CN106186087A - A kind of preparation method of feedstuff cobaltous sulfate - Google Patents
A kind of preparation method of feedstuff cobaltous sulfate Download PDFInfo
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- CN106186087A CN106186087A CN201610528024.3A CN201610528024A CN106186087A CN 106186087 A CN106186087 A CN 106186087A CN 201610528024 A CN201610528024 A CN 201610528024A CN 106186087 A CN106186087 A CN 106186087A
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- China
- Prior art keywords
- cobaltous sulfate
- feedstuff
- obtains
- mixed solution
- present
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Links
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 43
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 19
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 17
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 17
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 17
- 238000012805 post-processing Methods 0.000 claims abstract description 13
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000005083 Zinc sulfide Substances 0.000 claims abstract description 12
- 229910052984 zinc sulfide Inorganic materials 0.000 claims abstract description 12
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 44
- 239000001117 sulphuric acid Substances 0.000 claims description 24
- 235000011149 sulphuric acid Nutrition 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 23
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 13
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 13
- 239000012445 acidic reagent Substances 0.000 claims description 6
- 229910052793 cadmium Inorganic materials 0.000 abstract description 33
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 33
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 8
- 239000000654 additive Substances 0.000 abstract description 5
- 230000000996 additive effect Effects 0.000 abstract description 5
- 230000004044 response Effects 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 22
- 239000002244 precipitate Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 241001465754 Metazoa Species 0.000 description 8
- 230000018044 dehydration Effects 0.000 description 8
- 238000006297 dehydration reaction Methods 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 230000001105 regulatory effect Effects 0.000 description 7
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 5
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 4
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000003674 animal food additive Substances 0.000 description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 2
- 229940044175 cobalt sulfate Drugs 0.000 description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 102000001554 Hemoglobins Human genes 0.000 description 1
- 108010054147 Hemoglobins Proteins 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
- 241000220317 Rosa Species 0.000 description 1
- 229930003779 Vitamin B12 Natural products 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000001185 bone marrow Anatomy 0.000 description 1
- -1 can be with S2-React Chemical compound 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- FDJOLVPMNUYSCM-WZHZPDAFSA-L cobalt(3+);[(2r,3s,4r,5s)-5-(5,6-dimethylbenzimidazol-1-yl)-4-hydroxy-2-(hydroxymethyl)oxolan-3-yl] [(2r)-1-[3-[(1r,2r,3r,4z,7s,9z,12s,13s,14z,17s,18s,19r)-2,13,18-tris(2-amino-2-oxoethyl)-7,12,17-tris(3-amino-3-oxopropyl)-3,5,8,8,13,15,18,19-octamethyl-2 Chemical compound [Co+3].N#[C-].N([C@@H]([C@]1(C)[N-]\C([C@H]([C@@]1(CC(N)=O)C)CCC(N)=O)=C(\C)/C1=N/C([C@H]([C@@]1(CC(N)=O)C)CCC(N)=O)=C\C1=N\C([C@H](C1(C)C)CCC(N)=O)=C/1C)[C@@H]2CC(N)=O)=C\1[C@]2(C)CCC(=O)NC[C@@H](C)OP([O-])(=O)O[C@H]1[C@@H](O)[C@@H](N2C3=CC(C)=C(C)C=C3N=C2)O[C@@H]1CO FDJOLVPMNUYSCM-WZHZPDAFSA-L 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002607 hemopoietic effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 210000004994 reproductive system Anatomy 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011715 vitamin B12 Substances 0.000 description 1
- 235000019163 vitamin B12 Nutrition 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/10—Sulfates
-
- 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)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Fodder In General (AREA)
Abstract
The invention provides the preparation method of a kind of feedstuff cobaltous sulfate, cobaltous sulfate raw material, zinc sulfate, pH value regulator and water are mixed, obtains the mixed solution that pH value is 2.4～2.6；Described mixed solution is reacted with hydrogen sulfide, to there being zinc sulfide precipitation to produce, the material obtained is carried out post processing, obtains feedstuff cobaltous sulfate product.The method using the present invention to provide can make cadmium content in feedstuff cobaltous sulfate product less than 2ppm, meet the requirement of feedstuff additive standard.Additionally, required reagent is easily purchased and low cost in the method for present invention offer, i.e. can determine that reaction end by the obvious phenomenon occurred during direct observing response, simple to operate, the cadmium separated is the most molten.
