, wherein in step l), the drying equipment of the zinc sulfate monohydrate is selected from a rotary kiln, a belt dryer, a disc dryer, a rake dryer or a box dryer.
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| CN115215367A (en) * | 2022-07-21 | 2022-10-21 | 焦作市维联精细化工有限公司 | Process for preparing zinc sulfate monohydrate from zinc sulfate heptahydrate |
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| US4292283A (en) * | 1977-10-27 | 1981-09-29 | Klockner-Humboldt-Deutz Ag | Method for the recovery of zinc |
| CN101985361A (en) * | 2009-09-09 | 2011-03-16 | 王嘉兴 | Material circulating system formed by petrochemistry zinc slag and hydrochloric acid |
| CN103866139B (en) * | 2012-12-18 | 2015-07-08 | 宁波金田铜业(集团)股份有限公司 | Method for evaporation-free preparation of zinc sulfate from brass slag material |
| CN106755994A (en) * | 2017-01-12 | 2017-05-31 | 江苏凯力克钴业股份有限公司 | A kind of production method for comprehensively utilizing zinc cobalt raw material high |
| CN107385216B (en) * | 2017-07-20 | 2018-05-18 | 台山市化工厂有限公司 | The method that monohydrate zinc sulphate is prepared from utilising zinc containing waste residue |
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