CN107500325B - A kind of gangue produces nano alumina powder jointed method - Google Patents
A kind of gangue produces nano alumina powder jointed method Download PDFInfo
- Publication number
- CN107500325B CN107500325B CN201710991217.7A CN201710991217A CN107500325B CN 107500325 B CN107500325 B CN 107500325B CN 201710991217 A CN201710991217 A CN 201710991217A CN 107500325 B CN107500325 B CN 107500325B
- Authority
- CN
- China
- Prior art keywords
- gangue
- hydrochloric acid
- powder
- minutes
- alumina powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/441—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by calcination
-
- 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
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/08—Preparation by working up natural or industrial salt mixtures or siliceous minerals
-
- 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
- C01F7/22—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with halides or halogen acids
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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
Abstract
A kind of gangue produces nano alumina powder jointed method, includes the following steps: that gangue is handled the gangue powder to roast after powder, after being activated by (1)；(2) it is separated by solid-liquid separation after step (1) products therefrom being carried out hydro-thermal auxiliary acidleach processing with hydrochloric acid；(3) sodium hydroxide solution is added dropwise to liquid obtained by step (2) and is equal to 13~14 to pH, be separated by solid-liquid separation；(4) a small amount of hydrochloric acid is added into filtrate obtained by step (3) and is equal to 10~11 to pH, a small amount of soluble starch solution is then added dropwise, adds ammonium bicarbonate soln to pH and is equal to 7~8, washing sintering obtains Nano-sized Alumina Powder after separation.Method of the invention, which is compared with other methods, has that low energy consumption, and level of residue is few, the high feature of nano oxidized Al extraction efficiency, while the theory of resources circulation and environmental protection is realized in whole process, opens new method for the comprehensive utilization of gangue.
Description
Technical field
The comprehensive benefit for the solid waste discharged the invention belongs to generate electricity, in metallurgy, derived energy chemical synthetic production process
It is with technical field, in particular to a kind of that nano alumina powder jointed method is produced using gangue.
Background technique
Gangue refers to the solid waste and available resource generated during coal mining, dressing of coal by washing, tool
There is duality.Its main component is Al2O3、SiO2, in addition also contain Fe in varying numbers2O3、CaO、MgO、Na2O、K2O、P2O5、
SO3With micro rare element (gallium, vanadium, titanium, cobalt etc.).
From the point of view of coal mining, 100,000,000 tons of coals of Chinese every production discharge 14,000,000 tons of spoil or so；From coal washing plus
From the point of view of work, 100,000,000 tons of coking coals of every washing discharge 20,000,000 tons of spoil amount, often wash 100,000,000 tons of thermal coals, discharge spoil amount 15,000,000
Ton.A large amount of stackings of gangue, not only cover soil, influence ecological environment, and gangue leaching water will pollute surrounding soil and ground
It is lauched, and contains certain combustible in gangue, spontaneous combustion can occur under certain conditions, discharge sulfur dioxide, nitrogen oxygen
The pernicious gases such as compound, oxycarbide and flue dust pollute atmospheric environment, influence the health of Residents in Mining Area.
Just because of above-mentioned reason, processing and comprehensive utilization of resources to gangue are always by national height weight
Depending on.At present the main Land use systems of gangue be building materials, backfill, power generation, etc. application and part high-tech content, height
The Technology of Comprehensive Utilization of Coal Gangue and product of added value.It, can be with according to the composition of spoil due to containing a large amount of aluminium in gangue
For producing the products such as white carbon black, aluminium oxide, new industry chain of circular economy is formed, most important one product is aluminium oxide.
Currently, extracting the process of aluminium hydroxide powder using gangue mainly includes limestone sintering process, soda lime sintering process, acid
Leaching method, solubilization of microwave method, combination method etc..
