CN108328594A - The improved method for producing battery-grade iron phosphate using pyrite cinder - Google Patents
The improved method for producing battery-grade iron phosphate using pyrite cinder Download PDFInfo
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- CN108328594A CN108328594A CN201810268426.3A CN201810268426A CN108328594A CN 108328594 A CN108328594 A CN 108328594A CN 201810268426 A CN201810268426 A CN 201810268426A CN 108328594 A CN108328594 A CN 108328594A
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- Prior art keywords
- water
- hydrochloric acid
- once washing
- washing water
- evaporative condenser
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Classifications
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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
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
-
- 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
Abstract
A kind of improved method for producing battery-grade iron phosphate using pyrite cinder, includes the following steps：The washings containing hydrochloric acid are sent into electrolytic cell during ferric phosphate is produced, and obtain chlorine；Chlorine is passed through in yellow phosphorus water, is absorbed by yellow phosphorus water, the mixture of phosphoric acid and hydrochloric acid is obtained；The mixture of phosphoric acid and hydrochloric acid is reacted with pyrite cinder, obtains crude product ferric phosphate；In the present invention, after hydrochloric acid in once washing water is by cell reaction, chlorion generates chlorine, chlorine reacts the mixture for generating phosphoric acid and hydrochloric acid with yellow phosphorus water, the mixture of phosphoric acid and hydrochloric acid generates crude product ferric phosphate with pyrite cinder again, to which pyrite cinder be turned waste into wealth, and avoid the exhaust emission environment of chlorion, it is cationic then combined with hydroxyl to be formed precipitation discharge, avoid being continuously increased for cation concn, once washing water by electrolysis processing is recycled, realize the zero-emission of washings, hydrochloric acid in technical process is recycled simultaneously, realize the zero-emission of chlorion.
Description
Technical field
The present invention relates to ferric phosphate preparing technical fields, more particularly to a kind of to produce battery-grade iron phosphate using pyrite cinder
Improved method.
Background technology
Ferric phosphate can be used as preparing the source of iron of lithium ion battery anode material lithium iron phosphate, but its cost is higher, only phosphoric acid
Iron just accounts for nearly the half of cost of material, it is necessary to the cost of ferric phosphate be greatly lowered, meet the market demand with high performance-price ratio.Sulphur
Sour slag is that pyrite burning extracts the residue being discharged after sulphur.Iron is in slag mainly using ingredient.Currently, pyrite cinder
Comprehensively utilize it is unsatisfactory, it is most of to be handled using landfill other than small part is used as ironmaking and construction material, cause resource
Waste, environment pollution.And using pyrite cinder as the raw material for preparing ferric phosphate, it has no and has been reported that.Ferric phosphate production process
In need to wash it, the hydrochloric acid containing low concentration and some chlorates in washings, if do not handled, washings cannot follow
Ring uses, since hydrochloric acid, chlorination salinity are low, it is difficult to using conventional method processing, such as use neutralization displacement method, that is, use big
It measures lime and neutralization reaction occurs with waste hydrochloric acid.Hydrochloric acid in waste water is handled using this method, processing cost is high, and recovery value is very
It is low, a large amount of waste water are also will produce, environment is polluted, direct emission not only results in waste of resources, and certain shadow can be also caused to environment
It rings, especially chlorion is especially prominent to the pollution of environment.
Invention content
In view of this, against the above deficiency, it is necessary to propose that a kind of energy prepare ferric phosphate using pyrite cinder, and can be effective
The hydrochloric acid and washings in ferric phosphate washings are recycled, zero release of pollutant, the especially profit of chlorion zero-emission are met
The improved method for producing battery-grade iron phosphate with pyrite cinder.
