CN103435094B - Containing the production method of ferrous Zinc Sulphate Monohydrate - Google Patents
Containing the production method of ferrous Zinc Sulphate Monohydrate Download PDFInfo
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Abstract
Containing the production method of ferrous Zinc Sulphate Monohydrate, belong to biological fodder processing technique field.It comprises following processing step: the 1) preparation of raw materials for production; 2) leaching of raw materials for production; 3) purification of solution; 4) removal of impurities of solution; 5) precipitation of solution; 6) solution is concentrated; 7) work in-process are dried; 8) work in-process cooling; 9) work in-process classification.The present invention is for improving the rate of recovery and produce high quality feed grade Zinc Sulphate Monohydrate with leach liquor significant with reclaiming zinc containing Zn scrap returns.
Description
Technical field
The invention belongs to biological fodder processing technique field, be specifically related to the production method containing ferrous Zinc Sulphate Monohydrate.
Background technology
The production method of traditional Zinc Sulphate Monohydrate generates solution by containing zinc cigarette ash and sulfuric acid reaction, and be waste material is carried out three times to leach for improving zinc leaching rate, a meutral innersion, secondary acidic leaching, three washings are leached.Process application produces containing Zn scrap returns in a kind of zinc processing, and after secondary acidic leaching, leach liquor returns meutral innersion, and result meutral innersion temperature is low, acidic leaching impurity accumulates in meutral innersion, meutral innersion solid-liquor separation speed constantly slows down, and the quantity of slag constantly increases, and impact is produced.Infusion solution is by producing qualified solution after removing impurities by oxidation, qualified solution is dried through concentrated, obtains Zinc Sulphate Monohydrate.This product application is in fodder additives, and in actual husbandry sector, a wherein comparatively outstanding problem is the oxidisability of sulfuric acid monohydrate zinc product.The oxidisability of sulfuric acid monohydrate zinc product shows: can destroy micro-nutrient in feed pre-mixing material, as VITAMIN, amino acid etc., makes the variable color of Preblend product; Add the water absorbability of product, accelerate the loss of nutrient further.
Zinc is that animal sustains life and grows one of requisite nutrient substance, and zinc sulfate is zinc supplementing preparation important in fodder industry.Along with the fast development of fodder additives, harmful element in zinc sulfate is required that content is more and more higher, as every content from being less than 30mg/Kg in the past, be down to 10mg/Kg zinc sulfate product cadmium content reduce to solution of zinc sulfate in zinc sulfate production process except cadmium propose requirements at the higher level.How for the low solution of zinc sulfate of cupric cadmium, except cadmium reaches certain content and filtrate body can be produced and is less than 10 mg/Kg zinc sulfate products containing cadmium.
Current fodder additives zinc sulfate produce in low levels cadmium add zinc powder except the method for cadmium adopts, zinc powder except cadmium effect fast, but the zinc powder excessive zinc powder that causes waste, zinc powder is on the low side, except solution of zinc sulfate cadmium content instability during solid-liquor separation after cadmium.
Summary of the invention
For prior art Problems existing, the object of the invention is to design the technical scheme that a kind of production method containing ferrous Zinc Sulphate Monohydrate is provided.
