CN105753063A - Method for separating ferric oxide in coal-powder boiler fly ash - Google Patents
Method for separating ferric oxide in coal-powder boiler fly ash Download PDFInfo
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- CN105753063A CN105753063A CN201610066002.XA CN201610066002A CN105753063A CN 105753063 A CN105753063 A CN 105753063A CN 201610066002 A CN201610066002 A CN 201610066002A CN 105753063 A CN105753063 A CN 105753063A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention provides a method for separating ferric oxide in coal-powder boiler fly ash. According to the method, phosphoric acid and fly ash take low-temperature hydrothermal reaction, so that total Fe2O3 and FeO and partial amorphous state Al2O3 in the fly ash are dissolved out; then, ethanol is used for separating Fe2O3 and FeO in the solution to obtain high-purity ferric oxide. The method provided by the invention belongs to a method with the advantages that special requirements on equipment are not needed; low-temperature reaction is performed; the ferric oxide in the fly ash can be efficiently separated and extracted. The method provided by the invention has the advantages that 90 percent to 96 percent of aluminum oxide in the fly ash can be dissolved; 98 percent to 100 percent of ferric oxide can be dissolved out. By the technical scheme provided by the invention, resources of the fly ash are sufficiently used; the manufacturing process is simple; the production cost is low; the method is suitable for mass production.
Description
Technical field
The present invention relates to a kind of Ash Utilization Application way, separate the method for ferrum oxide in coal-powder boiler flyash in particular to a kind of.
Background technology
Coal fired power generation is one of commonly used power generation mode in countries in the world, and effective utilization of the coal-fired a large amount of flyash produced has become world subject.At present, China's electric power more than 70% is produced by coal fired power generation, and the yield about 30% of whole nation coal is used for generating electricity, and consequent flyash, if, with amount deficiency, not only occupies a large amount of soil, causes serious environmental pollution, be also the waste of a kind of resource.
From another angle, rich in many oxide in flyash, such as Al2O3, SiO2, Fe2O3, FeO, CaO, MgO, SO3, Na2O, K2O etc., additionally contain a small amount of rare earth element.These oxides separation and Extraction from flyash out and is prepared corresponding high value-added product, higher social economy's value can not only be produced, it is possible to alleviate the flyash harm to environment.
The comprehensive utilizating research of flyash, the particularly research of separation and Extraction aluminium oxide from flyash, from the forties in last century so far, many experts both domestic and external, scholar study at this and have carried out extensive work and proposed multiple separating and extracting process.But when extracting separation aluminium oxide, ferrum oxide is fallen as impurity treatment, not by Fe in flyash2O3With FeO recycling, cause the serious waste of resource.
And ferrum oxide is as a kind of inorganic pigment, it is widely used in the fields such as paint, rubber, plastic cosmetic, building ground material, accurate five metals instrument, optical glass, enamel, school supply and stationery, leather, magnetic alloy and high-grade alloy steel.
At present, Chinese scholars proposes certain methods for separation and Extraction ferrum oxide from flyash, such as: calcium oxide sintering process, soda lime sintering process etc., but these methods due to process conditions limit, the reason such as the ferrum oxide response rate is low, power consumption is big, production cost is high, bed drain purge is big, cause separation and Extraction ferrum oxide implementation result poor.
It is an object of the invention to utilize dust technology to react with common coal-powder boiler flyash low-temperature hydrothermal, make Fe whole in flyash2O3, FeO and part amorphous state Al2O3Dissolution, recycling separation of ethanol extracts the Fe in solution2O3, FeO, finally give the iron oxide product that purity is higher.
Summary of the invention
It is an object of the invention to provide and a kind of utilize the method for ferrum oxide in nitric acid and ethanol extraction flyash under cryogenic.
Technical scheme provided by the invention includes utilizing nitric acid to react with flyash low-temperature hydrothermal, makes Fe whole in flyash2O3, FeO and part amorphous state Al2O3Dissolution, recycling separation of ethanol extracts the Fe in solution2O3, FeO obtain highly purified ferrum oxide.Technical scheme processing technology provided by the invention is simple, reduce production cost, take full advantage of the resource of flyash, is suitable for large-scale production.