A kind of nano alumina powder jointed process, this method are extracted with gangue as CN 101209849A is disclosed
It is that original gangue is crushed, is levigate to certain particle size, in high-temperature roasting certain time, takes certain density hydrochloric acid that bastard coal is added
Stone is configured to the mixed liquor of certain solid-to-liquid ratio, is then separated by solid-liquid separation with centrifuge to it to get Al is arrived2O3.This method is not
Iron is removed by magnetic separator, when reaction will increase the consumption of hydrochloric acid, and obtained nano alumina powder jointed purity is not high.
CN 101450811A discloses a kind of gangue and extracts nano alumina powder jointed method, and this method is by bastard coal
It is calcined after mountain flour mill, except iron, is reacted with acid, obtain low temperature calcination after condensing crystallizing containing aluminum solutions, thick nano oxygen is made
Change aluminium powder body, then slightly nano alumina powder jointed will be reacted with sodium hydroxide, obtains sodium metaaluminate mother liquor, remove de-iron, titanium impurity, to
Aluminium hydroxide powder crystal seed is added in mother liquor and is passed through carbon dioxide gas and carries out kind point, obtains aluminium hydroxide powder precipitating,
It is nano alumina powder jointed that metallurgical grade is obtained by calcining.In addition this method complex operation is passed through carbon dioxide gas tune
It is not easy to control to save pH, the iron oxide etc. of removing not can be carried out resource utilization.
CN 101759209A disclose it is a kind of extracted from gangue it is nano alumina powder jointed with silica gel production method,
This method takes calcination activation, leaching to be separated by filtration, carbon point, sodium carbonate and water recycling, sial separation, pyrolysis, HCl recovery etc.
Step obtains nano alumina powder jointed and silica gel.This method is easy agglomeration when gangue and sodium carbonate are baking mixed, so that instead
It should be incomplete.In addition in H2SiO3With Al (OH)3Hydrochloric acid is added in mixture, is filtered after reaction, obtained AlCl3Solution is impure,
Silica obtained purity is not high.
CN 102180493A, which is disclosed, a kind of produces nano alumina powder jointed method with gangue.The main work of this method
Skill process is, after broken gangue and caustic soda are mixed in a certain ratio grinding, then passes through calcination activation, circulation leaching
It takes, precipitate filtering, calcining, auxiliary agent, washing and calcining, extract high purity nanometer alumina powder product.This method does not have
There is the processing problem in view of filter residue sodium metasilicate, in addition circulation leaching technology is complicated for operation used in this method and is difficult to obtain
High-purity alpha-alumina.
Summary of the invention
For this purpose, producing nano alumina powder jointed new method the object of the present invention is to provide a kind of gangue, this method is mentioned
High nano alumina powder jointed recovery rate.
In order to achieve the above object, the present invention adopts the following technical scheme:
A kind of gangue produces nano alumina powder jointed method, includes the following steps:
(1) gangue is handled to the gangue powder to roast after powder, after being activated；
(2) it is separated by solid-liquid separation after step (1) products therefrom being carried out hydro-thermal auxiliary acidleach processing with hydrochloric acid；
(3) sodium hydroxide solution is added dropwise to liquid obtained by step (2) and is equal to 13~14 to pH, at this time the iron in filtrate, magnesium
Plasma precipitates completely, and aluminium ion is dissolved among solution, forms meta-aluminic acid radical ion, is separated by solid-liquid separation；
(4) a small amount of hydrochloric acid is added into filtrate obtained by step (3) and is equal to 10~11 to pH, a small amount of solubility is then added dropwise and forms sediment
Powder solution adds ammonium bicarbonate soln to pH and is equal to 7~8, it is heavy that cotton-shaped aluminium hydroxide can be obtained to stable dispersion system
It forms sediment, washing sintering obtains Nano-sized Alumina Powder after separation.
