CN107236963A - A kind of method that chlorination ferroelectricity conversion directly prepares iron hydroxide or iron oxide - Google Patents
A kind of method that chlorination ferroelectricity conversion directly prepares iron hydroxide or iron oxide Download PDFInfo
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- CN107236963A CN107236963A CN201710324343.7A CN201710324343A CN107236963A CN 107236963 A CN107236963 A CN 107236963A CN 201710324343 A CN201710324343 A CN 201710324343A CN 107236963 A CN107236963 A CN 107236963A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/26—Chlorine; Compounds thereof
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Abstract
A kind of method that chlorination ferroelectricity conversion directly prepares iron hydroxide or iron oxide, belongs to iron-containing resource and utilizes field.This method is electrolysed to ferric chloride in aqueous solution, 10 DEG C≤temperature<100 DEG C, voltage >=2.2V of electrolysis；The pH value for controlling cathode chamber electrolyte in cationic membrane electrolytic cell is 8~12, makes to directly generate iron hydroxide in cationic membrane electric tank cathode room；The cathode chamber of cationic membrane electrolytic cell is stirred, cathode chamber electrolyte and iron hydroxide directed flow, through filter, separation of solid and liquid obtains iron hydroxide and filtrate, iron hydroxide is dried, and obtains iron hydroxide product.Obtained iron hydroxide product is calcined again, iron oxide, its purity >=95% is made.It this method solve high cost present in prior art, acid or alkali and consume the problems such as big, environmental pollution is serious, high with electrolysis process automaticity, it is easy to control, product purity is high, advantageously reduces the advantage of production cost.
Description
Technical field
Utilize field the invention belongs to iron-containing resource, and in particular to a kind of conversion of chlorination ferroelectricity directly prepare iron hydroxide or
The method of iron oxide.
Background technology
Iron dust is in the feeromagnetic metal of the VIIIth subgroup.Iron hydroxide is a kind of amorphous substance, can be used to pigment processed, medicine,
Water purification agent, it can also be used to cook the antidote of arsenic.Iron oxide (di-iron trioxide) is red-brown powder, industrially referred to as iron oxide
It is red, for painting, the coloring of rubber, plastics, building etc., it is inorganic pigment, rust resisting pigment is used as in coatings industry.Also serve as
Rubber, artificial marble, the colouring agent of ground terrazzo, the colouring agent of plastics, asbestos, artificial leather, leather casein finiss etc. and are filled out
Fill agent, raw material of precision instrument, the polishing agent of optical glass and manufacture magnetic material ferrite component etc..Because of its extensive use,
The iron hydroxide production method that research and development purity is high, technique is simple, environment-friendly have important practical significance with it is wide
Development prospect.
The preparation method of current iron hydroxide mainly has two kinds of wet method and dry method.Wet method is by a certain amount of 5% ferrous sulfate
Solution reacts (it is required that base excess) with excess sodium hydroxide solution rapidly, and air is passed through at normal temperatures, is allowed to all be changed into reddish brown
The ferric hydroxide colloid solution of color, is used as the nucleus of deposition of iron oxide.Using above-mentioned nucleus as carrier, using ferrous sulfate as medium,
Air is passed through, under 75~85 DEG C, metallic iron existence condition, ferrous sulfate and oxygen effect generation di-iron trioxide in air
(i.e. iron oxide red) is deposited on nucleus, and the sulfate radical in solution regenerates ferrous sulfate with metallic iron effect again, and ferrous sulfate is again
It is oxidised with air to iron oxide red to continue to deposit, is so recycled to whole process and terminates, generate red iron oxide.Dry way process is nitric acid
With iron filings reaction generation ferrous nitrate, through crystallisation by cooling, dehydrate, grind after, in 600~700 DEG C of 8~10h of calcining, then pass through
Iron oxide red product is made in washing, dry, crushing.Can also iron oxide yellow be raw material, through 600~700 DEG C calcining be made oxidation
Iron oxide red.The technique of both approaches is all long, process is cumbersome, consumes substantial amounts of alkali or acid, is unfavorable for environmental protection, and operation
Environment is poor.
