CN108190928A - A kind of method of aluminous fly-ash synthesizing mesoporous nano gama-alumina - Google Patents
A kind of method of aluminous fly-ash synthesizing mesoporous nano gama-alumina Download PDFInfo
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Abstract
A kind of method of aluminous fly-ash synthesizing mesoporous nano gamma-alumina, by aluminous fly-ash in aqueous slkali pre-desiliconizing；Desiliconization ash and lime stone are mixed, screening, calcine at high temperature, obtain sintered clinker from dusting；Sintered clinker and sodium carbonate liquor are mixed, reacted, obtains silico-calcium residue and sodium aluminate solution after separation；The CO of 15 30vol% is passed through into sodium aluminate solution after purification with microbubble aerating system2Gas reacts 1h, isolated sodium carbonate liquor and aluminium hydroxide presoma under the conditions of 20 80 DEG C；Presoma is dried, calcines 4 8h at 400 550 DEG C, meso-porous nano gamma-alumina product is obtained after cooling.This method had not only realized the high level recycling of aluminous fly-ash, but also had synthesized the meso-porous nano gamma-alumina of high value and silico-calcium residue can be used for CO in situ2Trapping；Meanwhile the technology need not add high template, production cost is greatly reduced, improves product combined coefficient, product crystallinity is high, has excellent meso-porous nano material property.
Description
Technical field
The invention belongs to Resource Recovery of Industrial Solid Waste utilize and meso-porous nano field of material synthesis technology, more particularly to one
The method of kind aluminous fly-ash synthesizing mesoporous nano gama-alumina.
Background technology
Since two thousand, the thermoelectricity installed capacity in China is in explosive growth, and the ratio of wherein coal fired power generation accounts for fire
More than 90% power power generation.Flyash is the tiny flying dust and furnace bottom that mineral and clay in fire coal etc. are generated through high-temperature calcination
Slag is the primary solids waste of coal-burning power plant.Coal-burning power plant of China flyash generated in 2015 has reached 6.20 hundred million tons, but comprehensive
Utilization rate is closed less than 70%.By year ends 2015, the volume of cargo in storage of China's flyash alreadys exceed 2,000,000,000 tons, and will also have a net increase of every year
200000000 tons.The flyash stored up year by year does not only take up large amount of land resources, also forms huge prestige to ecological environment and health
The side of body.《Total utilization of PCA management method》In point out, encourage to carry out that the high added value and large dosage of flyash are utilized.
Alumina content in flyash is generally 15-40%, mainly exists in the form of corundum and mullite, is a kind of
Very important non-bauxitic resource.In some areas such as Shanxi and the Inner Mongol, alumina content in flyash even can be with
Reach 40-55%, be equivalent to middle-low bauxite.The aluminous fly-ash (more than 37% alumina content) that China generates every year
Up to 50,000,000 tons or more, it is possible to provide 20,000,000 tons or more of alumina resource.On the other hand, China's bauxite resource is deficient,
And based on the diaspore of middle-low grade；52,050,000 tons of China's import bauxite in 2016, external dependence degree reaches
44.47%.Therefore, carry out aluminous fly-ash recycling aluminum oxide technology research, China's bauxite resource shortage can not only be alleviated
The problem of, additionally it is possible to realize the high level recycling of aluminous fly-ash.
In recent years, China has carried out the technical research of a large amount of aluminous fly-ash recycling alumina resources, mainly including lime
Stone sintering process, pre-desiliconizing-soda lime sintering process, acidleach are followed the example of with alkali leaching method etc..These technologies are realized from flyash
Aluminium oxide is extracted, and by technique and parameter optimization, gradually reduces cost, extraction efficiency up to 80-90%.But these skills
Art only conducts a research from the substance of aluminium oxide recycling angle, for how further to utilize and develop the alumina product after recycling
Not yet consider.Therefore, the alumina product recycled from aluminous fly-ash lacks the market competitiveness in quality and in price.
Meso-porous nano gama-alumina has regular pore structure, the crystal structure of stabilization, intrinsic soda acid characteristic,
Therefore it is widely used in various catalyst carriers.At present, meso-porous nano gama-alumina generally uses sol-gel self assembly skill
Art synthesizes：Using aluminium-alcohol salt or aluminate as presoma, under the auxiliary of template, by hydrolysis, aging, washing, separation, drying
Etc. obtain aluminium hydroxide presoma after processes, presoma obtains gama-alumina product after high-temperature calcination again.Usual gamma oxidation
The crystallization temperature of aluminium is at 800 DEG C or more, but high temperature is easily destroyed its regular pore structure, it is therefore desirable to study hydroxide
Influence of the aluminium presoma to crystallization temperature reduces the crystallization temperature of gama-alumina.And traditional technology needs to add expensive mould
Plate agent also constrains being widely used for meso-porous nano gama-alumina.