A kind of improved method for producing battery-grade iron phosphate using pyrite cinder, includes the following steps：Step 1：By sulfuric acid
Slag and the second phosphatase reaction, to obtain crude product ferric phosphate, wherein the mass percentage concentration of the second phosphoric acid is 20~80%；
Step 2：By the second dissolving with hydrochloric acid of crude product ferric phosphate, and clear liquid and filter residue is obtained by filtration, wherein the quality of the second hydrochloric acid
Percentage concentration is 20~30%；
Step 3：The clear liquid is distilled, to obtain gaseous hydrogen chloride and ferric phosphate crystallized product；
Step 4：Gaseous hydrogen chloride is condensed, the 4th hydrochloric acid is obtained, the 4th hydrochloric acid rectifying is obtained into the second hydrochloric acid, by this step
In obtained the second hydrochloric acid be back in step 2, to dissolve crude product ferric phosphate, wherein the mass percentage concentration of the 4th color
To be less than 5%；
Step 5：Ferric phosphate crystallized product is washed with second wash water, obtain purification of phosphoric acid iron and contains once washing water,
Wherein, the once washing water be containing mass percentage concentration be 1~5% the first hydrochloric acid washings, in the once washing water
Also contain chlorate, the corresponding hydroxide of cation of the chlorate is not soluble in water, and second wash water is removal chloride
Once washing water；
Step 6：Once washing water is sent into electrolysis unit electrolysis, to obtain chlorine, hydrogen, hydroxyl sediment, secondary washing
Water, hydrogen is discharged from hydrogen discharge mouth, and hydroxyl sediment is discharged from electrolytic cell, second wash water is back to step
Five, to wash ferric phosphate crystallized product, second wash water is changed into once washing water again；
Step 7：The chlorine is passed through in yellow phosphorus water, and is absorbed by yellow phosphorus water, to obtain the mixed of the first phosphoric acid and third hydrochloric acid
Close object；
Step 8：The mixture of first phosphoric acid and third hydrochloric acid is back in step 1, to be reacted with pyrite cinder；
Step 9：The purification of phosphoric acid iron obtained in step 5 is roasted, anhydrous iron phosphate is obtained.
In the present invention, after hydrochloric acid, phosphorus chloride, magnesium chloride, calcium chloride in once washing water are by cell reaction, chlorion
Chlorine is generated, chlorine reacts the mixture of generation the first phosphoric acid and third hydrochloric acid with yellow phosphorus water, the first phosphoric acid and third hydrochloric acid
Mixture generates crude product ferric phosphate with pyrite cinder again, to which pyrite cinder be turned waste into wealth by recycling for chlorion,
And avoid the exhaust emission environment of chlorion, it is cationic then combined with hydroxyl to be formed precipitation discharge, avoid cation concn
Be continuously increased so that by electrolysis processing once washing water can recycle, realize the zero-emission of washings, technique
Hydrochloric acid in the process is recycled by dissolving, filtering, distillation, condensation, rectification process, realizes the zero-emission of chlorion
It puts.
Description of the drawings
Fig. 1 is the flow chart for the improved method that battery-grade iron phosphate is produced using pyrite cinder.
Fig. 2 is the structural schematic diagram of the evaporative condenser.
Fig. 3 is the structural schematic diagram of the boiling wall.
Fig. 4 is the structural schematic diagram in condensation pipe main view direction.
Fig. 5 is the structural schematic diagram of the right apparent direction of the condensation pipe.
In figure：Evaporation boiler 10, water inlet line 11, the first solenoid valve 111, outlet conduit 12, second solenoid valve 121, condensation
Pipeline 13, condensation part 131, baffle plate 1311, fluid level controller 14, boiling wall 15, heating furnace 20, combustion chamber 21, Hydrogen Line
22, drainage pipeline 23, combustion gas duct 24.
Specific implementation mode
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be apparent that, drawings in the following description are some embodiments of the invention, common for this field
For technical staff, without creative efforts, other drawings may also be obtained based on these drawings.