The content of the invention
For the problems such as cost present in prior art is high, acid or alkali consumption are big, environmental pollution is serious, the present invention is provided
A kind of method that chlorination ferroelectricity conversion directly prepares iron hydroxide or iron oxide, it is therefore an objective to by electrolytic chlorination water solution straight
Obtain to obtain iron hydroxide product and byproduct hydrogen and chlorine.
In order to realize the purpose of the present invention, a kind of chlorination ferroelectricity conversion of the invention directly prepares iron hydroxide or iron oxide
Method, follow the steps below：
Step 1：Ferric chloride in aqueous solution is electrolysed, the technique of electrolysis is：10 DEG C≤temperature<100 DEG C, the voltage of electrolysis
≥2.2V；
Step 2：The pH value for controlling cathode chamber electrolyte in cationic membrane electrolytic cell is 8~12, makes cationic membrane electrolytic cell
Iron hydroxide is directly generated in cathode chamber；
Step 3：The cathode chamber of cationic membrane electrolytic cell is stirred, cathode chamber electrolyte and iron hydroxide oriented flow
It is dynamic, filtered by filter, separation of solid and liquid, obtain iron hydroxide and filtrate, filtrate cycle is back to cathode chamber conduct
Cathode chamber electrolyte；Anode chamber's solution is continuously extracted out, and anode chamber is returned to after adjusted concentration；Collect anodic gas and obtain byproduct
Chlorine, collects cathode gas and obtains byproduct hydrogen；
Step 4：Iron hydroxide is dried, iron hydroxide product is obtained.
The method that a kind of chlorination ferroelectricity conversion of the present invention directly prepares iron hydroxide or iron oxide, by above-mentioned step
1st, after step 2, step 3, step 4, then obtained iron hydroxide product calcined, iron oxide product, iron oxide production is made
Purity >=95% of product.
In described step 1, the mass concentration of described ferric chloride in aqueous solution is any concentration.
In described step 1, described electrolysis temperature is preferably 20~90 DEG C.
In described step 1, described electrolysis is carried out in electrolysis system, electrolysis system include cationic membrane electrolytic cell and
It is recovered by filtration and utilizes device；
Described cation electrolytic cell includes：Cell body, cathode chamber, anode chamber, cation-exchange membrane, agitator, direct current
Source；
Described being recovered by filtration includes filter, drying box, the first dissolving tank, the first pump, the second dissolving using device
Groove and the second pump；
Wherein, cell body is internally provided with cation-exchange membrane, and cell body is divided into anode chamber and cathode chamber by cation-exchange membrane,
Wherein, be connected with the positive pole of dc source for anode chamber, be connected with the negative pole of dc source for cathode chamber, in cathode chamber
Agitator is provided with, described agitator is stirred by electrode drive；
Filter is provided with below cathode chamber, filter is provided with solid outlet and liquid outlet, filtering dress
The solid outlet put is connected with drying box, and the liquid outlet of filter is connected with the second dissolving tank, and the second dissolving tank leads to
The second pump is crossed to communicate with cathode chamber；
Opening is set to be connected with the first dissolving tank in the downside of anode chamber, the first dissolving tank passes through the first pump and anode chamber
Communicate.
Described electrolysis system has the function of stirring and filtering.
In described step 2, the pH value control method of cathode chamber electrolyte is that control DC current flow density or addition are slow
Release agent to be adjusted, described sustained release agent is ammoniacal liquor.
In described step 3, described stirring is mechanical agitation or electromagnetic agitation, and the effect of the stirring is to suppress groove
Body bottom precipitation；
In described step 3, described directed flow is continuous flowing or intermittent flow, the time of described intermittent flow
It is spaced according to depending on filter plant difference used.
