CN110342481A - A method of phosphoric acid is prepared with ferrophosphorus - Google Patents
A method of phosphoric acid is prepared with ferrophosphorus Download PDFInfo
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- CN110342481A CN110342481A CN201910621520.7A CN201910621520A CN110342481A CN 110342481 A CN110342481 A CN 110342481A CN 201910621520 A CN201910621520 A CN 201910621520A CN 110342481 A CN110342481 A CN 110342481A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
- B03C1/30—Combinations with other devices, not otherwise provided for
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/185—Preparation neither from elemental phosphorus or phosphoric anhydride nor by reacting phosphate-containing material with an acid, e.g. by reacting phosphate-containing material with an ion-exchange resin or an acid salt used alone
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention discloses a kind of methods for preparing phosphoric acid with ferrophosphorus, comprising the following steps: S1. pulverization process: ferrophosphorus addition flour mill being ground, and sieves and obtains particulate material；S2. oxidizing roasting: roaster is added in the particulate material, and the particulate material is roasted to obtain mixed oxide to air is passed through, the mixed oxide includes Fe2O3、P2O5、SiO2；S3. heating reduction: high temperature furnace is added in the mixed oxide, and is passed through reducibility gas to the high temperature furnace under the high temperature conditions, reduzate is obtained after reaction, the reduzate includes P2O5、Fe、SiO2；S4. magnetic separation separates: magnetic separator is added in the reduzate, Fe is isolated by magnetic separation, obtains P2O5And SiO2Mixture；S5. it is separated by solid-liquid separation: by the P2O5And SiO2Mixture be added in cold water and reacted, and reaction solution and solid are separated by inoranic membrane, finally dry the solid and obtain SiO2；S6. it prepares phosphoric acid: the reaction solution being passed through hot water, end reaction obtains phosphoric acid solution.
Description
Technical field
The present invention relates to mineral chemical technology field, specifically a kind of method for preparing phosphoric acid with ferrophosphorus.
Background technique
Ferrophosphorus is the by-product in the production processes such as a kind of thermal method phosphorus or calcium magnesium phosphate, be a kind of phosphorous (P) 20~
26%, iron content (Fe) 35~47%, the symbiotic compound of siliceous (Si) 0.1~6%.The corrosion stability and chip of steel can be changed in ferrophosphorus
Property, as the alloy addition and deoxidier in metallurgy, automobile cylinder sleeve, engine roller bearing and Big Steel Castings forging piece are widely used in increase
Add the corrosion resistance and wearability of mechanical part.
According to statistics, ferrophosphorus by-product caused by every production 1t yellow phosphorus is up to 130~150kg, due to containing 20 in ferrophosphorus
~26% phosphorus.Currently, most of phosphorous chemical industry manufacturing enterprises, China are still insufficient to the utilization of by-product ferrophosphorus, some enterprises are direct
It is low so as to cause the ferrophosphorus resource utilization in phosphorous chemical industry as Solid state fermentation, in a disguised form cause the pole of ferrophosphorus resource
Big waste.However, phosphate rock resource is further exhausted with the manufacturing development of China's yellow phosphorus, while the yield of ferrophosphorus is also increasingly
Greatly.Therefore, it is just increasingly important that a large amount of ferrophosphorus caused by phosphorous chemical industry are rationally recycled.
Chinese patent literature CN201110262951.2, the applying date, title are as follows: utilize the preparation oxidation of yellow phosphorus by-product ferrophosphorus slag
The method of iron oxide red and sodium phosphate, discloses one kind using yellow phosphorus by-product ferrophosphorus slag as raw material, using ferrophosphorus slag and sodium hydroxide press than
The mode of example mixing, roasting, water logging obtains iron oxide red through separation of solid and liquid, washing, drying, then solution is concentrated, is crystallized, is dry
The dry method for obtaining sodium phosphate finished product.This method has easy to operate, and process flow is simple, resource utilization is high, economic benefit
The advantages that high.
Although the above method can solve the problem of ferrophosphorus utilizes, but there are the following problems:
1) a large amount of impurity is contained using the phosphate that this method is prepared；
2) due to the silicon in ferrophosphorus containing 0.1~6%, reaction produces silicates substance, can give birth to acid and alkali reaction
Agglutination substance not only increases operation difficulty and cost, but also can not so that slag liquid is difficult to separate the filtrate for obtaining high-purity and filter residue
Guarantee product purity；
3) this method does not carry out waste heat recycling, and the thermal efficiency is low.
