CN108190964A - A kind of method that ferrate solution is prepared using pyrite cinder - Google Patents
A kind of method that ferrate solution is prepared using pyrite cinder Download PDFInfo
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- CN108190964A CN108190964A CN201810269191.XA CN201810269191A CN108190964A CN 108190964 A CN108190964 A CN 108190964A CN 201810269191 A CN201810269191 A CN 201810269191A CN 108190964 A CN108190964 A CN 108190964A
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- pyrite cinder
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0081—Mixed oxides or hydroxides containing iron in unusual valence state [IV, V, VI]
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Abstract
The invention discloses a kind of methods that ferrate solution is prepared using pyrite cinder.Pyrite cinder is crushed first, obtains pyrite cinder powder；Sodium hydroxide solution is weighed, pyrite cinder powder is added in and stirs evenly, obtain mixed liquor；By mixed liquor, normal heating, heating postcooling carry out separation of solid and liquid under microwave condition, and gained solid phase is dried, and obtains solid phase fine powder；Solid phase fine powder is added in reactor, strong base solution is added in and NaClO solution stirs evenly；Then normal heating under microwave condition, through centrifuging or being obtained by filtration atropurpureus ferrate solution after heating.The method of the present invention is easy to operate, quick, energy saving, and the concentration of prepared ferrate solution is not less than the ferrate concentration prepared in the prior art using molysite or iron oxide as source of iron, has the value of popularization and application.
Description
First, technical field：
The present invention relates to a kind of preparation methods of ferrate solution, are prepared more particularly to a kind of using pyrite cinder
The method of ferrate solution.
2nd, background technology：
Pyrite cinder is the waste residue that roasting pyrite generates when producing sulfuric acid, and main component is Fe2O3And SiO2, this
Also contain CaO, MgO, AI outside2O3, the non-ferrous metals such as S and a small amount of copper-lead zinc gold and silver.The troilite place of production is different, slag ingredient
And content is also variant, such as：Part pyrite cinder is containing Fe (with Fe2O3Represent) it is 50~80%, SiO210~20%, containing S
Be more than 3% (yellow Changchun, from the research of Recovery of Iron From Pyrite Cinder fine powder, chemical-academic dissertation, 2013).Sulphur iron
Ore deposit slag is mainly used as construction material, iron system chemical products, molysite, iron pigment, magnetic iron oxide, water purification agent are produced in ironmaking,
Micro useful element of association etc. in also extractable raw ore.
Preparing water-purifying material using pyrite cinder also has relevant report.It is prepared in the prior art using pyrite cinder net
Water material generally using hydrochloric acid method and sulfuric acid process (such as：Poly-ferric chloride aluminium water purifying agent is prepared using pyrite slag；Pyrite
Slag recycling-production new series high efficiency composition Polyferric Sulfate water purification agent PISC；The technique of sulfuric acid plant's slag production bodied ferric sulfate is ground
Study carefully；A kind of preparation of new and effective water purification agent-polymeric aluminium ferrum silicate and property).
Ferrate typically refers to potassium ferrate, Na2Fe04, and wherein iron is sexavalence, has very strong oxidisability, is one
Kind integrates the excellent water purification agent of the multiple functions such as oxidation, sterilization, deodorization, flocculation, and in the selectivity of many organic matters
It has broad application prospects in terms of oxidation and environment protection type battery material.
At present, the existing method for preparing ferrate is wet chemical, it is to be sent out using chlorine and strong alkali solution as raw material
Raw reaction, makes hypochlorite oxidation's molysite of generation so as to obtain ferrate solution.It is used in the research of wet chemical
Source of iron be generally FeCl3、Fe(NO3)3, bodied ferric sulfate, FeCO3And Fe2O3Deng.
According to pertinent literature, being prepared for ferrate using pyrite cinder, (high honor etc., pyrite cinder prepare high ferro
Sour potassium and potassium ferrate solution stability, Wuhan Engineering Univ's journal, 11 phases in 2011), the preparation method be using acidolysis-
Water seaoning first prepares ferric sulfate, then ferrate is prepared by the use of ferrum sulfuricum oxydatum solutum as source of iron.
