CN107855105A - The method of porous beads and obtained porous beads are prepared using coal gasification fine slag - Google Patents
The method of porous beads and obtained porous beads are prepared using coal gasification fine slag Download PDFInfo
- Publication number
- CN107855105A CN107855105A CN201710157813.5A CN201710157813A CN107855105A CN 107855105 A CN107855105 A CN 107855105A CN 201710157813 A CN201710157813 A CN 201710157813A CN 107855105 A CN107855105 A CN 107855105A
- Authority
- CN
- China
- Prior art keywords
- acid
- slurry
- coal gasification
- fine slag
- gasification fine
- 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.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D24/00—Filters comprising loose filtering material, i.e. filtering material without any binder between the individual particles or fibres thereof
- B01D24/001—Making filter elements not provided for elsewhere
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
- B01J20/28073—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being in the range 0.5-1.0 ml/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Processing Of Solid Wastes (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of molten method for preparing porous beads of coal gasification fine slag acid, methods described includes：A. appropriate coal gasification fine slag is taken, adds water to prepare the coal gasification fine slag slurry for being contained in 10 30wt% admittedly；B. the slurry of step a configurations is sufficiently stirred, afterwards by gravity cyclonic separation, collects heavy separation product and obtain the compound slurry of Silicon-rich；C. appropriate acid solution and the Silicon-rich composite mortar are mixed to get mixed slurry, carry out the molten reaction of acid；D. separation of solid and liquid is carried out to the material after the molten reaction of acid, and washs, dries, obtain product；The invention also discloses the composite porous material being prepared.The present invention utilizes the high activity of sial calcium irony in coal gasification fine slag, regulate and control dissolution in a mild condition and obtain porous material, the material has good physics, chemisorbed performance, preparation technology is simple, cost is cheap, the metal ion of dissolution can further prepare water purification agent, realize the full constituent comprehensive utilization of coal gas slugging, turn waste into wealth.
Description
Technical field
The invention belongs to the technical field that solid waste resource recovery utilizes, the more particularly to a kind of molten system of coal gasification fine slag acid
The method of standby porous beads, and the porous material being prepared.
Background technology
Coal Gasification Technology is one of core content of clean coal technology, and coal is carried out into incomplete oxidation to obtain being available for downstream
Utilize can coal-fired gasification gas (such as raw gas), in recent years quickly as the important directions of coal resources and using energy source.Closely
Over 20 years, China has built one more in Yulin, Ordos, inner Mongolia, Shanxi Changzhi, the quasi- east in Xinjiang, Yi Li etc.
Coal chemical industry enterprises are criticized, are gone into operation successively, yield increases year by year, and the clean comprehensive utilization of coal resources forms a set pattern in China
Mould.
In Coal Gasification Technology system, by while carbonaceous part is largely converted into gas in coal, association in raw coal
Thoroughly remaining carbonaceous can not arranged in the form of residue (coal gas slugging) for inorganic mineral components, the catalyst added and gasification
Go out.Because discharging the difference of mode, coal gas slugging is divided into thick slag and fine slag again, wherein, the thick slag refers to via coal gasifier
The residue of furnace bottom discharge, and fine slag refers to be carried secretly by coal gasification gas and in the purification process after coal gasification gas leaves coal gasifier
Separate the residue of discharge.The yield of coal gasification residue with the development of Chemical Industry, increase quickly, land occupation during stacking,
Environment is polluted, has become new solid waste urgently to be resolved hurrily.
