CN104843790B - A kind of chromite oxidizing method preparing sodium chromate of acid - Google Patents
A kind of chromite oxidizing method preparing sodium chromate of acid Download PDFInfo
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Abstract
The invention discloses a kind of chromite oxidizing method preparing sodium chromate of acid, including: in the chromite grind to form breeze, add sulphuric acid, control reaction temperature, pressure and time, filter after having reacted, filtrate adds calcic Ore regulation pH value to 2 5.5, filter, add in filtrate alkaline matter regulation pH value to 4 6.5, filter add in filtrate alkaline matter regulation pH value to 6.5 9.5, be filtrated to get solid hydrogen chromium oxide；Chromic oxide gel is pulled an oar, alkaline matter regulation pH value is added to 8～14 in making beating liquid, control reaction temperature, pressure and time, alkaline matter regulation pH value is added to 9 14 after having reacted, filter and in filtrate, add alkaline matter regulation pH value to 69, filtering, filtrate obtains sodium chromate after concentrating, crystallizing.In the present invention chromite pressurization, in the environment of strong acid the reaction of oxidizer can destroy chromite spinel structure, improve the dissolution rate of chromite, and realize efficiently separating of chromium ion and impurity by regulation pH value.
Description
Technical field
The invention belongs to technical field of mineral processing, be specifically related to that the acid of a kind of chromite is oxidizing prepares chromic acid
The method of sodium.
Background technology
What at present prepared by sodium chromate is most with chromite as raw material, substantially uses several method: have calcium roasting,
Few calcium or calcium-free roasting, the oxidizing method of ferrochrome alkali, Pneumatic fluidized tower Continuous Liquid Phase oxidation technology, potassium system
Sub-molten salt liquid phase oxidations etc., by the roasting of chromite or add alkali high-temperature oxydation and obtain sodium chromate.
The major defect having calcium roasting is that deslagging is many, and slag is up to 1%～1.5% (with chromic acid containing Cr VI
Meter), especially with the acid-soluble Cr VI existed with solid solution form, it is difficult to detoxify or utilize, making
Becoming bigger environmental pollution, therefore the chromium recovery ratio in chromite is 75%～80%.
The grog of few calcium or calcium-free roasting does not has sour molten chromium, and oxygenation efficiency is consistent with the numerical value of conversion ratio, another
Aspect, owing to the technique return slag amount added is big, chrome content is high.A chromium slag part is as chromium salt production, separately
A part, as the raw material of production ferrochrome, the most a small amount of untreated chromium slag, is gone down for a long time, pollutes
Environment and increase loss.
The chromium slag that Pneumatic fluidized tower Continuous Liquid Phase oxidation technology, potassium system sub-molten salt liquid phase oxidation are produced can
As the additive of production cement after smelt iron or high-temperature detoxification, but the amount processed is limited and puts into
The big easily generation secondary pollution to environment.
The technology of currently used acid molten process chromite, the problem existed is mainly trivalent chromium and ferric iron
Separation.Trivalent chromium separates conventional to be to be first ferrous iron by ferric iron back, then add with ferric
Oxalic acid separates, and this separation method mesoxalic acid cost is high, and separating effect is general, it is impossible to realize chromium and ferrum
High efficiency separation, thus cause the content overproof of ferrum in the chromium product prepared to cause chromium product to be unsatisfactory for requirement.
Patent documentation CN101979679A discloses " a kind of method for the treatment of chromite by sulfuric acid leaching ",
Chromite " is ground to form breeze, adds sulphuric acid, stirring, add oxidant, oxygen in breeze by the method
Agent is chromic anhydride, potassium chlorate or Ammonium persulfate., and its addition is the 0.2%～7% of powdered ore quality, heating,
Heating-up temperature is 120～190 DEG C, and controlling reaction pressure is 0.2～1.2MPa, and the response time is 30～90min,
Filtering after having reacted, carry out solid-liquid separation, filtering residue is directly as the raw material of smelting duriron, by filter
Liquid carries out obtaining chromium sulfate solution except ferrum processes, and prepares chromic sulfate by the method for direct crystallization further ".
This method after completion of the reaction, has only been carried out except ferrum processes, and does not has detailed except ferrum processing method,
But containing the impurity such as a certain amount of magnesium, aluminum in chromite, if do not processed, the product obtained pure
Degree can not improve, and affects the quality of product, it is therefore desirable to carries out reasonably processing these impurity,
Additionally, the reaction pressure that the method uses is relatively low, cause its reaction effect poor.Academic dissertation " ferrochrome
Ore deposit sulfuric acid leaching is prepared chromium sulfate basic process for cleanly preparing and is studied, Shi Peiyang, Northeastern University, and 2002 "
Disclosing the method using sulfuric acid treatment chromite, but use synthesis under normal pressure in the method, it reacts effect
The poorest, and use complexity except ferrum processing method.
Summary of the invention
As various extensive and careful researchs and the result of experiment, it has been found by the inventor that
Chromite adds the reaction of oxidant in the environment of pressurization, strong acid can destroy chromite spinel structure,
Can improve the dissolution rate of chromite, and regulate pH can make ferrum, aluminum, magnesium etc. and chromium effectively point
From, make the response rate of chromite 85%～90%, the sodium chromate that purity is high can be obtained, based on this simultaneously
Plant and find, complete the present invention.
It is an object of the invention to solve at least the above and/or defect, and provide after at least and will say
Bright advantage.
It is a still further object of the present invention to provide a kind of chromite oxidizing method preparing sodium chromate of acid, bag
Include following steps:
Step one, chromite is ground to form the breeze that granularity is 100～200 mesh, then breeze is added anti-
Answer in still and add sulphuric acid, stirring with the speed of 300～800 revs/min, reacting by heating, and controlling reaction
Pressure and response time, after having reacted, obtain product feed liquid, product feed liquid is filtered and carries out solid-liquid
Separate, add in filtrate calcic Ore regulation pH value to 2-5.5, be filtered to remove calcium sulfate precipitation, then
Filtrate adds alkaline matter regulation pH value to 4-6.5, be filtered to remove precipitation, and in filtrate, add alkalescence
Material regulation pH value, to 6.5-9.5, is filtrated to get solid hydrogen chromium oxide；
Step 2, take the solid hydrogen chromium oxide obtained in 1 weight portion step one, add 0.5～1.5 weight portions
Pull an oar after water, obtain liquid of pulling an oar, making beating liquid is added in reactor, and add alkaline matter regulation pH
It is worth to 8～14, reacting by heating, and controls reaction pressure and response time, after having reacted, generated
Material liquid, in product feed liquid, addition alkaline matter regulation pH value is to 9-14, is filtered to remove precipitation,
And in filtrate, add alkaline matter regulation pH value to 6-9, be filtered to remove precipitation, filtrate through concentrating, knot
Sodium chromate is obtained after crystalline substance.