The present inventor had done correlative study for red mud, using red mud as source of iron, using its strong basicity environment, produced to obtain
Ferrate solution, it is determined that preparation condition and method for red mud (prepare the side of ferrate solution using red mud
Method).
Microwave heating be it is a kind of absorb microwave energy by object and convert thereof into thermal energy, make adding for itself whole heating simultaneously
Hot mode is different from other conventional heating modes completely.Traditional heating mode is to make heat according to heat transfer, convection current and radiation theory
Amount reaches material heat from outside, and heat always from outward appearance to inner essence transmits and carries out heated material, and temperature is inevitably present in material
Gradient is spent, therefore the material heated is uneven, material is caused hot-spot occur, microwave heating technique and traditional heating mode are not
Together, it is moved by heated object internal dipole molecule high-frequency reciprocating, is generated " interior frictional heat " and is made heating object material temperature degree
Raising, is not necessary to any heat transfer process, and with regard to material inside and outside portion can be made to heat while heat up simultaneously, heating speed is fast and uniform, only
Need the part or 1/tens of the energy consumption of traditional heating mode, so that it may reach heating purpose.
Chemical reaction is accelerated to have relevant report using microwave heating technique.Such as：1st, microwave heating technique is applied to multiple
Close the research of polyaluminium chloride silicic acid production；2nd, poly aluminum chloride compound silicic acid is produced with microwave heating technique.
3rd, invention content：
The technical problem to be solved by the present invention is to：According to the technology of preparing and pyrite cinder of existing ferrate solution
Utilization power, the present invention provides a kind of method that ferrate solution is prepared using pyrite cinder.The method of the present invention uses
Pyrite cinder is source of iron, and ferrate solution is prepared in alkaline process under the conditions of microwave radiation.
To solve the above-mentioned problems, the technical solution adopted by the present invention is that：
The present invention provides a kind of method that ferrate solution is prepared using pyrite cinder, the preparation method include with
Lower step：
A, pyrite cinder is crushed first, smashes it through 200 mesh sieve, obtain pyrite cinder powder；
B, sodium hydroxide solution is weighed, step a gained pyrite cinder powder is then added in and stirs evenly, control gained is mixed
The solid-to-liquid ratio for closing liquid is 1:3~6；
C, by mixed liquor obtained by step b, normal heating, heating time are 2~8min under microwave condition, are carried out after heating
Cooling, carries out separation of solid and liquid, gained solid phase is dried, and solid phase fine powder is obtained after drying after being cooled to room temperature；
D, solid phase fine powder obtained by step c is added in reactor, then adds in strong base solution and NaClO solution, stirring
Uniformly；Then normal heating 1~3 minute under microwave condition, it is molten through centrifuging or being obtained by filtration atropurpureus ferrate after heating
Liquid.
According to the above-mentioned method that ferrate solution is prepared using pyrite cinder, sodium hydroxide is molten described in step b
The mass percentage concentration of liquid is 35~45%.
According to the above-mentioned method that ferrate solution is prepared using pyrite cinder, normal pressure under microwave condition in step c
Frequency is 900MHz~3000MHz during heating.
According to the above-mentioned method that ferrate solution is prepared using pyrite cinder, when solid phase is dried in step c
Drying temperature is 240~260 DEG C, and drying time is 20~30min.
According to the above-mentioned method that ferrate solution is prepared using pyrite cinder, obtained after separation of solid and liquid in step c
Liquid phase recycle.
According to the above-mentioned method that ferrate solution is prepared using pyrite cinder, highly basic described in step d is NaOH
Or KOH.
According to the above-mentioned method that ferrate solution is prepared using pyrite cinder, strong base solution described in step d
Mass percentage concentration is 25~35%；The content of effective chlorine is 6~11% in the NaClO solution.
According to the above-mentioned method that ferrate solution is prepared using pyrite cinder, solid phase fine powder and highly basic in step d
The weight ratio of solution therebetween is 1：3.5~5.5, the weight ratio of solid phase fine powder and NaClO solution addition therebetween
Example is 1：2.5~4.5.
According to the above-mentioned method that ferrate solution is prepared using pyrite cinder, normal pressure under microwave condition in step d
Frequency during heating is 900MHz~3000MHz.