Realize the object of the invention technical scheme as follows:
A kind of separate the method for ferrum oxide in coal-powder boiler flyash, it is characterised in that described preparation method comprises the steps:
1) magnetic bead in magnetic separation separation of fine coal ash；
2) acidleach: at 70 DEG C～90 DEG C, mixes flyash with the nitric acid that concentration is 1%～5% with the ratio that solid-to-liquid ratio is 1:3～1:6 of nitric acid in flyash, reacts 1～4h；
3) solid-liquid separation: after reactant is cooled to room temperature, sucking filtration, the filter cake water washing that solid-to-liquid ratio is 2:1～1:2 by flyash Yu water, obtain the solution of ferric nitrate and aluminum nitrate；
4) separation of ethanol aluminum nitrate and ferrum oxide: ethanol and step 3) in the described solution that obtains mix by 2:1～5:1 volume ratio, again by the mol ratio of aluminium oxide Yu ammonium nitrate be 1:3～1:4 add formulating ammonium nitrate mixed liquor, after stirring 1～2h, sucking filtration, obtain aluminum nitrate filter cake；Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1～1:2 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed；
5) ferrum oxide reclaims: dropping ammonia, in described recovery filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Further, described flyash is following component by mass percentage:
Al2O3+SiO2+Fe2O3> 70%, CaO > 5%.
Further, described flyash following component by mass percentage: Al2O3, 29.87%；19.25%, 47.08%；Fe2O3, 7.01%；CaO, 6.98%；SO3, 1.2%；Loss on ignition, 7.68%.
Further, described step 1) in, carry out wet magnetic separation separation with wet type low-intensity (magnetic) separator.
Further, described wet type low-intensity (magnetic) separator magnetic induction 0.2T, pan feeding speed 500mL/min, material concentration 8%, magnetic separation 3～5 times.
Further, described step 1) purpose of magnetic separation is to isolate magnetic bead, that isolates magnetic bead in flyash is mainly composed of Fe3O4.Because of Fe3O4Stable chemical nature, not easily react with strong acid and strong base, therefore for make the ferrum oxide in flyash be totally separated extraction, it is necessary to add magnetic separation step.
With immediate prior art ratio, technical scheme provided by the invention has following excellent effect:
1, technical scheme provided by the invention, the ferrum oxide in energy fully high efficiency extraction flyash.
2, technical scheme provided by the invention, utilizes the method treated coal ash of low-temp reaction, to equipment without particular/special requirement.
3, technical scheme provided by the invention, can by the alumina leaching 90%～96% in flyash, ferrum oxide dissolution 98%～100%.
4, technical scheme provided by the invention, flyash is after magnetic separation, and the response rate of magnetic bead reaches more than 85%, and magnetic bead particle diameter is at 20～30um；From flyash, reclaim magnetic bead less costly, except nonmagnetic portion iron content is relatively low in the flyash after magnetic bead, be more beneficial for integrated application；With magnetic bead in conjunction with HGMS technology process waste water, can by effective for the tp removal rate in waste water, efficiency is high, treating capacity is big.
5, technical scheme provided by the invention, has widened the scope of total utilization of PCA.
Detailed description of the invention
Further technical scheme is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain, broadly fall into the scope of protection of the invention.