In recent years, the utilization around coal chemical industry slag started the concern for causing some scholars.The disclosures of CN 201510148929.3
A kind of light ceramic prepared using the gentle slugging of flyash and its methods and applications processed, are described and utilize flyash and gasification
Slag prepares light ceramic and its preparation method；CN 201510420421.4 disclose it is a kind of be used to producing the composition of ceramic for filtration with
And ceramic for filtration and its preparation method and application, describe the method for preparing ceramic for filtration using the slag that gasifies for key component；CN
201310207509.9 disclose the method that activation coal gasification lime-ash realizes the separation of ferro-aluminum calcium, describe and dry coal gas slugging
Afterwards, chilling obtains activated material after being calcined at 700 to 1100 DEG C 75 minutes, then by activated material and hydrochloric acid solution or sulfuric acid solution
Reaction, aluminium, iron, Calcium compounds separation are realized, and the calorific value of carbon residue in coal gasification lime-ash can be utilized；CN
201210511610.9 disclose a kind of processing method of coal chemical industry gasification slag, describe after the gentle slugging of coal slime uniformly mixing
Clay wash is added, using high-pressure pump pipe conveying technology, mixture is transported in the fluidized-bed combustion boiler stove outside hundreds of meters, is led to
Cross the utilization of burning again that fluidized-bed combustion boiler combustion technology realizes gasification slag；Shenhua Ningxia Coal Industry Group Co., Ltd. Yang Shuai and
Shi Lijun is in August, 2013《Coal chemical industry》On publish an article, describe Shenhua Ningxia Coal Industry Group Co., Ltd .'s coal chemical industry
Various oxide component contents and loss on ignition in 3 kinds of coal gasification fine slags of output, with reference to total utilization of PCA national standard and
Professional standard, cement, concrete and road foundation blend composition etc. are used for coal gasification fine slag and has carried out feasibility analysis, is proposed
Coal gasification fine slag, which mixes to burn, to be utilized and suggestion that sorting utilizes；Liu Ziliang etc., both at home and abroad using being summarized, wraps to gasification slag
Include in sewage disposal, build the road, applied in non-burning brick, cement and concrete etc..Data from recent years shows that people have recognized
To the harm of coal gas slugging, starting system research from different perspectives, it forms structure and characteristic, and starts to pay attention to its disposal and profit
Use problem.
On for example all kinds of synthetic zeolites of Porous materials, be the industries such as modern chemical industry, material, the energy be used to adsorbing, separate,
The indispensable material such as catalysis, catalyst carrier.Porous materials can be divided into micropore, mesopore and macropore according to pore size.With
In the raw material for synthesizing siliceous Porous materials can be the natural mineral raw of industrial chemicals or rich reserves.In recent years, with
The research on utilization for the silica solid discarded object such as flyash, gangue is increasingly paid attention to, and uses solid waste to be closed for raw material
Achievement in research into zeolite is also constantly seen in report.It is multiple that such as Sun Hong (2008) using gangue is prepared for zeolite-activated carbon
Condensation material；ZhonglinLi etc. (2014) has been delivered on adding pitch and solid silica synthesis particle shape in gangue
The achievement in research of X- types zeolite/absorbent charcoal composite material.
So far, using natural material or chemical reagent synthetic zeolite Porous materials, the mainly hydro-thermal in alkaline environment
Synthetic method, such as micropore, mesopore, orderly, unordered, high silicon or high aluminum molecular screen and mesoporous material, it is various in style.Using people
Work Hydrothermal Synthesiss technology needs special Hydrothermal Synthesiss equipment, and building-up process condition is harsh, is also needed when being synthesized for mesopore material
A large amount of templates are added, the later stage will remove template agent removing by heat treatment again, and synthesis cost is high, complex process, causes its product
It is expensive.
The content of the invention
It is an object of the invention to provide a kind of coal gasification fine slag molten method for preparing porous beads of acid and obtained porous
Microballon, microballon porous material prepared in accordance with the present invention is compared with conventional porous materials, without undergoing complicated Hydrothermal Synthesiss etc.
Process, preparation technology is simple, and cost is cheap.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of molten method for preparing porous beads of coal gasification fine slag acid, methods described include：
A. appropriate coal gasification fine slag is taken, adds water to prepare the coal gasification fine slag slurry for being contained in 10-30wt% admittedly；
B. the slurry of step a configurations is sufficiently stirred, afterwards by gravity cyclonic separation, collects heavy separation product
Obtain the compound slurry of Silicon-rich；
C. appropriate acid solution and the Silicon-rich composite mortar are mixed to get mixed slurry, carry out the molten reaction of acid；
D. separation of solid and liquid is carried out to the material after the molten reaction of acid, and washs, dries, obtain product.
In the present invention, the coal gasification fine slag is to be carried secretly by coal gasification gas and after coal gasification gas leaves coal gasifier
The residue of separation discharge in purification process (such as through cyclone dust removal, bag-type dust and/or washing), coal gasification course is this area
It is known, it will be appreciated by those skilled in the art that due to the inorganic mineral components of formation ash content of coal contained in feed coal, and in gas
The presence for the charcoal for not being gasified totally and remaining during change, solid phase group is inevitably carried secretly in coal gasification gas caused by coal gasification
Point, wherein the less solid phase components of granularity leave gasification furnace and form coal gasification fine slag, and the solid phase components are amorphous state, and particle diameter is usual
Less than 120 μm, such as 0.1-100 μm.
