CN103145161A - Method for preparing pseudo-boehmite co-preparation white carbon black by coal gangue - Google Patents
Method for preparing pseudo-boehmite co-preparation white carbon black by coal gangue Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides a method for preparing pseudo-boehmite co-preparation white carbon black by coal gangue. The method comprises the steps: the coal gangue is ground, roasted, alkaline-leached and filtered so that sodium silicate solution and alkaline leaching dregs are obtained, a dispersing agent is added to the sodium silicate solution and after gas containing CO2 is fed into the solution, a white carbon black product is prepared; lime and sodium carbonate are added into the alkaline leaching dregs for sintering, clinker obtained by the sintering is water-quenched to obtain NaAlO2 solution, the gas containing CO2 is added to the NaAlO2 solution for carbonation to form glue, ageing treatment is performed to seriflux after glue forming and powder-shaped pseudo-boehmite is obtained after the aged seriflux is washed, filtered, dried and smashed. The coal gangue serves as a raw material for preparation of the pseudo-boehmite and the white carbon black so that high-valued comprehensive utilization of industry solid wastes is achieved and an additional value of a product is high; all by-products can be recovered and recycled so that zero release, low energy consumption, economy and environment protection are achieved; and a requirement for a device is low, the while coal black prepared and the pseudo-boehmite prepared are high in purity, fine and even in granularity and high in specific surface area.
Description
Technical field
The present invention relates to a kind of method that is prepared the pseudo-boehmite co-producing white carbon black by coal gangue, relate in particular to a kind of method of utilizing the coal gangue alkaline process to prepare the pseudo-boehmite co-producing white carbon black.
Background technology
Coal gangue is to compose the main intergrowth mineral thing that is stored in coal measure strata, they generally are positioned at roof or base plate, or be present in the coal seam with the form of dirt band, often being used as solid waste in progress of coal mining abandons, not only cause the waste of resource, and the accumulation earth's surface, occupy the good farmland, cause serious environmental pollution.Based on comprehensive utilization of resources, environment protection and the requirement of developing a circular economy, carry out take coal gangue as raw material, produce the high added value Chemicals such as pseudo-boehmite and white carbon black and have very important economic implications and social effect.
At present, there has been the pseudo-boehmite production method of report to have a variety of.Representative method comprise disclosed slurries take aluminium hydroxide in CN 1247773 as raw material (these slurries by a kind of solution of aluminum contained compound and a kind of precipitant solution at least 50 ℃ of temperature with keep pH value 7.5～8.8 conditions under contact make), at the temperature of at least 50 ℃, add successively acid reagent and alkaline reagents in these slurries, the pH value of slurries is dropped to below 5, make again slurry pH value go back up to 9.4～10.4, filtration, washing, drying, obtain pseudo-boehmite, roasting again obtains gama-alumina.And the disclosed preparation process of pseudoboehmite of CN100999328, comprising: a) be enough to make under the acidic conditions of aluminum precipitation, the aluminium in the aqueous solution of precipitation aluminum contained compound is isolated to a kind of unbodied hydrated aluminum oxide; B) unbodied hydrated aluminum oxide, water and at least a water miscible alkali are mixed, pulp, slurries in 20 ℃ to 90 ℃ aging 0.2 hour to 6 hours, wherein, it is 6-11 that the consumption of described alkali makes the pH value of slurries.The preparation method of the disclosed pseudo-boehmite of CN101172631, sodium aluminate solution is carried out carbonating plastic, aging, separating, washing and drying, after it is characterized in that sodium aluminate solution carbonating plastic, at first carry out slurries and separate, then it is aging to carry out temperature raising after adding the wash water mixing to pull an oar filter cake.The preparation method of the disclosed pseudo-boehmite of CN101665262, comprise, with sodium aluminate solution carbonation become that slurries, slurries are warmed up to that aging temperature, slurries are aging, filtering separation, washing and dry step, wherein, also comprise in described method and add seed precipitation solution in the described slurries or plant minute washing lotion.The time that adds described seed precipitation solution or plant minute washing lotion is that described slurries are when being warmed up to aging temperature or in described slurries weathering process.