The described production method containing ferrous Zinc Sulphate Monohydrate, is characterized in that comprising following processing step:
1) preparation of raw materials for production
That selects zinc processing to produce contains Zn scrap returns, as containing ferrous Zinc Sulphate Monohydrate raw materials for production, mainly should contain zinc 31 ~ 60%, iron 0 ~ 2.5%, chlorine 0 ~ 1.2% and SiO containing Zn scrap returns
26 ~ 20%; To carry out stacking process containing Zn scrap returns, pilling up time is not less than 20 days; Carry out proportioning to containing Zn scrap returns, make containing Zn content 38 ~ 44%, iron level 1 ~ 2.0%, cl content 0.3 ~ 0.7% in Zn scrap returns;
2) leaching of raw materials for production
A, in primary first-order equation container, add mother liquid coming that step 6 produces and the waste water that step f produces, in conjunction with Zn content in waste water, allocate into and need consumption sulfuric acid total amount, zinc is dissolved;
B, by step 1) containing after Zn scrap returns breaks into pieces, particle evenly adds in primary first-order equation container;
C, when mother-in-law U.S. degree is 31 ~ 33 degree and pH 4.4 ~ 4.5 stops reinforced, continue stirring 180 ~ 400 minutes;
D, carry out solid-liquor separation when liquid pH is 4.7 ~ 4.9 in step c, obtain a leach liquor and filter residue;
E, in secondary reaction container, add the waste water that step g produces, add by solid-to-liquid ratio 1:1 the filter residue that step d) obtains, adding the vitriol oil to pH is 3.9 ~ 4.1, and stirring 0.5h, pH is 4.1 ~ 4.3;
F, in secondary reaction container, add the waste water that water or step g produce, make pH value of solution be 4.4 ~ 4.5, solid-liquor separation, obtains secondary leach liquor and filter residue;
G, in third-order reaction container, add clear water, add the filter residue of step f by solid-liquid 1:3 again, stir 30 ~ 60 minutes, solid-liquor separation, obtain three leach liquors and filter residue;
3) purification of solution
By step 2) an obtained leach liquor adds suspended impurity in flocculation agent removing liquid;
4) removal of impurities of solution
1. the solution that step 3) obtains is got;
2. add step solid 4. add step solution 1. in reaction vessel after, stir 30 minutes ~ 60 minutes, solid-liquor separation, obtains liquid and solid;
3. in reaction vessel, add the liquid that 2. step obtains, then add zinc powder 0.5 ~ 3g/L, stir 30 minutes, in zinc powder consumption to liquid, cadmium content is less than 5ppm;
4. solid-liquid in step 3. reaction tank being squeezed into volume is in the high bit strip stirred vessel of reaction vessel 1/3 ~ 1/4 size, allows solid-liquid naturally flow in pressure filter, carries out solid-liquor separation, obtains solid and cupric is less than 1ppm, containing cadmium 2 ~ 5ppm containing zinc liquid;
5) precipitation of solution: obtained for step 4) is delivered to settling tank precipitation containing zinc liquid, and precipitate more than 12 hours, solution is limpid;
6) solution is concentrated: deliver in concentrate container concentrated by supernatant obtained for step 5) containing zinc liquid, add 5 ~ 10g edible oil before heating up, evaporation concentration, be separated to obtain aqueous sulfuric acid zinc and mother liquor with whizzer, mother liquor returns step 2) in primary first-order equation container;
7) work in-process are dried: aqueous sulfuric acid zinc step 6) obtained is dried in rotary kiln dryer, obtain containing ferrous Zinc Sulphate Monohydrate;
8) work in-process cooling: the Zinc Sulphate Monohydrate containing ferrous iron step 7) obtained, enters in feed bin through rotary conveyor and lift;
9) work in-process classification: step 8) feed bin is obtained less than 250 μm containing ferrous Zinc Sulphate Monohydrate containing ferrous Zinc Sulphate Monohydrate through the classification of solid, powdery thing tripping device, should be made up of the composition of following weight percent containing ferrous Zinc Sulphate Monohydrate:
Zinc Sulphate Monohydrate is in zinc): >=% 33
Ferrous sulfate (in iron) :≤% 2
Chlorine :≤% 0.8
Plumbous :≤mg/Kg 10
Arsenic :≤mg/Kg 1
Cadmium :≤mg/Kg 10
The described production method containing ferrous Zinc Sulphate Monohydrate, is characterized in that the addition of flocculation agent in described step 3) is 1 ~ 2.0g/m
3.
The described production method containing ferrous Zinc Sulphate Monohydrate, is characterized in that evaporation concentration solid-liquor separation condition in described step 6): solids concn is greater than 1.6g/L, and temperature is greater than 80 DEG C.