Description
Technical field
The present invention relates to field of feed additive technology, particularly to the preparation method of a kind of feedstuff cobaltous sulfate.
Background technology
Cadmium is a kind of severe toxicity metallic element, is mainly entered in humans and animals body by food, water and air.Cadmium is people and moves
Object intracellular metabolite is relatively slow, easily in lung, liver, kidney and other organs deposition, and can be to the respiratory system of humans and animals and reproductive system
Cause huge destruction, particularly can cause humans and animals arthroncus, damage skeleton.Cadmium is not the required unit of humans and animals body
Element, the cadmium of excess can bring the biggest harm to humans and animals.
Cobalt is one of useful essential trace element of animals and plants, it is possible to stimulate the hemopoietic system of bone marrow in humans and animals body,
The synthesis and the RBC number purpose that promote hemoglobin increase.Cobalt participates in humans and animals with the form of composition vitamin B12 mostly
Internal physiological action.
Cobaltous sulfate is the one of feed additive, generally contains cadmium element in cobaltous sulfate raw material, and rapid determination of content of cadmium element is super
Cross 30ppm, and the standard of feedstuff cobaltous sulfate is cadmium content is less than 10ppm.Method for removing cadmium in traditional feedstuff cobaltous sulfate
It is to use extraction separation method, but uses cadmium content in the cobaltous sulfate that this extraction separation method obtains the highest.
Summary of the invention
It is an object of the invention to provide a kind of method removing cadmium from feedstuff cobaltous sulfate, the method energy that the present invention provides
Cadmium content in feedstuff cobaltous sulfate product is enough made to meet the requirement of feedstuff additive standard.
The invention provides the preparation method of a kind of feedstuff cobaltous sulfate, comprise the following steps:
(1) cobaltous sulfate raw material, zinc sulfate, pH value regulator and water are mixed, obtain the mixing that pH value is 2.4～2.6 molten
Liquid；
(2) mixed solution that described step (1) obtains is reacted with hydrogen sulfide, to there being zinc sulfide precipitation to produce, will obtain
Material carry out post processing, obtain feedstuff cobaltous sulfate product.
Preferably, the mass ratio of step (1) described cobaltous sulfate raw material and water is (10～20): 100.
Preferably, step (1) described pH value regulator includes acid reagent.
Preferably, in described step (2), hydrogen sulfide is obtained with sulfuric acid reaction by sodium sulfide.
Preferably, described step (2) particularly as follows:
(21) sulphuric acid is joined reaction in sodium sulfide and obtains hydrogen sulfide；
(22) mixed solution that the hydrogen sulfide described step (21) obtained and described step (1) obtain reacts, to there being sulfur
Change zinc precipitation to produce, stop adding sulphuric acid；
(23) material that described step (22) obtains is carried out post processing, obtain feedstuff cobaltous sulfate product.
Preferably, the mass concentration of described sulphuric acid is 92%～98%.
Preferably, the feed postition of described sulphuric acid is dropping.
Preferably, post processing in described step (2), particularly as follows: the pH value of regulation gained material is 4.9～5.1, obtains clear
Liquid；Described clear liquid is carried out concentration, obtains feedstuff cobaltous sulfate product.
Preferably, described clear liquid is filtrated to get.