The present invention adjusts pH by adding sodium hydroxide solution in filtrate containing aluminium, removes iron therein, magnesium plasma, from
And it overcomes in the prior art except the disadvantage that iron is not complete and magnetic separator iron removal is cumbersome.It is assisted using hydro-thermal this mild
Condition, hydrochloric acid acidification is energy saving by desilication, while reducing the generation of other wastes, instead of gangue with
NaOH mixture is sintered jointly generates sodium aluminosilicate (Na2O·Al2O3·2SiO2), to overcome sintering temperature height, Al2O3It mentions
Take the shortcoming that rate is low.Nano alumina powder jointed, energy consumption and the life in gangue are extracted using the mild method of hydro-thermal auxiliary
It produces cost to be effectively reduced, to for Technique Popularizing of the invention and realize that solid economic technology base has been established in industrialization
Plinth.
It is an object of the invention to overcome existing gangue to extract, nano alumina powder jointed technical process is many and diverse, equipment requirement
The disadvantages of height, high production cost, impure product.Basic fundamental approach of the invention is: cleaned using gangue as primary raw material
Drying, crushing and grinding, calcining and activating assist hydrochloric acid acidification using hydro-thermal, and filter residue can be used for extracting white carbon black, in filtrate
Carry out the enrichment of aluminium.Carrying out suitable pH adjusting to filtrate precipitates the Fe in gangue completely, by filtration treatment, in filtrate
Soluble starch is added, stirring in water bath can be cooperateed with, suitable ph is adjusted by ammonium bicarbonate soln, it is heavy to obtain aluminium hydroxide powder
It forms sediment, is obtained by calcine technology nano alumina powder jointed.Filtrate can be dried in the process, evaporative crystallization realizes by-product
The recycling of object sodium chloride.
Method of the invention be compared with other methods have low energy consumption, level of residue is few, the high spy of nano oxidized Al extraction efficiency
Point, while the theory of resources circulation and environmental protection is realized in whole process, new method is opened for the comprehensive utilization of gangue.
Preferably, in step (1) powder be 75 microns hereinafter, for example, 65 microns, 60 microns, 52 microns, 40 microns,
30 microns, 10 microns etc..
Preferably, the temperature of roasting is 800~900 DEG C, and the time is 60 minutes or more, preferably 120~180 minutes.
Gangue is preferably using Huainan, Anhui gangue as primary raw material.Gangue can be handled by using jaw crusher
For powder.
Preferably, in step (2) gangue and hydrochloric acid mass ratio 1:2~6, preferably 1:3~4, the volume of hydrochloric acid
Score is 10-40%, preferably 20%.
Preferably, the temperature of acidleach is 180~200 DEG C, and the time is 60 minutes or more, preferably 120 minutes~150 points
Clock.
Preferably, the filter residue after separation of solid and liquid can extract white carbon black.
In step (3) molar concentration of sodium hydroxide solution can be 1~3mol/L, preferably 1.5~2.5mol/L, preferably
It is added dropwise.Progress can be stirred under 90 DEG C of water bath conditions by being added when adjusting pH.
Preferably, the mass fraction of hydrochloric acid is 10~40% in step (4).
Preferably, the volume fraction of soluble starch solution is 0.5~2%, preferably 1%.
Preferably, soluble starch solution dripping quantity is 3~10 drops, preferably 5~8 drops.
Preferably, ammonium bicarbonate soln molar concentration is 0.5~2mol/L, preferably 0.5~1.5mol/L.
Ammonium bicarbonate soln can cooperate with stirring in water bath to be added under the conditions of 90 DEG C.
Soluble starch solution manufacturing method can are as follows: weighs 0.5~2g soluble starch and is put into small beaker, adds water
10mL stirs into paste and pours into 90mL boiling water, slightly boiled 2 minutes, is transferred to after cooling spare in 100mL reagent bottle.
Sodium chloride can be recycled in liquid after separation of solid and liquid.
Preferably, the temperature of sintering is 350~500 DEG C, and sintering time is 100 minutes or more, preferably 150~180 points
Clock.
It washs and distilled water can be used to carry out.It can be pre-dried before sintering.
Being separated by solid-liquid separation in the present invention can be carried out by the common methods such as filtering, being centrifuged, such as be carried out using centrifuge, such as logical
Cross supercentrifuge separation.