Preferably, also need to after described step one adding sulphuric acid add oxidant.
Preferably, described oxidant is sodium dichromate, oxygen, chromic anhydride, peroxide, persulfate
In the combination of one or more, its addition is the 0～50% of powdered ore quality.
Preferably, the one during described peroxide is sodium peroxide or hydrogen peroxide；Described persulfuric acid
Salt is the one in sodium peroxydisulfate or Ammonium persulfate..
Preferably, in described step one, the mass concentration of sulphuric acid is 1～90%, and its addition is breeze matter
0.3～0.9 times of amount.
Preferably, the one or several during described alkaline matter is sodium bicarbonate, sodium carbonate and oxygen sodium oxide
The combination planted；Described calcic Ore is the combination of one or more in quick lime, Calx, dolomite.
Preferably, in described step one, reaction temperature is 50～360 DEG C, and reaction pressure is 0.3～8MPa,
Response time is 10～400min.
Preferably, also needing to add oxygen in described step 2 before reacting by heating, its addition is hydrogen-oxygen
Change the 0～99% of chromium quality.
Preferably, in described step 2, reaction temperature is room temperature～360 DEG C, and reaction pressure is
0.01～8MPa, the response time is 1～400min.
Preferably, the reacting by heating in described step one and step 2 all uses microwave heating, and microwave
The microwave frequency of heating is 2450 ± 50MHz.
The composition of heretofore described chromite is as shown in table 1:
Table 1
In step one of the present invention, the composition in chromite is as follows with the main chemical reactions formula of sulfuric acid reaction:
Fe(CrO2)2+4H2SO4→FeSO4+Cr2(SO4)3+4H2O
(Mg, Fe) Cr2O4+5H2SO4→FeSO4+Cr2(SO4)3+MgSO4+5H2O
MgCr2O4+4H2SO4→MgSO4+Cr2(SO4)3+4H2O
(Mg, Fe)7Si8O22(OH)2+7H2SO4→7FeSiO3↓+7MgSO4↓+SiO2↓+8H2O
Wherein preferably oxidant sodium dichromate dissolves Fe (CrO2)2Master equation as follows:
Na2Cr2O7+2Fe(CrO2)2+10H2SO4→Fe2(SO4)3+2Cr2(SO4)3+Na2SO4+10H2O
Preferably oxidant oxygen and Fe (CrO2)2The master equation of reaction is as follows:
O2+4Fe(CrO2)2+18H2SO4→2Fe2(SO4)3+4Cr2(SO4)3+18H2O
Preferably oxidant chromic anhydride and Fe (CrO2)2The master equation of reaction is as follows:
2CrO3+6Fe(CrO2)2+30H2SO4→3Fe2(SO4)3+7Cr2(SO4)3+30H2O
Preferably oxidant persulfate dissolves Fe (CrO2)2The master equation of reaction is as follows:
S2O8 2-+2Fe(CrO2)2+8H2SO4→Fe2(SO4)3+2Cr2(SO4)3+8H2O+SO4 2-
Preferably oxidant peroxide dissolves Fe (CrO2)2The master equation of reaction is as follows:
O2 2-+2Fe(CrO2)2+9H2SO4→Fe2(SO4)3+2Cr2(SO4)3+9H2O+O2-
After oxidation reaction completes in the present invention, filter and carry out solid-liquid separation, the main one-tenth of the filtering residue obtained
It is divided into FeSiO3、SiO2Deng, these filtering residues can be as the raw material of smelting duriron；The filtrate obtained adds and contains
Calcium Ore regulation pH value is to 2-5.5, and in filtrate, excess sulfuric acid generates calcium sulfate precipitation with the calcium ion of addition,
Being filtered to remove calcium sulfate precipitation, filtering residue calcium sulfate can do Gypsum Fibrosum, then adds alkaline matter regulation in filtrate
PH value is to 4-6.5, and in this process, part magnesium ion, iron ion and the aluminium ion in filtrate can be with
Alkaline matter produces precipitation, is filtered to remove precipitation, and adds alkaline matter regulation pH value in filtrate extremely
6.5-9.5, chromium ion can produce precipitation, i.e. solid hydrogen chromium oxide with alkaline matter in this process.
The addition of oxidant in the present invention can improve the dissolution rate of chromite, and the kind of oxidant is red
The combination of one or more in vitriol sodium, oxygen, chromic anhydride, peroxide, persulfate, these oxygen
The use of agent will not bring other impurity into, it is ensured that the purity of final products.
One or more during alkaline matter is sodium bicarbonate, sodium carbonate and oxygen sodium oxide in the present invention
Combination, the alkaline matter of use is not in the case of bringing other impurity into, it is possible to effectively make iron ion,
Magnesium ion and aluminium ion precipitation, it is achieved that foreign ion separates with chromium ion.
In step 2 of the present invention, preferably can add oxygen promote that reaction is carried out, trivalent chromium oxidation is generated
Cr VI, after having reacted, adds alkaline matter regulation pH value to 9-14 in product feed liquid,
During this, impurity iron ion and alkaline matter produce precipitation, are filtered to remove precipitation, it is achieved Cr VI from
Son separate with iron ion, and add in filtrate alkaline matter regulation pH value to 6-9, in this process
Impurity aluminum ion produces precipitation with alkaline matter, is filtered to remove precipitation, it is achieved hexavalent chromium and aluminium ion
Separation, filtrate through concentration, crystallization after obtain sodium chromate.
In the present invention, the reacting by heating in step one and step 2 all uses microwave heating, and microwave is one
Planting the electromagnetic wave with special nature, its frequency is between radio wave and light wave, and its rate of heat addition is fast,
Raw material can be made to reach to react temperature required in short-term, and therefore energy consumption is relatively low, simultaneously in microwave heating process,
Material is self-heating, relative to the mode of existing air conduction, and temperature of charge projecting environment temperature
Degree, it is possible to make reaction more abundant.