The invention provides the preparation method of a kind of feedstuff cobaltous sulfate, by cobaltous sulfate raw material, zinc sulfate, pH value regulator
Mix with water, obtain the mixed solution that pH value is 2.4～2.6；Described mixed solution is reacted with hydrogen sulfide, sinks to there being zinc sulfide
Form sediment and produce, the material obtained is carried out post processing, obtains feedstuff cobaltous sulfate product.The method using the present invention to provide can make
Feedstuff less than 2ppm, meets the requirement of feedstuff additive standard with cadmium content in cobaltous sulfate product.Additionally, what the present invention provided
In method, required reagent is easily purchased and low cost, i.e. be can determine that instead by the obvious phenomenon occurred during direct observing response
Answering terminal, simple to operate, the cadmium separated is the most molten.
Accompanying drawing explanation
The present invention is further detailed explanation with detailed description of the invention below in conjunction with the accompanying drawings.
Fig. 1 is the structural representation that the feedstuff cobaltous sulfate that the embodiment of the present invention provides removes cadmium production equipment.
Detailed description of the invention
The invention provides a kind of method removing cadmium from feedstuff cobaltous sulfate, comprise the following steps:
(1) cobaltous sulfate raw material, zinc sulfate, pH value regulator and water are mixed, obtain the mixing that pH value is 2.4～2.6 molten
Liquid；
(2) mixed solution that described step (1) obtains is reacted with hydrogen sulfide, to there being zinc sulfide precipitation to produce, will obtain
Material carry out post processing, obtain feedstuff cobaltous sulfate product.
The method using the present invention to provide can make cadmium content in feedstuff cobaltous sulfate product less than 2ppm, meet feedstuff and use
The requirement of additive standard.Additionally, required reagent is easily purchased and low cost in the method for present invention offer, by directly observing
The obvious phenomenon occurred in course of reaction i.e. can determine that reaction end, and simple to operate, the cadmium separated is the most molten.
The method that the present invention provides uses zinc sulfate to be the removal degree that indicator judges cadmium in cobaltous sulfate, through the applicant
Research finds, in the system that pH value is 1.4～1.6, and Cd2+I.e. can be with S2-React, but the most do not do
Method completely removes Cd2+, the level of about 30ppm can only be accomplished；And Zn with this understanding2+With S2-Do not react.By system pH
Value regulation is to 2.4～2.6, Cd2+Can be with S2-React completely, Zn2+Can be with excess S in system2-Reaction；And in the case
Co2+Not with S2-Reaction, therefore cobalt does not lose.In the system that pH value is 2.4～2.6, hydrogen sulfide elder generation and Cd in system2+Instead
Should, then in system, excess hydrogen sulfide can be by Zn2+Sponge, stop environmental pollution, guarantee safe production.And the present invention adopts
With hydrogen sulfide and Cd in system2+And Zn2+Reaction, it is possible to be prevented effectively from metal sulfide, such as sodium sulfide, be added directly into reaction
In system, the pH value of local response system is caused to change greatly, it is impossible to the problem accurately judging reaction end.
Cobaltous sulfate raw material, zinc sulfate, pH value regulator and water are mixed by the present invention, obtain the mixing that pH value is 2.4～2.6
Solution.In the present invention, the mass ratio of described cobaltous sulfate raw material and water is preferably (10～20): 100, more preferably (13～
16): 100.In the present invention, described zinc sulfate is used for judging the removal degree of cadmium in cobaltous sulfate as indicator.The present invention couple
Consumption in described zinc sulfate does not has special requirement, uses the addition of indicator well known to those skilled in the art.
The charging sequence when present invention mixes for described cobaltous sulfate raw material, zinc sulfate, pH value regulator and water does not has special requirement,
Use the charging sequence that material well known to those skilled in the art mixes.Cobaltous sulfate raw material is the most first mixed by the present invention with water
Close, obtain cobalt sulfate solution, then described cobalt sulfate solution mixed with zinc sulfate, pH value regulator, obtain pH value be 2.4～
The mixed solution of 2.6.