Therefore, our urgent needs, which find one kind, can recycle thermal energy, and impurity in products is few, the side with high purity using ferrophosphorus
Method.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of methods for preparing phosphoric acid with ferrophosphorus, to reach
To recycling thermal energy, and the effect that impurity in products is few, with high purity.
In the present invention, mainly include following chemical reaction:
2FeP+4O2→Fe2O3+P2O5
4Fe2P+11O2→4Fe2O3+2P2O5
Si+O2→SiO2
Fe2O3+3CO→2Fe+3CO2
P2O5+H2O (cold water) → 2HPO3
HPO3+H2O (hot water) → H3PO4
The purpose of the present invention is achieved through the following technical solutions: a method of phosphoric acid being prepared with ferrophosphorus, it is described
Method the following steps are included:
S1. pulverization process: ferrophosphorus addition flour mill is ground, and sieves and obtains particulate material；
S2. oxidizing roasting: being homogeneously added into roaster for the particulate material, and be passed through air into the roaster, right
The particulate material obtains mixed oxide after being roasted, the mixed oxide includes Fe2O3、P2O5、SiO2；
S3. heating reduction: high temperature furnace is added in the mixed oxide, and is passed through under the high temperature conditions to the high temperature furnace
Reducibility gas, obtains reduzate after reaction, the reduzate includes P2O5、Fe、SiO2；
S4. magnetic separation separates: magnetic separator will be added after reduzate cooling, isolates Fe by magnetic separation, obtain P2O5With
SiO2Mixture；
S5. it is separated by solid-liquid separation: by the P2O5And SiO2Mixture be added cold water in reacted, and by inoranic membrane general
Obtained reaction solution and solid separation are reacted, it is finally that the solid is dry, obtain SiO2Solid；
S6. it prepares phosphoric acid: the reaction solution being passed through hot water, end reaction obtains phosphoric acid solution.
Through the above technical solutions, make the ferrophosphorus that oxidation reaction occur by roasting first, each member in the ferrophosphorus
The isolated Fe of element2O3、P2O5、SiO2, reducibility gas is added by Fe2O3It is reduced into the Fe simple substance of high value, has reached benefit
With the effect of ferrophosphorus output high value iron ore；Fe simple substance is separated in the way of magnetic separation, has reached the separation effect for improving Fe simple substance
The effect of rate；In addition, utilizing SiO2Principle insoluble in metaphosphoric acid, with inoranic membrane by SiO2Impurity removes, and has reached promotion product
The effect of purity；Meanwhile it can prevent high temperature from causing to the performance of the inoranic membrane using the inoranic membrane under normal temperature state
Influence, achieved the effect that protect inoranic membrane.
Preferably, in S1, the ferrophosphorus gets the particulate material after grinding, through 20 mesh screens.
Through the above technical solutions, being in particulate material by ferrophosphorus grinding, the contact area of oxidation reaction can be increased, reached
To being the fully oxidized effect of the ferrophosphorus.
Preferably, in S2, it is passed through air from the bottom of the roaster, the air carries out adsorption treatment through active carbon and obtains
It arrives.
Through the above technical solutions, can be blown afloat the particulate material from the air that the roasting furnace bottom enters, reach
Increase the effect of reaction contact area；In addition to this, air is handled using the activated carbon adsorption, the air can be prevented
In impurity participate in reaction, achieved the effect that improve product purity.
Preferably, in S3, reducibility gas is passed through from the bottom of the high temperature furnace.
Through the above technical solutions, the reducibility gas can be by Fe2O3It is reduced into Fe simple substance, has reached and has utilized ferrophosphorus
The effect of output high value iron ore.
Preferably, in S3, the reducibility gas is CO.
Through the above technical solutions, using the CO Fe can be being restored as reducibility gas2O3When, prevent
Only P2O5And SiO2With CO reduction reaction.
Preferably, in S4, the magnetic separator uses low-intensity (magnetic) separator, and the magnetic field strength of the weak magnetic magnetic separator is
6000~15000A/m.
Through the above technical solutions, using the low-intensity (magnetic) separator separate Fe simple substance, reached simplified lock out operation and
Improve the effect of high value iron ore yield.
Preferably, in S5, the inoranic membrane includes level-one inoranic membrane, second level inoranic membrane, the aperture of the level-one inoranic membrane
Greater than the aperture of the second level inoranic membrane；The mixture first passes through the level-one inoranic membrane when separation, then passes through the second level
Inoranic membrane.
Through the above technical solutions, the level-one inoranic membrane can initial gross separation bulky grain solid, the inorganic UF membrane of second level
Solid small particles, classification separation can prevent the blocking of inoranic membrane, achieve the effect that improve separative efficiency.
