CN107902683A - Method for extracting silicon product and aluminum oxide step by mixing, reducing and roasting fly ash and sulfuric acid - Google Patents
Method for extracting silicon product and aluminum oxide step by mixing, reducing and roasting fly ash and sulfuric acid Download PDFInfo
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- CN107902683A CN107902683A CN201711144546.4A CN201711144546A CN107902683A CN 107902683 A CN107902683 A CN 107902683A CN 201711144546 A CN201711144546 A CN 201711144546A CN 107902683 A CN107902683 A CN 107902683A
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- sulfuric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
- C01F7/26—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with sulfuric acids or sulfates
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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
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
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Abstract
The invention discloses a method for extracting silicon products and aluminum oxide step by mixing, reducing and roasting fly ash and sulfuric acid, belonging to the field of comprehensive utilization of fly ash. Mixing and batching the fly ash, a carbon-based solid reducing agent and concentrated sulfuric acid according to a certain proportion, directly feeding the mixture into roasting equipment to finish reduction roasting, then carrying out low-temperature alkaline leaching on the reduction roasted product to extract silicon to obtain a silicon solution and high-alumina slag, then carrying out high-temperature alkaline leaching on the high-alumina slag to extract alumina, wherein the silicon solution can be treated according to a conventional method to obtain a silicon product. The acidolysis and the reduction roasting are completed in one step, so that the ring formation of the rotary kiln is avoided, the flow is simplified, the investment is reduced, the energy consumption is saved, and the synergy of the efficient decomposition of the aluminum sulfate and the regulation and control of the reaction activity of the calcine alumina and the silica is realized.
Description
Technical field
The invention belongs to total utilization of PCA field, and in particular to one kind extracts aluminium oxide and silicon product from flyash
Method, mix reduction roasting, low-temperature alkaline leaching silicon, high-temperature alkali leaching aluminium especially by flyash and sulfuric acid, from
Aluminium oxide and silicon product are extracted in flyash.
Background technology
Flyash main component is aluminium oxide and silica, particularly some regional flyash it is salic up to 40% with
On, be a kind of potential alumina resource, but due in flyash silica content it is also very high, it is traditional also up to more than 40%
Bauxite into alumina technique is difficult to economic treatment flyash.Therefore, how both economical separation aluminium silicon, particularly into
Silica is preferentially removed or extracts before entering alkaline process production aluminium oxide, it is most important to flyash extraction aluminium oxide.
Silica in flyash is directly leached with sodium hydroxide solution, technique is simple, but due to more than aluminium in flyash with not
Carry out the compound form that stone etc. is stablized to exist, direct alkali leaching can only remove amorphous carbon/silicon dioxide, and total removal efficiency of silicon is low, leads to
Often there was only 40%~50%.A kind of method that aluminium oxide is extracted from aluminous fly-ash disclosed in CN101284668A, by high alumina
The sodium hydroxide solution pressure leaching of flyash concentration 15%~30%, makes part silicon dissolution, and siliceous leachate is used to produce
White carbon, the flyash after pre-desiliconizing sinter after being mixed with agstone, sodium carbonate liquor, then leach aluminium, but due to coal measures
The activated silica ratio of alkali soluble is less in solid waste, and the alumina silica ratio of material is still relatively low after pre-desiliconizing, follow-up sintered material
Amount is big, the high energy consumption of high temperature pre-desiliconizing and sintering, and red mud quantum of output is still very big.One kind disclosed in CN101125656A is from fine coal
The method of firstly extracting silicon and secondly extracting aluminum in ash, leaches flyash using concentrated alkali solution of the naoh concentration more than 40%, can improve
The pre- removal efficiency of silicon, then alkaline process, which sinters, extracts aluminium oxide.Since the desiliconization rate of direct alkali leaching is low, the aluminium silicon of flyash after desiliconization
Than only having 2 or so, cause to still need to supplying large quantities of lime during follow-up sintering, energy consumption, material consumption are high, and red mud quantum of output is big.