In a word, the preparation method of existing pseudo-boehmite is mainly that the raw materials cost of production is higher take aluminium hydroxide and industrial sodium metaaluminate as raw material production, and when containing siliceous composition in raw material, the overwhelming majority is effluxed as residue, and resource utilization is low, and environment is damaged.
Coal gangue contains abundant aluminum oxide and silicon-dioxide resource, is splendid production pseudo-boehmite and the raw material of white carbon black product.Be that the preparation that raw material carries out the pseudo-boehmite co-producing white carbon black becomes problems to be solved as coal gangue how.
Summary of the invention
The invention provides a kind of method that coal gangue alkaline process makes the pseudo-boehmite co-producing white carbon black; solve defective of the prior art, realize reducing raw materials cost, resource utilization is provided; in the time of protection of the environment, obtain pseudo-boehmite and white carbon black with good quality.
A kind of method of utilizing coal gangue to prepare the pseudo-boehmite co-producing white carbon black provided by the invention comprises the following steps:
1) the coal gangue powder of preparation activation: with cooling after coal gangue fragmentation, abrasive dust, removal of impurities, roasting, the coal gangue powder that obtains activating;
2) alkali soaks desiliconization: the coal gangue powder of above-mentioned activation is leached with sodium hydroxide solution, and filtration obtains sodium silicate solution and alkali soaks slag;
3) preparation white carbon black comprises:
A, add dispersion agent in described sodium silicate solution, and pass into and contain CO
2Gas carry out carbonating and process, carbonation reaction finishes when the pH of solution is 4 ~ 7, filters, and obtains orthosilicic acid precipitated filter cakes and filtrate;
B, described orthosilicic acid precipitated filter cakes is carried out ageing, roasting, pulverize and obtain white carbon black;
4) preparation pseudo-boehmite comprises:
A, with step 2) alkali that makes soak slag and mix with sodium carbonate and Wingdale after sintering, obtain grog, what produce in sintering process contains CO
2Gas recovery make carbonating and use;
Then b, cooling described grog obtain NaAlO through shrend, filtration
2Thick liquid and calcium silicate slag, described NaAlO
2Thick liquid obtains NaAlO after with the lime milk solution deep desilication
2Seminal fluid;
C, the described NaAlO of use distilled water diluting
2Seminal fluid obtains NaAlO
2Solution is to NaAlO
2Pass in solution and contain CO
2Gas carry out the carbonating plastic, after plastic reaction is completed, reacting slurry is carried out burin-in process, then filter and obtain glue and filtrate, glue obtains pulverous pseudo-boehmite through washing, dry, pulverization process.
In method provided by the invention, adopt alkaline process desiliconization and soda-lime sintering process, little to the corrosion of equipment, the by product that produces in method (as contains CO
2Gas, filtrate and a small amount of calcium silicate slag) all recycling uses, for example: what produce in sintering process contains CO
2Gas can pass into sodium silicate solution and/or NaAlO
2Carry out carbonating in solution and process, obtain orthosilicic acid precipitated filter cakes and filtrate after filtration, glue and filtrate (being generally dilute sodium carbonate solution) can recycle as raw material after evaporation concentration; Step 4-b) a small amount of calcium silicate slag that produces in can be made into high standard cement, makes whole processing method realize zero release.
In the solution of the present invention, step 1) prepare in the coal gangue powder process of activation: it is 50-300 purpose powder that coal gangue is broken into granularity, and the temperature range of roasting can be 700-1050 ℃, and the time of roasting can be 30 ~ 60 minutes.Be in order to make kaolinite activation wherein to the roasting of Coal gangue powder, reasonably grinding particle size can further improve the efficient of activation, when the temperature of roasting is 700-1050 ℃, and the SiO in kaolinite
2Change the amorphous Si O that is easy to alkali reaction into
2, the amorphous Al in kaolinite
2O
3Be converted into the γ-Al of crystalline state
2O
3, the γ-Al of crystalline state
2O
3Stable chemical nature, thus aluminium is stayed in desiliconization under the effect that alkali soaks; When being heated to 950-1050 ℃, SiO
2Stable the existing with metamict of energy, Al
2O
3Can be stably with γ-Al
2O
3Crystalline state exists, thereby further improves the desiliconization rate.