Preferably, in S5, after reaction solution and the solid separation for reaction being obtained by the inoranic membrane, be washed with water solid
Upper remaining reaction solution is collected cleaning solution and is added into the reaction solution, finally that the solid is dry, obtains SiO2Gu
Body.
Through the above technical solutions, washing the solid and the reaction solution being added in the cleaning solution, promotion is reached
The effect of phosphoric acid yield.
Preferably, the step of being recycled the method also includes thermal energy, one kind that thermal energy recycling includes the following steps or
Two kinds:
1) hot wind of the roaster discharge, dedusting are collected, and the hot wind after dedusting is used for the dry of solid described in S5
It is dry；
2) hot wind of the high temperature furnace discharge, dedusting are collected, and the hot wind after dedusting is used for the dry of solid described in S5
It is dry.
Through the above technical solutions, the hot wind collected from the roaster and high temperature furnace is used for drying, reach
Improve the effect of the heat energy recovery utilization rate in production.
The beneficial effects of the present invention are:
1. a kind of method for preparing phosphoric acid with ferrophosphorus of the invention, by the way that reducibility gas is added by Fe2O3It is reduced into high price
The Fe simple substance of value has achieved the effect that utilize ferrophosphorus output high value iron ore；Fe simple substance is separated in the way of magnetic separation, is reached
Improve the effect of the separative efficiency of Fe simple substance.
2. a kind of method for preparing phosphoric acid with ferrophosphorus of the invention, in P2O5It is reacted with cold water and generates metaphosphoric acid (HPO3) when,
Using SiO2 principle not soluble in water, SiO2 impurity is removed with inoranic membrane, has achieved the effect that promote product purity.
3. a kind of method for preparing phosphoric acid with ferrophosphorus of the invention carries out oxidation reaction or reduction reaction in the ferrophosphorus
When, it is passed through air or reducibility gas from the bottom of the roaster or high temperature furnace, reactant is blown afloat, having reached makes reaction more
Add sufficient effect.
4. a kind of method for preparing phosphoric acid with ferrophosphorus of the invention is added to the step of thermal energy recycles, has collected the roasting
The hot wind being discharged in furnace and high temperature furnace is burnt, and the hot wind after dedusting is used for the drying process in the method, has reached raising
The effect of heat energy recovery utilization rate.
Detailed description of the invention
Fig. 1 is a kind of process flow chart for the method that phosphoric acid is prepared with ferrophosphorus in the present invention.
Specific embodiment
Technical solution of the present invention is described in further detail with reference to the accompanying drawing, but protection scope of the present invention is not limited to
It is as described below.
Embodiment 1
In the present embodiment, the phosphorus content of ferrophosphorus used is 25.2%, and iron content 34.7% is a kind of to prepare phosphoric acid with ferrophosphorus
Method, comprising the following steps:
S1. pulverization process: 1000kg ferrophosphorus addition flour mill is ground, gets particulate material through 20 mesh screens；
S2. oxidizing roasting: particulate material is homogeneously added into roaster, and is passed through from the bottom of roaster through activated carbon adsorption
Air afterwards obtains mixed oxide after roasting 2h at 500 DEG C to particulate material, and mixed oxide includes Fe2O3、P2O5、SiO2；
At the same time, the hot wind of roaster discharge when collecting reaction, and to its dedusting, it may be assumed that
2FeP+4O2→Fe2O3+P2O5；
4Fe2P+11O2→4Fe2O3+2P2O5；
Si+O2→SiO2；
S3. heating reduction: being added high temperature furnace for mixed oxide, be passed through CO from the bottom of high temperature furnace, continues at 750 DEG C
Reduzate is obtained after reaction 1h, reduzate includes P2O5、Fe、SiO2；At the same time, high temperature furnace discharge when collecting reaction
Hot wind, and to its dedusting, it may be assumed that
Fe2O3+3CO→2Fe+3CO2；
S4. magnetic separation separates: the low-intensity (magnetic) separator that magnetic field strength is 12000A/m is added in reduzate after cooling, is passed through
Fe is isolated in magnetic separation, obtains P2O5And SiO2Mixture；
S5. it is separated by solid-liquid separation: by P2O5And SiO2Mixture be added in 10 DEG C of cold water and reacted to obtain metaphosphoric acid, and lead to
Cross reaction solution and unreacted SiO that level-one inoranic membrane and second level inoranic membrane obtain reaction2Solid separation, is washed with water solid
Upper remaining reaction solution is collected cleaning solution and is added into reaction solution, finally using the hot wind after dedusting to SiO2Solid into
Row drying；Level-one inoranic membrane and second level inoranic membrane are all made of ceramic inorganic film, and the aperture of level-one inoranic membrane is 10 μm, and second level is inorganic
The aperture of film is 1 μm, it may be assumed that
P2O5+H2O (cold water) → 2HPO3, because of SiO2It is dissolved in hot phosphoric acid but does not dissolve in metaphosphoric acid, therefore can Schilling P2O5With
Cold water reaction generates metaphosphoric acid, to reach separation SiO2Effect.