In the step a of the present invention, when being mixed and made into slurry using coal gasification fine slag and water, those skilled in the art's reason
Solution, the gasification fine slag can be that dry slag can also be wet slag, make the solid content of slurry in 10wt%~30wt%, further excellent
Between selecting 15wt%~25wt%, such as 20wt%.In a preferred embodiment, the coal gasification fine slag slurry of configuration
Follow-up stir process, such as 1.5h, 2h or 5h are carried out again after at least 1h, are fully contacted, are moistened with water so that coal gasification refines
It is wet, so as to be advantageous to follow-up cyclonic separation.
In step b in the present invention, slurry is stirred, then cyclonic separation obtains the compound slurry of rich charcoal；Wherein,
The stirring is processing means commonly used in the art, such as can be stirred using mixing plant, it is preferred to use reinforcement
Agitator is stirred.In a preferred embodiment, in the preparation process of Silicon-rich composite mortar, stirring condition turns for stirring
Speed is not less than 1500r/min, and mixing time is no less than 30min；Preferably, speed of agitator is 1800~3000r/min, during stirring
Between be 60min~180min；In order to follow-up cyclonic separation.Research is found, by above-mentioned strong stirring, especially for leaching
Pulp separation after bubble processing is better.It is processing means commonly used in the art in the cyclonic separation, such as can uses
Cyclone separator carry out cyclonic separation, in cyclonic separation, due to Action of Gravity Field, the less charcoal component of fine slag Midst density mainly from
Overflowed at the top of cyclone separator, and the sa component (heavy separation product) that density is larger is then mainly discharged from bottom, so as to
Realize separation.
In the step c of the present invention, appropriate aqueous acid and the Silicon-rich composite mortar are mixed to get mixed slurry, with
Carry out the molten reaction of acid；Because coal gasification fine slag experienced by the process of high temperature (such as 1300-1400 DEG C) to water quenching chilling, because
This, possesses very high chemical reactivity so that metal oxide therein can with acid reaction and dissolution, and with metal
The difference of Ion release amount, remaining siliceous component forms the different unordered porous beads state of porosity, thus, it is possible to obtain silicon
Matter skeletal porous material.Preferably, in step c, solid content is 10-35wt% in mixing gained slurry, such as 12wt%,
15wt% or 20wt%, acid concentration (liquid phase quality in sour quality divided by slurry in slurry, i.e. sour matter in the liquid phase of slurry
Amount fraction) be 5-25wt%, such as 8wt% or 12wt%, stirring 2-6h carry out the molten reaction of acid, advantageously ensure that sour molten reaction
Effect.The acid solution can be the acid solution of the metallic elements such as the aluminium calcium iron be advantageous in dissolution fine slag commonly used in the art,
Preferably, the acid solution is hydrochloric acid or aqueous solution of nitric acid.
In the step d of the present invention, separation of solid and liquid is carried out to the material after the molten reaction of acid, and wash, dry；Above-mentioned mistake
Journey is known in the art, such as carries out separation of solid and liquid by filtering, and washing solid makes its pH be more than 4；Again by solid in
80-120 DEG C of drying, that is, obtain the porous material of the molten regulation type of acid.Preferably, in step d products therefroms, carbon content is not more than
10wt%, preferably not greater than 8wt%, such as 5~8wt%.
Liquid product obtained by above-mentioned separation of solid and liquid mainly contains the metal ions such as aluminium, iron and calcium, can further prepare
Water purification agent, comprehensive utilization is realized, is further increased economic efficiency, wherein it is possible to be prepared by method commonly used in this field net
Aqua, for example, containing aluminium chloride, iron chloride and calcium chloride in dissolution fluid, material reaches concentration of aluminum chloride by simple adjustment
29wt% cans meet water purification agent requirement.
In a preferred embodiment of the present invention, methods described also includes step e：Step e：To step d product
Calcination processing is carried out, to remove residual carbon, calcining heat is 550-750 DEG C, such as 600 or 650 DEG C, it is functional so as to obtain
Siliceous porous beads material, may be used as catalyst carrier, functional stuffing etc..