The described production method containing ferrous Zinc Sulphate Monohydrate, is characterized in that controlling rotary kiln dryer flue-gas temperature 500 ~ 600 DEG C in described step 7).
Step of the present invention (1) object is that in control raw material, each constituent content is in reasonable level; Step (2) object is to leach zinc in raw material, the satisfactory zinc liquid of output; Step (3) is by microactuator suspension small-particle in flocculation agent removing solution; Step (4) carries out replacement(metathesis)reaction by copper, cadmium, lead in zinc powder and liquid, copper, cadmium, lead in removing solution, and ensures that copper in solution, lead, cadmium content meet the requirements; Step (5) is by impurity in precipitation further removing solution; Step (6) makes the aqueous sulfuric acid zinc of output pure white, loose; Step (7) makes that aqueous sulfuric acid zinc ridity is good, good fluidity; Step (8) makes oven dry Zinc Sulphate Monohydrate cool, and homogenizing, stablizes physicochemical property; Step (9) makes Zinc Sulphate Monohydrate granularity less than 250 μm be greater than 95%, improves liquidity further.
The above-mentioned Zinc Sulphate Monohydrate Measures compare produced containing ferrous Zinc Sulphate Monohydrate production method and existing strong oxidizer deironing has paid attention to material choice and production material formula, contributes to guarantee product uniqueness; Raw material leaches last pH for three times and is greater than 4.4, dissolves impurity level under contributing to reducing strong acid condition in zinc leaching process, and do not affecting in leaching result situation, solid-liquor separation is fast; Make use of the solid produced in production process, reduce zinc powder consumption; Utilize natural filtration, decrease when filtering by pump pressure and enter solution except cadmium slag wears filter, utilization to add before the final controlled filter of zinc powder amount cadmium content in solution, reduce zinc powder consumption, and solution cadmium content after reaching stable filtration, ensure that solution is dried output Zinc Sulphate Monohydrate cadmium content through condensing crystal and is less than 10ppm, eliminate by strong oxidizer deferrization process step, do not deposit the problem that strong oxidizer is in the product residual, and to retain iron be divalence.Whole production process is arranged outward without waste water.Containing ferrous Zinc Sulphate Monohydrate, white or off-white color good fluidity, not easily deliquescence.Product non-oxidative, water-soluble after potential value is less than distilled water.1 year quality guaranteed period, take use apart after being long placed in, good fluidity, do not lump.Produce for feed pre-mixing material and be easy to hybrid process, and effectively to alleviate in Preblend micro-nutrient as the destruction of the micronutrient such as VITAMIN, amino acid.Product uses so far through domestic Duo Jia large and medium-sized enterprise, and prove that product application is produced in Preblend, be easy to hybrid process, Preblend is not easy to change.
The present invention is for improving the rate of recovery and produce high quality feed grade Zinc Sulphate Monohydrate with leach liquor significant with reclaiming zinc containing Zn scrap returns.
Embodiment
Below by way of embodiment, further illustrate the present invention.The per-cent related in the present invention is all weight percentage.
Embodiment 1:
1) get the raw materials ready
Raw materials for production 771.0t, Zn content 27%-55%, zinc average content 41.38%, pilling up time 27 ~ 67 days before feeding intake, raw material is prepared burden on request, and raw material is divided into 163 batches of inputs.
2) leach
1. reaction time first add step 6. in waste water enter in primary first-order equation container, the reinforced later stage adds the waste water that other production process produces, according to entering wastewater flow rate and solution mother-in-law U.S. degree in reaction vessel, allocating 98% sulfuric acid to solution into, making solution mother-in-law U.S. degree concentration increase by 8 ~ 12 degree.
2. raw material spades is broken into pieces, evenly adds in reaction vessel and reacts.
3. stop feeding in raw material in filtrate mother-in-law U.S. degree 31 ~ 33 degree and PH=4.4 ~ 4.5, continue stirring 3.5 ~ 4.5 hours.