Preferably, production method of the present invention includes the following steps:
(1) crushing grinding: using coal gangue as raw material, washing and drying is carried out, is handled using jaw crusher crushing, through sieving
Get the following gangue powder of 200 mesh；
(2) high-temperature roasting: control temperature roasts under the conditions of 800~900 DEG C, and calcining time is 120~180 minutes, obtains
Gangue powder after to activation；
(3) hydro-thermal auxiliary acidleach processing: take gangue: the mass ratio that hydrochloric acid solution is 1:3~1:4 carries out acidleach, water
Hot auxiliary temperature is 180~200 DEG C, and the time is 2 hours, is separated after obtaining turbid solution using supercentrifuge；
(4) filter residue proposes silicon processing: obtained filter residue can carry out subsequent operation, extract white carbon black；
(5) sodium hydroxide solution iron, magnesium removal of impurities: is added dropwise in the filtrate obtained by step (3) dropwise to pH equal to 13~14, together
When stir, the iron in filtrate, magnesium plasma precipitate completely at this time, are separated by solid-liquid separation using centrifuge, aluminium ion is dissolved in molten
Among liquid, meta-aluminic acid radical ion is formed；
(6) a small amount of hydrochloric acid washing of precipitate: is added in the filtrate obtained by step (5) to pH equal to 10~11；It is added dropwise again a small amount of
Soluble starch solution ammonium bicarbonate soln is added in stirring in water bath to pH and is equal to 7~8 to stable dispersion system,
Cotton-shaped aluminum hydroxide precipitation can be obtained, while recycling sodium chloride；It is centrifuged to obtain filter residue through supercentrifuge, filter paper is placed on
In funnel, washing is filtered to filter residue with distilled water, just obtains aluminium-hydroxide powder after drying in air dry oven,
It is sintered 150~180 minutes at a temperature of 350~500 DEG C and obtains Nano-sized Alumina Powder.
It is provided by the invention that nano alumina powder jointed method is extracted from gangue, using gangue as primary raw material, warp
Cleaning, drying, crushing and grinding, calcining and activating, hydro-thermal auxiliary carry out acidification, filter residue for extracting white carbon black, in filtrate into
The enrichment of row aluminium.Carrying out pH adjusting to filtrate precipitates the Fe in gangue completely, and by centrifugal treating, being added in filtrate can
Soluble starch keeps dispersion to stablize as dispersing agent to be easily formed cotton-shaped product suspension.Stirring state is assisted in hydro-thermal
Under, ammonium bicarbonate soln is added dropwise dropwise can obtain cotton-shaped aluminum hydroxide precipitation, obtain high-purity nano oxygen by calcine technology
Change aluminium powder body.The recycling of sodium chloride can be realized in the process.This method be compared with other methods have low energy consumption, level of residue
It is few, the high feature of nano oxidized Al extraction efficiency, while the theory of resources circulation and environmental protection is realized in whole process, it is gangue
Comprehensive utilization open new method.The present invention can both make this solid waste of gangue obtain sufficiently beneficial benefit
With, and can solve the status of China's alumina scarcity of resources, significant contribution is made that for industrialized production.In addition, this method gram
It is big the nano alumina powder jointed difficulty of traditional gangue extraction is taken, the not high disadvantage of recovery rate.Meanwhile hard charcoal is extracted to gangue
Black method also provides method and reference significance.
Detailed description of the invention
Fig. 1 is that the hydro-thermal auxiliary gangue of one embodiment of the invention extracts the process flow of nano alumina powder jointed method
Figure；
Fig. 2 is the XRD spectrum for the aluminium hydroxide powder that 1 hydro-thermal of embodiment assists gangue to extract；
Fig. 3 is the XRD spectrum of alumina powder after 450 DEG C of calcinings in embodiment 2；
Fig. 4 is TEM photo nano alumina powder jointed after 450 DEG C of calcinings in embodiment 2.
Specific embodiment
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Fig. 1 is one embodiment of the present of invention, i.e., high purity nanometer alumina powder and white carbon black are extracted from gangue
Process flow chart.