The reaction principle of preparation method of the present invention is：First under microwave heating condition, (arteries and veins is destroyed using highly basic activation slag
Stone package bonding --- the main component of gangue is aluminium oxide and silica), wherein sulphur is made to be converted into the salt of dissolving and divide
From, and partial oxidation iron is made to be converted to ferrite NaFeO2, and then it is oxidized to ferric iron under alkalinity, microwave heating condition
Sexavalence molysite.Its correlated response formula is as follows：
The positive beneficial effect of the present invention：
1st, the present invention is raw material under the conditions of microwave radiation using pyrite cinder, and wet oxidation prepares ferrate solution,
A kind of new method is provided for pyrite cinder comprehensive utilization.
2nd, the present invention mutually wraps up for iron ore composition granule and impurity in pyrite cinder and gangue mineral particle, is mutually glutinous
It is lived in knot, slag containing a certain amount of sulphur impurity etc. to the preparation of ferrate and preservation rough sledding using microwave heating alkalinity
Change simultaneously sulphur removal, achieve ideal effect.
3rd, the method for the present invention is easy to operate, quick, energy saving, and the concentration of prepared ferrate solution is not less than existing skill
With the ferrate concentration that molysite (or iron oxide) is source of iron preparation in art, have the value of popularization and application.
4th, contained a small amount of copper-lead zinc gold and silver is enriched in residue more than the method for the present invention preparation institute in pyrite cinder,
The further leaching for being conducive to residue utilizes.
4th, specific embodiment：
The present invention is further explained with reference to embodiments, but is not intended to limit the range of technical solution of the present invention protection.
Embodiment 1：
The method that the present invention prepares ferrate solution using pyrite cinder, the detailed step of the preparation method are as follows：
A, pyrite cinder is crushed first, smashes it through 200 mesh sieve, obtain pyrite cinder powder；
B, it weighs the sodium hydroxide solution 120mL that mass percentage concentration is 40% to be placed in reaction vessel, then adds in step
Pyrite cinder powder 30g obtained by rapid a is stirred evenly；
C, by the normal heating under microwave condition of mixed liquor obtained by step b, frequency is 2450MHz during heating, heating time
It for 2min, is cooled down after heating, separation of solid and liquid is carried out after being cooled to room temperature, gained solid phase is dried (drying temperature 260
DEG C, drying time 20min), solid phase fine powder is obtained after drying (gained liquid phase recycles after separation)；
D, solid phase fine powder 6g obtained by step c is added in reactor, then adds in the hydrogen that mass percentage concentration is 32%
Sodium hydroxide solution 20mL and NaClO solution 10mL (available chlorine content 11%), stirs evenly；Then normal pressure under microwave condition
Heating 1 minute (frequency is 2450MHz during electromagenetic wave radiation), the atropurpureus that centrifuged concentration is about 4.5g/L after heating is high
Ferrous acid salting liquid.
Embodiment 2：
The method that the present invention prepares ferrate solution using pyrite cinder, the detailed step of the preparation method are as follows：
A, pyrite cinder is crushed first, smashes it through 200 mesh sieve, obtain pyrite cinder powder；
B, it weighs the sodium hydroxide solution 120mL that mass percentage concentration is 40% to be placed in reaction vessel, then adds in step
Pyrite cinder powder 30g obtained by rapid a is stirred evenly；
C, by the normal heating under microwave condition of mixed liquor obtained by step b, frequency is 2450MHz during heating, heating time
It for 2min, is cooled down after heating, separation of solid and liquid is carried out after being cooled to room temperature, gained solid phase is dried (drying temperature 260
DEG C, drying time 20min), solid phase fine powder is obtained after drying (gained liquid phase recycles after separation)；
D, solid phase fine powder 6g obtained by step c is added in reactor, then adds in the hydrogen that mass percentage concentration is 32%
Sodium hydroxide solution 20mL and NaClO solution 15mL (available chlorine content 11%), stirs evenly；Then normal pressure under microwave condition
Heating 1 minute (frequency is 2450MHz during electromagenetic wave radiation), it is high through the atropurpureus that concentration is about 4.8g/L is obtained by filtration after heating
Ferrous acid salting liquid.