The present inventor discloses a kind of extracted from coal solid waste pre-desiliconizing in CN104803403A and aoxidizes
The soda acid process integration of aluminium, flyash is uniform with a certain amount of concentrated sulfuric acid mix, first carried out at a temperature of 120 DEG C~500 DEG C
Acidolysis, cure pretreatment, then by the flyash after acidolysis under conditions of reducing agent is not added, in 900 DEG C~1200 DEG C temperature
Spend the lower fluosolids roasting that carries out and obtain calcining, gained calcining obtains high alumina slag through atmospheric low-temperature alkali leaching pre-desiliconizing, then uses and adds
Aluminium oxide is extracted in the leaching of super pressure-high temperature alkali from high alumina slag.The leaching rate of the method silicon is high, up to more than 70%, but due to acidolysis cure with
Separate operation is roasted, it is necessary to first that acidolysis feed powder is broken, then is warming up to firing temperature roasting, it is impossible to which realization is really continuously turned into
Industry, energy consumption increase.Simultaneously because Curing material is fine and close, stove ring formation is easy to cause, it is necessary to stop work and is cleared up and cleared up difficulty
It is larger.Additionally due to being roasted using non-reducing atmosphere, aluminium oxide easily changes to alpha-aluminium oxide when aluminum sulfate decomposes, and makes follow-up
Alkali extraction take aluminium oxide to become difficult.
The content of the invention
The purpose of the invention is to overcome the shortcomings of in existing flyash extraction aluminum oxide technology, especially for solution
It is insufficient present in flyash soda acid combined extracting alumina technology, there is provided a kind of flyash sulfuric acid mixing reduction roasting substep carries
The method for taking silicon product and aluminium oxide.
The present inventor, by repetition test exploration discovery, by flyash soda acid combined extracting alumina technology
Acidolysis, cure pretreatment and roasting, by two steps separated merge into a step complete, both simplify flow, eliminate acid
Solution material cooling, crush and etc., realize real continuous operations, improve production efficiency;Again can be by reducing agent so that
Acidolysis material is loose, avoids acid hemolysis process stove ring formation;Perfection is solved in existing flyash soda acid combined extracting alumina technology
Existing production process is discontinuous, acidolysis material densification causes the technical problem of stove ring formation, simultaneously because using reduction roasting, solution
Determine in acidolysis material the aluminium oxide problem difficult with the regulation and control of silica reactivity in aluminum sulfate efficient-decomposition, calcining.The present invention's
Purpose is achieved through the following technical solutions.
The method of flyash sulfuric acid mixing reduction roasting step by step arithmetic silica and aluminium oxide, it is characterised in that including with
Lower step:
(1) roasted after mixing flyash, the concentrated sulfuric acid and reducing agent in proportion, obtain reduced calcine;
(2) reduced calcine is taken into silicon using low-temperature alkaline extraction, obtains siliceous leachate and high alumina slag;
(3) high alumina slag is taken into aluminium using high-temperature alkali extraction, obtains sodium aluminate solution and leach residue;
(4) siliceous leachate is conventionally handled to obtain silicon product;
(5) sodium aluminate solution is conventionally handled to obtain aluminium oxide.
Further, the reducing agent is carbon-based solid reducing agent.
Further, the carbon-based solid reducing agent is the one or more in coal, coke, charcoal or petroleum coke, preferably
Fixed carbon content is not less than 50% coal dust.
Further, mass concentration >=80% of the concentrated sulfuric acid.
Further, the mixing in proportion described in step (1), refers to that aluminium oxide rubs with the sulfuric acid in the concentrated sulfuric acid in flyash
You are than being 1:2.5~1:5, aluminium oxide is 1 with the carbon containing molar ratio of reducing agent:1.5~1:5.
Further, the firing temperature of roasting is 850 DEG C~1200 DEG C in step (1).
Further, the equipment of roasting uses rotary kiln in step (1), and 900~1100 DEG C of firing temperature, controls rotary kiln
The programming rate of middle material, ensures residence time >=30min of the material in 100 DEG C~250 DEG C sections, preferably at 120 DEG C~200 DEG C
Residence time >=30min of section.