In a specific embodiment of the present invention, step 2) alkali soaks that to may be controlled in desiliconization process under 80 ~ 100 ℃ of conditions be the described coal gangue powder of 5-25% sodium hydroxide solution leaching 30 ~ 90 minutes with massfraction, and total consumption of sodium hydroxide is according to Na
2O:SiO
2=1.0 ~ 1.2 mol ratio is calculated.Further, can be the described coal gangue powder of 10% ~ 20% sodium hydroxide solution leaching 50 ~ 70 minutes with massfraction step 2).Further, can be the described coal gangue powder of 15% sodium hydroxide solution leaching 60 minutes with massfraction step 2).Carry out under these conditions alkali and soak and greatly to improve the alumina silica ratio that alkali soaks slag, not only satisfied the requirement of soda-lime sintering process to raw material, also greatly improved Al
2O
3Actual solubility rate, reduced the consumption of Wingdale, and can reduce the side reaction in the soda-lime sintering process, reduce the amount of by product calcium silicate slag.
In a specific embodiment of the present invention, in the process of preparation white carbon black, control step 3-a) condition of acidification can for: the quality of the dispersion agent that adds is 0.5 ~ 5% of sodium silicate solution, and what add contains CO
2Gas in CO
2Volumetric concentration be not less than 15%, 50 ~ 95 ℃ of the starting temperatures of carbonation reaction, pressure is 0.25 ~ 0.4Mpa, terminal temperature is 40 ~ 60 ℃, carbonation reaction finishes when the pH of solution is 6.Further, pass into step 3-a) and contain CO
2Volumetric concentration be that 30 ~ 60% gas carries out carbonating and processes.The quality of the dispersion agent that further, adds is sodium silicate solution or NaAlO
2Solution quality is 0.6 ~ 1%.Further, the dispersion agent step 3-a) is selected from one or more in Sodium hexametaphosphate 99, polyoxyethylene glycol, sodium lauryl sulphate, polyvinyl alcohol and trolamine.Further, dispersion agent is comprised of Sodium hexametaphosphate 99 and the polyoxyethylene glycol mass ratio by 1:1.
Step 3-b) in, the orthosilicic acid precipitated filter cakes is carried out ageing in the ageing tank of 75 ℃ of temperature, the time is 6 ~ 9 hours, dewaters under 200 ~ 250 ℃ of conditions, then 500 ~ 650 ℃ of roastings 1 hour, pulverizes and namely gets white carbon black.
In a specific embodiment of the present invention, can be ageing 6 ~ 9 hours under 5 ~ 7 condition in the pH value with the orthosilicic acid precipitated filter cakes, can obtain the more tiny uniform silicon-dioxide of particle, in 200 ~ 250 ℃ of dehydrations, then 500 ~ 650 ℃ of roastings 1 hour.
The particle diameter of the white carbon black that the inventive method makes is at 15 ~ 50nm, and can have 250-350m
2The specific surface area of/g, and the purity of 98% left and right.
In a specific embodiment of the present invention, the process of preparation pseudo-boehmite, step 4-a) may be controlled to alkali is soaked slag and sodium carbonate and Wingdale according to mol ratio: Ca/Si=2 ~ 3, mix Na/Al=1 ~ 1.2, carry out sintering under 1000～1350 ℃, obtain grog, sintering time is controlled to be 0.5 ~ 1 hour.Preferably, step 4-a): alkali is soaked slag, sodium carbonate and Wingdale according to mass ratio: Ca/Si=2, and Na/Al=1 mixes, and carries out sintering processes under 1200 ~ 1300 ℃, and the time is controlled at 50 minutes.Above-mentioned blending ratio and sintering time both can guarantee that each material can fully react in sintering process, again because alkali to soak in slag silicone content few, the consumption of the Wingdale of allocating into is few, has increased Al
2O
3With Na
2CO
3Contact, thereby greatly improve Al
2O
3Leaching yield.