Referring to Fig. 1, an embodiment of the present invention provides a kind of improved method for producing battery-grade iron phosphate using pyrite cinder,
Include the following steps：
Step S300：By pyrite cinder and the second phosphatase reaction, to obtain crude product ferric phosphate, wherein the quality percentage of the second phosphoric acid
A concentration of 20~80%；
Step S301：By the second dissolving with hydrochloric acid of crude product ferric phosphate, and clear liquid and filter residue is obtained by filtration, wherein the matter of the second hydrochloric acid
It is 20~30% to measure percentage concentration；
Step S302：The clear liquid is distilled, to obtain gaseous hydrogen chloride and ferric phosphate crystallized product；
Step S303：Gaseous hydrogen chloride is condensed, the 4th hydrochloric acid is obtained, the 4th hydrochloric acid rectifying is obtained into the second hydrochloric acid, this is walked
The second hydrochloric acid obtained in rapid is back in step S301, to dissolve crude product ferric phosphate, wherein the quality percentage of the 4th color
It is a concentration of to be less than 5%；
Step S304：Ferric phosphate crystallized product is washed with second wash water, purification of phosphoric acid iron is obtained and contains once washing
Water, wherein the once washing water be containing mass percentage concentration be 1~5% the first hydrochloric acid washings, the once washing
Also contain chlorate in water, the corresponding hydroxide of cation of the chlorate is not soluble in water, and second wash water is removal chlorination
The once washing water of object；
Step S305：Once washing water is sent into electrolysis unit electrolysis, to obtain chlorine, hydrogen, hydroxyl sediment, secondary wash
Water is washed, hydrogen is discharged from hydrogen discharge mouth, hydroxyl sediment is discharged from electrolytic cell, second wash water is back to step
S304, to wash ferric phosphate crystallized product, second wash water is changed into once washing water again, wherein second wash water is to go
Except the once washing water of chloride；
Step S306：The chlorine is passed through in yellow phosphorus water, and is absorbed by yellow phosphorus water, to obtain the first phosphoric acid and third hydrochloric acid
Mixture；
Step S307：The mixture of first phosphoric acid and third hydrochloric acid is back in step S300, to be reacted with pyrite cinder；
Step S308：The purification of phosphoric acid iron obtained in step S304 is roasted, anhydrous iron phosphate is obtained.
In wherein Fig. 1, one finger chlorine of reaction is reacted with yellow phosphorus water, and two finger phosphoric acid of reaction is reacted with pyrite cinder.
In the present invention, after hydrochloric acid, phosphorus chloride, magnesium chloride, calcium chloride in once washing water are by cell reaction, chlorion
Chlorine is generated, chlorine reacts the mixture of generation the first phosphoric acid and third hydrochloric acid with yellow phosphorus water, the first phosphoric acid and third hydrochloric acid
Mixture generates crude product ferric phosphate with pyrite cinder again, to which pyrite cinder be turned waste into wealth by recycling for chlorion,
And avoid the exhaust emission environment of chlorion, it is cationic then combined with hydroxyl to be formed precipitation discharge, avoid cation concn
Be continuously increased so that by electrolysis processing once washing water can recycle, realize the zero-emission of washings, technique
Hydrochloric acid in the process is recycled by dissolving, filtering, distillation, condensation, rectification process, realizes the zero-emission of chlorion
It puts.
Referring to Fig. 1, further, the once washing water in step 304 passes through pretreated step before being electrolysed in step 305
Suddenly, which is that once washing water is passed through evaporative condenser, the washings for being 1~5% by mass percentage concentration
Concentration, the evaporative condenser use the hydrogen heating discharged in step 305.
In present embodiment, the hydrogen that cell reaction is generated is used for the evaporation and concentration of once washing, is once washed with improving
Water electrolysis efficiency is washed, electrolysis energy consumption is reduced, while both having avoided the exhaust emission environment of hydrogen, in turn avoids energy waste.