S6. it prepares phosphoric acid: reaction solution being passed through 75 DEG C of hot water, reaction obtains 100L phosphoric acid solution, it may be assumed that
HPO3+H2O (hot water) → H3PO4。
Test effect
In order to verify it is of the invention it is a kind of with ferrophosphorus prepare the method for phosphoric acid made from iron simple substance and phosphoric acid yield, carry out
Following operation:
1) 1L phosphoric acid solution will be randomly selected, sufficiently drying removes moisture and obtains liquid phosphoric acid at 110 DEG C, is cooled to room
Temperature
It is weighed afterwards to it and carries out purity detecting；
2) weight of gained Fe simple substance is weighed.
It is obtained by above-mentioned steps, the weight of gained phosphoric acid is 7.794kg in step 1), and purity 99.52% is calculated and known
The yield of phosphoric acid is 97.79%；The weight of Fe simple substance is 333.81kg in step 2), and the rate of recovery of iron is known to calculating
96.20%.
Embodiment 2
In the present embodiment, the phosphorus content of ferrophosphorus used is 21.7%, and iron content 37.3% is a kind of to prepare phosphoric acid with ferrophosphorus
Method, comprising the following steps:
S1. pulverization process: 1000kg ferrophosphorus addition flour mill is ground, gets particulate material through 20 mesh screens；
S2. oxidizing roasting: particulate material is homogeneously added into roaster, and is passed through from the bottom of roaster through activated carbon adsorption
Air afterwards obtains mixed oxide after roasting 2h at 500 DEG C to particulate material, and mixed oxide includes Fe2O3、P2O5、SiO2；
At the same time, the hot wind of roaster discharge when collecting reaction, and to its dedusting, it may be assumed that
2FeP+4O2→Fe2O3+P2O5；
4Fe2P+11O2→4Fe2O3+2P2O5；
Si+O2→SiO2；
S3. heating reduction: being added high temperature furnace for mixed oxide, be passed through CO from the bottom of high temperature furnace, continues at 800 DEG C
Reduzate is obtained after reaction 1h, reduzate includes P2O5、Fe、SiO2；At the same time, high temperature furnace discharge when collecting reaction
Hot wind, and to its dedusting, it may be assumed that
Fe2O3+3CO→2Fe+3CO2；
S4. magnetic separation separates: the low-intensity (magnetic) separator that magnetic field strength is 15000A/m is added in reduzate after cooling, is passed through
Fe is isolated in magnetic separation, obtains P2O5And SiO2Mixture；
S5. it is separated by solid-liquid separation: by P2O5And SiO2Mixture be added in 10 DEG C of cold water and reacted to obtain metaphosphoric acid, and lead to
Cross reaction solution and unreacted SiO that level-one inoranic membrane and second level inoranic membrane obtain reaction2Solid separation, is washed with water solid
Upper remaining reaction solution is collected cleaning solution and is added into reaction solution, finally using the hot wind after dedusting to SiO2Solid into
Row drying；Level-one inoranic membrane and second level inoranic membrane are all made of ceramic inorganic film, and the aperture of level-one inoranic membrane is 10 μm, and second level is inorganic
The aperture of film is 1 μm, it may be assumed that
P2O5+H2O (cold water) → 2HPO3, because of SiO2It is dissolved in hot phosphoric acid but does not dissolve in metaphosphoric acid, therefore can Schilling P2O5With
Cold water reaction generates metaphosphoric acid, to reach separation SiO2Effect.
S6. it prepares phosphoric acid: reaction solution being passed through 75 DEG C of hot water, reaction obtains 100L phosphoric acid solution, it may be assumed that
HPO3+H2O (hot water) → H3PO4。
Test effect
In order to verify it is of the invention it is a kind of with ferrophosphorus prepare the method for phosphoric acid made from iron simple substance and phosphoric acid yield, carry out
Following operation:
1) 1L phosphoric acid solution will be randomly selected, sufficiently drying removes moisture and obtains liquid phosphoric acid at 110 DEG C, is cooled to room
Temperature
It is weighed afterwards to it and carries out purity detecting；
2) weight of gained Fe simple substance is weighed.