Further, the clinker cooling to 600 of sintering ~ 700 ℃ can be taken out the β-2CaOSiO in grog from agglomerating plant (for example: alkali melts device)
2Change rapidly γ-2CaOSiO into
2, volumetric expansion, proportion reduces, and causes crystal to become fine powder, and grog is produced from efflorescence.Thereby make soda-lime sintering process technique have more excellent economy.
Further, step 4-b) in, the temperature of shrend can be controlled at 20 ℃-30 ℃, and the time can be controlled at 30 ~ 60min, and the condition of deep desilication is: lime milk solution concentration is 5 ~ 25wt%, and total consumption of calcium hydroxide is according to Ca
2O:SiO
2=0.8 ~ 1.2 mol ratio is calculated, and the deep desilication time is 3 ~ 10 minutes.
Step 4-c) in to NaAlO
2Pass in solution and contain CO
2Volumetric concentration is that 30 ~ 50% gas carries out the carbonating plastic, and the plastic reaction conditions is temperature: 20 ~ 45 ℃, and the time: 45 ~ 90 minutes.Further, NaAlO step 4-c)
2Solution is to make the Al that is diluted with distilled water into
2O
3Concentration is rare NaAlO of 30 ~ 65g/L
2Solution.
Further, at step 4-c) in to NaAlO
2After adding the expanding agent of 0.1 ~ 0.5wt% in solution, under the stirring velocity of 800-2000r/min, pass into and contain CO
2Volumetric concentration is that 30 ~ 50% gas carries out the carbonating plastic, and the plastic reaction conditions is temperature: 20 ~ 45 ℃, the time: 45 ~ 90 minutes, described expanding agent was one or more in gac, polyvinyl alcohol, polyacrylamide, Mierocrystalline cellulose, urea and starch.
Step 4-c) after in, the plastic reaction is completed, described reacting slurry is warmed up to 60 ~ 100 ℃, is incubated aging 2 ~ 6 hours.
In another embodiment of the present invention, step 2) alkali soaks in desiliconization process sodium hydroxide solution and divides and can add the described coal gangue powder of leaching for twice, the massfraction of the sodium hydroxide solution that adds is 15 ~ 20%, the quality that adds for the first time sodium hydroxide is the 50-80% of sodium hydroxide total amount, and alkali time of soaking is 30 ~ 40 minutes for the first time; The sodium hydroxide that adds for the second time residual mass, alkali time of soaking is 20 ~ 30 minutes for the second time.
due in soaking the process of desiliconization with alkali, soak the continuation of time along with alkali, the viscosity of sodium silicate solution constantly increases, desilication efficiency is more and more lower, alkali soaks weak effect, in prior art, in order to improve desiliconization speed and desiliconization rate, adopt two sections stripping desiliconizations, namely carry out solid-liquid separation after desiliconization for some time, and filter cake is reentered into continuation stirring stripping in new alkali lye, but two sections stripping desiliconizations have increased processing step and cost, extended total operating time, increased the aluminium loss amount, simultaneously, the high co-producing white carbon black of abandoning of aluminum content in sodium silicate solution due to alkali after soaking, make a low multiple use, value-added content of product is low.
add sodium hydroxide solution leaching powder twice of the present invention's employing, the massfraction of sodium hydroxide solution is 15 ~ 20%, the amount that adds for the first time sodium hydroxide is the 50-80% of sodium hydroxide total amount, under this condition, desilication reaction can carry out with speed of reaction faster in the early stage, when reaction proceeds to certain degree, it is large that the viscosity of reaction solution becomes, at this moment add remaining sodium hydroxide solution, both replenished the amount of sodium hydroxide in the reaction solution, again reaction solution has been played diluting effect, reduced the viscosity of reaction solution, make desilication reaction to go on speed faster, improved the efficient of desiliconization.Add sodium hydroxide solution leaching powder for twice, the one, improved the efficient of desiliconization, thereby improved the utilization ratio of silicon and increased alumina silica ratio, the carrying out that is conducive to follow-up white lime sintering process, the 2nd, greatly reduce alkali and soaked the aluminium loss amount of process, be conducive to improve the utilization ratio of aluminium, reduced simultaneously the aluminium content in the alkali immersion liquid, be conducive to the purification in subsequent production white carbon black process.