The present invention does not has special requirement for the temperature of described mixed solution, uses energy well known to those skilled in the art
Enough ensure the non crystallized temperature of described mixed solution.In the present invention, the temperature of described mixed solution is preferably 20～50
DEG C, more preferably 22～30 DEG C.Concrete, in an embodiment of the present invention, described by cobaltous sulfate raw material, zinc sulfate, pH value tune
Joint agent and water mixing, obtaining mixed solution is at room temperature to carry out, it is not necessary to heat described mixed solution without carrying out
Cooling.
The present invention does not has special requirement for kind and the source of described pH value regulator, uses those skilled in the art
Known to the pH value of described mixed solution can be regulated the compound to 2.4～2.6.In the present invention, described pH value
Regulator preferably includes acid reagent.The present invention does not has special requirement for the kind of described acid reagent, uses this area
The pH value of described mixed solution can be regulated the acid compound to 2.4～2.6 known to technical staff.The present invention is excellent
Choosing uses sulfuric acid solution as acid reagent.In the present invention, the mass concentration of described sulfuric acid solution is preferably 15～25%, more
It is preferably 18～22%.In the present invention, described pH value regulator the most also includes alkaline reagent.In actual production, if
Use acid reagent to be regulated by the pH value of described mixed solution to less than required pH value, then need to use alkaline reagent to continue regulation
The pH value of mixed solution, the pH value finally making described mixed solution is 2.4～2.6.The present invention is for the kind of described alkaline reagent
Class does not has special requirement, uses the alkali compounds for regulating solution ph well known to those skilled in the art.This
Invention preferably employs sodium carbonate liquor as alkaline reagent.In the present invention, the mass concentration of described sodium carbonate liquor is preferably
15～25%, more preferably 18～22%.The present invention does not has special requirement for the equipment monitoring described mixed solution pH value,
Use the equipment that can monitor solution ph well known to those skilled in the art.Present invention preferably employs acidometer and monitor institute
State the pH value of mixed solution.
After obtaining described mixed solution, described mixed solution is reacted by the present invention with hydrogen sulfide, produces to there being zinc sulfide precipitation
Raw, the material obtained is carried out post processing, obtains feedstuff cobaltous sulfate product.In the present invention, described hydrogen sulfide is preferably by sulfur
Change sodium to obtain with sulfuric acid reaction.In the present invention, in described mixed solution, the mol ratio of cadmium and described hydrogen sulfide is preferably 1:
(1.05～1.10).
After obtaining described mixed solution, sulphuric acid is preferably joined reaction in sodium sulfide and obtains hydrogen sulfide, then by the present invention
Described hydrogen sulfide is reacted with described mixed solution, to there being zinc sulfate precipitation to produce, stops adding sulphuric acid, the material obtained is entered
Row post processing, obtains feedstuff cobaltous sulfate product.In the present invention, the mass concentration of described sulphuric acid is preferably 92%～98%.
In the present invention, described sulphuric acid is preferably joined in sodium sulfide by dropping mode.The present invention is for the dropping speed of described sulphuric acid
Rate does not has special restriction, uses the dropping liquid judging reaction end by controlling drop rate well known to those skilled in the art
The technical scheme of body material.Specifically, in actual production, if the volume of described mixed solution is 1000～1500L, then
The drop rate of described sulphuric acid is preferably 100～280mL/min, more preferably 130～230mL/min.In the present invention, control
The feed postition of described sulphuric acid facilitates look at the phenomenon occurred in reaction, and then accurately judges reaction end, determines that stopping adds
Enter the opportunity of sulphuric acid.In the present invention, the mixed solution including cobaltous sulfate is rose, after adding sulphuric acid in sodium sulfide,
The hydrogen sulfide produced first reacts with cadmium ion in mixed solution, then reacts with zinc ion, therefore first produces sulfuration in reaction system
Cadmium bright yellow precipitate, then produces zinc sulfide milky white precipitate, and now zinc ion does not react with cobalt ion, therefore does not results in cobalt
Loss.Therefore, the present invention, according to reacting phenomenon, can accurately judge reaction end by the addition controlling sulphuric acid.