Present invention also offers the porous beads material being prepared according to the above method；Preferably, the porous beads
The content range of silica is 60-95wt% in material, such as 80wt% or 90wt%.
Compared with prior art, the present invention has advantages below：
The present invention can realize to be developed to coal gasification fine slag high value added product, and coal gasification fine slag used is coal through high temperature
After gasification, amorphous silicon aluminum material that the inorganic mineral of siliceous in coal, aluminium etc. is transformed into from high-temperature fusion to water quenching chilling
(while also containing calcium, iron etc.) and the mixture of residual charcoal.From conventional pulverized coal grey different, microballon and flyash in coal gasification fine slag
In microballon significant difference be its component all with amorphous state state exist, chemism is good, wherein the aluminium contained, calcium, iron
It is easy to Deng metal oxide at low temperature with acid reaction and dissolution, the dissolution degree of metal ion can be adjusted by sour dosage
Control；
These microballons after aluminium calcium iron component dissolution therein, can obtain loose porous siliceous glass through Low-temperature acid soluble
Microballon, the porous beads specific surface area is big, pore volume is high, heat endurance is good, intensity is high, can turn into absorption, filtering, catalyst load
Body or functional stuffing etc., so as to realize the high value added product exploitation of coal gas slugging solid waste, and preparation technology letter
Single, cost is cheap；Meanwhile the metal ion of dissolution can further prepare water purification agent, the full constituent for realizing coal gas slugging is comprehensive
Close and utilize, turn waste into wealth.
Embodiment
Below with reference to embodiment, the present invention is described in detail, but the present invention is not limited to this.
In following examples/comparative example, coal gasification fine slag used is from the industry of Ordos, inner Mongolia Jungar Banner main road
Garden, its property/combination are as follows：Carbon content 40.2wt%, silica 20.1wt%；Aluminum oxide is 10.9wt%, calcium oxide
For 12.4wt%, iron oxide 5.3wt%.
In following examples, agents useful for same is pure to analyze if not otherwise specified.
Embodiment 1
100g coal gasification fine slags are weighed, it is 10wt% to be diluted with water to solid content, and high velocity dispersators are used under normal temperature
(Foshan Yi Fu Machinery Co., Ltd.s) stirs, speed of agitator 1800r/min, mixing time 30min；Slurry is imported
Being separated in cyclone separator, obtained bottom slurry is Silicon-rich composite mortar, isolates solid constituent, solid amount about 60g,
Wherein carbon content is about 6wt%；
36wt% concentrated hydrochloric acid 130ml separately are taken, are added in above-mentioned solid constituent, it is 360ml to add water regulation slurry cumulative volume,
The slurry acid concentration reaches about 15.6wt%, solid content about 14.5wt%, stirs 6h under normal temperature, separation of solid and liquid, is washed to afterwards
PH is equal to 4；The calcium chloride isolated, aluminium chloride, chlorination iron mixed solution can be used for aluminum chlorate of polymerized silicic acid product development；
For the solid isolated in 100 DEG C of dryings, obtained product is charcoal silicon composite porous material.The product alumina obtained under the conditions of this
Dissolution rate is 88%, and oxidation dissoluble rate of calcium is 93%, and iron oxide dissolution rate is 91%；It is 390m to determine its specific surface area2/ g, hole
Hold for 0.6748cm3/g.Aperture 3.54nm.
By above-mentioned composite porous material through being heat-treated 3h carbon removal in 580 DEG C of air, siliceous glass microballon Porous materials are obtained, are surveyed
Its fixed specific surface area is 289m2/ g, pore volume 0.5426cm3/ g, aperture 3.48nm.