In described step 3, described filtrate adds water and adjusted to original content, is recycled back to cathode chamber as cathode chamber
Electrolyte, anode chamber's electrolyte is added after extracting out after iron chloride adjustment concentration to initial reaction ferric chloride concn, is back to anode
Room, realizes recycling for iron chloride.
In described step 4, described drying, drying condition is：20~80 DEG C of drying of vacuum.
The key reaction that the method that a kind of chlorination ferroelectricity conversion of the present invention directly prepares iron hydroxide is related to is as follows：
Anode reaction：2Cl-- 2e=Cl2 (1)
Cathode reaction：2H2O+2e=H2+2OH- (2)
Overall reaction：
A kind of method that chlorination ferroelectricity conversion directly prepares iron oxide, the calcination reaction being related to is as follows：
Calcination reaction：2Fe(OH)3=Fe2O3+3H2O↑
Check in, at 25 DEG C, standard production potential V1=-1.3583V, V2=-0.8277V, then EAlways=-2.186V, so,
Tank voltage necessarily be greater than 2.186V.
Compared with prior art, the method that a kind of chlorination ferroelectricity of the invention conversion directly prepares iron hydroxide or iron oxide
Have the advantages that：
1. using the method for electrolysis, iron chloride can directly prepare iron hydroxide, electrolysis process automaticity therein
High, it is easy to control, product purity is high, advantageously reduces production cost.
2. electrolyte can be the ferric chloride solution of any concentration.
3. the electrolysis system that the present invention is used, its cathode chamber electrolyte is continuously circulated through filter, adjustment solution is dense
Cathode chamber is returned after degree, the continuous production of iron hydroxide product can be achieved.
4. this invention removes the consumption and environmental pollution of a large amount of alkali in traditional iron hydroxide and iron oxide production process.
Brief description of the drawings
Fig. 1 is the structural representation of electrolysis system of the present invention.
Wherein, 1- cathode chambers；2- anode chambers；3- cation-exchange membranes；4- agitators；5- dc sources；6- filters；
7- drying boxes；The dissolving tanks of 8- first；The pumps of 9- first；The dissolving tanks of 10- second；The pumps of 11- second；12- cell bodies.
Embodiment
With reference to embodiment, the present invention is described in further detail.
In following examples, electrolysis is carried out in electrolysis system, and the structural representation of electrolysis system is shown in Fig. 1, electrolysis system
Including cationic membrane electrolytic cell and it is recovered by filtration and utilizes device；
Described cation electrolytic cell includes：Cell body 12, cathode chamber 1, anode chamber 2, cation-exchange membrane 3, the and of agitator 4
Dc source 5；
Described being recovered by filtration includes filter 6, drying box 7, the first dissolving tank 8, the first pump 9, second using device
The pump 11 of dissolving tank 10 and second；
Wherein, cell body 12 is internally provided with cation-exchange membrane 3, and cell body is divided into anode chamber and the moon by cation-exchange membrane 3
Pole room, wherein, be connected with the positive pole of dc source 5 for anode chamber 2, be connected with the negative pole of dc source 5 for cathode chamber 1,
Agitator 4 is provided with cathode chamber 1, described agitator 4 is stirred by electrode drive；
Filter 6 is provided with the lower section of cathode chamber 1, filter 6 is provided with solid outlet and liquid outlet, filtered
The solid outlet of device is connected with drying box 7, and the liquid outlet of filter is connected with the second dissolving tank 10, the second dissolving
Groove 10 is communicated by the second pump 11 with the upside of cathode chamber 1；
Opening is set to be connected with the first dissolving tank 8 in the downside of anode chamber 2, the first dissolving tank 8 passes through the first pump 9 and sun
The upside of pole room 2 is communicated.