4. check filtrate PH=4.7 ~ 4.9 in reaction vessel, reaction vessel solid-liquor separation, obtains a leach liquor and filter residue, temperature 60 ~ 75 DEG C, and solid-liquid separation is fast, and filter cake is shaping.
5. in secondary reaction container, add the waste water produced in 7. step, match by solid-to-liquid ratio 1:1 and filter residue, add step 4. filter residue, add the vitriol oil while stirring and make PH=3.9 ~ 4.1 to reaction vessel, then stir half an hour, PH=4.1 ~ 4.3.
6. in secondary reaction container, add step 7. middle remaining waste water, make PH=4.4 ~ 4.5, solid-liquor separation, obtain secondary leach liquor and filter residue, solid-liquor separation is fast, and filter cake is shaping.
7. in third-order reaction container, add step 6. filter residue, add clear water by solid-to-liquid ratio 1:3 and stir 30-60 minute, solid-liquor separation obtains three leach liquors and filter residue, and solid-liquor separation is fast, and filter cake is shaping.
3) purify
Get 50g-80g flocculation agent and pour 46m into hot water dissolving
3stir 5-10 minute containing in a leach liquor container, stop stirring.
4) removal of impurities
Leaching reaction produces low levels copper cadmium solution of zinc sulfate wherein cadmium content 32ppm ~ 60ppm, and copper 239ppm ~ 500ppm, zinc 118g/L ~ 125g/l, squeeze into 46m by above-mentioned content solution
3container in, what add output in production process stirs 30 minutes except cadmium slag, uses pressure filter solid-liquor separation, extrudes liquid and enter an other 46m
3container in, disposablely add zinc powder, on average add zinc powder amount 54Kg, after stirring half an hour, measure the average 0.8 ~ 3ppm of solution cadmium content.Liquid-solidly squeeze into volume 17m
3container in, naturally flow in pressure filter and filter, final solution is on average containing cadmium 2 ~ 5ppm.
5) precipitate
Above-mentioned filtrate sent settling tank to precipitate and reach more than 12 hours.According to settling tank water quality situation, limpid the using containing zinc water of solution in selective precipitation pond.
6) concentrated
Put into transition pond containing zinc liquid concentrate limpid in settling tank with being pumped to concentrate container, add several edible oils, be warming up to 80 DEG C, stop concentrated after being concentrated into concentration 1.6g/L, solid-liquor separation while hot, output aqueous sulfuric acid zinc, mother liquor returns reaction vessel.
7) classification is dried
Aqueous sulfuric acid zinc is 500 ~ 600 DEG C by automatic control rotary kiln flue-gas temperature in rotary kiln dryer dries, dry grading, obtain product meter 28 batches, totally 711.2 tons, average containing zinc 33.18%, iron content scope 0.9 ~ 1.8%, chloride scope 0.3 ~ 0.55%, leaded scope 1 ~ 7mg/Kg, containing cadmium scope 2 ~ 8mg/Kg.
Embodiment 2:
1) get the raw materials ready
Raw materials for production 2014.1t, Zn content 27%-55%, zinc average content 41.9%, pilling up time 25 days-70 days before feeding intake, raw material is prepared burden on request, and raw material is divided into 455 batches of inputs.
2) leach
1. first add during reaction 6. in step waste water enter in reaction vessel, the reinforced later stage adds the waste water that other production process produces.According to entering wastewater flow rate and solution mother-in-law U.S. degree in reaction vessel, allocating 98% sulfuric acid to solution into, making solution mother-in-law U.S. degree concentration increase by 8 ~ 12 degree.
2. raw material spades is broken into pieces, evenly adds in reaction vessel and reacts.
3. stop feeding in raw material in filtrate mother-in-law U.S. degree 30-34 degree and PH=4.4 ~ 4.5, continue stirring 3.5 ~ 4.5 hours.
4. check filtrate PH=4.6 ~ 5.0 in reaction vessel, reaction vessel solid-liquor separation, obtains a leach liquor and filter residue, temperature 60 ~ 75 DEG C, and solid-liquid separation is fast, and filter cake is shaping.