The particle diameter of the pseudo-boehmite that the inventive method makes is at 35 ~ 100nm, and can have 300-350m
2The specific surface area of/g, the pore volume of 1.2-2.0ml/g is better than existing macropore pseudo-boehmite specific surface area (250m
2/ g) and the performance index of pore volume (0.3-1.0ml/g).
Scheme provided by the invention has the following advantages:
1. the present invention adopts coal gangue as the raw material of producing pseudo-boehmite and white carbon black, has realized the high-valued comprehensive utilization of industrial solid castoff, and value-added content of product is high;
2. in the present invention, all by product is all recyclable, has realized zero release, and energy consumption is low, economic environmental protection;
3. utilization of the present invention utilizes alkaline process desiliconization and soda-lime sintering process, to equipment require low;
4. the white carbon black of producing and pseudo-boehmite purity is high, uniform particles, fine size.
Description of drawings
The X-ray diffractogram of the pseudo-boehmite powder of Fig. 1 embodiment 1 preparation.
Embodiment
Below in conjunction with embodiment, the present invention is described in more detail; but not thereby limiting the invention; under the prerequisite that does not break away from design philosophy of the present invention, the various changes and modifications that those skilled in the art make technical scheme of the present invention all belong to protection scope of the present invention.
Embodiment 1
Essential mineral composition in the present embodiment in coal gangue is kaolinite, and impure mineral content is extremely low; Aluminum oxide, silicon-dioxide, loss on ignition account for respectively 40.08%, 37.65% and 17.32%.
1) the coal gangue powder of preparation activation: take coal gangue 50 grams, be broken for the 50-300 order, obtain the coal gangue powder of activation by naturally cooling through abrasive dust, removal of impurities, roasting;
2) alkali soaks desiliconization: the coal gangue powder of above-mentioned activation is placed in leacher, is that 20% diluted sodium hydroxide solution leaches 30 minutes under 90 ℃ of conditions with massfraction, and total consumption of sodium hydroxide is according to Na
2O:SiO
2=1.0 mass ratio calculates, react complete after, filtration obtains sodium silicate solution and alkali soaks slag;
3) preparation white carbon black:
A, add Sodium hexametaphosphate 99 in above-mentioned sodium silicate solution, the quality of Sodium hexametaphosphate 99 is 0.5% of sodium silicate solution quality, passes into to contain CO
2Gas carry out carbonating and process, carbonation reaction finishes when the pH of solution is 4, filters, and obtains orthosilicic acid precipitated filter cakes and sodium carbonate filtrate; The described CO that contains
2Gas in CO
2Volumetric concentration be not less than 15%;
B, described orthosilicic acid precipitated filter cakes is carried out ageing, roasting, pulverizing namely make white carbon black;
4) preparation pseudo-boehmite:
A, with step 2) alkali that makes soaks slag and sodium carbonate and Wingdale according to mass ratio: Ca/Si=2, puts into alkali after Na/Al=1 mixes and melts device, obtains grog in 1 hour at 1350 ℃ of lower sintering; What produce in sintering process contains CO
2Gas recovery make carbonating and use;
B, this grog is melted device from alkali and takes out being cooled to 600 ℃, achieve from efflorescence, will carry out shrend, filtration from the powder of efflorescence, obtain NaAlO
2Thick liquid and calcium silicate slag, described NaAlO
2Thick liquid obtains NaAlO after the lime milk solution deep desilication
2Seminal fluid;
C, described seminal fluid are for to become Al by distilled water diluting
2O
3Concentration is rare NaAlO of 60g/L
2Solution is with above-mentioned rare NaAlO
2After solution is heated to 30 ℃, passes into and contain CO
2Volumetric concentration is that 35% gas carried out the carbonating plastic 1 hour, then reacting slurry is continued to be warming up to 80 ℃, be incubated aging 4 hours, then filter and obtain glue and filtrate, glue is the gained powder after washing, drying, pulverizing, be pseudo-boehmite through the X-ray powder diffraction analysis, the X-ray powder diffraction analysis chart as shown in Figure 1.