Invention content
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide a kind of aluminous fly-ash is synthesising mesoporous
The method of nanometer gama-alumina, using aluminous fly-ash as raw material, using pre-desiliconizing-limestone sintering technology extraction aluminium oxide,
CO2Microbubble sedimentation synthesizing mesoporous nano gama-alumina product, being capable of recycling aluminous fly-ash, promotion oxidation
Aluminium properties of product；Meanwhile the silico-calcium residue extracted after aluminium oxide can be used for the CO of coal-burning power plant in situ2Trapping.In addition, synthesis
CO used by meso-porous nano gama-alumina product2Microbubble is capable of the effect of alternate template agent, be greatly reduced production into
Originally product combined coefficient, is improved.Realize the high level recycling of aluminous fly-ash.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of method of aluminous fly-ash synthesizing mesoporous nano gama-alumina, includes the following steps：
(A) pre-desiliconizing with high alumina fly ash：Aluminous fly-ash and sodium hydroxide solution are mixed, through hydro-thermal reaction, solid-liquid point
From rear, desiliconization ash and sodium silicate solution are obtained；
(B) raw material are prepared：Desiliconization ash in lime stone and step (A) is mixed, after screening, it is spare to obtain raw material；
(C) sintered clinker is prepared：Raw material in step (B) are calcined at high temperature, sintered product are taken out, fast quickly cooling
But, sintered product obtains sintered clinker from after dusting；
(D) sodium metaaluminate is dissolved out：Sintered clinker in step (C) and sodium carbonate liquor are mixed, after hydro-thermal reaction, generation
The mix products of silico-calcium residue and sodium aluminate solution；
(E) it detaches, purify sodium aluminate solution：By the mix products separation of solid and liquid in step (D), filter residue is that silico-calcium is residual
Slag adds in calcium hydroxide solution into filtrate, removes impurity, obtains purifying sodium aluminate solution after separation of solid and liquid again；
(F) aluminium hydroxide presoma is synthesized：Led to microbubble aerating system into the purifying sodium aluminate solution of step (E)
Enter the CO of 15-30vol%2Gas, CO2After sodium metaaluminate reaction, separation of solid and liquid, aluminium hydroxide presoma and sodium carbonate are obtained
Solution；
(G) synthesizing mesoporous nano gama-alumina：By the aluminium hydroxide presoma drying removal absorption water in step (F), then
Calcined dehydration, crystallization obtain meso-porous nano gama-alumina product after cooling.
In the step (A), aluminous fly-ash and 25wt% sodium hydroxide solutions are mixed, sodium hydrate solid and high alumina
The mass ratio of flyash is 0.5:1；Solution after mixing is placed in 110 DEG C of high-temperature high-pressure reaction kettle, the reaction time is
30min；Mix products are detached with Suction filtration device, and filter residue is desiliconization ash, and filtrate is sodium silicate solution.
In the step (B), using the desiliconization ash in planetary ball mill mixing lime stone and step (A), ball milling used
Tank is corundum material, abrading-ball is zirconium oxide material, drum's speed of rotation 180rpm, Ball-milling Time 10min；Lime stone in raw material
Meet with the ratio of desiliconization ash：N (CaO)=2 × n (SiO2)+ 12/7×n(Al2O3)+2×n(Fe2O3)；It is sieved using 200 mesh
Device sieves the raw material after ball milling, and it is spare less than 74 μm of raw material to obtain grain size.
In the step (C), when high temperature Muffle furnace is warming up to 800 DEG C, the raw material in step (B) are put into, after of continuing rising
Temperature to calcination temperature (1350-1400 DEG C) calcines 0.5-2h afterwards, takes out, is quickly cooled down when product to be sintered is cooled to 800 DEG C,
Sintered product obtains sintered clinker from after dusting.Chemical reaction such as formula (1-3) in raw material sintering process：
SiO2+2CaO→2CaO·SiO2 (1)
3Al2O3·2SiO2+7CaO→3(CaO·Al2O3)+2(2CaO·SiO2) (3)
In the step (D), the sodium carbonate liquor of the sintered clinker in step (C) and 0.9mol/L are mixed, liquid-solid ratio
For 10-20, mixed solution is placed in 30-70 DEG C of reaction kettle, reacts 15- under the conditions of magnetic agitation (300rpm)
30min generates the mix products of silico-calcium residue and sodium aluminate solution；The chemical reaction of sintered clinker and sodium carbonate liquor such as formula
(4)：
12CaO·7Al2O3+12Na2CO3+5H2O→12CaCO3+14NaAlO2+10NaOH (4)
In the step (E), the mix products in step (D) are detached with Suction filtration device, filter residue is silico-calcium residue, can be former
Position is used for the CO of coal-burning power plant2Trapping；Appropriate calcium hydroxide solution is added in into filtrate, removes silicic acid sodium impurity, again with pumping
After filtering device separation, gained filtrate is to purify sodium aluminate solution.