The present invention at least includes following beneficial effect:
(1) in the present invention, chromite can destroy in pressurization, the reaction that adds oxidant in the environment of strong acid
Chromite spinel structure, improve chromite dissolution rate, and by regulation pH value make ferrum, aluminum, silicon,
Magnesium plasma efficiently separates with chromium ion；
(2) in the filtering residue produced in the preparation process of the present invention, chromic content is less than 0.01%,
Total chrome content is less than 0.3%, and the response rate of chromite, 85%～90%, processes preparation with existing chromite
The method of sodium chromate compares, and has technological process feature short, that discharge, filtering residue content without " three wastes "
Less and without Cr VI, following of resource can be improve as smelting duriron, the raw material of preparing Gypsum Fibrosum etc.
Ring utilizes.
Part is embodied by the further advantage of the present invention, target and feature by description below, and part also will
By the research of the present invention and practice are understood by the person skilled in the art.
Accompanying drawing illustrates:
Fig. 1 is that chromite of the present invention acid is oxidizing prepares the process chart of step one in sodium chromate method；
Fig. 2 is that chromite of the present invention acid is oxidizing prepares the process chart of step 2 in sodium chromate method；
Detailed description of the invention:
The present invention is described in further detail below in conjunction with the accompanying drawings, to make those skilled in the art's reference
Description word can be implemented according to this.
Should be appreciated that used herein such as " have ", " comprising " and " including " term also
Do not allot other element one or more or the existence of a combination thereof or interpolation.
Embodiment 1:
A kind of chromite oxidizing method preparing sodium chromate of acid, comprises the following steps:
Step one, chromite is ground to form the breeze that granularity is 200 mesh, then breeze is added reactor
In and to add mass concentration be 20% sulphuric acid, sulphuric acid is 0.9 times of powdered ore quality, then with 500
Rev/min speed stir and add oxidant sodium dichromate, sodium dichromate addition is the 10% of powdered ore quality,
Reacting by heating temperature is 50 DEG C, and to control reaction pressure be 1.0MPa and response time 100min；
Above-mentioned technical process main chemical reactions is as follows:
Fe(CrO2)2+4H2SO4→FeSO4+Cr2(SO4)3+4H2O
(Mg, Fe) Cr2O4+5H2SO4→FeSO4+Cr2(SO4)3+MgSO4+5H2O
MgCr2O4+4H2SO4→MgSO4+Cr2(SO4)3+4H2O
(Mg, Fe)7Si8O22(OH)2+7H2SO4→7FeSiO3↓+7MgSO4↓+SiO2↓+8H2O
Oxidant sodium dichromate dissolves Fe (CrO2)2Master equation as follows:
Na2Cr2O7+2Fe(CrO2)2+10H2SO4→Fe2(SO4)3+2Cr2(SO4)3+Na2SO4+10H2O
Obtaining product feed liquid after having reacted, product feed liquid filtered and carry out solid-liquid separation, filtering residue can
As the raw material of smelting duriron, add in filtrate quick lime regulation pH value to 2, generate calcium sulfate precipitation,
Being filtered to remove calcium sulfate precipitation, filtering residue calcium sulfate can do Gypsum Fibrosum, and then adding weight ratio in filtrate is 1:1
Sodium bicarbonate and sodium hydroxide regulation pH value to 4, in this process, part magnesium ion in filtrate,
Iron ion and aluminium ion can produce precipitation with alkaline matter, are filtered to remove precipitation, and add weight in filtrate
Than be the sodium bicarbonate of 1:1 and sodium hydroxide regulation pH value to 8, chromium ion meeting and alkali in this process
Property material produce precipitation, be filtrated to get solid hydrogen chromium oxide；
Step 2, take the solid hydrogen chromium oxide obtained in 1 weight portion step one, after adding 1 weight parts water
Making beating, obtains liquid of pulling an oar, and is added in reactor by making beating liquid, and adds the bicarbonate that weight ratio is 1:1
Sodium and sodium hydroxide regulation pH value, to 8, are subsequently adding oxygen, and the amount of oxygen is chromic oxide gel quality
60%, reacting by heating temperature is 90 DEG C, and controls reaction pressure 2MPa and response time 100min, instead
After should completing, obtaining product feed liquid, adding weight ratio in product feed liquid is the sodium bicarbonate of 1:1
With sodium hydroxide regulation pH value to 9, impurity iron ion produces precipitation with alkaline matter in this process,
It is filtered to remove precipitation, it is achieved hexavalent chromium separates with iron ion, and to add weight ratio in filtrate be 1:1
Sodium bicarbonate and sodium hydroxide regulation pH value to 6, impurity aluminum ion and alkaline matter in this process
Produce precipitation, be filtered to remove precipitation, it is achieved hexavalent chromium separates with aluminum ions, filtrate process concentration,
Sodium chromate is obtained after crystallization.Impurity in this technical process is detected, finds that chromic content is
Less than 0.01%, the content of total chromium is less than 0.3%, and the response rate of chromite reaches 90%.