After testing, the aluminum oxide in coal gangue and silicon-dioxide utilization ratio are respectively 97.3%, 95.1%, and sodium carbonate, carbonic acid gas, water circuit rate of utilization are all over 95%.The particle diameter that obtains the pseudo-boehmite powder is 50 ~ 100nm, and specific surface area is 302m
2/ g, pore volume are 1.2ml/g; The white carbon black particle diameter is 20 ~ 50nm, and the purity of white carbon black is 98.0%, and specific surface area is 267m
2/ g has reached the quality product requirement of pseudo-boehmite and white carbon black.
Embodiment 2
In the coal gangue that adopts in the present embodiment, aluminum oxide, silicon-dioxide, loss on ignition account for respectively 37.36%, 42.79%, 15.60%.
1) the coal gangue powder of preparation activation: take coal gangue 50 grams, be broken for 50-300 order, abrasive dust, removal of impurities, obtain the coal gangue powder of activation 800 ℃ of roastings by naturally cooling.
2) alkali soaks desiliconization: the coal gangue powder of above-mentioned activation is placed in leacher, and adding at twice massfraction is that 18% sodium hydroxide solution carries out alkali and soaks: add for the first time the 50-80% of total amount, the alkali time of soaking is 30 ~ 40 minutes; Add for the second time remaining sodium hydroxide solution, the alkali time of soaking is 20 ~ 30 minutes; Total consumption of sodium hydroxide is according to Na
2O:SiO
2=1.1 mass ratio calculates, react complete after, filtration obtains sodium silicate solution and alkali soaks slag.
3) preparation white carbon black:
A, add Sodium hexametaphosphate 99 in above-mentioned sodium silicate solution, the quality of Sodium hexametaphosphate 99 is 0.6% of sodium silicate solution quality, passes into to contain CO
2Gas carry out carbonating and process, carbonation reaction finishes when the pH of solution is 6, filters, and obtains orthosilicic acid precipitated filter cakes and sodium carbonate filtrate.The described CO that contains
2Gas in CO
2Volumetric concentration be not less than 15%, 50 ~ 80 ℃ of the starting temperatures of carbonation reaction, pressure is 0.25 ~ 0.4Mpa, terminal temperature is 40 ~ 50 ℃.
B, the ageing in ageing tank of orthosilicic acid precipitated filter cakes was filtered after 6 ~ 9 hours, and dewater under 200 ~ 250 ℃ of conditions, then 500 ~ 650 ℃ of roastings 1 hour, pulverize and namely get white carbon black.
4) preparation pseudo-boehmite:
A, with step 2) alkali that makes soaks slag and sodium carbonate and Wingdale according to mass ratio: Ca/Si=3, puts into alkali after Na/Al=1.2 mixes and melts device, obtains grog in 50 minutes at 1000 ℃ of lower sintering; What produce in sintering process contains CO
2Gas recovery make carbonating and use.
B, this clinker cooling to 600 ℃ is melted device from alkali take out, achieve from efflorescence, will carry out shrend, filtration from the powder of efflorescence, obtain NaAlO
2Thick liquid and calcium silicate slag, described NaAlO
2Thick liquid obtains NaAlO after rare lime milk solution deep desilication
2Seminal fluid.The temperature of shrend is controlled at 20 ℃, and the time is controlled at 30 ~ 60min, and the condition of deep desilication is: lime milk solution concentration is 5%, and total consumption of calcium hydroxide is according to Ca
2O:SiO
2=0.8 mol ratio is calculated, and the deep desilication time is 3min.
C, described seminal fluid are the Al that becomes by distilled water diluting
2O
3Concentration is rare NaAlO of 75g/L
2Solution is with above-mentioned rare NaAlO
2After solution is heated to 30 ℃, passes into and contain CO
2Volumetric concentration is that 45% gas carried out the reaction of carbonating plastic after 70 minutes, then reacting slurry is continued to be warming up to 100 ℃, be incubated aging 5 hours, filtration obtains glue and filtrate, glue is the gained powder after washing, drying, pulverizing, detecting through X-ray diffraction analysis is the pseudo-boehmite powder, and X-ray diffraction analysis figure and Fig. 1 are similar.