Embodiment 3：
The method that the present invention prepares ferrate solution using pyrite cinder, the detailed step of the preparation method are as follows：
A, pyrite cinder is crushed first, smashes it through 200 mesh sieve, obtain pyrite cinder powder；
B, it weighs the sodium hydroxide solution 120mL that mass percentage concentration is 40% to be placed in reaction vessel, then adds in step
Pyrite cinder powder 30g obtained by rapid a is stirred evenly；
C, by the normal heating under microwave condition of mixed liquor obtained by step b, frequency is 2450MHz during heating, heating time
It for 2min, is cooled down after heating, separation of solid and liquid is carried out after being cooled to room temperature, gained solid phase is dried (drying temperature 250
DEG C, drying time 30min), solid phase fine powder is obtained after drying (gained liquid phase recycles after separation)；
D, solid phase fine powder 6g obtained by step c is added in reactor, then adds in the hydrogen that mass percentage concentration is 32%
Sodium hydroxide solution 20mL and NaClO solution 10mL (available chlorine content 8%), stirs evenly；Then normal pressure under microwave condition
Heating 1 minute (frequency is 2450MHz during electromagenetic wave radiation), the atropurpureus that centrifuged concentration is about 3.2g/L after heating is high
Ferrous acid salting liquid.
Embodiment 4：
The method that the present invention prepares ferrate solution using pyrite cinder, the detailed step of the preparation method are as follows：
A, pyrite cinder is crushed first, smashes it through 200 mesh sieve, obtain pyrite cinder powder；
B, it weighs the sodium hydroxide solution 120mL that mass percentage concentration is 40% to be placed in reaction vessel, then adds in step
Pyrite cinder powder 30g obtained by rapid a is stirred evenly；
C, by the normal heating under microwave condition of mixed liquor obtained by step b, frequency is 2450MHz during heating, heating time
It for 2min, is cooled down after heating, separation of solid and liquid is carried out after being cooled to room temperature, gained solid phase is dried (drying temperature 240
DEG C, drying time 30min), solid phase fine powder is obtained after drying (gained liquid phase recycles after separation)；
D, solid phase fine powder 6g obtained by step c is added in reactor, then adds in the hydrogen that mass percentage concentration is 25%
Sodium hydroxide solution 20mL and NaClO solution 10mL (available chlorine content 8%), stirs evenly；Then normal pressure under microwave condition
Heating 1 minute (frequency is 2450MHz during electromagenetic wave radiation), the atropurpureus that centrifuged concentration is about 1.8g/L after heating is high
Ferrous acid salting liquid.
Embodiment 5：
The method that the present invention prepares ferrate solution using pyrite cinder, the detailed step of the preparation method are as follows：
A, pyrite cinder is crushed first, smashes it through 200 mesh sieve, obtain pyrite cinder powder；
B, it weighs the sodium hydroxide solution 120mL that mass percentage concentration is 40% to be placed in reaction vessel, then adds in step
Pyrite cinder powder 30g obtained by rapid a is stirred evenly；
C, by the normal heating under microwave condition of mixed liquor obtained by step b, frequency is 2450MHz during heating, heating time
It for 2min, is cooled down after heating, separation of solid and liquid is carried out after being cooled to room temperature, gained solid phase is dried (drying temperature 260
DEG C, drying time 20min), solid phase fine powder is obtained after drying (gained liquid phase recycles after separation)；
D, solid phase fine powder 6g obtained by step c is added in reactor, then adds in the hydrogen that mass percentage concentration is 35%
Sodium hydroxide solution 20mL and NaClO solution 15mL (available chlorine content 11%), stirs evenly；Then normal pressure under microwave condition
Heating 1 minute (frequency is 2450MHz during electromagenetic wave radiation), it is high through the atropurpureus that concentration is about 5.2g/L is obtained by filtration after heating
Ferrous acid salting liquid.