Embodiment 2
100g coal gasification fine slags are weighed, it is 10wt% to be diluted with water to solid content, and high velocity dispersators are used under normal temperature
(Foshan Yi Fu Machinery Co., Ltd.s) stirs, speed of agitator 1600r/min, mixing time 40min；Slurry is imported
Being separated in cyclone separator, obtained bottom slurry is Silicon-rich composite mortar, isolates the total amount about 60g of solid constituent, its
Middle carbon content is about 6wt%；
36wt% concentrated hydrochloric acid 100ml separately are taken, 130ml is diluted with water to and is added to afterwards in above-mentioned solid constituent, add water to adjust
Material-saving slurry cumulative volume is 360ml, the slurry acid concentration about 12.2wt%, solid content about 14.7wt%, stirring at normal temperature 4h, Zhi Hougu
Liquid separates, and is washed to pH equal to 4, and the calcium chloride isolated, aluminium chloride, chlorination iron mixed solution can be used for PAFC net
Aqua product is developed；For the solid isolated in 100 DEG C of dryings, the product obtained is porous siliceous microballon and compound new of porous charcoal
Porous materials.The product alumina dissolution rate obtained under the conditions of this is 74%, and oxidation dissoluble rate of calcium is 81%, and iron oxide dissolution rate is
69%；It is 342m to determine its specific surface area2/ g, pore volume 0.531cm3/ g, aperture 3.59nm.
By above-mentioned composite porous material through being heat-treated 3h carbon removal in 600 DEG C of air, siliceous glass microballon Porous materials are obtained, are surveyed
Its fixed specific surface area is 238m2/ g, pore volume 0.4919cm3/g.Aperture 2.97nm.
Embodiment 3
100g coal gasification fine slags are weighed, it is 10wt% to be diluted with water to solid content, and high velocity dispersators are used under normal temperature
(Foshan Yi Fu Machinery Co., Ltd.s) stirs, speed of agitator 1700r/min, mixing time 30min；Slurry is imported
Being separated in cyclone separator, obtained bottom slurry is Silicon-rich composite mortar, isolates the total amount about 62g of solid constituent, its
Middle carbon content is about 6.5wt%；
36wt% concentrated hydrochloric acid 75ml separately are taken, 130ml is diluted with water to and is added to afterwards in above-mentioned solid constituent, add water to adjust
Slurry cumulative volume is 360ml, now slurry acid concentration about 9.3wt%, solid content about 15.3wt%, stirring at normal temperature 4h, Zhi Hougu
Liquid separates, and is washed to pH equal to 4, and the calcium chloride isolated, aluminium chloride, chlorination iron mixed solution can be used for PAFC net
Aqua product is developed；For the solid isolated in 100 DEG C of dryings, the product obtained is porous siliceous microballon and compound new of porous charcoal
Porous materials.The product alumina dissolution rate obtained under the conditions of this is 53%, and oxidation dissoluble rate of calcium is 67%, and iron oxide dissolution rate is
55%；It is 309m to determine its specific surface area2/ g, pore volume 0.4541cm3/ g, aperture 3.18nm.
By above-mentioned composite porous material through being heat-treated 3h carbon removal in 600 DEG C of air, siliceous glass microballon Porous materials are obtained, are surveyed
Its fixed specific surface area is 198m2/ g, pore volume 0.3982cm3/ g, aperture 2.19nm.
Embodiment 4
100g coal gasifications fine slag (wherein aqueous 50wt%) is weighed, it is 10wt% to be diluted with water to solid content, is adopted under normal temperature
Stirred with high velocity dispersators (Foshan Yi Fu Machinery Co., Ltd.s), speed of agitator 1600r/min, mixing time is
40min；Slurry is imported in cyclone separator and separated, obtained bottom slurry is Silicon-rich composite mortar, isolates solid group
The total amount about 60g divided, wherein carbon content is about 6wt%；
70wt% concentrated nitric acid 28ml separately are taken, 130ml is diluted with water to and is added to afterwards in above-mentioned solid constituent, add water to adjust
Slurry cumulative volume is 360ml, the slurry concentration of nitric acid about 7.25wt%, solid content about 14.8%, and 4h, Zhi Hougu are stirred under normal temperature
Liquid separates, and is washed to pH equal to 4, for the solid isolated in 100 DEG C of dryings, obtained product is porous siliceous microballon and porous charcoal
Compound new Porous materials.The product alumina dissolution rate obtained under the conditions of this is 90%, and oxidation dissoluble rate of calcium is 95%, oxidation
Iron dissolution rate is 93%；It is 410m to determine its specific surface area2/ g, pore volume 0.6925cm3/g.Aperture 3.50nm.
By above-mentioned composite porous material through being heat-treated 3h carbon removal in 600 DEG C of air, siliceous glass microballon Porous materials are obtained, are surveyed
Its fixed specific surface area is 295m2/ g, pore volume 0.5523cm3/ g, aperture 3.46nm.