5. in secondary reaction container, add the step 7. middle waste water produced, match by solid-to-liquid ratio 1:1 and filter residue, add step 4. filter residue, add the vitriol oil while stirring and make PH=3.9 ~ 4.1 to reaction vessel, then stir PH=4.1 ~ 4.3 half an hour.
6. in secondary reaction container, add step 7. middle remaining waste water, make PH=4.4 ~ 4.5, solid-liquor separation, obtain secondary leach liquor and filter residue, solid-liquor separation is fast, and filter cake is shaping.
7. in third-order reaction container, add step 6. filter residue, add clear water by solid-to-liquid ratio 1:3 and stir 30 ~ 60 minutes, solid-liquor separation obtains three leach liquors and filter residue, and solid-liquor separation is fast, and filter cake is shaping.
3) purify
Get 50g-80g flocculation agent and pour 46m into hot water dissolving
3stir 5 ~ 10 minutes containing in the container of a leach liquor, stop stirring.
4) removal of impurities
Leaching reaction produces low levels copper cadmium solution of zinc sulfate, and wherein cadmium content 42ppm ~ 110ppm, copper 250ppm ~ 500ppm, zinc 112g/L ~ 126g/l, squeeze into 46m by above-mentioned content solution
3container in, what add output in production process stirs 30 minutes except cadmium slag, uses pressure filter solid-liquor separation, extrudes liquid and enter an other 46m
3container in, once add zinc powder, on average add zinc powder amount 62Kg, stir after half an hour and measure the average 1.5 ~ 3ppm of solution cadmium content.Liquid-solidly squeeze into volume 17m
3container in, naturally flow in pressure filter and filter, final solution is on average containing cadmium 2.2 ~ 5ppm.
5) precipitate
Above-mentioned filtrate sent settling tank to precipitate and reach more than 12 hours.According to settling tank water quality situation, limpid the using containing zinc water of solution in selective precipitation pond.
6) concentrated
Put into transition pond containing zinc liquid concentrate limpid in settling tank with being pumped to concentrate container, add several edible oils, heating up, it is concentrated to stop after being concentrated into concentration 1.6g/L, and solid-liquor separation while hot, output aqueous sulfuric acid zinc, mother liquor returns reaction vessel.
7) classification is dried
Aqueous sulfuric acid zinc is 500 ~ 600 DEG C by automatic control rotary kiln flue-gas temperature in rotary kiln dryer dries, dry grading, obtain product meter 67 batches, totally 1894 tons, average containing zinc 33.28%, containing zinc-iron scope 0.9-1.8%, chloride scope 0.3-0.55%, leaded scope 1-7mg/Kg, containing cadmium 2-8 mg/Kg.
Claims (4)
1., containing the production method of ferrous Zinc Sulphate Monohydrate, it is characterized in that comprising following processing step:
1) preparation of raw materials for production
That selects zinc processing to produce contains Zn scrap returns, as containing ferrous Zinc Sulphate Monohydrate raw materials for production, mainly should contain zinc 31 ~ 60%, iron 0 ~ 2.5%, chlorine 0 ~ 1.2% and SiO containing Zn scrap returns
26 ~ 20%; To carry out stacking process containing Zn scrap returns, pilling up time is not less than 20 days; Prepare burden to containing Zn scrap returns, make containing Zn content 38 ~ 44%, iron level 1 ~ 2.0%, cl content 0.3 ~ 0.7% in Zn scrap returns;
2) leaching of raw materials for production
A, in primary first-order equation container, add mother liquid coming that step 6) produces and the waste water that step f produces, according to entering wastewater flow rate and solution degree Beaume in reaction vessel, allocate 98% sulfuric acid to solution into, make solution degree Beaume concentration increase by 8 ~ 12 degree;
B, by step 1) containing after Zn scrap returns breaks into pieces, particle evenly adds in primary first-order equation container;
C, when degree Beaume is 31 ~ 33 degree and pH 4.4 ~ 4.5 stops reinforced, continue stirring 180 ~ 400 minutes;