Embodiment 2:
A kind of chromite oxidizing method preparing sodium chromate of acid, comprises the following steps:
Step one, chromite is ground to form the breeze that granularity is 200 mesh, then breeze is added reactor
In and to add mass concentration be 40% sulphuric acid, sulphuric acid is 0.7 times of powdered ore quality, then with 500
Rev/min speed stir and add oxidant oxygen, oxygen addition is the 20% of powdered ore quality, heating
Reaction temperature is 140 DEG C, and to control reaction pressure be 2.0MPa and response time 150min；
Above-mentioned technical process main chemical reactions is as follows:
Fe(CrO2)2+4H2SO4→FeSO4+Cr2(SO4)3+4H2O
(Mg, Fe) Cr2O4+5H2SO4→FeSO4+Cr2(SO4)3+MgSO4+5H2O
MgCr2O4+4H2SO4→MgSO4+Cr2(SO4)3+4H2O
(Mg, Fe)7Si8O22(OH)2+7H2SO4→7FeSiO3↓+7MgSO4↓+SiO2↓+8H2O
Oxidant oxygen and Fe (CrO2)2The master equation of reaction is as follows:
O2+4Fe(CrO2)2+18H2SO4→2Fe2(SO4)3+4Cr2(SO4)3+18H2O
Obtaining product feed liquid after having reacted, product feed liquid filtered and carry out solid-liquid separation, filtering residue can
As the raw material of smelting duriron, add in filtrate dolomite regulation pH value to 5.5, generate calcium sulfate precipitation,
Being filtered to remove calcium sulfate precipitation, filtering residue calcium sulfate can do Gypsum Fibrosum, and then adding weight ratio in filtrate is 1:1:
Sodium bicarbonate, sodium hydroxide and the sodium carbonate regulation pH value of 1 are to 6.5, in this process, in filtrate
Part magnesium ion, iron ion and aluminium ion can with alkaline matter produce precipitation, be filtered to remove precipitation, and
Filtrate adds weight ratio be the sodium bicarbonate of 1:1:1, sodium hydroxide and sodium carbonate regulation pH value to 9,
Chromium ion can produce precipitation with alkaline matter in this process, is filtrated to get solid hydrogen chromium oxide；
Step 2, take the solid hydrogen chromium oxide obtained in 1 weight portion step one, add 1.5 weight parts waters
Rear making beating, obtains liquid of pulling an oar, and is added in reactor by making beating liquid, and adds the carbonic acid that weight ratio is 1:1:1
Hydrogen sodium, sodium hydroxide and sodium carbonate regulation pH value, to 14, are subsequently adding oxygen, and the amount of oxygen is hydrogen-oxygen
Changing the 70% of chromium quality, reacting by heating temperature is 180 DEG C, and when controlling reaction pressure 4MPa and reaction
Between 200min, after having reacted, obtain product feed liquid, in product feed liquid add weight ratio be 1:1:1
Sodium bicarbonate, sodium hydroxide and sodium carbonate regulation pH value to 14, impurity iron ion in this process
Produce precipitation with alkaline matter, be filtered to remove precipitation, it is achieved hexavalent chromium separates with iron ion, and
Filtrate adds weight ratio be the sodium bicarbonate of 1:1:1, sodium hydroxide and sodium carbonate regulation pH value to 9,
Impurity aluminum ion produces precipitation with alkaline matter in this process, is filtered to remove precipitation, it is achieved Cr VI
Ion separates with aluminum ions, and filtrate obtains sodium chromate after concentrating, crystallizing.To in this technical process
Impurity detect, find chromic content for less than 0.01%, the content of total chromium is less than 0.3%,
And the response rate of chromite reaches 88%.
Embodiment 3:
A kind of chromite oxidizing method preparing sodium chromate of acid, comprises the following steps:
Step one, chromite is ground to form the breeze that granularity is 200 mesh, then breeze is added reactor
In and to add mass concentration be 50% sulphuric acid, sulphuric acid is 0.6 times of powdered ore quality, then with 500
Rev/min speed stir and add oxidant oxygen, oxygen addition is the 30% of powdered ore quality, heating
Reaction temperature is 200 DEG C, and to control reaction pressure be 4.0MPa and response time 200min；
Above-mentioned technical process main chemical reactions is as follows:
Fe(CrO2)2+4H2SO4→FeSO4+Cr2(SO4)3+4H2O
(Mg, Fe) Cr2O4+5H2SO4→FeSO4+Cr2(SO4)3+MgSO4+5H2O
MgCr2O4+4H2SO4→MgSO4+Cr2(SO4)3+4H2O
(Mg, Fe)7Si8O22(OH)2+7H2SO4→7FeSiO3↓+7MgSO4↓+SiO2↓+8H2O
Oxidant oxygen and Fe (CrO2)2The master equation of reaction is as follows:
O2+4Fe(CrO2)2+18H2SO4→2Fe2(SO4)3+4Cr2(SO4)3+18H2O
Obtaining product feed liquid after having reacted, product feed liquid filtered and carry out solid-liquid separation, filtering residue can
As the raw material of smelting duriron, add in filtrate dolomite regulation pH value to 4, generate calcium sulfate precipitation,
Being filtered to remove calcium sulfate precipitation, filtering residue calcium sulfate can do Gypsum Fibrosum, and then adding weight ratio in filtrate is 1:2:
Sodium bicarbonate, sodium hydroxide and the sodium carbonate regulation pH value of 1 are to 6, in this process, in filtrate
Part magnesium ion, iron ion and aluminium ion can produce precipitation with alkaline matter, are filtered to remove precipitation, and
Filtrate adds weight ratio be the sodium bicarbonate of 1:2:1, sodium hydroxide and sodium carbonate regulation pH value to 8,
Chromium ion can produce precipitation with alkaline matter in this process, is filtrated to get solid hydrogen chromium oxide；
Step 2, take the solid hydrogen chromium oxide obtained in 1 weight portion step one, after adding 1 weight parts water
Making beating, obtains liquid of pulling an oar, and is added in reactor by making beating liquid, and adds the bicarbonate that weight ratio is 1:2:1
Sodium, sodium hydroxide and sodium carbonate regulation pH value, to 10, are subsequently adding oxygen, and the amount of oxygen is hydroxide
The 80% of chromium quality, reacting by heating temperature is 240 DEG C, and controls reaction pressure 6MPa and response time
300min, after having reacted, obtains product feed liquid, and adding weight ratio in product feed liquid is 1:2:1
Sodium bicarbonate, sodium hydroxide and sodium carbonate regulation pH value to 12, impurity iron ion in this process
Produce precipitation with alkaline matter, be filtered to remove precipitation, it is achieved hexavalent chromium separates with iron ion, and
Filtrate adds weight ratio be the sodium bicarbonate of 1:2:1, sodium hydroxide and sodium carbonate regulation pH value to 8,
Impurity aluminum ion produces precipitation with alkaline matter in this process, is filtered to remove precipitation, it is achieved Cr VI
Ion separates with aluminum ions, and filtrate obtains sodium chromate after concentrating, crystallizing.To in this technical process
Impurity detect, find chromic content for less than 0.01%, the content of total chromium is less than 0.3%,
And the response rate of chromite reaches 90%.