Referring to Fig. 2, further, evaporative condenser includes evaporation boiler 10, heating furnace 20, and hydrogen is equipped on heating furnace 20
Pipeline 22, drainage pipeline 23, combustion gas duct 24 are equipped with water inlet line 11, outlet conduit 12, condensation on evaporation boiler 10
Pipeline 13, fluid level controller 14, evaporation boiler 10 pass through the round hole of 20 roof of heating furnace, and are nested into internally heated oven 20, evaporate
The round hole internal ring wall of pot 10 top external annulus and 20 roof of heating furnace is fixed, is tightly connected, one end of Hydrogen Line 22 with add
21 bottom of combustion chamber of hot stove 20 is connected to, and the other end of Hydrogen Line 22 is connected to the hydrogen discharge mouth of electrolysis unit, heating furnace
20 21 bottom of combustion chamber is communicated with drainage pipeline 23, the water generated after combustion of hydrogen is discharged, the combustion chamber of heating furnace 20
21 bottoms are communicated with combustion gas duct 24, and air is passed through in the combustion chamber 21 of heating furnace 20, and evaporative condenser top connects
It is connected to water inlet line 11, once washing water to be pre-treated is passed through evaporative condenser, is equipped on water inlet line 11
One solenoid valve 111, evaporative condenser lower part are connected with outlet conduit 12, and the once washing after being concentrated by evaporation is passed through electrolysis
Slot, is equipped with second solenoid valve 121 on outlet conduit 12, and after the water evaporation in above-mentioned evaporative condenser, water vapour is evaporating
Condenser overhead is delivered to use from the water outlet at the top of evaporative condenser at condensed water, the condensed water by condensation pipe 13
Point is equipped with fluid level controller 14, fluid level controller 14 and control mould to wash ferric phosphate crystallized product in evaporative condenser
Block is electrically connected, and control module is electrically connected with the first solenoid valve 111, second solenoid valve 121, and the water level in evaporative condenser exists
When low water level, fluid level controller 14 sends out the low signal of water level to control module, and controller module controls the first solenoid valve 111 and beats
It opens, the closing of second solenoid valve 121, for the water level in evaporative condenser in high water level, fluid level controller 14 sends out the high letter of water level
Number give control module, control module control the first solenoid valve 111 close, second solenoid valve 121 open.
In the present embodiment, the first solenoid valve 111 is controlled by fluid level controller 14 and is closed, second solenoid valve 121 is intermittently opened
Or close, to control the liquid level of once washing water in evaporative condenser, to which indirect control is washed by pretreated first
The mass percentage concentration of the middle hydrochloric acid of water, to provide the hydrochloric acid required containing specified mass percentage concentration for electrolysis unit interval
Once washing water.
Referring to Fig. 2 and Fig. 3, further, in evaporative condenser has and contacted with the raw water in it, and to heat raw water
Boil wall 15, and the side that boiling wall 15 is contacted with raw water is densely covered with tiny protrusion, and the free end of protrusion is arranged to tip.
In the present embodiment, part that evaporative condenser is contacted with water, and heated to water is arranged to the wall 15 that boils, and one
Aspect increases disengagement area by densely covered tiny protrusion, is on the other hand gas by the way that the free end of protrusion is arranged to tip
Bubble production provides growth cores, to promote the evaporation of water.
Referring to Fig. 2, Fig. 4, Fig. 5, further, 13 section of condensation pipe is rectangular, square along its length in condensation pipe 13
Multiple condensation parts 131 are inserted to uniform intervals, condensation part 131 includes two baffle plates 1311, and two baffle plates 1311 are reversed
It is obliquely installed, each baffle plate 1311 is trapezoidal, and vertical with exhaust duct inside side walls.
Baffle plate 1311 adjusts the mobility status of vapor in condensation pipe 13, after vapor encounters baffle plate 1311, one
Small part condensed water flows downward along baffle plate 1311, while multiple baffle plates 1311 increase the heat exchange area of vapor,
Accelerate the cohesion of vapor, after the condensation film to certain thickness on baffle plate 1311, edge under the action of gravity and air-flow
It baffle plate 1311 and is gathered in 13 bottom of condensation pipe, point of use is flow to further along 13 bottom of condensation pipe, to wash phosphoric acid
Iron crystallized product effectively accelerates vapor condensation effect, which neither additionally increases device structure, and can be fully
Using the space in the pipeline of existing device, and acceleration vapor condensation effect, simple structure, practicality are reached.