Embodiment 1
Washing and drying is carried out to gangue, it is screened to obtain 75 microns of bastard coals below using jaw crusher crushing
Stone powder.Gangue powder is placed in Muffle furnace and is sintered, for control temperature at 850 DEG C, the time is 120 minutes, after obtaining activation
Gangue powder.Gangue 70g is taken, mass fraction is that 20% hydrochloric acid is 210ml, and it is anti-that mixing is placed on hydro-thermal in 30 minutes
It answers and carries out acidleach in kettle, under the action of hydro-thermal auxiliary, controlled at 180 DEG C, the time is 2 hours, obtains turbid solution progress
Centrifuge separation.
Sodium hydroxide solution is added dropwise dropwise in filtrate to be equal to 13.05 to pH and stir, at this time the iron in filtrate, magnesium ion
Precipitating, aluminium ion are dissolved among solution completely.Be added a small amount of mass fraction be 20% hydrochloric acid to pH be equal to 10.55,90
The soluble starch solution that 5 drop volume scores are 1%, the agitated ammonium bicarbonate soln that 1mol/L is added are added dropwise in DEG C water-bath
It is equal to 7.95 to pH, aluminium hydroxide powder precipitating can be obtained, while recycling sodium chloride；It is just obtained through filtration washing drying and processing
Aluminium-hydroxide powder, XRD spectrum at 20 ° with 40 ° of left-right position main peaks as shown in Figure 1, coincide preferably, it can be seen that obtains
For aluminium hydroxide powder not with the presence of impurity phase, quality is higher.It is sintered 180 minutes at a temperature of 450 DEG C and obtains high-purity nano oxygen
Change aluminium powder body.
By measurement, nano alumina powder jointed purity is 96.43%, average grain diameter 23nm, and extraction rate is
84.86%.
Embodiment 2
Washing and drying is carried out to gangue, it is screened to obtain 75 microns of bastard coals below using jaw crusher crushing
Stone powder.Gangue powder is placed in Muffle furnace and is sintered, for control temperature at 850 DEG C, the time is 120 minutes, after obtaining activation
Gangue powder.Gangue 70g is taken, volume fraction is that 30% hydrochloric acid is 210ml, and it is anti-that mixing is placed on hydro-thermal in 30 minutes
It answers and carries out acidleach in kettle, under the action of hydro-thermal auxiliary, controlled at 140 DEG C, the time is 2 hours, obtains turbid solution progress
Centrifuge separation.
Sodium hydroxide solution is added dropwise dropwise in filtrate to be equal to 13.90 to pH and stir, at this time the iron in filtrate, magnesium ion
Precipitating, aluminium ion are dissolved among solution completely.Be added a small amount of mass fraction be 20% hydrochloric acid to pH be equal to 10.97,90
The soluble starch solution that 5 drop volume scores are 1%, the agitated ammonium bicarbonate soln that 1mol/L is added are added dropwise in DEG C water-bath
It is equal to 7.95 to pH, aluminium hydroxide powder precipitating can be obtained, while recycling sodium chloride；It is just obtained through filtration washing drying and processing
The XRD spectrum of aluminium-hydroxide powder, alumina powder is as shown in Figure 3, it can be seen that and alumina powder crystalline condition is good,
450 DEG C of calcinings obtain aluminium oxide not with the presence of impurity phase, and aluminium oxide characteristic diffraction peak significantly wideization.In 450 DEG C of temperature
Lower sintering obtains high-purity nano alumina powder in 180 minutes, and nano alumina powder jointed TEM photo is as shown in Figure 4 after calcining.
As shown in Figure 4: the crystallite dimension of alumina powder is about 20nm~30nm.
By measurement, nano alumina powder jointed purity is 97.29%, average grain diameter 21nm, and extraction rate is
74.08%.