Embodiment 4:
A kind of chromite oxidizing method preparing sodium chromate of acid, comprises the following steps:
Step one, chromite is ground to form the breeze that granularity is 200 mesh, then breeze is added reactor
In and to add mass concentration be 60% sulphuric acid, sulphuric acid is 0.53 times of powdered ore quality, then with 500
Rev/min speed stir and add oxidant persulfate, persulfate addition is powdered ore quality
35%, reacting by heating temperature is 240 DEG C, and to control reaction pressure be 5.0MPa and response time 250min；
Above-mentioned technical process main chemical reactions is as follows:
Fe(CrO2)2+4H2SO4→FeSO4+Cr2(SO4)3+4H2O
(Mg, Fe) Cr2O4+5H2SO4→FeSO4+Cr2(SO4)3+MgSO4+5H2O
MgCr2O4+4H2SO4→MgSO4+Cr2(SO4)3+4H2O
(Mg, Fe)7Si8O22(OH)2+7H2SO4→7FeSiO3↓+7MgSO4↓+SiO2↓+8H2O
Oxidant persulfate and Fe (CrO2)2The master equation of reaction is as follows:
S2O8 2-+2Fe(CrO2)2+8H2SO4→Fe2(SO4)3+2Cr2(SO4)3+8H2O+SO4 2-
Obtaining product feed liquid after having reacted, product feed liquid filtered and carry out solid-liquid separation, filtering residue can
As the raw material of smelting duriron, add in filtrate quick lime regulation pH value to 3.5, generate calcium sulfate precipitation,
Being filtered to remove calcium sulfate precipitation, filtering residue calcium sulfate can do Gypsum Fibrosum, then hydro-oxidation sodium regulation in filtrate
PH value is to 5, and in this process, part magnesium ion, iron ion and the aluminium ion in filtrate can be with alkalescence
Material produces precipitation, is filtered to remove precipitation, and in filtrate hydro-oxidation sodium regulation pH value to 8.5,
During this, chromium ion can produce precipitation with alkaline matter, is filtrated to get solid hydrogen chromium oxide；
Step 2, take the solid hydrogen chromium oxide obtained in 1 weight portion step one, add 0.5 weight parts water
Rear making beating, obtains liquid of pulling an oar, and is added in reactor by making beating liquid, and adds sodium hydroxide regulation pH value
To 11, being subsequently adding oxygen, the amount of oxygen is the 90% of chromic oxide gel quality, and reacting by heating temperature is
360 DEG C, and control reaction pressure 8MPa and response time 400min, after having reacted, obtain product
Feed liquid, in product feed liquid, addition sodium hydroxide regulation pH value is to 13, impurity iron in this process
Ion produces precipitation with alkaline matter, is filtered to remove precipitation, it is achieved hexavalent chromium separates with iron ion,
And in filtrate hydro-oxidation sodium regulation pH value to 9, impurity aluminum ion and alkaline matter in this process
Produce precipitation, be filtered to remove precipitation, it is achieved hexavalent chromium separates with aluminum ions, filtrate process concentration,
Sodium chromate is obtained after crystallization.Impurity in this technical process is detected, finds that chromic content is
Less than 0.01%, the content of total chromium is less than 0.3%, and the response rate of chromite reaches 85%.
Embodiment 5:
A kind of chromite oxidizing method preparing sodium chromate of acid, comprises the following steps:
Step one, chromite is ground to form the breeze that granularity is 200 mesh, then breeze is added reactor
In and to add mass concentration be 70% sulphuric acid, sulphuric acid is 0.7 times of powdered ore quality, then with 500
Rev/min speed stir and add oxidant peroxide, peroxide charge is powdered ore quality
40%, reacting by heating temperature is 300 DEG C, and to control reaction pressure be 6.0MPa and response time 310min；
Above-mentioned technical process main chemical reactions is as follows:
Fe(CrO2)2+4H2SO4→FeSO4+Cr2(SO4)3+4H2O
(Mg, Fe) Cr2O4+5H2SO4→FeSO4+Cr2(SO4)3+MgSO4+5H2O
MgCr2O4+4H2SO4→MgSO4+Cr2(SO4)3+4H2O
(Mg, Fe)7Si8O22(OH)2+7H2SO4→7FeSiO3↓+7MgSO4↓+SiO2↓+8H2O
Oxidant peroxide and Fe (CrO2)2The master equation of reaction is as follows:
O2 2-+2Fe(CrO2)2+9H2SO4→Fe2(SO4)3+2Cr2(SO4)3+9H2O+O2-
Obtaining product feed liquid after having reacted, product feed liquid filtered and carry out solid-liquid separation, filtering residue can
As the raw material of smelting duriron, add in filtrate Calx regulation pH value to 3, generate calcium sulfate precipitation,
Being filtered to remove calcium sulfate precipitation, filtering residue calcium sulfate can do Gypsum Fibrosum, then hydro-oxidation sodium regulation in filtrate
PH value is to 6, and in this process, part magnesium ion, iron ion and the aluminium ion in filtrate can be with alkalescence
Material produces precipitation, is filtered to remove precipitation, and hydro-oxidation sodium regulation pH value is to 7 in filtrate, at this
During individual, chromium ion can produce precipitation with alkaline matter, is filtrated to get solid hydrogen chromium oxide；
Step 2, take the solid hydrogen chromium oxide obtained in 1 weight portion step one, after adding 1 weight parts water
Making beating, obtains liquid of pulling an oar, and is added in reactor by making beating liquid, and adds sodium hydroxide regulation pH value to 9,
Being subsequently adding oxygen, the amount of oxygen is the 99% of chromic oxide gel quality, and reacting by heating temperature is 180 DEG C,
And control reaction pressure 4MPa and response time 200min, after having reacted, obtain product feed liquid,
In product feed liquid add sodium hydroxide regulation pH value to 12, in this process impurity iron ion with
Alkaline matter produces precipitation, is filtered to remove precipitation, it is achieved hexavalent chromium separates with iron ion, and
In filtrate, hydro-oxidation sodium regulation pH value is to 8, and impurity aluminum ion produces with alkaline matter in this process
Precipitation, is filtered to remove precipitation, it is achieved hexavalent chromium separates with aluminum ions, and filtrate is through concentrating, tying
Sodium chromate is obtained after crystalline substance.Impurity in this technical process is detected, finds that chromic content is little
In 0.01%, the content of total chromium is less than 0.3%, and the response rate of chromite reaches 89%.