Embodiment 6：
The method that the present invention prepares ferrate solution using pyrite cinder, the detailed step of the preparation method are as follows：
A, pyrite cinder is crushed first, smashes it through 200 mesh sieve, obtain pyrite cinder powder；
B, it weighs the sodium hydroxide solution 120mL that mass percentage concentration is 40% to be placed in reaction vessel, then adds in step
Pyrite cinder powder 30g obtained by rapid a is stirred evenly；
C, by the normal heating under microwave condition of mixed liquor obtained by step b, frequency is 2450MHz during heating, heating time
It for 2min, is cooled down after heating, separation of solid and liquid is carried out after being cooled to room temperature, gained solid phase is dried (drying temperature 250
DEG C, drying time 20min), solid phase fine powder is obtained after drying (gained liquid phase recycles after separation)；
D, solid phase fine powder 12g obtained by step c is added in reactor, then adds in the hydrogen that mass percentage concentration is 35%
Sodium hydroxide solution 30mL and NaClO solution 20mL (available chlorine content 11%), stirs evenly；Then normal pressure under microwave condition
Heating 1 minute (frequency is 2450MHz during electromagenetic wave radiation), the atropurpureus that centrifuged concentration is about 5.6g/L after heating is high
Ferrous acid salting liquid.
Embodiment 7：
The method that the present invention prepares ferrate solution using pyrite cinder, the detailed step of the preparation method are as follows：
A, pyrite cinder is crushed first, smashes it through 200 mesh sieve, obtain pyrite cinder powder；
B, it weighs the sodium hydroxide solution 120mL that mass percentage concentration is 35% to be placed in reaction vessel, then adds in step
Pyrite cinder powder 30g obtained by rapid a is stirred evenly；
C, by the normal heating under microwave condition of mixed liquor obtained by step b, frequency is 2450MHz during heating, heating time
It for 4min, is cooled down after heating, separation of solid and liquid is carried out after being cooled to room temperature, gained solid phase is dried (drying temperature 240
DEG C, drying time 30min), solid phase fine powder is obtained after drying (gained liquid phase recycles after separation)；
D, solid phase fine powder 6g obtained by step c is added in reactor, then adds in the hydrogen that mass percentage concentration is 32%
Sodium hydroxide solution 20mL and NaClO solution 10mL (available chlorine content 11%), stirs evenly；Then normal pressure under microwave condition
Heating 1 minute (frequency is 2450MHz during electromagenetic wave radiation), the atropurpureus that centrifuged concentration is about 4.6g/L after heating is high
Ferrous acid salting liquid.
Embodiment 8：
The method that the present invention prepares ferrate solution using pyrite cinder, the detailed step of the preparation method are as follows：
A, pyrite cinder is crushed first, smashes it through 200 mesh sieve, obtain pyrite cinder powder；
B, it weighs the sodium hydroxide solution 120mL that mass percentage concentration is 35% to be placed in reaction vessel, then adds in step
Pyrite cinder powder 30g obtained by rapid a is stirred evenly；
C, by the normal heating under microwave condition of mixed liquor obtained by step b, frequency is 2450MHz during heating, heating time
It for 2min, is cooled down after heating, separation of solid and liquid is carried out after being cooled to room temperature, gained solid phase is dried (drying temperature 260
DEG C, drying time 20min), solid phase fine powder is obtained after drying (gained liquid phase recycles after separation)；
D, solid phase fine powder 6g obtained by step c is added in reactor, then adds in the hydrogen that mass percentage concentration is 32%
Sodium hydroxide solution 20mL and NaClO solution 10mL (available chlorine content 11%), stirs evenly；Then normal pressure under microwave condition
Heating 1 minute (frequency is 2450MHz during electromagenetic wave radiation), it is high through the atropurpureus that concentration is about 3.8g/L is obtained by filtration after heating
Ferrous acid salting liquid.
Embodiment 9：
The method that the present invention prepares ferrate solution using pyrite cinder, the detailed step of the preparation method are as follows：
A, pyrite cinder is crushed first, smashes it through 200 mesh sieve, obtain pyrite cinder powder；
B, it weighs the sodium hydroxide solution 120mL that mass percentage concentration is 45% to be placed in reaction vessel, then adds in step
Pyrite cinder powder 30g obtained by rapid a is stirred evenly；
C, by the normal heating under microwave condition of mixed liquor obtained by step b, frequency is 2450MHz during heating, heating time
It for 4min, is cooled down after heating, separation of solid and liquid is carried out after being cooled to room temperature, gained solid phase is dried (drying temperature 250
DEG C, drying time 20min), solid phase fine powder is obtained after drying (gained liquid phase recycles after separation)；
D, solid phase fine powder 6g obtained by step c is added in reactor, then adds in the hydrogen that mass percentage concentration is 32%
Sodium hydroxide solution 20mL and NaClO solution 15mL (available chlorine content 11%), stirs evenly；Then normal pressure under microwave condition
Heating 1 minute (frequency is 2450MHz during electromagenetic wave radiation), it is high through the atropurpureus that concentration is about 6.1g/L is obtained by filtration after heating
Ferrous acid salting liquid.