Embodiment 3
Washing and drying is carried out to gangue, it is screened to obtain 75 microns of bastard coals below using jaw crusher crushing
Stone powder.Gangue powder is placed in Muffle furnace and is sintered, for control temperature at 850 DEG C, the time is 120 minutes, after obtaining activation
Gangue powder.Gangue 70g is taken, volume fraction is that 40% hydrochloric acid is 210ml, and it is anti-that mixing is placed on hydro-thermal in 30 minutes
It answers and carries out acidleach in kettle, under the action of hydro-thermal auxiliary, controlled at 180 DEG C, the time is 2 hours, obtains turbid solution progress
Centrifuge separation.
Sodium hydroxide solution is added dropwise dropwise in filtrate to be equal to 13.55 to pH and stir, at this time the iron in filtrate, magnesium ion
Precipitating, aluminium ion are dissolved among solution completely.Be added a small amount of mass fraction be 30% hydrochloric acid to pH be equal to 10.87,90
The soluble starch solution that 5 drop volume scores are 1% is added dropwise in DEG C water-bath, the agitated ammonium hydrogen carbonate that 1.5mol/L is added is molten
Liquid is equal to 7.62 to pH, aluminium hydroxide powder precipitating can be obtained, while recycling sodium chloride；Just through filtration washing drying and processing
To aluminium hydroxide powder, it is sintered 180 minutes at a temperature of 450 DEG C and obtains high-purity nano alumina powder.
By measurement, nano alumina powder jointed purity is 97.01%, average grain diameter 25nm, and extraction rate is
72.03%.
Embodiment 4
Washing and drying is carried out to gangue, it is screened to obtain 75 microns of bastard coals below using jaw crusher crushing
Stone powder.Gangue powder is placed in Muffle furnace and is sintered, for control temperature at 800 DEG C, the time is 100 minutes, after obtaining activation
Gangue powder.Gangue 70g is taken, volume fraction is that 10% hydrochloric acid is 100ml, and it is anti-that mixing is placed on hydro-thermal in 30 minutes
It answers and carries out acidleach in kettle, under the action of hydro-thermal auxiliary, controlled at 180 DEG C, the time is 2 hours, obtains turbid solution progress
Centrifuge separation.
Sodium hydroxide solution is added dropwise dropwise in filtrate to be equal to 13.25 to pH and stir, at this time the iron in filtrate, magnesium ion
Precipitating, aluminium ion are dissolved among solution completely.Be added a small amount of mass fraction be 30% hydrochloric acid to pH be equal to 10.21,90
The soluble starch solution that 5 drop volume scores are 1%, the agitated ammonium bicarbonate soln that 2mol/L is added are added dropwise in DEG C water-bath
It is equal to 7.42 to pH, aluminium hydroxide powder precipitating can be obtained, while recycling sodium chloride；It is just obtained through filtration washing drying and processing
Aluminium hydroxide powder is sintered 150 minutes at a temperature of 450 DEG C and obtains high-purity nano alumina powder.
By measurement, nano alumina powder jointed purity is 95.57%, average grain diameter 27nm, and extraction rate is
65.36%.
Embodiment 5
Washing and drying is carried out to gangue, it is screened to obtain 50 microns of bastard coals below using jaw crusher crushing
Stone powder.Gangue powder is placed in Muffle furnace and is sintered, for control temperature at 850 DEG C, the time is 120 minutes, after obtaining activation
Gangue powder.Gangue 70g is taken, volume fraction is that 30% hydrochloric acid is 300ml, and it is anti-that mixing is placed on hydro-thermal in 30 minutes
Answer and carry out acidleach in kettle, under the action of hydro-thermal auxiliary, controlled at 190 DEG C, the time is 150 minutes, obtain turbid solution into
Row centrifuge separation.
Sodium hydroxide solution is added dropwise dropwise in filtrate to be equal to 13.22 to pH and stir, at this time the iron in filtrate, magnesium ion
Precipitating, aluminium ion are dissolved among solution completely.Be added a small amount of mass fraction be 20% hydrochloric acid to pH be equal to 10.71,90
The soluble starch solution that 5 drop volume scores are 1%, the agitated ammonium bicarbonate soln that 2mol/L is added are added dropwise in DEG C water-bath
It is equal to 7.92 to pH, aluminium hydroxide powder precipitating can be obtained, while recycling sodium chloride；It is just obtained through filtration washing drying and processing
Aluminium hydroxide powder is sintered 100 minutes at a temperature of 500 DEG C and obtains high-purity nano alumina powder.