Embodiment 6:
A kind of chromite oxidizing method preparing sodium chromate of acid, comprises the following steps:
Step one, chromite is ground to form the breeze that granularity is 200 mesh, then breeze is added reactor
In and to add mass concentration be 80% sulphuric acid, sulphuric acid is 0.7 times of powdered ore quality, then with 500
Rev/min speed stir and add oxidant chromic anhydride, chromic anhydride addition is the 50% of powdered ore quality,
Reacting by heating temperature is 360 DEG C, and to control reaction pressure be 8.0MPa and response time 400min；
Above-mentioned technical process main chemical reactions is as follows:
Fe(CrO2)2+4H2SO4→FeSO4+Cr2(SO4)3+4H2O
(Mg, Fe) Cr2O4+5H2SO4→FeSO4+Cr2(SO4)3+MgSO4+5H2O
MgCr2O4+4H2SO4→MgSO4+Cr2(SO4)3+4H2O
(Mg, Fe)7Si8O22(OH)2+7H2SO4→7FeSiO3↓+7MgSO4↓+SiO2↓+8H2O
Oxidant chromic anhydride and Fe (CrO2)2The master equation of reaction is as follows:
2CrO3+6Fe(CrO2)2+30H2SO4→3Fe2(SO4)3+7Cr2(SO4)3+30H2O
Obtaining product feed liquid after having reacted, product feed liquid filtered and carry out solid-liquid separation, filtering residue can
As the raw material of smelting duriron, add in filtrate quick lime and dolomite regulation pH value to 4.5, generate sulfur
Acid calcium deposit, is filtered to remove calcium sulfate precipitation, and filtering residue calcium sulfate can do Gypsum Fibrosum, then adds carbon in filtrate
Acid hydrogen sodium regulation pH value to 5, in this process, part magnesium ion, iron ion and the aluminum in filtrate from
Son can produce precipitation with alkaline matter, is filtered to remove precipitation, and adds sodium bicarbonate regulation pH in filtrate
Value is to 8, and chromium ion can produce precipitation with alkaline matter in this process, is filtrated to get solid hydrogen oxidation
Chromium；
Step 2, take the solid hydrogen chromium oxide obtained in 1 weight portion step one, add 1.5 weight parts waters
Rear making beating, obtains liquid of pulling an oar, and is added in reactor by making beating liquid, and adds sodium bicarbonate regulation pH value
To 13, being subsequently adding oxygen, the amount of oxygen is the 70% of chromic oxide gel quality, and reacting by heating temperature is
180 DEG C, and control reaction pressure 4MPa and response time 200min, after having reacted, obtain product
Feed liquid, in product feed liquid add sodium bicarbonate regulation pH value to 9, in this process impurity iron from
Son produces precipitation with alkaline matter, is filtered to remove precipitation, it is achieved hexavalent chromium separates with iron ion,
And add in filtrate sodium bicarbonate regulation pH value to 9, impurity aluminum ion and alkaline matter in this process
Produce precipitation, be filtered to remove precipitation, it is achieved hexavalent chromium separates with aluminum ions, filtrate process concentration,
Sodium chromate is obtained after crystallization.Impurity in this technical process is detected, finds that chromic content is
Less than 0.01%, the content of total chromium is less than 0.3%, and the response rate of chromite reaches 87%.
Embodiment 7:
A kind of chromite oxidizing method preparing sodium chromate of acid, comprises the following steps:
Step one, chromite is ground to form the breeze that granularity is 200 mesh, then breeze is added reactor
In and to add mass concentration be 50% sulphuric acid, sulphuric acid is 0.7 times of powdered ore quality, then with 500
Rev/min speed stirring, reacting by heating temperature is 340 DEG C, and to control reaction pressure be 7.0MPa and anti-
It is 300min between Ying Shi；
Above-mentioned technical process main chemical reactions is as follows:
Fe(CrO2)2+4H2SO4→FeSO4+Cr2(SO4)3+4H2O
(Mg, Fe) Cr2O4+5H2SO4→FeSO4+Cr2(SO4)3+MgSO4+5H2O
MgCr2O4+4H2SO4→MgSO4+Cr2(SO4)3+4H2O
(Mg, Fe)7Si8O22(OH)2+7H2SO4→7FeSiO3↓+7MgSO4↓+SiO2↓+8H2O
Obtaining product feed liquid after having reacted, product feed liquid filtered and carry out solid-liquid separation, filtering residue can
As the raw material of smelting duriron, add in filtrate dolomite regulation pH value to 4, generate calcium sulfate precipitation,
Being filtered to remove calcium sulfate precipitation, filtering residue calcium sulfate can do Gypsum Fibrosum, then hydro-oxidation sodium regulation in filtrate
PH value is to 6, and in this process, part magnesium ion, iron ion and the aluminium ion in filtrate can be with alkalescence
Material produces precipitation, is filtered to remove precipitation, and hydro-oxidation sodium regulation pH value is to 9 in filtrate, at this
During individual, chromium ion can produce precipitation with alkaline matter, is filtrated to get solid hydrogen chromium oxide；
Step 2, take the solid hydrogen chromium oxide obtained in 1 weight portion step one, after adding 1 weight parts water
Making beating, obtains liquid of pulling an oar, and is added in reactor by making beating liquid, and adds sodium hydroxide regulation pH value to 9,
Being subsequently adding oxygen, the amount of oxygen is the 70% of chromic oxide gel quality, and reacting by heating temperature is 180 DEG C,
And control reaction pressure 4MPa and response time 200min, after having reacted, obtain product feed liquid,
In product feed liquid add sodium hydroxide regulation pH value to 14, in this process impurity iron ion with
Alkaline matter produces precipitation, is filtered to remove precipitation, it is achieved hexavalent chromium separates with iron ion, and
In filtrate, hydro-oxidation sodium regulation pH value is to 9, and impurity aluminum ion produces with alkaline matter in this process
Precipitation, is filtered to remove precipitation, it is achieved hexavalent chromium separates with aluminum ions, and filtrate is through concentrating, tying
Sodium chromate is obtained after crystalline substance.Impurity in this technical process is detected, finds that chromic content is little
In 0.01%, the content of total chromium is less than 0.3%, and the response rate of chromite reaches 89%.