Further, the extraction of low-temperature alkaline described in step (2) takes silicon, is by reduced calcine Na250~150g/L of O concentration
Sodium hydroxide solution leach silicon, leach solid-liquid mass ratio 1:3~1:25,50~100 DEG C of extraction temperature, extraction time 30~
240min。
Further, the extraction of high-temperature alkali described in step (3) takes aluminium, is by high alumina slag Na2150~300g/L of O concentration
Sodium hydroxide solution leach aluminium, leach solid-liquid mass ratio 1:3~1:20, lime-crushed stone pile is the 0~15% of high alumina slag quality,
150~300 DEG C of extraction temperature, 15~120min of extraction time.
In the implementation of the present invention, it is allowed to containing certain moisture in flyash, but the moisture in flyash should be controlled, its
Moisture allows content to be limited with the h 2 so 4 concentration after mixed ingredients not less than 70%.
The flue gas that reduction roasting obtains is used for relieving haperacidity production sulfuric acid for recycling.The siliceous solution that low-temperature alkaline soaks can
Further produce silicon product, such as white carbon etc.;The sodium aluminate solution that high-temperature alkali is soaked is through kind point or carbon method production metallurgy
Grade aluminum oxide, seed precipitation solution can return to recycling.
The method of flyash sulfuric acid mixing reduction roasting step by step arithmetic silicon product and aluminium oxide provided by the invention, by fine coal
After ash is mixed in a certain ratio dispensing with carbon-based solid reducing agent, the concentrated sulfuric acid, it is sent directly into roasting apparatus and completes roasting, acidolysis
Completed with roasting in same equipment, between acidolysis and roasting, no first-hand datum crushing-fine grinding, clinker and reducing agent mixed ingredients
Deng intermediate step, a step obtains reduced calcine, simplifies flow, saves energy consumption, reduces investment;And in flyash, carbon-based solid
Reducing agent, the concentrated sulfuric acid mixture in, due to the supplying of carbon-based solid reducing agent, acidolysis, roasting material can be made loose, so as to avoid
Ring formation of rotary kiln, beneficial to rotary kiln operation;Simultaneously as using reduction roasting, while aluminum sulfate decomposition efficiency is improved, solution
Determine aluminium oxide and the problem of silica reactivity regulation and control in calcining, so as to improve the step by step arithmetic of silica and aluminium oxide
Rate;Silicon removal efficiency is up to 80% or so, obtains the high alumina slag of alumina silica ratio more than 7.
Brief description of the drawings
Fig. 1 is the principle flow chart of the method for the present invention.
Embodiment
Further explanation is made to the present invention below in conjunction with Fig. 1.
The present invention flyash sulfuric acid mixing reduction roasting step by step arithmetic silicon product and aluminium oxide method, by flyash,
The concentrated sulfuric acid and reducing agent roast after mixing in proportion, obtain reduced calcine;Reduced calcine is taken into silicon using low-temperature alkaline extraction, is obtained
Siliceous leachate and high alumina slag;High alumina slag is taken into aluminium using high-temperature alkali extraction, sodium aluminate solution is obtained and leaches residue;By aluminic acid
Sodium solution conventionally handles to obtain aluminium oxide.
When implementing, for the concentrated sulfuric acid used for the sulfuric acid of mass concentration >=80%, reducing agent is coal, coke, charcoal or stone
The carbon-based solid reducing agent such as oil coke, the carbon content in reducing agent are not less than 50%.The mixture of flyash, the concentrated sulfuric acid and reducing agent
In proportioning, aluminium oxide and the sulfuric acid molar ratio in the concentrated sulfuric acid are 1 in flyash:2.5~1:5, aluminium oxide and reducing agent institute are carbon containing
Molar ratio be 1:1.5~1:5.
Roasting apparatus uses rotary kiln, controls the programming rate of material in rotary kiln, 850 DEG C~1200 DEG C of firing temperature,
And control material is in residence time >=30min of 100 DEG C~250 DEG C sections, preferably 120 DEG C~200 DEG C sections residence time >=
30min。
Reduced calcine uses Na2The sodium hydroxide solution of 50~150g/L of O concentration leaches silicon, leaches solid-liquid mass ratio 1:3
~1:25,50~100 DEG C of extraction temperature, 30~240min of extraction time.