After producing to there being zinc sulfide precipitation, the material obtained is carried out post processing by the present invention, obtains feedstuff cobaltous sulfate and produces
Product.In the present invention, described post processing preferably particularly as follows: the pH value of regulation gained material is 4.9～5.1, obtains clear liquid；By institute
State clear liquid and carry out concentration, obtain feedstuff cobaltous sulfate product.The present invention is the most special for the mode obtaining described clear liquid
Requirement, use and well known to those skilled in the art be obtained in that the mode of clear liquid in solid-liquid mixture.In the present invention
In, described clear liquid is preferably filtrated to get.The present invention does not has special requirement for the equipment that described filtration is used, and uses
The equipment that can be used in filtering well known to those skilled in the art.Present invention preferably employs pressure filter and carry out described filtration.
After obtaining described clear liquid, described clear liquid is preferably carried out concentration by the present invention, obtains feedstuff cobaltous sulfate product.
The present invention does not has special requirement for the mode that described concentration is used, and uses concentration well known to those skilled in the art
Processing mode.The heating of described clear liquid is preferably carried out concentration by the present invention.The present invention does not has for the mode of described heating
There is special restriction, use heating well known to those skilled in the art to realize the technical scheme of concentration.In reality
In production, in the material obtained after described heating carries out concentration, the Baume degrees of described cobaltous sulfate is preferably 40～45 °
Bé。
After completing described concentration, the material cooling that the present invention preferably will obtain after concentration, obtain after cooling
Cobaltous sulfate crystalline solid centrifuge dehydration, obtain feedstuff cobaltous sulfate product.The present invention will obtain after concentration for described
The mode that material carries out cooling down does not has special requirement, uses the mode of cooling well known to those skilled in the art.This
The material natural cooling obtained after bright the most just concentration.The equipment that the present invention is used for described centrifuge dehydration does not has
Special requirement, uses the equipment for centrifuge dehydration well known to those skilled in the art.Present invention preferably employs centrifugal
Machine carries out described centrifuge dehydration.In the present invention, the rotating speed of described centrifuge dehydration is preferably 800～1200r/min, more preferably
900～1100r/min；Time is preferably 4～6min.
Below in conjunction with actual process production procedure, technical scheme is further described.
Fig. 1 is the structural representation that the feedstuff cobaltous sulfate that the embodiment of the present invention provides removes cadmium production equipment, including reaction
Still (1), reaction tank (2), water-jet pump (3), reactor motor (4), water pump (5), stirring paddle (6), sewage draining exit (7),
Discharging opening (8) and dog-house (9), wherein, the bottom of reactor (1) is provided with sewage draining exit (7), the top of described reactor (1)
Being provided with sodium sulfide dog-house (9) and reactor motor (4), described reactor (1) is internal to be provided with and described reactor motor
(4) stirring paddle (6) connected, described reactor (1) is connected with water-jet pump (3) by pipeline, described water injection vacuum
Pump (3) is arranged on the top of reaction tank (2), and described water-jet pump (3) is connected with water pump (5) by pipeline, described water pump
(5) being connected with the bottom of reaction tank (2) by pipeline, the bottom of described reaction tank (2) is provided with discharging opening (8).