Embodiment 8:
A kind of chromite oxidizing method preparing sodium chromate of acid, comprises the following steps:
Step one, chromite is ground to form the breeze that granularity is 100 mesh, then breeze is added reactor
In and to add mass concentration be 10% sulphuric acid, sulphuric acid is 0.7 times of powdered ore quality, then with 500
Rev/min speed stir and add oxidant chromic anhydride, chromic anhydride addition is the 50% of powdered ore quality,
Microwave heating reaction temperature is 100 DEG C, and microwave frequency is 2450 ± 50MHz, and controls reaction pressure and be
8.0MPa and response time 100min；Obtain product feed liquid after having reacted, product feed liquid is filtered
Carrying out solid-liquid separation, filtering residue can add quick lime as the raw material of smelting duriron and dolomite adjusted in filtrate
Joint pH value, to 4, generates calcium sulfate precipitation, is filtered to remove calcium sulfate precipitation, and filtering residue calcium sulfate can do Gypsum Fibrosum,
Then add in filtrate sodium bicarbonate regulation pH value to 5, in this process, the part magnesium in filtrate from
Son, iron ion and aluminium ion can produce precipitation with alkaline matter, are filtered to remove precipitation, and add in filtrate
Sodium bicarbonate regulation pH value is to 9, and chromium ion can produce precipitation with alkaline matter in this process, filters
Obtain solid hydrogen chromium oxide；
Step 2, take the solid hydrogen chromium oxide obtained in 1 weight portion step one, after adding 1 weight parts water
Making beating, obtains liquid of pulling an oar, and is added in reactor by making beating liquid, and adds sodium bicarbonate regulation pH value extremely
12, it is subsequently adding oxygen, the amount of oxygen is the 70% of chromic oxide gel quality, and microwave heating reaction temperature is
180 DEG C, microwave frequency is 2450 ± 50MHz, and controls reaction pressure 8MPa and response time 100min,
After having reacted, obtain product feed liquid, in product feed liquid, add sodium bicarbonate regulation pH value extremely
12, impurity iron ion produces precipitation with alkaline matter in this process, is filtered to remove precipitation, it is achieved six
Valency chromium ion separates with iron ion, and add in filtrate sodium bicarbonate regulation pH value to 8, in this mistake
In journey, impurity aluminum ion produces precipitation with alkaline matter, is filtered to remove precipitation, it is achieved hexavalent chromium and aluminum
The separation of ion, filtrate obtains sodium chromate after concentrating, crystallizing.Impurity in this technical process is entered
Row detection, finds that chromic content is that the content of total chromium is less than 0.3%, and chromium less than 0.01%
The response rate of iron mine reaches 90%.
Embodiment 9:
A kind of chromite oxidizing method preparing sodium chromate of acid, comprises the following steps:
Step one, chromite is ground to form the breeze that granularity is 200 mesh, then breeze is added reactor
In and to add mass concentration be 40% sulphuric acid, sulphuric acid is 0.7 times of powdered ore quality, then with 500
Rev/min speed stir and add the compounding oxygen that weight ratio is the sodium dichromate of 1:1:1, oxygen and chromic anhydride
Agent, its addition is the 20% of powdered ore quality, and reacting by heating temperature is 140 DEG C, and controls reaction pressure
Power is 2.0MPa and response time 150min；
Obtaining product feed liquid after having reacted, product feed liquid filtered and carry out solid-liquid separation, filtering residue can
As the raw material of smelting duriron, add in filtrate dolomite regulation pH value to 5.5, generate calcium sulfate precipitation,
Being filtered to remove calcium sulfate precipitation, filtering residue calcium sulfate can do Gypsum Fibrosum, and then adding weight ratio in filtrate is 1:1:
Sodium bicarbonate, sodium hydroxide and the sodium carbonate regulation pH value of 1 are to 6.5, in this process, in filtrate
Part magnesium ion, iron ion and aluminium ion can with alkaline matter produce precipitation, be filtered to remove precipitation, and
Filtrate adds weight ratio be the sodium bicarbonate of 1:1:1, sodium hydroxide and sodium carbonate regulation pH value to 9,
Chromium ion can produce precipitation with alkaline matter in this process, is filtrated to get solid hydrogen chromium oxide；
Step 2, take the solid hydrogen chromium oxide obtained in 1 weight portion step one, add 1.5 weight parts waters
Rear making beating, obtains liquid of pulling an oar, and is added in reactor by making beating liquid, and adds the carbonic acid that weight ratio is 1:1:1
Hydrogen sodium, sodium hydroxide and sodium carbonate regulation pH value are to 14, and reacting by heating temperature is 180 DEG C, and controls
Reaction pressure 4MPa and response time 200min, after having reacted, obtain product feed liquid, to generation
In material liquid add weight ratio be the sodium bicarbonate of 1:1:1, sodium hydroxide and sodium carbonate regulation pH value to 14,
Impurity iron ion produces precipitation with alkaline matter in this process, is filtered to remove precipitation, it is achieved Cr VI
Ion separates with iron ion, and add in filtrate weight ratio be the sodium bicarbonate of 1:1:1, sodium hydroxide and
Sodium carbonate regulation pH value is to 9, and impurity aluminum ion produces precipitation with alkaline matter in this process, filters
Removing precipitation, it is achieved hexavalent chromium separates with aluminum ions, filtrate obtains chromium after concentrating, crystallizing
Acid sodium.Impurity in this technical process is detected, finds that chromic content is less than 0.01%,
The content of total chromium is less than 0.3%, and the response rate of chromite reaches 85%.
In order to the effect of the present invention is described, inventor provides contrast experiment as follows:
Comparative example 1:
In step one of the present invention, the reaction pressure of employing is 0.2MPa, and it is less than model of the present invention
Enclosing, remaining parameter is identical with embodiment 6, and technical process is the most identical.To this technique mistake
Impurity in journey detects, and finds that chromic content is 0.05%, and the content of total chromium is 0.6%, and
And the response rate of chromite is 70%.
Comparative example 2:
In step one of the present invention, the reaction pressure of employing is 9MPa, and it is more than scope of the present invention,
Remaining parameter is identical with embodiment 6, and technical process is the most identical.To in this technical process
Impurity detect, find chromic content for less than 0.01%, the content of total chromium is less than 0.3%,
And the response rate of chromite reaches 87%.