After testing, the aluminum oxide in coal gangue and silicon-dioxide utilization ratio are respectively 97.3%, 95.1%, and sodium carbonate, carbonic acid gas, water circuit rate of utilization are all over 95%.The particle diameter that obtains the pseudo-boehmite powder is 45 ~ 70nm, and specific surface area is 325m
2/ g, pore volume are 1.6ml/g; The white carbon black particle diameter is 20 ~ 50nm, and the purity of white carbon black is 98.0%, and specific surface area is 267m
2/ g.
Embodiment 3
In the coal gangue that adopts in the present embodiment, aluminum oxide, silicon-dioxide, loss on ignition account for respectively 40.08%, 37.65%, 17.32%.
1) the coal gangue powder of preparation activation: take coal gangue 50 grams, be broken for 50-300 order, abrasive dust, removal of impurities, obtain the coal gangue powder of activation 1000 ℃ of roastings by naturally cooling;
2) alkali soaks desiliconization: the coal gangue powder of above-mentioned activation is placed in leacher, and adding at twice massfraction is that 15% sodium hydroxide solution carries out alkali and soaks: add for the first time the 50-80% of total amount, the alkali time of soaking is 30 ~ 40 minutes; Add for the second time remaining sodium hydroxide solution, the alkali time of soaking is 20 ~ 30 minutes; Total consumption of sodium hydroxide is according to Na
2O:SiO
2=1.1 mass ratio calculates, react complete after, filtration obtains sodium silicate solution and alkali soaks slag.
3) preparation white carbon black:
A, add polyoxyethylene glycol in above-mentioned sodium silicate solution, addition is 1% of sodium silicate solution quality, passes into to contain CO
2Gas carry out carbonating and process, carbonation reaction finishes when the pH of solution is 4, filters, and obtains orthosilicic acid precipitated filter cakes and sodium carbonate filtrate.The described CO that contains
2Gas in CO
2Volumetric concentration be 30-60%, 50 ~ 80 ℃ of the starting temperatures of carbonation reaction, pressure is 0.25 ~ 0.4Mpa, terminal temperature is 40 ~ 50 ℃.
B, the ageing in the ageing tank of 75 ℃ of orthosilicic acid precipitated filter cakes was filtered after 6 ~ 9 hours, and dewater under 200 ~ 250 ℃ of conditions, then 500 ~ 650 ℃ of roastings 1 hour, pulverize and namely get white carbon black.
4) preparation pseudo-boehmite:
A, with step 2) alkali that makes soaks slag and sodium carbonate and Wingdale according to mass ratio: Ca/Si=2, puts into alkali after Na/Al=1 mixes and melts device, obtains grog in 1 hour 1350 ℃ of lower sintering processes; What produce in sintering process contains CO
2Gas recovery make carbonating and use.
B, this sintered clinker is cooled to 600 ℃ melts device from alkali and take out, achieve from efflorescence, will carry out shrend, filtration from the powder of efflorescence, obtain NaAlO
2Thick liquid and calcium silicate slag, described NaAlO
2Thick liquid obtains NaAlO after rare lime milk solution deep desilication
2Seminal fluid.
C, described seminal fluid become Al by distilled water diluting
2O
3Concentration is rare NaAlO of 80g/L
2Solution is with above-mentioned rare NaAlO
2After solution is heated to 40 ℃, passes into and contain CO
2Volumetric concentration is that 35% gas carried out the carbonating plastic 1 hour, then reacting slurry is continued to be warming up to 90 ℃, be incubated aging 4.5 hours, filtration obtains glue and filtrate, glue is the gained powder after washing, drying, pulverizing, detecting through X-ray diffraction analysis is the pseudo-boehmite powder, and X-ray diffraction analysis figure and Fig. 1 are similar.
After testing, the aluminum oxide in coal gangue and silicon-dioxide utilization ratio are respectively 97.3%, 95.1%, and sodium carbonate, carbonic acid gas, water circuit rate of utilization are all over 95%.The particle diameter that obtains the pseudo-boehmite powder is 45 ~ 70nm, and specific surface area is 325m
2/ g, pore volume are 1.6ml/g; The white carbon black particle diameter is 15 ~ 40nm, and the purity of white carbon black is 98.0%, and specific surface area is 314m
2/ g.