Embodiment 1
A kind of method that chlorination ferroelectricity conversion directly prepares iron hydroxide or iron oxide, is followed the steps below：
Step 1：The ferric chloride in aqueous solution of mass concentration 10% is electrolysed, the technique of electrolysis is：20 DEG C of electrolysis temperature,
The voltage of electrolysis is 2.2V；
Step 2：Cathode chamber electrolyte ph is controlled in cationic membrane electrolytic cell by control electric current density in 8-12 models
In enclosing, make to directly generate iron hydroxide in cationic membrane electric tank cathode room；
Step 3：Mechanical agitation is carried out to the cathode chamber of cationic membrane electrolytic cell, cathode chamber electrolyte and iron hydroxide are continuous
Directed flow, is filtered by filter, separation of solid and liquid, obtains iron hydroxide and filtrate, filtrate add water adjust to
10% is recycled back to cathode chamber as cathode chamber electrolyte；Anode chamber's solution is continuously extracted out, adds iron chloride adjustment concentration extremely
After initial reaction ferric chloride concn (10%), anode chamber is returned to；Collect anodic gas and obtain byproduct chlorine, collect cathode gas
Obtain byproduct hydrogen；
Step 4：Iron hydroxide is placed in 20 DEG C of drying of vacuum, iron hydroxide product is obtained.
Obtained iron hydroxide product is calcined, iron oxide product is made, the purity of iron oxide product is 95%.
Embodiment 2
A kind of method that chlorination ferroelectricity conversion directly prepares iron hydroxide or iron oxide, is followed the steps below：
Step 1：The ferric chloride in aqueous solution of mass concentration 12% is electrolysed, the technique of electrolysis is：90 DEG C of electrolysis temperature,
The voltage of electrolysis is 20V；
Step 2：Cathode chamber electrolyte ph is controlled in cationic membrane electrolytic cell by control electric current density in 8-12 models
In enclosing, make to directly generate iron hydroxide in cationic membrane electric tank cathode room；
Step 3：Mechanical agitation is carried out to the cathode chamber of cationic membrane electrolytic cell, cathode chamber electrolyte and iron hydroxide are continuous
Directed flow, is filtered by filter, separation of solid and liquid, obtains iron hydroxide and filtrate, filtrate add water adjust to
12% is recycled back to cathode chamber as cathode chamber electrolyte；Anode chamber's solution is continuously extracted out, adds iron chloride adjustment concentration extremely
After initial reaction ferric chloride concn (12%), anode chamber is returned to；Collect anodic gas and obtain byproduct chlorine, collect cathode gas
Obtain byproduct hydrogen；
Step 4：Iron hydroxide is placed in 60 DEG C of drying of vacuum, iron hydroxide product is obtained.
Obtained iron hydroxide product is calcined, iron oxide product is made, the purity of iron oxide product is 96%.
Embodiment 3
A kind of method that chlorination ferroelectricity conversion directly prepares iron hydroxide or iron oxide, is followed the steps below：
Step 1：The ferric chloride in aqueous solution of mass concentration 8% is electrolysed, the technique of electrolysis is：10 DEG C of electrolysis temperature,
The voltage of electrolysis is 2.2V；
Step 2：Cathode chamber electrolyte ph is controlled in cationic membrane electrolytic cell by control electric current density in 8-12 models
In enclosing, make to directly generate iron hydroxide in cationic membrane electric tank cathode room；
Step 3：Electromagnetic agitation is carried out to the cathode chamber of cationic membrane electrolytic cell, cathode chamber electrolyte and iron hydroxide are continuous
Directed flow, is filtered by filter, separation of solid and liquid, obtains iron hydroxide and filtrate, and filtrate adds water and adjusted to 8%
Cathode chamber is recycled back to as cathode chamber electrolyte；Anode chamber's solution is continuously extracted out, is added iron chloride and is adjusted concentration to initial
React after ferric chloride concn (8%), return to anode chamber；Collect anodic gas and obtain byproduct chlorine, collect cathode gas and obtain
Byproduct hydrogen；
Step 4：Iron hydroxide is placed in 80 DEG C of drying of vacuum, iron hydroxide product is obtained.
Obtained iron hydroxide product is calcined, iron oxide product is made, the purity of iron oxide product is 95.8%.