In actual production, the present invention uses production equipment shown in Fig. 1 to carry out except cadmium process, specifically includes following steps:
In reaction tank (2), add cobaltous sulfate and water, be subsequently adding zinc sulfate and pH value regulator, monitor institute with acidometer
The pH value stating mixed solution is 2.4～2.6；Water is added, to the water surface higher than stirring paddle (6) in reactor (1)；Switch on the pump
(5), described reaction tank (2) interior mixed solution is circulated in reaction tank (2) and pipeline by water-jet pump (3)；
Start reactor motor (4), in reactor (1), put into sodium sulfide by dog-house (9)；
In reactor (1), add sulphuric acid, first have bright yellow precipitate (cadmium sulfide) to produce to reaction tank (2) interior mixed solution
Raw, then there is milky white precipitate (zinc sulfide) to produce, stop adding sulphuric acid；
Described water-jet pump (3), reactor motor (4) and water pump (5) cuts out after continuing idle running 4～7 minutes,
Gas is not had to produce in ensureing reactor (1)；
The material obtained after discharging opening (8) releasing processes, the pH value of regulation gained material is 4.9～5.1, obtains clear
Liquid；Described clear liquid is carried out concentration, obtains feedstuff cobaltous sulfate product.
Below in conjunction with the embodiment in the present invention, the technical scheme in the present invention is clearly and completely described.Aobvious
So, described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the reality in the present invention
Execute example, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, all belong to
In the scope of protection of the invention.
Embodiment 1:
(1) it is based on 10: 100 by the mass ratio of cobaltous sulfate raw material and water, cobaltous sulfate raw material, water are mixed with indicator zinc sulfate
Close, be 2.5 with the pH value of the sulfuric acid solution regulation gained mixed solution that mass concentration is 15%；
(2) step (1) described mixed solution is reacted with hydrogen sulfide, first have to mixed solution cadmium sulfide bright yellow precipitate to produce
Raw, then there is zinc sulfide milky white precipitate to produce；Wherein, described hydrogen sulfide is obtained with sulfuric acid reaction by sodium sulfide, described sulphuric acid
Mass concentration be 92%；
(3) pH value of regulating step (2) gained material is 5.0, uses pressure filter to filter, the clear liquid heating that will obtain
Carry out concentration, obtain the material that cobaltous sulfate Baume degrees is 40 ° of B é, natural cooling, centrifuge dehydration 6min under 800r/min,
Obtain feedstuff cobaltous sulfate product.
Cadmium in the feedstuff cobaltous sulfate product that embodiment 1 prepares is measured according to method described in GB/T 13082-1991
Content, result shows, cadmium content is 1.8ppm.
Embodiment 2:
(1) it is based on 20: 100 by the mass ratio of cobaltous sulfate raw material and water, cobaltous sulfate raw material, water are mixed with indicator zinc sulfate
Close, be 2.4 with the pH value of the sulfuric acid solution regulation gained mixed solution that mass concentration is 25%；
(2) step (1) described mixed solution is reacted with hydrogen sulfide, first have to mixed solution cadmium sulfide bright yellow precipitate to produce
Raw, then there is zinc sulfide milky white precipitate to produce；Wherein, described hydrogen sulfide is obtained with sulfuric acid reaction by sodium sulfide, described sulphuric acid
Mass concentration be 98%；
(3) pH value of regulating step (2) gained material is 5.1, uses pressure filter to filter, the clear liquid heating that will obtain
Carry out concentration, obtain the material that cobaltous sulfate Baume degrees is 45 ° of B é, natural cooling, centrifuge dehydration under 1200r/min
4min, obtains feedstuff cobaltous sulfate product.
Cadmium in the feedstuff cobaltous sulfate product that embodiment 1 prepares is measured according to method described in GB/T 13082-1991
Content, result shows, cadmium content is 1.2ppm.
Embodiment 3:
(1) it is based on 15: 100 by the mass ratio of cobaltous sulfate raw material and water, cobaltous sulfate raw material, water are mixed with indicator zinc sulfate
Close, be 2.6 with the pH value of the sulfuric acid solution regulation gained mixed solution that mass concentration is 20%；
(2) step (1) described mixed solution is reacted with hydrogen sulfide, first have to mixed solution cadmium sulfide bright yellow precipitate to produce
Raw, then there is zinc sulfide milky white precipitate to produce；Wherein, described hydrogen sulfide is obtained with sulfuric acid reaction by sodium sulfide, described sulphuric acid
Mass concentration be 95%；
(3) pH value of regulating step (2) gained material is 4.9, uses pressure filter to filter, the clear liquid heating that will obtain
Carry out concentration, obtain the material that cobaltous sulfate Baume degrees is 43 ° of B é, natural cooling, centrifuge dehydration under 1000r/min
5min, obtains feedstuff cobaltous sulfate product.