Further, the electrolytic process of once washing water is in step S305, will pass through by pretreated once washing water
Diaphragm or cationic membrane electrolytic cell are that anode obtains chlorine and hydrogen using copper mesh as cathode, titanium alloy, and electrolysis uses continuous multi-stage
Mode, i.e., row supplements new once washing water and carries out two level electrolysis the once washing water after level-one electrolysis again, after two level electrolysis
Once washing water be supplemented new once washing water and carry out three-level electrolysis, and so on.
It in present embodiment, uses copper mesh for cathode, chlorion can be effectively reduced in diffusion length in the electrolytic solution, subtracted
Small electrolysis energy consumption is more suitable for the preparing chlorine by electrolysis gas of low concentration of salt aqueous acid.
The steps in the embodiment of the present invention can be sequentially adjusted, merged and deleted according to actual needs.
Module or unit in device of the embodiment of the present invention can be combined, divided and deleted according to actual needs.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, those skilled in the art can understand all or part of the processes for realizing the above embodiment, and is wanted according to right of the present invention
Equivalent variations made by asking, still belong to the scope covered by the invention.
Claims (6)
1. a kind of improved method for producing battery-grade iron phosphate using pyrite cinder, it is characterised in that include the following steps：
Step 1：By pyrite cinder and the second phosphatase reaction, to obtain crude product ferric phosphate, wherein the quality percentage of the second phosphoric acid is dense
Degree is 20~80%；
Step 2：By the second dissolving with hydrochloric acid of crude product ferric phosphate, and clear liquid and filter residue is obtained by filtration, wherein the quality of the second hydrochloric acid
Percentage concentration is 20~30%；
Step 3：The clear liquid is distilled, to obtain gaseous hydrogen chloride and ferric phosphate crystallized product；
Step 4：Gaseous hydrogen chloride is condensed, the 4th hydrochloric acid is obtained, the 4th hydrochloric acid rectifying is obtained into the second hydrochloric acid, by this step
In obtained the second hydrochloric acid be back in step 2, to dissolve crude product ferric phosphate, wherein the mass percentage concentration of the 4th color
To be less than 5%；
Step 5：Ferric phosphate crystallized product is washed with second wash water, obtain purification of phosphoric acid iron and contains once washing water,
Wherein, the once washing water be containing mass percentage concentration be 1~5% the first hydrochloric acid washings, in the once washing water
Also contain chlorate, the corresponding hydroxide of cation of the chlorate is not soluble in water, and second wash water is removal chloride
Once washing water；
Step 6：Once washing water is sent into electrolysis unit electrolysis, to obtain chlorine, hydrogen, hydroxyl sediment, secondary washing
Water, hydrogen is discharged from hydrogen discharge mouth, and hydroxyl sediment is discharged from electrolytic cell, second wash water is back to step
Five, to wash ferric phosphate crystallized product, second wash water is changed into once washing water again；
Step 7：The chlorine is passed through in yellow phosphorus water, and is absorbed by yellow phosphorus water, to obtain the mixed of the first phosphoric acid and third hydrochloric acid
Close object；
Step 8：The mixture of first phosphoric acid and third hydrochloric acid is back in step 1, to be reacted with pyrite cinder；
Step 9：The purification of phosphoric acid iron obtained in step 5 is roasted, anhydrous iron phosphate is obtained.
2. the improved method for producing battery-grade iron phosphate using pyrite cinder as described in claim 1, it is characterised in that：Step
Once washing water in five passes through pretreated step before being electrolysed in step 6, which is, by once washing
By evaporative condenser, the washings that mass percentage concentration is 1~5% are concentrated, the evaporative condenser uses in step 6
The hydrogen of discharge heats.