Claims (8)
1. a kind of molten method for preparing porous beads of coal gasification fine slag acid, methods described include：
A. appropriate coal gasification fine slag is taken, adds water to prepare the coal gasification fine slag slurry for being contained in 10-30wt% admittedly；
B. the slurry of step a configurations is sufficiently stirred, afterwards by gravity cyclonic separation, collects heavy separation product and obtain
The compound slurry of Silicon-rich；
C. appropriate acid solution and the Silicon-rich composite mortar are mixed to get mixed slurry, carry out the molten reaction of acid；
D. separation of solid and liquid is carried out to the material after the molten reaction of acid, and washs, dries, obtain product.
2. according to the method for claim 1, it is characterised in that in step d products therefroms, carbon content is not more than 10wt%,
Preferably 5~8wt%.
3. method according to claim 1 or 2, it is characterised in that methods described also includes step e：To step d product
Calcination processing is carried out, to remove remaining char, calcining heat is 550-750 DEG C.
4. according to the method any one of claim 1-3, it is characterised in that in step b, stirring condition is speed of agitator
Not less than 1500r/min, mixing time is no less than 30min；Preferably, speed of agitator is 1800~3000r/min, mixing time
For 40min~180min；It is further preferred that carry out step b's again after the coal gasification fine slag slurry at least 1h of step a configurations
Stir process.
5. according to the method any one of claim 1-4, it is characterised in that in step c, contain admittedly in gained mixed slurry
Measure as 10-35wt%, acid concentration 5-25wt%, stirring 2-6h is to carry out the molten reaction of acid.
6. according to the method any one of claim 1-5, it is characterised in that the acid solution is that hydrochloric acid or nitric acid are water-soluble
Liquid.
7. according to the method any one of claim 1-6, it is characterised in that the acid water for obtaining the separation of solid and liquid
Solution further prepares water purification agent.
8. the porous beads material being prepared according to method any one of claim 1-7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710157813.5A CN107855105B (en) | 2017-03-16 | 2017-03-16 | Method for preparing porous microspheres by using coal gasification fine slag and prepared porous microspheres |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710157813.5A CN107855105B (en) | 2017-03-16 | 2017-03-16 | Method for preparing porous microspheres by using coal gasification fine slag and prepared porous microspheres |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107855105A true CN107855105A (en) | 2018-03-30 |
| CN107855105B CN107855105B (en) | 2020-02-18 |
Family
ID=61699043
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710157813.5A Active CN107855105B (en) | 2017-03-16 | 2017-03-16 | Method for preparing porous microspheres by using coal gasification fine slag and prepared porous microspheres |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107855105B (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585779A (en) * | 2018-05-04 | 2018-09-28 | 中国科学院过程工程研究所 | A method of preparing Al-Si composites using gasification slag |
| CN110452012A (en) * | 2019-08-23 | 2019-11-15 | 成都德菲环境工程有限公司 | A kind of method that gangue cooperates with resource utilization to prepare haydite with coal gas slugging |
| CN110465300A (en) * | 2019-08-23 | 2019-11-19 | 吉林大学 | A kind of heterogeneous fenton catalyst and its preparation method and application |
| CN110624506A (en) * | 2019-10-24 | 2019-12-31 | 陕西利人之星环保科技有限公司 | Method for preparing water purifying agent by utilizing coal gasification furnace slag and obtained water purifying agent |
| CN112661162A (en) * | 2020-12-16 | 2021-04-16 | 青岛惠城环保科技股份有限公司 | Method for treating petroleum coke hydrogen production ash and mesoporous silicon material |
| CN113308025A (en) * | 2021-05-25 | 2021-08-27 | 内蒙古万邦清源环保科技有限公司 | Method for directly preparing high-activity micro-nano superfine powder material for highway asphalt by utilizing gasified slag |