Embodiment 10：(pyrite cinder is unprocessed)
The method that ferrate solution is prepared using pyrite cinder, the detailed step of the preparation method are as follows：
It directly weighs pyrite cinder fine powder (200 mesh are crossed in fine grinding) 6g to be added in reactor, adds in mass percentage concentration
For 32% sodium hydroxide solution 20ml, the NaClO solution 15ml of available chlorine content 11% are added, are stirred evenly；
Normal heating 1min under the microwave condition of 2450MHz, the ferrate solution that centrifuged concentration is about 0.8g/L.
Claims (9)
- A kind of 1. method that ferrate solution is prepared using pyrite cinder, which is characterized in that the preparation method include with Lower step：A, pyrite cinder is crushed first, smashes it through 200 mesh sieve, obtain pyrite cinder powder；B, sodium hydroxide solution is weighed, step a gained pyrite cinder powder is then added in and stirs evenly, control gained mixed liquor Solid-to-liquid ratio be 1:3~6；C, by mixed liquor obtained by step b, normal heating, heating time are 2~8min under microwave condition, are cooled down after heating, Separation of solid and liquid is carried out after being cooled to room temperature, gained solid phase is dried, and solid phase fine powder is obtained after drying；D, solid phase fine powder obtained by step c is added in reactor, then adds in strong base solution and NaClO solution, stir evenly； Then normal heating 1~3 minute under microwave condition, through centrifuging or being obtained by filtration atropurpureus ferrate solution after heating.
- 2. the method according to claim 1 that ferrate solution is prepared using pyrite cinder, it is characterised in that：Step The mass percentage concentration of sodium hydroxide solution described in b is 35~45%.
- 3. the method according to claim 1 that ferrate solution is prepared using pyrite cinder, it is characterised in that：Step Frequency is 900MHz~3000MHz during normal heating under microwave condition in c.
- 4. the method according to claim 1 that ferrate solution is prepared using pyrite cinder, it is characterised in that：Step Drying temperature is 240~260 DEG C when solid phase is dried in c, and drying time is 20~30min.
- 5. the method according to claim 1 that ferrate solution is prepared using pyrite cinder, it is characterised in that：Step The liquid phase obtained after separation of solid and liquid in c recycles.
- 6. the method according to claim 1 that ferrate solution is prepared using pyrite cinder, it is characterised in that：Step Highly basic described in d is NaOH or KOH.
- 7. the method according to claim 1 that ferrate solution is prepared using pyrite cinder, it is characterised in that：Step The mass percentage concentration of strong base solution described in d is 25~35%；The content of effective chlorine is 6~11% in the NaClO solution.
- 8. the method according to claim 1 that ferrate solution is prepared using pyrite cinder, it is characterised in that：Step Solid phase fine powder and the weight ratio of strong base solution therebetween are 1 in d：3.5~5.5, both solid phase fine powder and NaClO solution it Between addition weight ratio be 1：2.5~4.5.
- 9. the method according to claim 1 that ferrate solution is prepared using pyrite cinder, it is characterised in that：Step Frequency in d under microwave condition during normal heating is 900MHz~3000MHz.
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| CN109133190A (en) * | 2018-08-03 | 2019-01-04 | 武钢资源集团有限公司 | The processing method of magnetic iron ore |
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| CN109133190A (en) * | 2018-08-03 | 2019-01-04 | 武钢资源集团有限公司 | The processing method of magnetic iron ore |
| CN109133190B (en) * | 2018-08-03 | 2020-12-29 | 武钢资源集团大冶铁矿有限公司 | Processing method of pyrrhotite |
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