Embodiment 1, flyash through 3 magnetic separation, then with 5% nitric acid mix by solid-to-liquid ratio 1:3, and at 80 DEG C, react 4h；Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 2:1 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature；It is that 2:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:3 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 2h, sucking filtration, obtain aluminum nitrate filter cake；Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 2, flyash through 4 magnetic separation, then with 4% nitric acid mix by solid-to-liquid ratio 1:4, and at 75 DEG C, react 3h；Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 1:2 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature；It is that 3:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:4 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 1h, sucking filtration, obtain aluminum nitrate filter cake；Then by the absolute ethanol washing that solid-to-liquid ratio is 1:2 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 3, flyash through 5 magnetic separation, then with 3% nitric acid mix by solid-to-liquid ratio 1:5, and at 70 DEG C, react 3h；Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 2:1 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature；It is that 4:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:3 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 1.5h, sucking filtration, obtain aluminum nitrate filter cake；Then by the absolute ethanol washing that solid-to-liquid ratio is 2:3 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 4, flyash through 5 magnetic separation, then with 5% nitric acid mix by solid-to-liquid ratio 1:5, and at 90 DEG C, react 3h；Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 2:3 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature；It is that 5:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:3 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 2h, sucking filtration, obtain aluminum nitrate filter cake；Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 5, flyash through 5 magnetic separation, then with 2% nitric acid mix by solid-to-liquid ratio 1:6, and at 85 DEG C, react 4h；Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 4:3 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature；It is that 5:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:4 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 2h, sucking filtration, obtain aluminum nitrate filter cake；Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 6, flyash through 4 magnetic separation, then with 3% nitric acid mix by solid-to-liquid ratio 1:3, and at 75 DEG C, react 4h；Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 5:4 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature；It is that 3:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:4 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 1h, sucking filtration, obtain aluminum nitrate filter cake；Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 7, flyash through 5 magnetic separation, then with 5% nitric acid mix by solid-to-liquid ratio 1:4, and at 70 DEG C, react 2h；Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 2:1 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature；It is that 3:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:3 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 1h, sucking filtration, obtain aluminum nitrate filter cake；Then by the absolute ethanol washing that solid-to-liquid ratio is 1:2 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 8, flyash through 4 magnetic separation, then with 5% nitric acid mix by solid-to-liquid ratio 1:6, and at 85 DEG C, react 3h；Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 2:1 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature；It is that 4:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:4 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 2h, sucking filtration, obtain aluminum nitrate filter cake；Then by the absolute ethanol washing that solid-to-liquid ratio is 5:4 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 9, flyash through 3 magnetic separation, then with 1% nitric acid mix by solid-to-liquid ratio 1:3, and at 90 DEG C, react 4h；Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 4:1 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature；It is that 7:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:3 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 2h, sucking filtration, obtain aluminum nitrate filter cake；Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Embodiment 10, flyash through 5 magnetic separation, then with 4% nitric acid mix by solid-to-liquid ratio 1:4, and at 80 DEG C, react 3h；Reaction end after sucking filtration obtains filter cake, and with the water washing that solid-to-liquid ratio is 1:2 of flyash Yu water, obtains the solution of ferric nitrate and aluminum nitrate after being cooled to room temperature；It is that 2:1 preparation adds ethanol by the volume ratio of ethanol with ferric nitrate and aluminum nitrate solution, then is that 1:3 adds formulating ammonium nitrate mixed liquor by the mol ratio of aluminium oxide Yu ammonium nitrate, after stirring 1h, sucking filtration, obtain aluminum nitrate filter cake；Then by the absolute ethanol washing that solid-to-liquid ratio is 1:2 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed；Dropping ammonia is in reclaiming in filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
Gained sample in above-described embodiment is carried out performance test respectively, obtains data as shown in table 1 below.
Table 1
Above example is only in order to illustrate that technical scheme is not intended to limit; those of ordinary skill in the field are to be understood that; the specific embodiment of the present invention can being modified with reference to above-described embodiment or equivalent replacement, these are all being applied within the claims awaited the reply without departing from any amendment or equivalent replacement of spirit and scope of the invention.