Embodiment 4
A kind of method that chlorination ferroelectricity conversion directly prepares iron hydroxide or iron oxide, is followed the steps below：
Step 1：The ferric chloride in aqueous solution of mass concentration 10% is electrolysed, the technique of electrolysis is：50 DEG C of electrolysis temperature,
The voltage of electrolysis is 10V；
Step 2：By adding sustained release agent --- ammoniacal liquor controls the cathode chamber electrolyte ph in cationic membrane electrolytic cell to exist
In the range of 8-12, make to directly generate iron hydroxide in cationic membrane electric tank cathode room；
Step 3：Mechanical agitation is carried out to the cathode chamber of cationic membrane electrolytic cell, cathode chamber electrolyte and iron hydroxide are continuous
Directed flow, is filtered by filter, separation of solid and liquid, obtains iron hydroxide and filtrate, filtrate add water adjust to
10% is recycled back to cathode chamber as cathode chamber electrolyte；Anode chamber's solution is continuously extracted out, adds iron chloride adjustment concentration extremely
After initial reaction ferric chloride concn (10%), anode chamber is returned to；Collect anodic gas and obtain byproduct chlorine, collect cathode gas
Obtain byproduct hydrogen；
Step 4：Iron hydroxide is placed in 40 DEG C of drying of vacuum, iron hydroxide product is obtained.
Obtained iron hydroxide product is calcined, iron oxide product is made, the purity of iron oxide product is 95%.
Claims (10)
1. a kind of method that chlorination ferroelectricity conversion directly prepares iron hydroxide or iron oxide, it is characterised in that according to following steps
Carry out：
Step 1：Ferric chloride in aqueous solution is electrolysed, the technique of electrolysis is：10 DEG C≤temperature<100 DEG C, the voltage of electrolysis >=
2.2V；
Step 2：The pH value for controlling cathode chamber electrolyte in cationic membrane electrolytic cell is 8~12, makes cationic membrane electric tank cathode
Interior directly generates iron hydroxide；
Step 3：The cathode chamber of cationic membrane electrolytic cell is stirred, cathode chamber electrolyte and iron hydroxide directed flow, led to
Cross filter to be filtered, separation of solid and liquid, obtain iron hydroxide and filtrate, filtrate cycle is back to cathode chamber as cathode chamber
Electrolyte；Anode chamber's solution is continuously extracted out, and anode chamber is returned to after adjusted concentration；Collect anodic gas and obtain byproduct chlorine,
Collect cathode gas and obtain byproduct hydrogen；
Step 4：Iron hydroxide is dried, iron hydroxide product is obtained.
2. a kind of method that chlorination ferroelectricity conversion directly prepares iron hydroxide or iron oxide, it is characterised in that pass through claim 1
After described step 1, step 2, step 3, step 4, then obtained iron hydroxide product calcined, iron oxide production is made
Product, purity >=95% of iron oxide product.
3. the method that a kind of chlorination ferroelectricity conversion as claimed in claim 1 or 2 directly prepares iron hydroxide or iron oxide, it is special
Levy and be, in described step 1, the mass concentration of described ferric chloride in aqueous solution is any concentration.
4. the method that a kind of chlorination ferroelectricity conversion as claimed in claim 1 or 2 directly prepares iron hydroxide or iron oxide, it is special
Levy and be, in described step 1, described electrolysis temperature is preferably 20~90 DEG C.