From above-mentioned it can be seen that work as the reaction pressure used comparative example 1 step one less than of the present invention
Scope time, impurity finding, chromic content is 0.05%, the content of total chromium is 0.6%, and chromium
The response rate of iron mine is 70%, and effect is poor.The reaction pressure used in comparative example 2 step one is more than this
Scope described in invention, its experiment effect is identical with embodiment 6, illustrates to use higher than institute of the present invention
When stating the pressure of scope, it is impossible to improve experiment effect further, and equipment can be produced higher requirement.
Comparative example 3:
In step 2 of the present invention, after having reacted, in product feed liquid, add sodium hydroxide regulation pH
Value is to 8, and it is not in scope of the present invention, and remaining parameter is identical with embodiment 6,
Technical process is the most identical.The sodium chromate prepared is detected, compared with Example 6, right
In the sodium chromate of ratio 3, the content of ferrum is higher than embodiment 6.Illustrate only at the tune of pH of the present invention
Adjusting range can prepare the sodium chromate that purity is high.
Comparative example 4:
In step 2 of the present invention, after having reacted, second time regulation pH value is to 5, and it is less than the present invention
The scope of described pH value 6～9, remaining parameter is identical with embodiment 6, and technical process is also
Identical.The sodium chromate prepared is detected, compared with Example 6, the chromium of comparative example 4
In acid sodium, the content of aluminum is higher than embodiment 6.
Comparative example 5:
In step 2 of the present invention, after having reacted, second time regulation pH value is to 10, and it is more than this
The scope of bright described pH value 6～9, remaining parameter is identical with embodiment 6, technical process
The most identical.The sodium chromate prepared is detected, compared with Example 6, comparative example 4
In sodium chromate, the content of aluminum is higher than embodiment 6.
From comparative example 4 and comparative example 5 it can be seen that step 2 of the present invention, after having reacted,
It is high that Secondary Control pH value only can prepare purity in the range of accommodation of pH of the present invention
Sodium chromate.
Visible, in the present invention, chromite can break in pressurization, the reaction that adds oxidant in the environment of strong acid
Bad chromite spinel structure, improve chromite dissolution rate, and by regulation pH value make ferrum, aluminum,
Silicon, magnesium plasma efficiently separate with chromium ion.
Although embodiment of the present invention are disclosed as above, but it is not restricted to description and embodiment party
Listed utilization in formula, it can be applied to various applicable the field of the invention completely, for being familiar with ability
For the personnel in territory, be easily achieved other amendment, therefore without departing substantially from claim and etc. homotype
Enclosing under limited general concept, the present invention is not limited to specific details and shown here as the figure with description
Example.
Claims (10)
1. the chromite oxidizing method preparing sodium chromate of acid, it is characterised in that comprise the following steps:
Step one, chromite is ground to form the breeze that granularity is 100～200 mesh, then breeze is added anti-
Answer in still and add sulphuric acid, stirring with the speed of 300～800 revs/min, reacting by heating, and controlling reaction
Pressure and response time, after having reacted, obtain product feed liquid, product feed liquid is filtered and carries out solid-liquid
Separate, filtrate adds calcic Ore regulation pH value to 2-5.5, generate calcium sulfate precipitation, be filtered to remove
Calcium sulfate precipitation, then add in filtrate alkaline matter regulation pH value to 4-6.5, be filtered to remove precipitation,
And add in filtrate alkaline matter regulation pH value to 6.5-9.5, be filtrated to get solid hydrogen chromium oxide；
Step 2, take the solid hydrogen chromium oxide obtained in 1 weight portion step one, add 0.5～1.5 weight portions
Pull an oar after water, obtain liquid of pulling an oar, making beating liquid is added in reactor, and add alkaline matter regulation pH
It is worth to 8～14, reacting by heating, and controls reaction pressure and response time, after having reacted, generated
Material liquid, in product feed liquid, addition alkaline matter regulation pH value is to 9-14, is filtered to remove precipitation,
And in filtrate, add alkaline matter regulation pH value to 8-9, be filtered to remove precipitation, filtrate through concentrating, knot
Sodium chromate is obtained after crystalline substance.
2. the chromite oxidizing method preparing sodium chromate of acid as claimed in claim 1, it is characterised in that
Also need to after described step one adds sulphuric acid add oxidant.
3. the chromite oxidizing method preparing sodium chromate of acid as claimed in claim 2, it is characterised in that
Described oxidant is one or more in sodium dichromate, oxygen, chromic anhydride, peroxide, persulfate
Combination, its addition is the 0～50% of powdered ore quality.
4. the chromite oxidizing method preparing sodium chromate of acid as claimed in claim 3, it is characterised in that
Described peroxide is the one in sodium peroxide or hydrogen peroxide；Described persulfate be sodium peroxydisulfate or
One in Ammonium persulfate..
5. the chromite oxidizing method preparing sodium chromate of acid as claimed in claim 1, it is characterised in that
In described step one, the mass concentration of sulphuric acid is 1～90%, and its addition is 0.3～0.9 times of powdered ore quality.
6. the chromite oxidizing method preparing sodium chromate of acid as claimed in claim 1, it is characterised in that
Described alkaline matter is the combination of one or more in sodium bicarbonate, sodium carbonate and oxygen sodium oxide；Described
Calcic Ore is the combination of one or more in quick lime, Calx, dolomite.
7. the chromite oxidizing method preparing sodium chromate of acid as claimed in claim 1, it is characterised in that
In described step one, reaction temperature is 50～360 DEG C, and reaction pressure is 0.3～8MPa, and the response time is
10～400min.
8. the chromite oxidizing method preparing sodium chromate of acid as claimed in claim 1, it is characterised in that
Also needing to before reacting by heating in described step 2 add oxygen, its addition is chromic oxide gel quality
0～99%.
9. the chromite oxidizing method preparing sodium chromate of acid as claimed in claim 1, it is characterised in that
In described step 2, reaction temperature is room temperature～360 DEG C, and reaction pressure is 0.01～8MPa, and the response time is
1～400min.
10. the chromite oxidizing method preparing sodium chromate of acid as claimed in claim 1, its feature exists
In, the reacting by heating in described step one and step 2 all uses microwave heating, and the microwave of microwave heating
Frequency is 2450 ± 50MHz.
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