3. the improved method for producing battery-grade iron phosphate using pyrite cinder as claimed in claim 2, it is characterised in that：It is described
Evaporative condenser includes evaporation boiler, heating furnace, and Hydrogen Line, drainage pipeline, combustion gas duct are equipped on heating furnace,
Water inlet line, outlet conduit, condensation pipe, fluid level controller are installed, the evaporation boiler passes through heating furnace roof on evaporation boiler
Round hole, and be nested into internally heated oven, the round hole internal ring wall of evaporation boiler top external annulus and heating furnace roof fixes,
It is tightly connected, one end of the Hydrogen Line is connected to the bottom of combustion chamber of heating furnace, the other end and the electricity of the Hydrogen Line
The hydrogen discharge mouth connection of device is solved, the bottom of combustion chamber of the heating furnace is communicated with drainage pipeline, will be raw after combustion of hydrogen
At water discharge, the bottom of combustion chamber of the heating furnace is communicated with combustion gas duct, air is passed through to the burning of heating furnace
Interior, the evaporative condenser top are connected with water inlet line, and once washing water to be pre-treated is passed through evaporative condenser,
First solenoid valve is installed on water inlet line, the evaporative condenser lower part is connected with outlet conduit, after being concentrated by evaporation
Once washing be passed through electrolytic cell, second solenoid valve is installed on outlet conduit, after the water evaporation in above-mentioned evaporative condenser,
For water vapour at condensed water at the top of evaporative condenser, the condensed water is defeated by condensation pipe from the water outlet at the top of evaporative condenser
It send to point of use, to wash ferric phosphate crystallized product, fluid level controller, the liquid level control is installed in the evaporative condenser
Device processed is electrically connected with control module, and the control module is electrically connected with the first solenoid valve, second solenoid valve, evaporative condenser
For interior water level in low water level, fluid level controller sends out the low signal of water level to control module, the first electricity of controller module control
Magnet valve is opened, second solenoid valve is closed, and for the water level in evaporative condenser in high water level, fluid level controller sends out the high letter of water level
Number give control module, control module control the first solenoid valve close, second solenoid valve open.
4. the improved method for producing battery-grade iron phosphate using pyrite cinder as claimed in claim 3, it is characterised in that：It is described
Have in evaporative condenser and contacted with the raw water in it, and to heat the boiling wall of raw water, the boiling wall is contacted with raw water
Side be densely covered with tiny protrusion, the free end of the protrusion is arranged to tip.
5. the improved method for producing battery-grade iron phosphate using pyrite cinder as claimed in claim 3, it is characterised in that：It is described
Condensation pipe section is rectangular, and uniform intervals have inserted multiple condensation parts, the condensation along its length in condensation pipe
Portion includes two baffle plates, and the setting of two baffle plate reversed dips, each baffle plate is trapezoidal, and with side on the inside of exhaust duct
Wall is vertical.
6. the improved method for producing battery-grade iron phosphate using pyrite cinder as described in claim 1, it is characterised in that：Step
The electrolytic process of once washing water is in six, will pass through pretreated once washing water by diaphragm or cationic membrane electrolytic cell,
It is that anode obtains chlorine and hydrogen using copper mesh as cathode, titanium alloy, is electrolysed by the way of continuous multi-stage, i.e., after level-one electrolysis
Row supplements new once washing water progress two level electrolysis to once washing water again, and the once washing water after two level electrolysis is supplemented new
Once washing water carries out three-level electrolysis, and so on.
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| CN201810268426.3A CN108328594A (en) | 2018-03-29 | 2018-03-29 | The improved method for producing battery-grade iron phosphate using pyrite cinder |
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| CN201810268426.3A CN108328594A (en) | 2018-03-29 | 2018-03-29 | The improved method for producing battery-grade iron phosphate using pyrite cinder |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092698A (en) * | 2010-12-03 | 2011-06-15 | 何侠 | Method for preparing sulfuric-acid burned slag into phosphate with chemical method |
-
2018
- 2018-03-29 CN CN201810268426.3A patent/CN108328594A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102092698A (en) * | 2010-12-03 | 2011-06-15 | 何侠 | Method for preparing sulfuric-acid burned slag into phosphate with chemical method |
Non-Patent Citations (2)
| Title |
|---|
| 《简明化学试剂手册》编写组 编: "《简明化学试剂手册》", 31 January 1991, 上海科学技术出版社 * |
| 贾素云: "《化工环境科学与安全技术》", 28 February 2009, 北京：国防工业出版社 * |
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