D, carry out solid-liquor separation when liquid pH is 4.7 ~ 4.9 in step c, obtain a leach liquor and filter residue;
E, in secondary reaction container, add the waste water that step g produces, add by solid-to-liquid ratio 1:1 the filter residue that step d) obtains, adding the vitriol oil to pH is 3.9 ~ 4.1, and stirring 0.5h, pH is 4.1 ~ 4.3;
F, in secondary reaction container, add the waste water that water or step g produce, make pH value of solution be 4.4 ~ 4.5, solid-liquor separation, obtains secondary leach liquor and filter residue;
G, in third-order reaction container, add clear water, be the filter residue that 1:3 adds step f again by solid-to-liquid ratio, stir 30 ~ 60 minutes, solid-liquor separation, obtain three leach liquors and filter residue;
3) purification of solution
By step 2) an obtained leach liquor adds suspended impurity in flocculation agent removing liquid;
4) removal of impurities of solution
1. the solution that step 3) obtains is got;
2. add step solid 4. add step solution 1. in reaction vessel after, stir 30 minutes ~ 60 minutes, solid-liquor separation, obtains liquid and solid;
3. in reaction vessel, add the liquid that 2. step obtains, add zinc powder 0.5 ~ 3g again in every L liquid, stir 30 minutes, in zinc powder consumption to liquid, cadmium content is less than 5ppm;
4. material in step 3. reaction tank being squeezed into volume is in the high bit strip stirred vessel of reaction vessel 1/3 ~ 1/4 size, allows material naturally flow in pressure filter, carries out solid-liquor separation, obtains solid and cupric is less than 1ppm, containing cadmium 2 ~ 5ppm containing zinc liquid;
5) precipitation of solution: obtained for step 4) is delivered to settling tank precipitation containing zinc liquid, and precipitate more than 12 hours, solution is limpid;
6) solution is concentrated: deliver in concentrate container concentrated by supernatant obtained for step 5) containing zinc liquid, add 5 ~ 10g edible oil before heating up, evaporation concentration, be separated to obtain aqueous sulfuric acid zinc and mother liquor with whizzer, mother liquor returns step 2) in primary first-order equation container;
7) work in-process are dried: aqueous sulfuric acid zinc step 6) obtained is dried in rotary kiln dryer, obtain containing ferrous Zinc Sulphate Monohydrate;
8) work in-process cooling: the Zinc Sulphate Monohydrate containing ferrous iron step 7) obtained, enters in feed bin through rotary conveyor and lift;
9) work in-process classification: step 8) feed bin is obtained less than 250 μm containing ferrous Zinc Sulphate Monohydrate containing ferrous Zinc Sulphate Monohydrate through the classification of solid, powdery thing tripping device, should be made up of the composition of following weight percent containing ferrous Zinc Sulphate Monohydrate:
Zinc Sulphate Monohydrate (in zinc): >=% 33
Ferrous sulfate (in iron) :≤% 2
Chlorine :≤% 0.8
Plumbous :≤mg/kg 10
Arsenic :≤mg/kg 1
Cadmium :≤mg/kg 10.
2. the production method containing ferrous Zinc Sulphate Monohydrate as claimed in claim 1, is characterized in that the addition of flocculation agent in described step 3) is 1 ~ 2.0g/m
3.
3. the production method containing ferrous Zinc Sulphate Monohydrate as claimed in claim 1, is characterized in that evaporation concentration solid-liquor separation condition in described step 6): solids concn is greater than 1.6g/L, and temperature is greater than 80 DEG C.
4. the production method containing ferrous Zinc Sulphate Monohydrate as claimed in claim 1, is characterized in that controlling rotary kiln dryer flue-gas temperature 500 ~ 600 DEG C in described step 7).
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| CN113511669A (en) * | 2021-07-13 | 2021-10-19 | 常州市武进康佳化工有限公司 | Recovery and purification process of blast furnace zinc ash for preparing zinc carbonate |
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