It is obtained by above-mentioned steps, the weight of gained phosphoric acid is 6.72kg in step 1), and purity 99.34% is calculated and known
The yield of phosphoric acid is 97.96%；The weight of Fe simple substance is 362.56kg in step 2), and the rate of recovery of iron is known to calculating
97.20%.By embodiment 1 with embodiment 2 it is found that tune can be passed through for for the different ferrophosphorus of P elements, iron content
The magnetic field strength of whole reduction temperature and magnetic separator guarantees the gained yield of phosphoric acid, purity and the rate of recovery of iron.
In conclusion a kind of method for preparing phosphoric acid with ferrophosphorus of the invention, can not only be made the iron ore of high yield from
And improve the rate of recovery of iron, moreover it is possible to improve the yield and purity of gained phosphoric acid.
The above is only a preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form should not be regarded as an exclusion of other examples, and can be used for other combinations, modifications, and environments, and can be at this
In the text contemplated scope, modifications can be made through the above teachings or related fields of technology or knowledge.And those skilled in the art institute into
Capable modifications and changes do not depart from the spirit and scope of the present invention, then all should be in the protection scope of appended claims of the present invention
It is interior.
Claims (9)
1. a kind of method for preparing phosphoric acid with ferrophosphorus, it is characterised in that: the described method comprises the following steps:
S1. pulverization process: ferrophosphorus addition flour mill is ground, and sieves and obtains particulate material；
S2. oxidizing roasting: the particulate material is homogeneously added into roaster, and is passed through air into the roaster, to described
Particulate material obtains mixed oxide after being roasted；
S3. heating reduction: high temperature furnace is added in the mixed oxide, and is passed through reduction to the high temperature furnace under the high temperature conditions
Property gas, obtains reduzate after reaction；
S4. magnetic separation separates: magnetic separator will be added after reduzate cooling, isolates Fe by magnetic separation, obtain mixture；
S5. it is separated by solid-liquid separation: the reaction solution that the mixture is added in cold water and is reacted, and is obtained reaction by inoranic membrane
It is separated with solid, it is finally that the solid is dry；
S6. it prepares phosphoric acid: the reaction solution being passed through hot water, end reaction obtains phosphoric acid solution.
2. a kind of method for preparing phosphoric acid with ferrophosphorus according to claim 1, it is characterised in that: in S1, the ferrophosphorus exists
After grinding, get the particulate material through 20 mesh screens.
3. a kind of method for preparing phosphoric acid with ferrophosphorus according to claim 1, it is characterised in that: in S2, from the roasting
The bottom of furnace is passed through air, and the air carries out adsorption treatment through active carbon and obtains.
4. a kind of method for preparing phosphoric acid with ferrophosphorus according to claim 1, it is characterised in that: in S3, from the high temperature
The bottom of furnace is passed through reducibility gas.
5. a kind of method for preparing phosphoric acid with ferrophosphorus according to claim 1, it is characterised in that: in S3, the reproducibility
Gas is CO.
6. a kind of method for preparing phosphoric acid with ferrophosphorus according to claim 1, it is characterised in that: in S4, the magnetic separator
Using low-intensity (magnetic) separator, the magnetic field strength of the weak magnetic magnetic separator is 6000~15000A/m.
7. a kind of method for preparing phosphoric acid with ferrophosphorus according to claim 1, it is characterised in that: in S5, the inoranic membrane
Including level-one inoranic membrane, second level inoranic membrane, the aperture of the level-one inoranic membrane is greater than the aperture of the second level inoranic membrane；When separation
The mixture first passes through the level-one inoranic membrane, then passes through the second level inoranic membrane.
8. a kind of method for preparing phosphoric acid with ferrophosphorus according to claim 1, it is characterised in that: in S5, pass through the nothing
After reaction solution and the solid separation that machine film obtains reaction, remaining reaction solution on solid is washed with water, collection cleaning solution simultaneously will
It is added in the reaction solution, finally that the solid is dry.
9. a kind of method for preparing phosphoric acid with ferrophosphorus according to claim 1, it is characterised in that: the method also includes heat
Recoverable step, the thermal energy recycle the one or two included the following steps:
1) hot wind of roaster discharge is collected, dedusting, and the hot wind after dedusting is used for the drying of solid described in S5；
2) hot wind of high temperature furnace discharge is collected, dedusting, and the hot wind after dedusting is used for the drying of solid described in S5.
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| WO2022267190A1 (en) * | 2021-06-23 | 2022-12-29 | 中钢设备有限公司 | Method for treating high-phosphorus oolitic iron ores |
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