By measurement, nano alumina powder jointed purity is 96.82%, average grain diameter 23nm, and extraction rate is
82.19%.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (13)
1. a kind of gangue produces nano alumina powder jointed method, include the following steps:
(1) gangue is handled to the gangue powder to roast after powder, after being activated；
(2) it is separated by solid-liquid separation after step (1) products therefrom being carried out hydro-thermal auxiliary acidleach processing with hydrochloric acid；
(3) sodium hydroxide solution is added dropwise to liquid obtained by step (2) and is equal to 13~14 to pH, be separated by solid-liquid separation；
(4) a small amount of hydrochloric acid is added into filtrate obtained by step (3) and is equal to 10~11 to pH, it is molten that a small amount of soluble starch is then added dropwise
Liquid adds ammonium bicarbonate soln to pH and is equal to 7~8, and washing sintering obtains Nano-sized Alumina Powder after separation.
2. the method according to claim 1, wherein powder is 75 microns or less in step (1).
3. the method according to claim 1, wherein step (1) in roast temperature be 800~900 DEG C, the time
It is 60 minutes or more.
4. according to the method described in claim 3, it is characterized in that, the time of roasting is 120~180 minutes.
5. method according to claim 1-4, which is characterized in that the quality of gangue and hydrochloric acid in step (2)
Than 1:2~6, the mass fraction of hydrochloric acid is 10-40%.
6. according to the method described in claim 5, it is characterized in that, in step (2) mass ratio of gangue and hydrochloric acid be 1:3~
4, the mass fraction of hydrochloric acid is 20%.
7. method according to claim 1-4, which is characterized in that in step (2) temperature of acidleach be 180~
200 DEG C, the time is 60 minutes or more.
8. the method according to the description of claim 7 is characterized in that the time of acidleach is 120 minutes~150 points in step (2)
Clock.
9. method according to claim 1-4, which is characterized in that the filter residue after being separated by solid-liquid separation in step (2) mentions
Take white carbon black.
10. method according to claim 1-4, which is characterized in that the mass fraction of hydrochloric acid is 10 in step (4)
~40%；
The volume fraction of soluble starch solution is 0.5~2%；
Soluble starch solution dripping quantity is 3~10 drops；
Ammonium bicarbonate soln molar concentration is 0.5~2mol/L.
11. according to the method described in claim 10, it is characterized in that, the mass fraction of hydrochloric acid is 10~40% in step (4)；
The volume fraction of soluble starch solution is 1%；
Soluble starch solution dripping quantity is 5~8 drops；
Ammonium bicarbonate soln molar concentration is 0.5~1.5mol/L.
12. method according to claim 1-4, which is characterized in that the temperature being sintered in step (4) is 350~