In the step (F), a concentration of 0.1-0.4mol/L of purifying sodium aluminate solution in regulating step (E), by it
It is placed in 20-80 DEG C of reaction kettle, 15- is passed through thereto with microbubble aerating system under the conditions of magnetic agitation (300rpm)
The CO of 30vol%2Gas adjusts CO2A diameter of 1-5mm of microbubble, reaction time 1h, adjusting gas flow cause n
(CO2):n(NaAlO2)=1.6:1；Mix products are detached with Suction filtration device, and filter residue is aluminium hydroxide presoma, and filtrate is carbonic acid
Sodium solution, by recycling sodium carbonate by-product after purifying, crystallizing.CO2Chemical reaction such as formula (5) with sodium metaaluminate：
2NaAlO2+CO2+3H2O→Na2CO3+2Al(OH)3↓ (5)
In the step (G), by the aluminium hydroxide presoma in step (F), dry 2h removals are inhaled in 105 DEG C of baking oven
Attached water, then 4-8h dehydrations, crystallization are calcined in 400-550 DEG C of Muffle furnace, the production of meso-porous nano gama-alumina is obtained after cooling
Product.
Compared with prior art, the beneficial effects of the invention are as follows：
1. using industrial solid wastes as raw material, the high level recycling of aluminous fly-ash had not only been realized, but also has synthesized height
The meso-porous nano gama-alumina and silico-calcium residue of value can be used for the CO of coal-burning power plant in situ2Trapping is a kind of zero-emission, can
Lasting Green Chemistry process.
2. using CO2Microbubble sedimentation, can synthesizing mesoporous nano γ-oxidation without adding high template
Aluminium is greatly reduced production cost, improves product combined coefficient.
3. the product crystallinity is high, has excellent meso-porous nano material property, have well-regulated hexagonal hole road structure, ratio
Surface area is more than 200m2/ g, average pore size 3.5-4.0nm.
Description of the drawings
Fig. 1 is present invention process flow chart.
Fig. 2 is the graph of pore diameter distribution of sample in embodiment 3-5.
Fig. 3 is the small angle X-ray diffraction collection of illustrative plates of sample in embodiment 4.
Fig. 4 is the X ray diffracting spectrum of sample in embodiment 4.
Fig. 5 is the transmission electron microscope picture of sample in embodiment 4.
Specific embodiment
The technological process of the present invention is as shown in Figure 1, the embodiment party that the present invention will be described in detail with reference to the accompanying drawings and examples
Formula, but be not limited to the examples.
Aluminous fly-ash used picks up from Inner Mongol thermal power plant, main oxides composition in case study on implementation in detail below
Including：SiO2(52.00wt%), aluminium oxide (36.51wt%), Fe2O3(5.03wt%), CaO (2.61wt%), TiO2
(1.80wt%), K2O (0.77wt%), MgO (0.33wt%), Na2O (0.14 wt%) and other (0.81wt%).
Embodiment 1
(A) 25g NaOH solids, 50g aluminous fly-ash and 75mL pure water accurately are weighed, the high temperature for being added to 1000mL is high
It presses in inner liner of reaction kettle, reacts 30min under the conditions of 110 DEG C；Mix products are detached with Suction filtration device, and filter residue is desiliconization ash, is filtered
Liquid is sodium silicate solution.
(B) 20 desiliconization ashes and 40g lime stones accurately are weighed, be added in 250mL corundum ball grinders, adjust drum's speed of rotation
For 180rpm, Ball-milling Time 10min；Using 200 mesh sifters, the raw material after ball milling are sieved, obtain grain size less than 74 μm
Raw material it is spare.
(C) raw material in step (B) are placed in 100mL alumina crucibles, when high temperature Muffle furnace is warming up to 800 DEG C,
It puts it into Muffle furnace, calcines 2h after being continuously heating to 1350 DEG C of calcination temperature, product to be sintered takes when being cooled to 800 DEG C
Go out, be quickly cooled down, sintered product obtains sintered clinker from after dusting.
(D) 10g sintered clinkers and 200mL sodium carbonate liquors (0.9mol/L) accurately are weighed, is added to the reaction of 250mL
In kettle liner, 30min is reacted under the conditions of 30 DEG C and magnetic agitation (300rpm), generates silico-calcium residue and sodium aluminate solution
Mix products.
(E) mix products in step (D) are detached with Suction filtration device, filter residue is silico-calcium residue, can be used for fire coal in situ
The CO of power plant2Trapping；Appropriate calcium hydroxide solution is added in into filtrate, silicic acid sodium impurity is removed, is detached again with Suction filtration device
Afterwards, gained filtrate is to purify sodium aluminate solution.
(F) it is inclined accurately to weigh 50 mL purifying by a concentration of 0.1mol/L of purifying sodium aluminate solution in regulating step (E)
Sodium aluminate solution (0.1mol/L), is added in the pyroreaction kettle liner of 100mL, in 20 DEG C and magnetic agitation (300rpm)
Under the conditions of, it is passed through the CO of 15vol% thereto with microbubble aerating system2Gas adjusts CO2A diameter of 1mm of microbubble, gas
Body flow velocity is 20mL/min, reaction time 1h；Mix products are detached with Suction filtration device, and filter residue is aluminium hydroxide presoma, is filtered
Liquid is sodium carbonate liquor, by recycling sodium carbonate by-product after purifying, crystallizing.
(G) by the aluminium hydroxide presoma in step (F), dry 2h removals adsorb water, then 550 in 105 DEG C of baking oven
DEG C Muffle furnace in calcining 4h dehydration, crystallization, meso-porous nano gama-alumina product is obtained after cooling.
Embodiment 2
(A) 25g NaOH solids, 50g aluminous fly-ash and 75mL pure water accurately are weighed, the high temperature for being added to 1000mL is high
It presses in inner liner of reaction kettle, reacts 30min under the conditions of 110 DEG C；Mix products are detached with Suction filtration device, and filter residue is desiliconization ash, is filtered
Liquid is sodium silicate solution.
(B) 20 desiliconization ashes and 40g lime stones accurately are weighed, be added in 250mL corundum ball grinders, adjust drum's speed of rotation
For 180rpm, Ball-milling Time 10min；Using 200 mesh sifters, the raw material after ball milling are sieved, obtain grain size less than 74 μm
Raw material it is spare.
(C) raw material in step (B) are placed in 100mL alumina crucibles, when high temperature Muffle furnace is warming up to 800 DEG C,
It puts it into Muffle furnace, calcines 2h after being continuously heating to 1360 DEG C of calcination temperature, product to be sintered takes when being cooled to 800 DEG C
Go out, be quickly cooled down, sintered product obtains sintered clinker from after dusting.
(D) 10g sintered clinkers and 200mL sodium carbonate liquors (0.9mol/L) accurately are weighed, is added to the reaction of 250mL
In kettle liner, 30min is reacted under the conditions of 40 DEG C and magnetic agitation (300rpm), generates silico-calcium residue and sodium aluminate solution
Mix products.
(E) mix products in step (D) are detached with Suction filtration device, filter residue is silico-calcium residue, can be used for fire coal in situ
The CO of power plant2Trapping；Appropriate calcium hydroxide solution is added in into filtrate, silicic acid sodium impurity is removed, is detached again with Suction filtration device
Afterwards, gained filtrate is to purify sodium aluminate solution.
(F) it is inclined accurately to weigh 50 mL purifying by a concentration of 0.1mol/L of purifying sodium aluminate solution in regulating step (E)
Sodium aluminate solution (0.1mol/L), is added in the pyroreaction kettle liner of 100mL, in 35 DEG C and magnetic agitation (300rpm)
Under the conditions of, it is passed through the CO of 30vol% thereto with microbubble aerating system2Gas adjusts CO2A diameter of 2mm of microbubble, gas
Body flow velocity is 10mL/min, reaction time 1h；Mix products are detached with Suction filtration device, and filter residue is aluminium hydroxide presoma, is filtered
Liquid is sodium carbonate liquor, by recycling sodium carbonate by-product after purifying, crystallizing.
(G) by the aluminium hydroxide presoma in step (F), dry 2h removals adsorb water, then 550 in 105 DEG C of baking oven
DEG C Muffle furnace in calcining 4h dehydration, crystallization, meso-porous nano gama-alumina product is obtained after cooling.
Embodiment 3
(A) 25g NaOH solids, 50g aluminous fly-ash and 75mL pure water accurately are weighed, the high temperature for being added to 1000mL is high
It presses in inner liner of reaction kettle, reacts 30min under the conditions of 110 DEG C；Mix products are detached with Suction filtration device, and filter residue is desiliconization ash, is filtered
Liquid is sodium silicate solution.
(B) 20 desiliconization ashes and 40g lime stones accurately are weighed, be added in 250mL corundum ball grinders, adjust drum's speed of rotation
For 180rpm, Ball-milling Time 10min；Using 200 mesh sifters, the raw material after ball milling are sieved, obtain grain size less than 74 μm
Raw material it is spare.
(C) raw material in step (B) are placed in 100mL alumina crucibles, when high temperature Muffle furnace is warming up to 800 DEG C,
It puts it into Muffle furnace, calcines 1.5h after being continuously heating to 1370 DEG C of calcination temperature, product to be sintered takes when being cooled to 800 DEG C
Go out, be quickly cooled down, sintered product obtains sintered clinker from after dusting.
(D) 10g sintered clinkers and 150mL sodium carbonate liquors (0.9mol/L) accurately are weighed, is added to the reaction of 250mL
In kettle liner, 25min is reacted under the conditions of 50 DEG C and magnetic agitation (300rpm), generates silico-calcium residue and sodium aluminate solution
Mix products.
(E) mix products in step (D) are detached with Suction filtration device, filter residue is silico-calcium residue, can be used for fire coal in situ
The CO of power plant2Trapping；Appropriate calcium hydroxide solution is added in into filtrate, silicic acid sodium impurity is removed, is detached again with Suction filtration device
Afterwards, gained filtrate is to purify sodium aluminate solution.
(F) it is inclined accurately to weigh 50 mL purifying by a concentration of 0.2mol/L of purifying sodium aluminate solution in regulating step (E)
Sodium aluminate solution (0.2mol/L), is added in the pyroreaction kettle liner of 100mL, in 50 DEG C and magnetic agitation (300rpm)
Under the conditions of, it is passed through the CO of 15vol% thereto with microbubble aerating system2Gas adjusts CO2A diameter of 3mm of microbubble, gas
Body flow velocity is 40mL/min, reaction time 1h；Mix products are detached with Suction filtration device, and filter residue is aluminium hydroxide presoma, is filtered
Liquid is sodium carbonate liquor, by recycling sodium carbonate by-product after purifying, crystallizing.
(G) by the aluminium hydroxide presoma in step (F), dry 2h removals adsorb water, then 550 in 105 DEG C of baking oven
DEG C Muffle furnace in calcining 4h dehydration, crystallization, meso-porous nano gama-alumina product is obtained after cooling.
Embodiment 4
(A) 25g NaOH solids, 50g aluminous fly-ash and 75mL pure water accurately are weighed, the high temperature for being added to 1000mL is high
It presses in inner liner of reaction kettle, reacts 30min under the conditions of 110 DEG C；Mix products are detached with Suction filtration device, and filter residue is desiliconization ash, is filtered
Liquid is sodium silicate solution.
(B) 20 desiliconization ashes and 40g lime stones accurately are weighed, be added in 250mL corundum ball grinders, adjust drum's speed of rotation
For 180rpm, Ball-milling Time 10min；Using 200 mesh sifters, the raw material after ball milling are sieved, obtain grain size less than 74 μm
Raw material it is spare.
(C) raw material in step (B) are placed in 100mL alumina crucibles, when high temperature Muffle furnace is warming up to 800 DEG C,
It puts it into Muffle furnace, calcines 1.5h after being continuously heating to 1380 DEG C of calcination temperature, product to be sintered takes when being cooled to 800 DEG C
Go out, be quickly cooled down, sintered product obtains sintered clinker from after dusting.
(D) 10g sintered clinkers and 150mL sodium carbonate liquors (0.9mol/L) accurately are weighed, is added to the reaction of 250mL
In kettle liner, 20min is reacted under the conditions of 60 DEG C and magnetic agitation (300rpm), generates silico-calcium residue and sodium aluminate solution
Mix products.
(E) mix products in step (D) are detached with Suction filtration device, filter residue is silico-calcium residue, can be used for fire coal in situ
The CO of power plant2Trapping；Appropriate calcium hydroxide solution is added in into filtrate, silicic acid sodium impurity is removed, is detached again with Suction filtration device
Afterwards, gained filtrate is to purify sodium aluminate solution.
(F) it is inclined accurately to weigh 50 mL purifying by a concentration of 0.2mol/L of purifying sodium aluminate solution in regulating step (E)
Sodium aluminate solution (0.2mol/L), is added in the pyroreaction kettle liner of 100mL, in 65 DEG C and magnetic agitation (300rpm)
Under the conditions of, it is passed through the CO of 30vol% thereto with microbubble aerating system2Gas adjusts CO2A diameter of 4mm of microbubble, gas
Body flow velocity is 20mL/min, reaction time 1h；Mix products are detached with Suction filtration device, and filter residue is aluminium hydroxide presoma, is filtered
Liquid is sodium carbonate liquor, by recycling sodium carbonate by-product after purifying, crystallizing.
(G) by the aluminium hydroxide presoma in step (F), dry 2h removals adsorb water, then 550 in 105 DEG C of baking oven
DEG C Muffle furnace in calcining 4h dehydration, crystallization, meso-porous nano gama-alumina product is obtained after cooling.
Embodiment 5
(A) 25g NaOH solids, 50g aluminous fly-ash and 75mL pure water accurately are weighed, the high temperature for being added to 1000mL is high
It presses in inner liner of reaction kettle, reacts 30min under the conditions of 110 DEG C；Mix products are detached with Suction filtration device, and filter residue is desiliconization ash, is filtered
Liquid is sodium silicate solution.
(B) 20 desiliconization ashes and 40g lime stones accurately are weighed, be added in 250mL corundum ball grinders, adjust drum's speed of rotation
For 180rpm, Ball-milling Time 10min；Using 200 mesh sifters, the raw material after ball milling are sieved, obtain grain size less than 74 μm
Raw material it is spare.
(C) raw material in step (B) are placed in 100mL alumina crucibles, when high temperature Muffle furnace is warming up to 800 DEG C,
It puts it into Muffle furnace, calcines 1h after being continuously heating to 1390 DEG C of calcination temperature, product to be sintered takes when being cooled to 800 DEG C
Go out, be quickly cooled down, sintered product obtains sintered clinker from after dusting.
(D) 10g sintered clinkers and 100mL sodium carbonate liquors (0.9mol/L) accurately are weighed, is added to the reaction of 250mL
In kettle liner, 15min is reacted under the conditions of 70 DEG C and magnetic agitation (300rpm), generates silico-calcium residue and sodium aluminate solution
Mix products.
(E) mix products in step (D) are detached with Suction filtration device, filter residue is silico-calcium residue, can be used for fire coal in situ
The CO of power plant2Trapping；Appropriate calcium hydroxide solution is added in into filtrate, silicic acid sodium impurity is removed, is detached again with Suction filtration device
Afterwards, gained filtrate is to purify sodium aluminate solution.
(F) it is inclined accurately to weigh 50 mL purifying by a concentration of 0.4mol/L of purifying sodium aluminate solution in regulating step (E)
Sodium aluminate solution (0.4mol/L), is added in the pyroreaction kettle liner of 100mL, in 80 DEG C and magnetic agitation (300rpm)
Under the conditions of, it is passed through the CO of 15vol% thereto with microbubble aerating system2Gas adjusts CO2A diameter of 5mm of microbubble, gas
Body flow velocity is 80mL/min, reaction time 1h；Mix products are detached with Suction filtration device, and filter residue is aluminium hydroxide presoma, is filtered
Liquid is sodium carbonate liquor, by recycling sodium carbonate by-product after purifying, crystallizing.
(G) by the aluminium hydroxide presoma in step (F), dry 2h removals adsorb water, then 550 in 105 DEG C of baking oven
DEG C Muffle furnace in calcining 4h dehydration, crystallization, meso-porous nano gama-alumina product is obtained after cooling.
Embodiment 6
(A) 25g NaOH solids, 50g aluminous fly-ash and 75mL pure water accurately are weighed, the high temperature for being added to 1000mL is high
It presses in inner liner of reaction kettle, reacts 30min under the conditions of 110 DEG C；Mix products are detached with Suction filtration device, and filter residue is desiliconization ash, is filtered
Liquid is sodium silicate solution.
(B) 20 desiliconization ashes and 40g lime stones accurately are weighed, be added in 250mL corundum ball grinders, adjust drum's speed of rotation
For 180rpm, Ball-milling Time 10min；Using 200 mesh sifters, the raw material after ball milling are sieved, obtain grain size less than 74 μm
Raw material it is spare.
(C) raw material in step (B) are placed in 100mL alumina crucibles, when high temperature Muffle furnace is warming up to 800 DEG C,
It puts it into Muffle furnace, calcines 0.5h after being continuously heating to 1400 DEG C of calcination temperature, product to be sintered takes when being cooled to 800 DEG C
Go out, be quickly cooled down, sintered product obtains sintered clinker from after dusting.
(D) 10g sintered clinkers and 100mL sodium carbonate liquors (0.9mol/L) accurately are weighed, is added to the reaction of 250mL
In kettle liner, 15min is reacted under the conditions of 70 DEG C and magnetic agitation (300rpm), generates silico-calcium residue and sodium aluminate solution
Mix products.
(E) mix products in step (D) are detached with Suction filtration device, filter residue is silico-calcium residue, can be used for fire coal in situ
The CO of power plant2Trapping；Appropriate calcium hydroxide solution is added in into filtrate, silicic acid sodium impurity is removed, is detached again with Suction filtration device
Afterwards, gained filtrate is to purify sodium aluminate solution.
(F) it is inclined accurately to weigh 50 mL purifying by a concentration of 0.4mol/L of purifying sodium aluminate solution in regulating step (E)
Sodium aluminate solution (0.4mol/L), is added in the pyroreaction kettle liner of 100mL, in 80 DEG C and magnetic agitation (300rpm)
Under the conditions of, it is passed through the CO of 30vol% thereto with microbubble aerating system2Gas adjusts CO2A diameter of 5mm of microbubble, gas
Body flow velocity is 40mL/min, reaction time 1h；Mix products are detached with Suction filtration device, and filter residue is aluminium hydroxide presoma, is filtered
Liquid is sodium carbonate liquor, by recycling sodium carbonate by-product after purifying, crystallizing.
(G) by the aluminium hydroxide presoma in step (F), dry 2h removals adsorb water, then 400 in 105 DEG C of baking oven
DEG C Muffle furnace in calcining 8h dehydration, crystallization, meso-porous nano gama-alumina product is obtained after cooling.
To embodiment product analysis and comparison：
(1) alumina extraction efficiency comparative
Using the silent winged inductively coupled plasma spectrum generator of match, the aluminium element measured in purifying sodium aluminate solution is dense
Degree.Extraction efficiency (the η of aluminium oxide in aluminous fly-ash is calculated using formula (6)Al2O3, %), wherein MAl2O3And MAlIt is respectively
Al2O3Relative molecular mass, c with AlAlBe purify sodium aluminate solution in aluminium element concentration (mg/L), mSMIt is single experiment
Dosage (g), the V of sintered clinker are the volume (mL) for purifying sodium aluminate solution, WAl2O3It is the matter of aluminium oxide in sintered clinker
Measure score.
The extraction efficiency of aluminium oxide is as shown in table 1, and extraction efficiency calcines 1.0h items more than 75%, and at 1390 DEG C
Extraction efficiency can reach 87.42% under part.The extracting method cost of material is low, extraction efficiency is high, than existing report method more
Highly effective.
The extraction efficiency comparison of aluminium oxide in 1 embodiment 1-6 of table
(2) meso-porous nano gama-alumina structural parameters compare
The structural parameters of meso-porous nano gama-alumina product are measured using Mike's ASAP2020 nitrogen adsorptions instrument.According to sample
Nitrogen adsorption/desorption curve of product is as a result, be respectively adopted the ratio that BET formula, BJH formula and maximum single-point adsorbance calculate sample
Surface area, average pore size and pore volume, the results are shown in Table 2.The meso-porous nano gama-alumina of this technology synthesis has excellent
Structural behaviour, specific surface area are more than 200m2/ g, average pore size 3.5-4.0nm.The graph of pore diameter distribution of sample is as shown in Fig. 2, table
The pore-size distribution of bright sample is uniform, concentrates on 2-5nm, is typical ordered mesopore structure feature.
The structural parameters comparison of 2 embodiment 3-5 intermediary hole nanometer gama-alumina products of table
(3) the X-ray diffractogram spectrum analysis of 4 product of embodiment
Meso-porous nano gama-alumina is measured using X ray high-resolution diffractometer (Rigaku, D/max 2500PC types)
The diffraction maximum of product, instrument radiation source select Cu-K α (λ=0.15406nm).
Fig. 3 is small angle X-ray diffraction figure, and 2 0.6-5 ° of θ angular regions, sweep speed is 0.5 °/min.The result shows that sample
Occur apparent diffraction maximum at 2 θ=1.24 °, corresponded to (1 0 0) diffraction crystal face of sample, it was demonstrated that sample has formd
The hexagonal hole road structure of sequence.
Fig. 4 is X-ray diffractogram, and 2 10-90 ° of θ angular regions, sweep speed is 6 °/min.The result shows that sample 2 θ=
There is apparent diffraction maximum at 37.603 °, 45.862 ° and 67.032 °, corresponded to (the 31 of gama-alumina crystal respectively
1), (4 0 0) and (4 4 0) diffraction crystal face illustrates that the crystallinity of sample is high.
(4) the transmission electron microscope map analysis of 4 product of embodiment
Using the microscopic pattern of JEOL 2010F transmission electron microscope analysis meso-porous nano gama-alumina products, accelerating potential is
200kV.Fig. 5 the result shows that, sample shows parallel clearly black and white strip, illustrate sample form rule duct knot
Structure.
Claims (10)
- A kind of 1. method of aluminous fly-ash synthesizing mesoporous nano gama-alumina, which is characterized in that include the following steps：(A) pre-desiliconizing with high alumina fly ash：Aluminous fly-ash desiliconization is obtained into desiliconization ash；(B) raw material are prepared：Desiliconization ash in lime stone and step (A) is mixed, after screening, it is spare to obtain raw material；(C) sintered clinker is prepared：Raw material in step (B) are calcined at high temperature, sintered product is taken out, is quickly cooled down, are burnt Knot product obtains sintered clinker from after dusting；(D) sodium metaaluminate is dissolved out：Sintered clinker in step (C) and sodium carbonate liquor are mixed, after hydro-thermal reaction, generate silico-calcium The mix products of residue and sodium aluminate solution；(E) it detaches, purify sodium aluminate solution：By the mix products separation of solid and liquid in step (D), filter residue is silico-calcium residue, to Calcium hydroxide solution is added in filtrate, removes impurity, obtains purifying sodium aluminate solution after separation of solid and liquid again；(F) aluminium hydroxide presoma is synthesized：It is passed through with microbubble aerating system into the purifying sodium aluminate solution of step (E) The CO of 15-30vol%2Gas, CO2After sodium metaaluminate reaction, separation of solid and liquid, obtain aluminium hydroxide presoma and sodium carbonate is molten Liquid；(G) synthesizing mesoporous nano gama-alumina：By the aluminium hydroxide presoma drying removal absorption water in step (F), then calcine Dehydration, crystallization, obtain meso-porous nano gama-alumina product after cooling.
- 2. the method for aluminous fly-ash synthesizing mesoporous nano gama-alumina according to claim 1, which is characterized in that described In step (A), aluminous fly-ash and sodium hydroxide solution mixing after hydro-thermal reaction, separation of solid and liquid, obtain desiliconization ash and silicic acid Sodium solution.
- 3. the method for aluminous fly-ash synthesizing mesoporous nano gama-alumina according to claim 2, which is characterized in that described In step (A), concentration of sodium hydroxide solution 25wt%, the mass ratio of sodium hydrate solid and flyash is 0.5:1,110 DEG C high-temperature high-pressure reaction kettle in react 30min.
- 4. the method for aluminous fly-ash synthesizing mesoporous nano gama-alumina according to claim 1, which is characterized in that described In step (B), using planetary ball mill mixing lime stone and desiliconization ash, ball grinder used is corundum material, abrading-ball is oxidation Zirconium material, drum's speed of rotation 180rpm, Ball-milling Time 10min；Using 200 mesh sifters, the raw material after ball milling are sieved, It is spare less than 74 μm of raw material to obtain grain size.
- 5. according to the method for the aluminous fly-ash synthesizing mesoporous nano gama-alumina of claim 1 or 4, which is characterized in that institute It states in step (B), the ratio of lime stone and desiliconization ash meets in raw material：N (CaO)=2 × n (SiO2)+12/7×n(Al2O3)+2 ×n(Fe2O3)。
- 6. the method for aluminous fly-ash synthesizing mesoporous nano gama-alumina according to claim 1, which is characterized in that described In step (C), the charging temperature and tapping temperature of raw material are 800 DEG C, and calcination temperature is 1350-1400 DEG C, and calcination time is 0.5-2h；In the step (D), sodium carbonate liquor a concentration of 0.9mol/L, liquid-solid ratio 10-20, clinker and sodium carbonate liquor Mixing is placed in 30-70 DEG C of reaction kettle, reacts 15-30min under the conditions of the magnetic agitation of 300rpm.
- 7. the method for aluminous fly-ash synthesizing mesoporous nano gama-alumina according to claim 1, which is characterized in that described In step (E), silico-calcium residue is used for the CO of coal-burning power plant in situ2Trapping, it is mainly sodium metasilicate to remove impurity；The step (F) In, the sodium carbonate liquor is by recycling sodium carbonate by-product after purifying, crystallizing.
- 8. the method for aluminous fly-ash synthesizing mesoporous nano gama-alumina according to claim 1, which is characterized in that described In step (F), purifying a concentration of 0.1-0.4mol/L of sodium aluminate solution is first adjusted, is placed it in 20-80 DEG C of reaction kettle, The CO of 15-30vol% is passed through under the conditions of the magnetic agitation of 300rpm2Gas, reaction time 1h, adjusting gas flow cause n(CO2):n(NaAlO2)=1.6:1.
- 9. the method for aluminous fly-ash synthesizing mesoporous nano gama-alumina according to claim 8, which is characterized in that described In step (F), CO2Gas is passed into using microbubble aerating system in reaction kettle, is passed through CO2A diameter of 1-5mm of microbubble.
- 10. the method for aluminous fly-ash synthesizing mesoporous nano gama-alumina according to claim 1, which is characterized in that described In step (G), aluminium hydroxide presoma dry 2h removals absorption water in 105 DEG C of baking oven, then in 400-550 DEG C of Muffle furnace Middle calcining 4-8h dehydrations, crystallization.
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