5. the method that a kind of chlorination ferroelectricity conversion as claimed in claim 1 or 2 directly prepares iron hydroxide or iron oxide, it is special
Levy and be, in described step 1, described electrolysis is carried out in electrolysis system, electrolysis system include cationic membrane electrolytic cell and
It is recovered by filtration and utilizes device；
Described cation electrolytic cell includes：Cell body, cathode chamber, anode chamber, cation-exchange membrane, agitator, dc source；
It is described be recovered by filtration using device include filter, drying box, the first dissolving tank, the first pump, the second dissolving tank and
Second pump；
Wherein, cell body is internally provided with cation-exchange membrane, and cell body is divided into anode chamber and cathode chamber by cation-exchange membrane, its
In, be connected with the positive pole of dc source for anode chamber, be connected with the negative pole of dc source for cathode chamber, set in cathode chamber
Agitator is equipped with, described agitator is stirred by electrode drive；
Filter is provided with below cathode chamber, filter is provided with solid outlet and liquid outlet, filter
Solid outlet is connected with drying box, and the liquid outlet of filter is connected with the second dissolving tank, and the second dissolving tank passes through
Two pumps are communicated with cathode chamber；
Opening is set to be connected with the first dissolving tank in the downside of anode chamber, the first dissolving tank passes through the first pump and anode chamber's phase
It is logical.
6. the method that a kind of chlorination ferroelectricity conversion as claimed in claim 1 or 2 directly prepares iron hydroxide or iron oxide, it is special
Levy and be, in described step 2, the pH value control method of cathode chamber electrolyte is control DC current flow density or addition sustained release
Agent is adjusted, and described sustained release agent is ammoniacal liquor.
7. the method that a kind of chlorination ferroelectricity conversion as claimed in claim 1 or 2 directly prepares iron hydroxide or iron oxide, it is special
Levy and be, in described step 3, described stirring is mechanical agitation or electromagnetic agitation.
8. the method that a kind of chlorination ferroelectricity conversion as claimed in claim 1 or 2 directly prepares iron hydroxide or iron oxide, it is special
Levy and be, in described step 3, described directed flow is continuous flowing or intermittent flow, the time of described intermittent flow
It is spaced according to depending on filter plant difference used.
9. the method that a kind of chlorination ferroelectricity conversion as claimed in claim 1 or 2 directly prepares iron hydroxide or iron oxide, it is special
Levy and be, in described step 3, described filtrate addition water, which is adjusted to original content, is recycled back to cathode chamber as cathode chamber electricity
Liquid is solved, anode chamber's electrolyte is added after extracting out after iron chloride adjustment concentration to initial reaction ferric chloride concn, is back to anode chamber,
Realize recycling for iron chloride.
10. the method that a kind of chlorination ferroelectricity conversion as claimed in claim 1 or 2 directly prepares iron hydroxide or iron oxide, its
It is characterised by, in described step 4, described drying, drying condition is：20~80 DEG C of drying of vacuum.
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| CN201710324343.7A CN107236963A (en) | 2017-05-10 | 2017-05-10 | A kind of method that chlorination ferroelectricity conversion directly prepares iron hydroxide or iron oxide |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1151193A (en) * | 1994-05-26 | 1997-06-04 | 弗劳恩霍夫促进应用研究协会 | Electrochemical process and device for the production of metal hydroxides and/or metal oxide hydroxides |
| CN1210153A (en) * | 1998-02-27 | 1999-03-10 | 郑州大学 | One-step process of nickle hydroxide electrolysing |
| CN1614095A (en) * | 2004-09-16 | 2005-05-11 | 黑龙江科技学院 | Preparation of superfine metal oxide by electrolytic method |
| CN102732902A (en) * | 2011-04-15 | 2012-10-17 | 洪若瑜 | Preparation method of conductive metal oxide nanorod |
-
2017
- 2017-05-10 CN CN201710324343.7A patent/CN107236963A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1151193A (en) * | 1994-05-26 | 1997-06-04 | 弗劳恩霍夫促进应用研究协会 | Electrochemical process and device for the production of metal hydroxides and/or metal oxide hydroxides |
| CN1210153A (en) * | 1998-02-27 | 1999-03-10 | 郑州大学 | One-step process of nickle hydroxide electrolysing |
| CN1614095A (en) * | 2004-09-16 | 2005-05-11 | 黑龙江科技学院 | Preparation of superfine metal oxide by electrolytic method |
| CN102732902A (en) * | 2011-04-15 | 2012-10-17 | 洪若瑜 | Preparation method of conductive metal oxide nanorod |
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Application publication date: 20171010 |