Cadmium in the feedstuff cobaltous sulfate product that embodiment 1 prepares is measured according to method described in GB/T 13082-1991
Content, result shows, cadmium content is 0.8ppm.
As can be seen from the above embodiments, the method using the present invention to provide can make cadmium in feedstuff cobaltous sulfate product contain
Amount, less than 2ppm, meets the requirement of feedstuff additive standard.Additionally, required reagent is easily purchased in the method for present invention offer
And low cost, i.e. can determine that reaction end by the obvious phenomenon occurred during direct observing response, simple to operate, isolate
The cadmium come is the most molten.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For Yuan, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a preparation method for feedstuff cobaltous sulfate, comprises the following steps:
(1) cobaltous sulfate raw material, zinc sulfate, pH value regulator and water are mixed, obtain the mixed solution that pH value is 2.4～2.6；
(2) mixed solution that described step (1) obtains is reacted with hydrogen sulfide, to there being zinc sulfide precipitation to produce, the thing that will obtain
Material carries out post processing, obtains feedstuff cobaltous sulfate product.
Method the most according to claim 1, it is characterised in that the mass ratio of step (1) described cobaltous sulfate raw material and water is
(10～20): 100.
Method the most according to claim 1, it is characterised in that step (1) described pH value regulator includes acid reagent.
Method the most according to claim 1, it is characterised in that in described step (2), hydrogen sulfide is anti-with sulphuric acid by sodium sulfide
Should obtain.
Method the most according to claim 4, it is characterised in that described step (2) particularly as follows:
(21) sulphuric acid is joined reaction in sodium sulfide and obtains hydrogen sulfide；
(22) mixed solution that the hydrogen sulfide described step (21) obtained and described step (1) obtain reacts, to there being zinc sulfide
Precipitation produces, and stops adding sulphuric acid；
(23) material that described step (22) obtains is carried out post processing, obtain feedstuff cobaltous sulfate product.
Method the most according to claim 5, it is characterised in that the mass concentration of described sulphuric acid is 92%～98%.
7. according to the method described in claim 4 or 5, it is characterised in that the feed postition of described sulphuric acid is dropping.
Method the most according to claim 1, it is characterised in that post processing in described step (2) is particularly as follows: regulate gains
The pH value of material is 4.9～5.1, obtains clear liquid；Described clear liquid is carried out concentration, obtains feedstuff cobaltous sulfate product.
Method the most according to claim 8, it is characterised in that described clear liquid is filtrated to get.
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| CN102126761A (en) * | 2011-04-22 | 2011-07-20 | 桂金鸣 | Method for preparing cobaltous sulfate |
| US20150151981A1 (en) * | 2012-07-10 | 2015-06-04 | Basf Se | Process for preparing aqueous solutions of cobalt sulfate |
| CN105668651A (en) * | 2016-02-03 | 2016-06-15 | 广东佳纳能源科技有限公司 | Production method for cobaltous sulfate heptahydrate |
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| CN102126761A (en) * | 2011-04-22 | 2011-07-20 | 桂金鸣 | Method for preparing cobaltous sulfate |
| US20150151981A1 (en) * | 2012-07-10 | 2015-06-04 | Basf Se | Process for preparing aqueous solutions of cobalt sulfate |
| CN105668651A (en) * | 2016-02-03 | 2016-06-15 | 广东佳纳能源科技有限公司 | Production method for cobaltous sulfate heptahydrate |
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| CN112320856A (en) * | 2020-11-19 | 2021-02-05 | 湖南新发展农牧科技有限公司 | Preparation method of cobalt sulfate for feed |
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