500 DEG C, sintering time is 100 minutes or more.
13. according to the method for claim 12, which is characterized in that sintering time is 150~180 minutes in step (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710991217.7A CN107500325B (en) | 2017-10-23 | 2017-10-23 | A kind of gangue produces nano alumina powder jointed method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710991217.7A CN107500325B (en) | 2017-10-23 | 2017-10-23 | A kind of gangue produces nano alumina powder jointed method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107500325A CN107500325A (en) | 2017-12-22 |
| CN107500325B true CN107500325B (en) | 2019-02-15 |
Family
ID=60700719
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710991217.7A Active CN107500325B (en) | 2017-10-23 | 2017-10-23 | A kind of gangue produces nano alumina powder jointed method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107500325B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109019646A (en) * | 2018-08-28 | 2018-12-18 | 太原理工大学 | A method of Aluminum sol is prepared using gangue |
| CN113461030A (en) * | 2021-07-30 | 2021-10-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for synergistically and deeply removing Al, Mg, Ca, Ti and carbonate in NaCl brine recovered from chlorination residues |
| CN113860780B (en) * | 2021-11-04 | 2022-08-09 | 福州大学 | Preparation method of high-activity spherical calcined coal gangue powder |
| CN114014329B (en) * | 2021-12-10 | 2023-08-29 | 黑龙江省能源环境研究院 | Method for preparing white carbon black by utilizing coal gangue ash low-temperature roasting hydrothermal combined activation method |
| CN114849643A (en) * | 2022-04-27 | 2022-08-05 | 西安建筑科技大学 | Coal gangue-based porous material taking actinomycetes as template and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101209849A (en) * | 2007-12-22 | 2008-07-02 | 河南理工大学 | Novel technique for extracting aluminum oxide from coal gangue |
| CN101450811A (en) * | 2008-10-23 | 2009-06-10 | 长春市超威新材料科技有限公司 | Method for extracting alumina from coal gangue |
| CN101850998A (en) * | 2010-06-18 | 2010-10-06 | 长春市超威新材料科技有限公司 | Method for co-producing aluminum oxide and sodium carbonate from coal gangue |
| CN105712385B (en) * | 2016-04-14 | 2018-02-27 | 王嘉兴 | A kind of preparation method of aluminium hydroxide |
-
2017
- 2017-10-23 CN CN201710991217.7A patent/CN107500325B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN107500325A (en) | 2017-12-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107500325B (en) | A kind of gangue produces nano alumina powder jointed method | |
| CN100584764C (en) | Method for reclaiming ferric oxide from coal ash and coal gangue | |
| CN103121700B (en) | Method for preparing ultrafine alumina and coproducing and white carbon black by utilizing coal series kaolin | |
| CN107326182A (en) | High-value comprehensive utilization method for red mud | |
| CN106745027B (en) | A kind of method of flyash synthesis analcime | |
| CN108941167A (en) | Mechanochemistry conversion and recovery method in a kind of waste cathode of aluminum electrolytic cell carbon block containing sodium, fluorochemical | |
| CN109336116A (en) | A method of photovoltaic high purity quartz emery dust is prepared containing feldspar ore type quartzite | |
| CN104445313A (en) | Method for extracting aluminum oxide from fly ash by acid-base combination | |
| CN102153070A (en) | Method for purifying calcined petroleum coke | |
| CN106745128A (en) | A kind of method of aluminium lime-ash removal of impurities | |
| CN103031443A (en) | Method of dealkalizing red mud and recovering aluminum and iron | |
| CN111792650A (en) | Full-element recycling process of coal ash or coal gangue by hot-melt salt method | |
| CN103420386A (en) | Method for preparing silica through coal gangue aluminum extraction waste slag | |
| CN103738972B (en) | A kind of residue of aluminum-extracted pulverized fuel ash prepares the method for silicon powder | |
| CN113233482A (en) | Secondary aluminum ash resource utilization method | |
| CN105197973B (en) | Method of utilizing low-quality bauxite to prepare aluminum oxide | |
| CN101306819B (en) | Process for abstracting white carbon black from fly ash or slag | |
| CN1257292C (en) | Method for recovering nickel and aluminum from waste aluminum based nickel-containing catalyst | |
| CN112095017B (en) | Method for recycling fly ash based on reduction roasting-acid leaching | |
| CN103864086A (en) | Method of producing borax by utilizing boron-rich slag | |
| WO2014047767A1 (en) | Method for producing nanometer lithopone from electrolytic zinc acid leaching residue | |
| CN103408050B (en) | Method of efficient extraction of aluminum, iron, and titanium in coal gangue | |
| CN105668597B (en) | The method of flyash soda acid combined extracting aluminium base product and silica-based products | |
| CN106698490B (en) | A kind of method that aluminium predecessor is prepared from flyash and its prepares nano aluminium oxide | |
| CN103342376B (en) | Process for extracting valuable metal from coal gangues |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |