CN104892010A - A method of extracting a silicon-aluminum composite refractory material from fly ash - Google Patents
A method of extracting a silicon-aluminum composite refractory material from fly ash Download PDFInfo
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Abstract
A method of extracting a silicon-aluminum composite refractory material from fly ash is disclosed. Traditional fly ash activation mainly adopts a mixed calcinating manner and is high in energy consumption. According to the method, fly ash is firstly mixed with an activating agent and water, and activation effects can be achieved in short time at a low temperature by an ultrasonic treatment manner. Extraction rates of silicon and aluminum can be effectively increased. An added auxiliary agent can effectively improve material compatibility, and enhance stability and fire resistance of a finished product. The method can be applied to steel, nonferrous metals, glass, cement, ceramics, petrochemicals, machines, boilers, the light industry, electricity, the military industry, and other fields of national economy, and is nontoxic, pollution-free, safe and environmental friendly.
Description
Technical field
The present invention relates generally to and extracts aluminium field, particularly relates to a kind of method extracting silicon, aluminium composite refractory from flyash.
Background technology
Flyash is the solid waste that coal-burning power plant discharges.Total volume of cargo in storage of current China flyash, more than 1,000,000,000 t, increase with the speed of annual 8000 ten thousand t now, and the utilization of flyash is less than 50%.Flyash is stored up and is not only taken a large amount of soils, contaminate environment, also jeopardize biological and people's health, and the many useful components in flyash can not get rational utilization, cause the wasting of resources.
In concrete, adding coal ash has saved a large amount of cement and fine aggregate; Decrease water consumption; Improve the workability of concrete batching system; The pumpability of Concrete Structure; Decrease concrete creeping; Reduce hydration heat, heat energy swelling property; Improve concrete impervious ability; Increase concrete modified.GB one-level: the modern concrete new technology adopting high-quality fly ash and high efficiency water reducing agent compounding technology to produce high-grade concrete develops rapidly in the whole nation.GB secondary: high-quality fly ash is specially adapted to preparation pump concrete, mass concrete, impervious structural concrete, sulfate resistance concrete and anti-soft water corrosion concrete and underground, underwater engineering concrete, intrusion concrete and roller compacted concrete.GB three grades: flyash concrete has the advantages such as workability is good, pumpability strong, finish improvement, impact resistance raising, frost resistance enhancing.Flyash is the one seemingly pozzolana mixed material that coal dust is formed after high-temp combustion.It is the coal dust that coal is worn into less than 100 microns by the power station of coal combustion, sprays into burner hearth become suspended state to burn with preheated air, produces and mixes the high-temperature flue gas having a large amount of incombustible substance, just obtains flyash through particle collector trapping.The chemical constitution of flyash is similar to clayey, and main component is silicon-dioxide, aluminium sesquioxide, ferric oxide, calcium oxide and uncompleted burned carbon.Flyash is mainly used to produce pulverized fuel ash cement, flyash brick, fly ash silicate building block, powder ash air-entrained concrete and other material of construction, also can be used as agricultural fertilizer and soil improvement agent, reclaims industrial raw material and makes environmentally conscious materials.The application of flyash in Cement industry and concrete works: flyash replaces raw clay to produce cement; add the levigate hydraulic glue gel material made of proper amount of gypsum by Portland clinker and flyash, Cement industry employing flyash batching can utilize unburnt carbon wherein; Flyash makes cement mixture; Flyash produces low-temperature synthesizing water mud, and production principle is that first for admixtion vapor cure is generated hydrate, then forms cement minerals through dehydration and low-temperature solid phase reaction; Flyash makes clinker-free cement; comprise lime fly ash cement and pure fly ash cement; lime fly ash cement the flyash of drying is mixed the unslaked lime of 10%-30% or slaked lime and a small amount of gypsum combined grinding, or the hydraulic cementing materials evenly made of levigate rear remix respectively; Flyash makes mortar or concrete Additive, in concrete, adding coal ash replaces part of cement or fine aggregate, can not only reduce costs, and concrete workability can be improved, improve waterproof, gas, Sulphate-resistant property and chemistry-resistant characteristic, reduction hydration heat, improve concrete resistance to elevated temperatures, alleviate particle separation and bleed phenomenon, reduce concrete contraction and cracking and suppress stray current to the corrosion of reinforcement in concrete.The application of flyash in building product: steam flyash brick; with fly ash in electric power plant and unslaked lime or other alkali-activators for main raw material; also appropriate gypsum can be mixed; and add the aggregates such as a certain amount of cinder or water-granulated slag, a kind of materials for wall formed after processing, stirring, digestion, rolling, compression moulding, normal pressure or autoclave curing; Fired fly ash brick, with flyash, clay and other industrial wastes for raw material, makes brick through Raw material processing, stirring, shaping, dry, roast; Steam pressure produces foam powder coal ash insulating brick, is main raw material, adds a certain amount of lime and foaming agent with flyash, through a kind of novel insulating brick of prepare burden, stir, burn injection forming and steam pressure; Fly ash silicate building block, with flyash, lime, gypsum for gelling material, cinder, blast-furnace slag etc. are aggregate, the materials for wall of add water stirring, vibratory compaction, vapor cure; Powder ash air-entrained concrete, take flyash as raw material, adds unslaked lime, cement, gypsum and aluminium powder in right amount, adds water and stirs in slurry, inject a kind of porous light material of construction that mould is steam-cured; Lytag, is main raw material with flyash, mixes a small amount of binding agent and solid fuel, through mixing, balling-up, high temperature roast and a kind of artificial lightweight aggregate made; Coal ash light heat insulation brick, be carry out batching with flyash, scoria, soft soil and wood chip to form, have insulating efficiency high, refractoriness is done, thermal conductivity is little, can alleviate furnace wall thickness, shortens firing time, reduces fuel consumption, improves thermo-efficiency, reduce costs.Flyash makes agricultural fertilizer and soil improvement agent: flyash has good physicochemical property, can be widely used in transforming heavy clay, the immature soil, sour earth and saline-alkali soil, make up the defect that its sour thin plate is sticky, containing necessary nutritive elements of farm crop such as a large amount of solubility in citric acid silicon-calcium-magnesium phosphorus in flyash, therefore agricultural fertilizer can be used as.Reclaim industrial raw material: reclaiming coal resource, utilize flotation process to add flotation reagent in containing the grey pulp-water of coal powder coal ash, then adopt air flotation technology, make coal grain adhere to bubble floating and be separated with lime-ash; Containing Fe in Footwall drift material flyash
2o
3, Al
2o
3, and a large amount of rare metal; Sorting cenosphere, cenosphere has that quality is little, high strength, high temperature resistant and good insulating, may be used for the ideal filler of plastics, and for lightweight refractory and thermal insulation material, for petrochemical industry, for military industry field, tank brakes.Make environment-friendly materials: utilize flyash can manufacture the environment-friendly materials such as molecular sieve, flocculation agent and sorbing material; Flyash also can be used for process fluoride waste, electroplating wastewater and contains heavy metal example waste water and oily(waste)water, the Al contained in flyash
2o
3, CaO isoreactivity component, can title complex be produced with fluorine or produce colloid ion fluorine being had to throwing out, also containing zeolite, mullite, carbon granule and silica gel etc., there is mineral ion commutativity and adsorption and decoloration.
Summary of the invention
The object of the invention is just to provide a kind of method extracting aluminium from flyash.
The present invention is achieved by the following technical solutions:
From flyash, extract a method for silicon, aluminium composite refractory, it is characterized in that comprising the following steps:
(1) flyash being ground to fineness is 200-300 order, adds activator, water, supersound process 4-6 minute under the frequency of 70-100kHz;
(2) material after above-mentioned supersound process is heated to water at 680-700 DEG C do, sends in retort furnace, roasting 30-40 minute at 900-1000 DEG C;
(3) above-mentioned roasting material is cooled to normal temperature, adds the sodium hydroxide of 6-10mol/l, insulation reaction 1-2 hour at 60-80 DEG C, filter, obtain siliceous filtrate and filter residue;
(4) joined by filter residue in its weight 1.8-2 hydrochloric acid soln doubly, concentration of hydrochloric acid is 30-40%, insulation reaction 1-2 hour at 100-120 DEG C, filters, obtains secondary filtrate and secondary filter residue;
(5) adjusting secondary filtrate PH value is 4-5, after precipitation, filtration, obtain three filter residues and three filtrates, and three times filter residue calcines 50-60 minute after washing, oven dry at 1000-1200 DEG C, obtains aluminum oxide;
(6) by above-mentioned siliceous filtrate, secondary filter residue, aluminum oxide mixing, add auxiliary agent, drying treatment at supersound process 10-12 minute, 100-120 DEG C under the frequency of 30-60kHz, wear into fine powder after drying completely, obtain described refractory materials.
From flyash, extract a method for silicon, aluminium composite refractory, the activator described in step (1) is made up of the raw material of following weight parts: Sodium dodecylbenzene sulfonate 1-weight part, Amino Trimethylene Phosphonic Acid 2-3 part, Sodium Silicofluoride 6-10 part, potassium tetraborate 1-2 part; The part by weight of described activator, water and flyash is 1-2:100:31-50.
A kind of method extracting silicon, aluminium composite refractory from flyash, auxiliary agent described in step (6) is made up of the raw material of following weight parts: zirconium dioxide 3-5 weight part, tea saponin 1-2 weight part, calcium oxide 6-10 weight part, hexagonal boron nitride 4-6 weight part, aluminium dihydrogen phosphate 1-2 weight part, organosilicon crylic acid latex 3-4 weight part, deionized water 100-120 weight part, and the weight ratio of described auxiliary agent and siliceous filtrate, secondary filter residue, aluminum oxide compound is 10:1-1.2.
From flyash, extract a method for silicon, aluminium composite refractory, the preparation method of the auxiliary agent described in step (6) comprises the following steps:
Calcium oxide is joined in the deionized water of 3-4 times of weight, stir, obtain liquid a;
Tea saponin is joined in the deionized water of 6-10 times of weight, stir, obtain liquid b;
Joined in remaining deionized water by organosilicon crylic acid latex, add aluminium dihydrogen phosphate, raised temperature is 60-65 DEG C, adds liquid a, liquid b, insulated and stirred 20-30 minute, and add a residue raw material, 500-1000 rev/min of dispersed with stirring 3-5 minute, obtains described auxiliary agent.
Advantage of the present invention is:
Traditional flyash activating is mostly all by baking mixed method, energy consumption is higher, the present invention is first by flyash and activator, water mixes, by the mode of supersound process, can in the short period of time, lesser temps is issued to activation effect, effectively can improve silicon, the extraction yield of aluminium, the auxiliary agent added not only effectively can improve the consistency of each storeroom, stability and the resistivity against fire of finished product can also be improved, iron and steel can be applied to, non-ferrous metal, glass, cement, pottery, petrochemical industry, machinery, boiler, light industry, electric power, the every field of the national economy such as military project, nontoxic without pollution-free, safety and environmental protection.
Embodiment
Chemical composition in the flyash adopted in the embodiment of the present invention consists of:
SiO
254.34%；
Al
2O
326.17%；
Fe
2O
312.31%；
CaO 5.03%；
MgO 1.79%；
SO
3 0.19%；
Remaining is loss on ignition.
Embodiment 1:
From flyash, extract a method for silicon, aluminium composite refractory, it is characterized in that comprising the following steps:
(1) flyash being ground to fineness is 300 orders, adds activator, water, supersound process 4 minutes under the frequency of 90kHz;
(2) material after above-mentioned supersound process is heated to water at 700 DEG C do, sends in retort furnace, roasting 31 minutes at 1000 DEG C;
(3) above-mentioned roasting material is cooled to normal temperature, adds the sodium hydroxide of 9mol/l, insulation reaction 1 hour at 80 DEG C, filter, obtain siliceous filtrate and filter residue;
(4) joined by filter residue in its weight 1.8-2 hydrochloric acid soln doubly, concentration of hydrochloric acid is 33%, insulation reaction 1 hour at 120 DEG C, filters, obtains secondary filtrate and secondary filter residue;
(5) adjusting secondary filtrate PH value is 4, after precipitation, filtration, obtain three filter residues and three filtrates, and three times filter residue is calcined 60 minutes after washing, oven dry at 1200 DEG C, obtains aluminum oxide;
(6) by above-mentioned siliceous filtrate, secondary filter residue, aluminum oxide mixing, add auxiliary agent, supersound process 12 minutes under the frequency of 30-60kHz, drying treatment at 120 DEG C, wear into fine powder after drying completely, obtain described refractory materials.
From flyash, extract a method for silicon, aluminium composite refractory, the activator described in step (1) is made up of the raw material of following weight parts: Sodium dodecylbenzene sulfonate 1-weight part, Amino Trimethylene Phosphonic Acid 2 parts, Sodium Silicofluoride 10 parts, potassium tetraborate 2 parts; The part by weight of described activator, water and flyash is 1:100:43.
A kind of method extracting silicon, aluminium composite refractory from flyash, auxiliary agent described in step (6) is made up of the raw material of following weight parts: zirconium dioxide 3 weight part, tea saponin 1.4 weight part, calcium oxide 8 weight part, hexagonal boron nitride 4 weight part, aluminium dihydrogen phosphate 1.5 weight part, organosilicon crylic acid latex 3 weight part, deionized water 100 weight part, and the weight ratio of described auxiliary agent and siliceous filtrate, secondary filter residue, aluminum oxide compound is 10:1.
From flyash, extract a method for silicon, aluminium composite refractory, the preparation method of the auxiliary agent described in step (6) comprises the following steps:
Calcium oxide is joined in the deionized water of 3 times of weight, stir, obtain liquid a;
Tea saponin is joined in the deionized water of 8 times of weight, stir, obtain liquid b;
Joined in remaining deionized water by organosilicon crylic acid latex, add aluminium dihydrogen phosphate, raised temperature is 65 DEG C, adds liquid a, liquid b, insulated and stirred 30 minutes, adds a residue raw material, and 700 revs/min of dispersed with stirring 4 minutes, obtain described auxiliary agent.
Embodiment 2
From flyash, extract a method for silicon, aluminium composite refractory, comprise the following steps:
(1) flyash being ground to fineness is 200 orders, adds activator, water, supersound process 5 minutes under the frequency of 100kHz;
(2) material after above-mentioned supersound process is heated to water at 700 DEG C do, sends in retort furnace, roasting 37 minutes at 1000 DEG C;
(3) above-mentioned roasting material is cooled to normal temperature, adds the sodium hydroxide of 10mol/l, insulation reaction 1 hour at 80 DEG C, filter, obtain siliceous filtrate and filter residue;
(4) joined by filter residue in the hydrochloric acid soln of its weight 1.8 times, concentration of hydrochloric acid is 40%, insulation reaction 1 hour at 120 DEG C, filters, obtains secondary filtrate and secondary filter residue;
(5) adjusting secondary filtrate PH value is 4, after precipitation, filtration, obtain three filter residues and three filtrates, and three times filter residue is calcined 55 minutes after washing, oven dry at 1100 DEG C, obtains aluminum oxide;
(6) by above-mentioned siliceous filtrate, secondary filter residue, aluminum oxide mixing, add auxiliary agent, supersound process 11 minutes under the frequency of 50kHz, drying treatment at 110 DEG C, wear into fine powder after drying completely, obtain described refractory materials.
From flyash, extract a method for silicon, aluminium composite refractory, the activator described in step (1) is made up of the raw material of following weight parts: Sodium dodecylbenzene sulfonate 1 weight part, Amino Trimethylene Phosphonic Acid 2 parts, Sodium Silicofluoride 9 parts, potassium tetraborate 1 part; The part by weight of described activator, water and flyash is 1:100:33.
A kind of method extracting silicon, aluminium composite refractory from flyash, auxiliary agent described in step (6) is made up of the raw material of following weight parts: zirconium dioxide 4 weight part, tea saponin 1 weight part, calcium oxide 7 weight part, hexagonal boron nitride 5 weight part, aluminium dihydrogen phosphate 1 weight part, organosilicon crylic acid latex 3 weight part, deionized water 110 weight part, and the weight ratio of described auxiliary agent and siliceous filtrate, secondary filter residue, aluminum oxide compound is 10:1.
From flyash, extract a method for silicon, aluminium composite refractory, the preparation method of the auxiliary agent described in step (6) comprises the following steps:
Calcium oxide is joined in the deionized water of 3-4 times of weight, stir, obtain liquid a;
Tea saponin is joined in the deionized water of 6-10 times of weight, stir, obtain liquid b;
Joined in remaining deionized water by organosilicon crylic acid latex, add aluminium dihydrogen phosphate, raised temperature is 60 DEG C, adds liquid a, liquid b, insulated and stirred 27 minutes, adds a residue raw material, and 800 revs/min of dispersed with stirring 3 minutes, obtain described auxiliary agent.
Embodiment 3
From flyash, extract a method for silicon, aluminium composite refractory, it is characterized in that comprising the following steps:
(1) flyash being ground to fineness is 300 orders, adds activator, water, supersound process 4 minutes under the frequency of 100kHz;
(2) material after above-mentioned supersound process is heated to water at 700 DEG C do, sends in retort furnace, roasting 40 minutes at 1000 DEG C;
(3) above-mentioned roasting material is cooled to normal temperature, adds the sodium hydroxide of 10mol/l, insulation reaction 1 hour at 80 DEG C, filter, obtain siliceous filtrate and filter residue;
(4) joined by filter residue in the hydrochloric acid soln of its weight 1.8 times, concentration of hydrochloric acid is 40%, insulation reaction 1 hour at 120 DEG C, filters, obtains secondary filtrate and secondary filter residue;
(5) adjusting secondary filtrate PH value is 5, after precipitation, filtration, obtain three filter residues and three filtrates, and three times filter residue is calcined 60 minutes after washing, oven dry at 1200 DEG C, obtains aluminum oxide;
(6) by above-mentioned siliceous filtrate, secondary filter residue, aluminum oxide mixing, add auxiliary agent, supersound process 12 minutes under the frequency of 60kHz, drying treatment at 120 DEG C, wear into fine powder after drying completely, obtain described refractory materials.
From flyash, extract a method for silicon, aluminium composite refractory, the activator described in step (1) is made up of the raw material of following weight parts: Sodium dodecylbenzene sulfonate 1-weight part, Amino Trimethylene Phosphonic Acid 2 parts, Sodium Silicofluoride 10 parts, potassium tetraborate 1 part; The part by weight of described activator, water and flyash is 2:100:50.
A kind of method extracting silicon, aluminium composite refractory from flyash, auxiliary agent described in step (6) is made up of the raw material of following weight parts: zirconium dioxide 5 weight part, tea saponin 2 weight part, calcium oxide 6-10 weight part, hexagonal boron nitride 4 weight part, aluminium dihydrogen phosphate 1 weight part, organosilicon crylic acid latex 4 weight part, deionized water 120 weight part, and the weight ratio of described auxiliary agent and siliceous filtrate, secondary filter residue, aluminum oxide compound is 10:1.2.
From flyash, extract a method for silicon, aluminium composite refractory, the preparation method of the auxiliary agent described in step (6) comprises the following steps:
Calcium oxide is joined in the deionized water of 3-4 times of weight, stir, obtain liquid a;
Tea saponin is joined in the deionized water of 6-10 times of weight, stir, obtain liquid b;
Joined in remaining deionized water by organosilicon crylic acid latex, add aluminium dihydrogen phosphate, raised temperature is 65 DEG C, adds liquid a, liquid b, insulated and stirred 30 minutes, adds a residue raw material, and 1000 revs/min of dispersed with stirring 5 minutes, obtain described auxiliary agent.
Claims (4)
1. from flyash, extract a method for silicon, aluminium composite refractory, it is characterized in that comprising the following steps:
(1) flyash being ground to fineness is 200-300 order, adds activator, water, supersound process 4-6 minute under the frequency of 70-100kHz;
(2) material after above-mentioned supersound process is heated to water at 680-700 DEG C do, sends in retort furnace, roasting 30-40 minute at 900-1000 DEG C;
(3) above-mentioned roasting material is cooled to normal temperature, adds the sodium hydroxide of 6-10mol/L, insulation reaction 1-2 hour at 60-80 DEG C, filter, obtain siliceous filtrate and filter residue;
(4) joined by filter residue in its weight 1.8-2 hydrochloric acid soln doubly, concentration of hydrochloric acid is 30-40%, insulation reaction 1-2 hour at 100-120 DEG C, filters, obtains secondary filtrate and secondary filter residue;
(5) adjusting secondary filtrate PH value is 4-5, after precipitation, filtration, obtain three filter residues and three filtrates, and three times filter residue calcines 50-60 minute after washing, oven dry at 1000-1200 DEG C, obtains aluminum oxide;
(6) by above-mentioned siliceous filtrate, secondary filter residue, aluminum oxide mixing, add auxiliary agent, drying treatment at supersound process 10-12 minute, 100-120 DEG C under the frequency of 30-60kHz, wear into fine powder after drying completely, obtain described refractory materials.
2. a kind of method extracting silicon, aluminium composite refractory from flyash according to claim 1, is characterized in that what the activator described in step (1) was made up of the raw material of following weight parts: Sodium dodecylbenzene sulfonate 1-weight part, Amino Trimethylene Phosphonic Acid 2-3 part, Sodium Silicofluoride 6-10 part, potassium tetraborate 1-2 part; The part by weight of described activator, water and flyash is 1-2:100:31-50.
3. a kind of method extracting silicon, aluminium composite refractory from flyash according to claim 1, it is characterized in that what the auxiliary agent described in step (6) was made up of the raw material of following weight parts: zirconium dioxide 3-5 weight part, tea saponin 1-2 weight part, calcium oxide 6-10 weight part, hexagonal boron nitride 4-6 weight part, aluminium dihydrogen phosphate 1-2 weight part, organosilicon crylic acid latex 3-4 weight part, deionized water 100-120 weight part, the weight ratio of described auxiliary agent and siliceous filtrate, secondary filter residue, aluminum oxide compound is 10:1-1.2.
4. a kind of method extracting silicon, aluminium composite refractory from flyash according to claim 1, is characterized in that the preparation method of the auxiliary agent described in step (6) comprises the following steps:
Calcium oxide is joined in the deionized water of 3-4 times of weight, stir, obtain liquid a;
Tea saponin is joined in the deionized water of 6-10 times of weight, stir, obtain liquid b;
Joined in remaining deionized water by organosilicon crylic acid latex, add aluminium dihydrogen phosphate, raised temperature is 60-65 DEG C, adds liquid a, liquid b, insulated and stirred 20-30 minute, and add a residue raw material, 500-1000 rev/min of dispersed with stirring 3-5 minute, obtains described auxiliary agent.
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| CN201510253290.5A CN104892010B (en) | 2015-05-19 | 2015-05-19 | It is a kind of that silicon, the method for aluminium composite refractory are extracted from flyash |
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| CN107445185A (en) * | 2017-09-29 | 2017-12-08 | 广州百兴网络科技有限公司 | A kind of coal ash for manufacturing for aluminium polychloride method |
| CN117602917A (en) * | 2024-01-22 | 2024-02-27 | 中建八局西南建设工程有限公司 | Solid waste base composite curing agent and preparation method thereof |
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| CN101700491A (en) * | 2009-11-09 | 2010-05-05 | 中国海洋石油总公司 | Method for modifying fly ash |
| CN102923742A (en) * | 2012-11-19 | 2013-02-13 | 河北工程大学 | Method for comprehensively extracting aluminum and lithium from coal ash |
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| CN101700491A (en) * | 2009-11-09 | 2010-05-05 | 中国海洋石油总公司 | Method for modifying fly ash |
| CN102923742A (en) * | 2012-11-19 | 2013-02-13 | 河北工程大学 | Method for comprehensively extracting aluminum and lithium from coal ash |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107445185A (en) * | 2017-09-29 | 2017-12-08 | 广州百兴网络科技有限公司 | A kind of coal ash for manufacturing for aluminium polychloride method |
| CN117602917A (en) * | 2024-01-22 | 2024-02-27 | 中建八局西南建设工程有限公司 | Solid waste base composite curing agent and preparation method thereof |
| CN117602917B (en) * | 2024-01-22 | 2024-03-22 | 中建八局西南建设工程有限公司 | Solid waste base composite curing agent and preparation method thereof |
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