The high alumina slag obtained after leaching silicon, uses Na2The sodium hydroxide solution of 150~300g/L of O concentration leaches aluminium, leaches solid-liquid
Mass ratio 1:3~1:20, lime-crushed stone pile is the 0~15% of high alumina slag quality, 150~300 DEG C of extraction temperature, extraction time 15
~120min.
In some embodiments, it is allowed to containing certain moisture in flyash, but the moisture in flyash should be controlled,
Its moisture allows content to be limited with the h 2 so 4 concentration after mixed ingredients not less than 70%.
The method of the present invention is further described with nonlimiting examples below, to help to understand the present invention's
Content and its advantage, and determined not as limiting the scope of the present invention, protection scope of the present invention by claims.
Embodiment 1
Take that 1000g is salic 50%, the flyash of silica 38%, by 4 times of supplyings of wherein alumina molar number
The concentrated sulfuric acid of mass concentration 93%, is mixed into the coal dust containing fixed carbon 60% by 5 times of alumina molar number and is uniformly mixed, Ran Houjia
Enter in roaster, control stove programming rate, allow mixture to stop 60min in 120 DEG C~200 DEG C, be then warming up to 1050
15min is roasted at DEG C, obtains reduced calcine, by reduced calcine Na2The sodium hydroxide solution of O concentration 100g/L leaches, and leaches
Solid-liquid mass ratio 1:10,85 DEG C, extraction time 60min of extraction temperature, is obtained by filtration the high alumina of siliceous leachate and alumina silica ratio 8
Slag;Obtained high alumina slag Na2The sodium hydroxide solution of O concentration 200g/L leaches aluminium, leaches solid-liquid mass ratio 1:5, lime
Additive amount is the 5% of high alumina slag quality, 250 DEG C, extraction time 30min of extraction temperature, aluminium leaching rate 85%, the aluminium leached
Acid sodium solution is purified, kind point, calcining production aluminium oxide.
Embodiment 2
1000g flyash is taken, by the concentrated sulfuric acid of 4 times of supplying mass concentrations 93% of wherein alumina molar number, by oxidation
3 times of aluminium molal quantity are mixed into the coal dust containing fixed carbon 70% and are uniformly mixed, and then add in roaster, control stove heating speed
Degree, allows mixture to stop 60min in 120 DEG C~200 DEG C, is then warming up to 950 DEG C of roasting 15min, obtains reduced calcine, will
Reduced calcine Na2The sodium hydroxide solution of O concentration 50g/L leaches, and leaches solid-liquid mass ratio 1:5,85 DEG C of extraction temperature, is leached
Time 60min, is obtained by filtration siliceous leachate and high alumina slag, the leaching rate 80% of silicon, alumina silica ratio 7.5 in high alumina slag;It is resulting
High alumina slag Na2The sodium hydroxide solution of O concentration 200g/L leaches aluminium, leaches solid-liquid mass ratio 1:5, lime-crushed stone pile is height
The 10% of aluminium slag quality, 250 DEG C, extraction time 30min of extraction temperature, aluminium leaching rate 87%.
Embodiment 3
The concentrated sulfuric acid of the flyash by 3 times of supplying mass concentrations 93% of wherein alumina molar number is taken, by alumina molar
Several 2 times are mixed into the coal dust containing fixed carbon 70% and are uniformly mixed, and then add in roaster, control stove programming rate, allow mixed
Close material and stop 60min in 120 DEG C~200 DEG C, roast 15min at 1000 DEG C, reduced calcine is obtained, by reduced calcine Na2O
The sodium hydroxide solution of concentration 100g/L leaches, and leaches solid-liquid mass ratio 1:20,85 DEG C, extraction time 60min of extraction temperature, mistake
Filter obtains siliceous leachate and high alumina slag;By obtained high alumina slag Na2The sodium hydroxide solution of O concentration 220g/L leaches
Aluminium, leaches solid-liquid mass ratio 1:5,250 DEG C of extraction temperature, extraction time 30min, is filtered after leaching, obtained sodium aluminate solution
Purified, kind point, calcining production aluminium oxide.