| CN113843262A (en) * | 2021-10-07 | 2021-12-28 | 喻勇 | Rotary flushing process for coal chemical gasification slag |
| CN114308977A (en) * | 2020-09-29 | 2022-04-12 | 吉林大学 | Method for preparing composite conductive filler by using coal gasification fine slag and prepared filler |
| CN114950523A (en) * | 2022-05-23 | 2022-08-30 | 榆林学院 | Semi-coke wastewater treatment catalyst and preparation method and application thereof |
| CN114985435A (en) * | 2022-08-05 | 2022-09-02 | 中国科学院过程工程研究所 | Method for comprehensively utilizing waste salt and various solid wastes |
| CN116140341A (en) * | 2022-11-16 | 2023-05-23 | 山东大学 | Gasification slag high-value recycling method |
| CN117339552A (en) * | 2023-11-21 | 2024-01-05 | 陕西科技大学 | Gas-based residue adsorption-flocculation multifunctional water purifying agent and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1927716A (en) * | 2006-08-29 | 2007-03-14 | 吉林大学 | Preparation method of alumina |
| CN103305686A (en) * | 2013-05-30 | 2013-09-18 | 华东理工大学 | Method for realizing separation of aluminium, iron and calcium by activating coal gasification ash |
| CN104987107A (en) * | 2015-07-16 | 2015-10-21 | 神华集团有限责任公司 | Composition for filtering ceramic production, filtering ceramic, and preparation method and application of filtering ceramic |
| CN105524669A (en) * | 2014-09-29 | 2016-04-27 | 大唐国际化工技术研究院有限公司 | Separating and recycling method for fine slag of coal gasification |
-
2017
- 2017-03-16 CN CN201710157813.5A patent/CN107855105B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1927716A (en) * | 2006-08-29 | 2007-03-14 | 吉林大学 | Preparation method of alumina |
| CN103305686A (en) * | 2013-05-30 | 2013-09-18 | 华东理工大学 | Method for realizing separation of aluminium, iron and calcium by activating coal gasification ash |
| CN105524669A (en) * | 2014-09-29 | 2016-04-27 | 大唐国际化工技术研究院有限公司 | Separating and recycling method for fine slag of coal gasification |
| CN104987107A (en) * | 2015-07-16 | 2015-10-21 | 神华集团有限责任公司 | Composition for filtering ceramic production, filtering ceramic, and preparation method and application of filtering ceramic |
Non-Patent Citations (1)
| Title |
|---|
| 马小路等: "活化煤气化粗渣盐酸浸取机理研究", 《无机盐工业》 * |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585779B (en) * | 2018-05-04 | 2021-10-15 | 中国科学院过程工程研究所 | Method for preparing aluminum-silicon composite material by using gasified slag |
| CN108585779A (en) * | 2018-05-04 | 2018-09-28 | 中国科学院过程工程研究所 | A method of preparing Al-Si composites using gasification slag |
| CN110452012A (en) * | 2019-08-23 | 2019-11-15 | 成都德菲环境工程有限公司 | A kind of method that gangue cooperates with resource utilization to prepare haydite with coal gas slugging |
| CN110465300A (en) * | 2019-08-23 | 2019-11-19 | 吉林大学 | A kind of heterogeneous fenton catalyst and its preparation method and application |
| CN110465300B (en) * | 2019-08-23 | 2020-09-25 | 吉林大学 | Heterogeneous Fenton catalyst and preparation method and application thereof |
| CN110624506A (en) * | 2019-10-24 | 2019-12-31 | 陕西利人之星环保科技有限公司 | Method for preparing water purifying agent by utilizing coal gasification furnace slag and obtained water purifying agent |
| CN110624506B (en) * | 2019-10-24 | 2022-04-08 | 陕西利人之星环保科技有限公司 | Method for preparing water purifying agent by utilizing coal gasification furnace slag and obtained water purifying agent |
| CN114308977A (en) * | 2020-09-29 | 2022-04-12 | 吉林大学 | Method for preparing composite conductive filler by using coal gasification fine slag and prepared filler |
| CN112661162A (en) * | 2020-12-16 | 2021-04-16 | 青岛惠城环保科技股份有限公司 | Method for treating petroleum coke hydrogen production ash and mesoporous silicon material |
| CN113308025A (en) * | 2021-05-25 | 2021-08-27 | 内蒙古万邦清源环保科技有限公司 | Method for directly preparing high-activity micro-nano superfine powder material for highway asphalt by utilizing gasified slag |
| CN113843262A (en) * | 2021-10-07 | 2021-12-28 | 喻勇 | Rotary flushing process for coal chemical gasification slag |
| CN114950523A (en) * | 2022-05-23 | 2022-08-30 | 榆林学院 | Semi-coke wastewater treatment catalyst and preparation method and application thereof |
| CN114950523B (en) * | 2022-05-23 | 2024-01-26 | 榆林学院 | Semi-coke wastewater treatment catalyst and preparation method and application thereof |