Claims (5)
1. one kind separates the method for ferrum oxide in coal-powder boiler flyash, it is characterised in that described preparation method comprises the steps:
1) magnetic bead in magnetic separation separation of fine coal ash；
2) acidleach: at 70 DEG C～90 DEG C, mixes flyash with the nitric acid that concentration is 1%～5% with the ratio that solid-to-liquid ratio is 1:3～1:6 of nitric acid in flyash, reacts 1～4h；
3) solid-liquid separation: after reactant is cooled to room temperature, sucking filtration, the filter cake water washing that solid-to-liquid ratio is 2:1～1:2 by flyash Yu water, obtain the solution of ferric nitrate and aluminum nitrate；
4) separation of ethanol aluminum nitrate and ferrum oxide: ethanol and step 3) in the described solution that obtains mix by 2:1～5:1 volume ratio, again by the mol ratio of aluminium oxide Yu ammonium nitrate be 1:3～1:4 add formulating ammonium nitrate mixed liquor, after stirring 1～2h, sucking filtration, obtain aluminum nitrate filter cake；Then by the absolute ethanol washing that solid-to-liquid ratio is 2:1～1:2 of aluminium oxide Yu dehydrated alcohol, and filtrate is reclaimed；
5) ferrum oxide reclaims: dropping ammonia, in described recovery filtrate, to pH value of solution > 8, filters, obtains hydrated ferric oxide..
2. as claimed in claim 1 a kind of separate the method for ferrum oxide in coal-powder boiler flyash, it is characterised in that described flyash is following component by mass percentage:
Al2O3+SiO2+Fe2O3> 70%, CaO > 5%.
3. as claimed in claim 2 a kind of separate the method for ferrum oxide in coal-powder boiler flyash, it is characterised in that described flyash following component by mass percentage: Al2O3, 29.87%；19.25%, 47.08%；Fe2O3, 7.01%；CaO, 6.98%；SO3, 1.2%；Loss on ignition, 7.68%.
4. as claimed in claim 1 a kind of separate the method for ferrum oxide in coal-powder boiler flyash, it is characterised in that described step 1) in, carry out wet magnetic separation separation with wet type low-intensity (magnetic) separator.
5. as claimed in claim 4 a kind of separate the method for ferrum oxide in coal-powder boiler flyash, it is characterised in that described wet type low-intensity (magnetic) separator magnetic induction 0.2T, pan feeding speed 500mL/min, material concentration 8%, magnetic separation 3～5 times.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20230045286A1 (en) * | 2019-01-24 | 2023-02-09 | Elixsys, Inc. | Systems and Methods to Recover Value-Added Materials from Gypsum |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6241721A (en) * | 1985-08-19 | 1987-02-23 | Nisshin Steel Co Ltd | Method of recovering iron oxide |
| CN101870489A (en) * | 2010-04-27 | 2010-10-27 | 中国神华能源股份有限公司 | Method for producing superfine aluminium hydroxide and aluminium oxide by using flyash |
| CN102101689A (en) * | 2010-12-23 | 2011-06-22 | 内蒙古昶泰资源循环再生利用科技开发有限责任公司 | Technological method for producing high-purity low-iron aluminum sulfate by using coal ash and comprehensively utilizing coal ash |
| CN104445212A (en) * | 2013-09-16 | 2015-03-25 | 贵阳铝镁设计研究院有限公司 | Method for processing fly ash used for circulating fluidized bed |
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- 2016-01-29 CN CN201610066002.XA patent/CN105753063A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6241721A (en) * | 1985-08-19 | 1987-02-23 | Nisshin Steel Co Ltd | Method of recovering iron oxide |
| CN101870489A (en) * | 2010-04-27 | 2010-10-27 | 中国神华能源股份有限公司 | Method for producing superfine aluminium hydroxide and aluminium oxide by using flyash |
| CN102101689A (en) * | 2010-12-23 | 2011-06-22 | 内蒙古昶泰资源循环再生利用科技开发有限责任公司 | Technological method for producing high-purity low-iron aluminum sulfate by using coal ash and comprehensively utilizing coal ash |
| CN104445212A (en) * | 2013-09-16 | 2015-03-25 | 贵阳铝镁设计研究院有限公司 | Method for processing fly ash used for circulating fluidized bed |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20230045286A1 (en) * | 2019-01-24 | 2023-02-09 | Elixsys, Inc. | Systems and Methods to Recover Value-Added Materials from Gypsum |
| US11912582B2 (en) * | 2019-01-24 | 2024-02-27 | Davy Powersports Inc. | Systems and methods to recover value-added materials from gypsum |
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Application publication date: 20160713 |