Embodiment 4
The concentrated sulfuric acid of the flyash by 3 times of supplying mass concentrations 93% of wherein alumina molar number is taken, by alumina molar
The 2.5 times of several coal dusts of addition containing fixed carbon 70%, add in roaster, control stove programming rate, allow mixed after mixing
Close material and stop 60min in 120 DEG C~200 DEG C, roast 15min at 950 DEG C, obtain reduced calcine, reduced calcine is used
Na2The sodium hydroxide solution of O concentration 50g/L leaches 60min, leaches solid-liquid mass ratio 1:5,95 DEG C of extraction temperature, is obtained by filtration
Siliceous leachate and high alumina slag;By high alumina slag Na2The sodium hydroxide solution of O concentration 200g/L leaches aluminium, leaches solid-liquid quality
Than 1:5, lime-crushed stone pile is the 10% of high alumina slag quality, and 250 DEG C of extraction temperature, extraction time 30min, filters after leaching, obtain
The sodium aluminate solution that arrives is purified, kind point, calcining production aluminium oxide.
Embodiment 5
Flyash and the concentrated sulfuric acid, the coal dust containing fixed carbon 60% of mass concentration 93% are mixed in proportion, wherein
Concentrated sulfuric acid amount presses aluminium oxide and the sulfuric acid molar ratio 1 in the concentrated sulfuric acid in flyash:3.5 add, and are aoxidized by coal dust amount in flyash
Aluminium and the carbon containing molar ratio 1 of coal dust:3 add, and then continuously and uniformly add mixture in rotary kiln from rotary kiln,
Temperature gradient in rotary kiln is controlled, allows mixture to stop 60min in 120 DEG C~200 DEG C, burns till section temperature control at 950 DEG C
~1050 DEG C, a section residence time 30min is burnt till, kiln hood discharges to obtain reduced calcine, and reduced calcine is first taken through low-temperature alkaline extraction
Silicon, then high-temperature alkali extraction take aluminium.Rotary kiln stops material after 7 days continuously run and checks, is exported in kiln from feed points to kiln, inner wall
Without ring formation phenomenon.
For ease of contrast, be not added with mixture the oven test of reducing agent, i.e.,:By flyash and mass concentration
93% concentrated sulfuric acid mixes in proportion, and concentrated sulfuric acid amount presses aluminium oxide and the sulfuric acid molar ratio 1 in the concentrated sulfuric acid in flyash:
3.5 add, and then mixture is continuously and uniformly added in rotary kiln from rotary kiln, controls temperature gradient in rotary kiln,
Allow mixture to stop 60min in 120 DEG C~200 DEG C, burn till section temperature control at 950 DEG C~1050 DEG C, when burning till section stop
Between 30min, kiln hood discharges to obtain reduced calcine, after rotary kiln continuously runs 12h, can not be fed because formation rings in a kiln is serious.
Claims (10)
1. the method for flyash sulfuric acid mixing reduction roasting step by step arithmetic silicon product and aluminium oxide, it is characterised in that including following
Step:
(1) roasted after mixing flyash, the concentrated sulfuric acid and reducing agent in proportion, obtain reduced calcine;
(2) reduced calcine is taken into silicon using low-temperature alkaline extraction, obtains siliceous leachate and high alumina slag;
(3) high alumina slag is taken into aluminium using high-temperature alkali extraction, obtains sodium aluminate solution and leach residue;
(4) siliceous leachate is conventionally handled to obtain silicon product;
(5) sodium aluminate solution is conventionally handled to obtain aluminium oxide.
2. according to the method described in claim 1, it is characterized in that, the reducing agent described in step (1) is carbon-based solid reducing agent.
3. according to the method described in claim 2, it is characterized in that, the carbon-based solid reducing agent is coal, coke, charcoal or stone
One or more in oil coke, preferably fixed carbon content are not less than 50% coal dust.
4. according to the method described in claim 1, it is characterized in that, mass concentration >=80% of the concentrated sulfuric acid.
5. according to the method described in claim 1, it is characterized in that, mixing in proportion described in step (1), refers in flyash
Aluminium oxide is 1 with the sulfuric acid molar ratio in the concentrated sulfuric acid:2.5~1:5, aluminium oxide is 1 with the carbon containing molar ratio of reducing agent:1.5
~1:5.
6. according to the method described in claim 5, it is characterized in that, it is allowed to contain a certain amount of moisture in flyash, its moisture allows
Content is limited with the h 2 so 4 concentration after mixed ingredients not less than 70%.
7. according to the method described in claim 1, it is characterized in that, the firing temperature of roasting is 850 DEG C~1200 in step (1)
℃。
8. according to the method described in claim 1, it is characterized in that, step (1) in roasting equipment use rotary kiln, burn till temperature
Degree 900~1100 DEG C, control rotary kiln in material programming rate, ensure material 100 DEG C~250 DEG C sections residence time >=
30min, preferably residence time >=30min in 120 DEG C~200 DEG C sections.
9. according to the method described in claim 1, it is characterized in that low-temperature alkaline described in step (2) extraction take silicon, be to reduce
Calcining Na2The sodium hydroxide solution of 50~150g/L of O concentration leaches silicon, leaches solid-liquid mass ratio 1:3~1:25, extraction temperature
50~100 DEG C, 30~240min of extraction time.
10. according to the method described in claim 1, it is characterized in that high-temperature alkali described in step (3) extraction take aluminium, be by high alumina
Slag Na2The sodium hydroxide solution of 150~300g/L of O concentration leaches aluminium, leaches solid-liquid mass ratio 1:3~1:20, lime addition
Measure as the 0~15% of high alumina slag quality, 150~300 DEG C of extraction temperature, 15~120min of extraction time.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110404936A (en) * | 2019-07-30 | 2019-11-05 | 江苏省沙钢钢铁研究院有限公司 | Comprehensive treatment method for semi-dry desulfurized fly ash |
CN112095017A (en) * | 2020-09-15 | 2020-12-18 | 中南大学 | Method for recycling fly ash based on reduction roasting-acid leaching |
CN113376194A (en) * | 2021-05-25 | 2021-09-10 | 中国铝业股份有限公司 | X-ray fluorescence melting sample preparation method for aluminum nitride |
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CN104445312A (en) * | 2014-10-30 | 2015-03-25 | 北京矿冶研究总院 | Method for extracting aluminum oxide by synergistic treatment of fly ash and coal gangue |
CN104787790A (en) * | 2015-04-17 | 2015-07-22 | 北京矿冶研究总院 | Method for extracting aluminum oxide and silicon oxide from coal-based solid waste |
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CN104445312A (en) * | 2014-10-30 | 2015-03-25 | 北京矿冶研究总院 | Method for extracting aluminum oxide by synergistic treatment of fly ash and coal gangue |
CN104787790A (en) * | 2015-04-17 | 2015-07-22 | 北京矿冶研究总院 | Method for extracting aluminum oxide and silicon oxide from coal-based solid waste |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110404936A (en) * | 2019-07-30 | 2019-11-05 | 江苏省沙钢钢铁研究院有限公司 | Comprehensive treatment method for semi-dry desulfurized fly ash |
CN112095017A (en) * | 2020-09-15 | 2020-12-18 | 中南大学 | Method for recycling fly ash based on reduction roasting-acid leaching |
CN112095017B (en) * | 2020-09-15 | 2021-10-22 | 中南大学 | Method for recycling fly ash based on reduction roasting-acid leaching |
CN113376194A (en) * | 2021-05-25 | 2021-09-10 | 中国铝业股份有限公司 | X-ray fluorescence melting sample preparation method for aluminum nitride |
CN113376194B (en) * | 2021-05-25 | 2023-09-12 | 中国铝业股份有限公司 | X-ray fluorescence melting sample preparation method of aluminum nitride |
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