| CN114985435A (en) * | 2022-08-05 | 2022-09-02 | 中国科学院过程工程研究所 | Method for comprehensively utilizing waste salt and various solid wastes |
| CN116140341A (en) * | 2022-11-16 | 2023-05-23 | 山东大学 | Gasification slag high-value recycling method |
| CN117339552A (en) * | 2023-11-21 | 2024-01-05 | 陕西科技大学 | Gas-based residue adsorption-flocculation multifunctional water purifying agent and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107855105B (en) | 2020-02-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107855105A (en) | The method of porous beads and obtained porous beads are prepared using coal gasification fine slag | |
| CN107855104A (en) | The thick slag of coal gasification prepares the method for complex mesoporous material and obtained mesoporous material | |
| CN107857496B (en) | Comprehensive utilization method of coal gasification fine slag | |
| CN107855103B (en) | Using coal gasification fine slag prepare adsorbent material method and adsorbent material obtained | |
| CN108622904A (en) | The method of mesoporous microballon and mesoporous microballon obtained are prepared using coal gasification fine slag | |
| CN104437355B (en) | Preparation method of coal ash-based CuO-CeO2/FAU desulfurizer | |
| CN107855108B (en) | Method for synthesizing zeolite by utilizing coal gasification fine slag and prepared zeolite material | |
| CN104291349B (en) | A kind of take flyash as the method that P type molecular sieve prepared by raw material | |
| CN109650429B (en) | Carbide slag recycling treatment process | |
| CN107857499B (en) | Prepare method, cement admixture and the cement composition of cement admixture | |
| CN109621925B (en) | Carbon dioxide trapping agent and application thereof | |
| CN100595154C (en) | Method for extracting aluminum oxide from fly ash and coproducing cement by carbide slag or cyanamide slag | |
| Zou et al. | Sorption capacity and mechanism of Cr3+ on tobermorite derived from fly ash acid residue and carbide slag | |
| CN102311136A (en) | Method for producing low iron aluminum sulfate by utilization of coal gangue | |
| CN107857274A (en) | The synthetic method and tobermorite fibrous material of tobermorite fibrous material | |
| CN113716583A (en) | Method for preparing 4A zeolite by using MSWI fly ash and red mud hydrothermal method | |
| CN116078348A (en) | Comprehensive utilization method of gas slag | |
| CN111939745A (en) | Method for preparing desulfurizer from carbide slag, efficiently desulfurizing and utilizing desulfurized gypsum | |
| CN108906316A (en) | A method of desulfurizing agent is prepared using carbide slag | |
| CN114212799B (en) | Fly ash pretreatment method for molecular sieve preparation | |
| CN109695059B (en) | Preparation method of gypsum whisker | |
| CN105984885A (en) | Method for synthesizing ZSM-5 molecular sieve by using silica fume | |
| CN107857275A (en) | The preparation method of xonotlite fiber material and obtained xonotlite fiber material | |
| CN108558245A (en) | A kind of sludge base cement mixture and preparation method thereof | |
| CN106495173A (en) | A kind of method for producing tobermorite with siliceous discarded object and carbide slag heating using microwave |
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 | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wei Cundi Inventor after: Zhu Dandan Inventor after: Wei Jilun Inventor after: Cheng Pan Inventor after: Jiang Yinshan Inventor after: Yang Dianfan Inventor after: Ai Weidong Inventor before: Wei Cundi Inventor before: Zhu Dandan Inventor before: Cheng Pan Inventor before: Jiang Yinshan Inventor before: Yang Dianfan Inventor before: Wei Jilun Inventor before: Ai Weidong |
|
| CB03 | Change of inventor or designer information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20200810 Address after: Office 1506, Wanzheng building, opposite Dongsheng District Hospital, Ordos City, Inner Mongolia Autonomous Region Patentee after: Ordos Huiheng Technology Co., Ltd Address before: 130012 Changchun Qianjin Street, Jilin, No. 2699 Patentee before: Jilin University |
|
| TR01 | Transfer of patent right |