Embodiment 4
In the coal gangue that adopts in the present embodiment, aluminum oxide, silicon-dioxide, loss on ignition account for respectively 40.08%, 37.65%, 17.32%.
1) the coal gangue powder of preparation activation: take coal gangue 50 grams, be broken for 50-300 order, abrasive dust, removal of impurities, obtain the coal gangue powder of activation 700 ℃ of roastings by naturally cooling;
2) alkali soaks desiliconization: the coal gangue powder of above-mentioned activation is placed in leacher, is that 15% diluted sodium hydroxide solution leaches 85 minutes under 80 ℃ of conditions with massfraction, and total consumption of sodium hydroxide is according to Na
2O:SiO
2=1.1 mass ratio calculates, react complete after, filtration obtains sodium silicate solution and alkali soaks slag;
3) preparation white carbon black:
A, add in the above-mentioned sodium silicate solution polyoxyethylene glycol and Sodium hexametaphosphate 99 according to the mixing solutions of 1:1 proportional arrangement, addition is 0.5% of sodium silicate solution quality, passes into to contain CO
2Gas carry out carbonating and process, carbonation reaction finishes when the pH of solution is 4, filters to get orthosilicic acid precipitated filter cakes and sodium carbonate filtrate; The described CO that contains
2Gas in CO
2Volumetric concentration be 30-50%, 50 ~ 80 ℃ of the starting temperatures of carbonation reaction, pressure is 0.25 ~ 0.4Mpa, terminal temperature is 40 ~ 50 ℃.
B, the silicic acid precipitated filter cakes is carried out ageing, drying, pulverizing namely get white carbon black;
4) preparation pseudo-boehmite:
A, with step 2) alkali that makes soaks slag and sodium carbonate and Wingdale according to mass ratio: Ca/Si=2, put into alkali after Na/Al=1 mixes and melt device at 1 hour acquisition grog of 1350 ℃ of lower sintering; What produce in sintering process contains CO
2Gas recovery make carbonating and use;
B, this clinker cooling to 600 ℃ is melted device from alkali take out, achieve from efflorescence, will carry out shrend, filtration from the powder of efflorescence, obtain NaAlO
2Thick liquid and calcium silicate slag, described NaAlO
2Thick liquid obtains NaAlO after rare lime milk solution deep desilication
2Seminal fluid; The temperature of shrend is controlled at 30 ℃, and the time is controlled at 30 ~ 60min, and the condition of deep desilication is: lime milk solution concentration is 10wt%, and total consumption of calcium hydroxide is according to Ca
2O:SiO
2=1.0 mol ratio is calculated, and the deep desilication time is 5 minutes.
C, described seminal fluid become Al by distilled water diluting
2O
3Concentration is rare NaAlO of 65g/L
2Solution is with above-mentioned rare NaAlO
2After solution is heated to 35 ℃, passes into and contain CO
2Volumetric concentration is that 50% gas carried out the carbonating plastic 75 minutes, then reacting slurry is continued to be warming up to 90 ℃, be incubated aging 3.5 hours, filtration obtains glue and filtrate, glue is the gained powder after washing, drying, pulverizing, detecting through X-ray diffraction analysis is the pseudo-boehmite powder, and X-ray diffraction analysis figure and Fig. 1 are similar.
After testing, the aluminum oxide in coal gangue and silicon-dioxide utilization ratio are respectively 97.3%, 95.1%, and sodium carbonate, carbonic acid gas, water circuit rate of utilization are all over 95%.The particle diameter that obtains the pseudo-boehmite powder is 45 ~ 70nm, and specific surface area is 325m
2/ g, pore volume are 1.6ml/g; The white carbon black particle diameter is 15 ~ 25nm, and the purity of white carbon black is 98.0%, and specific surface area is 346m
2/ g.
Embodiment 5
In the coal gangue that adopts in the present embodiment, aluminum oxide, silicon-dioxide, loss on ignition account for respectively 40.08%, 37.65%, 17.32%.
1) the coal gangue powder of preparation activation: take coal gangue 50 grams, be broken for 50-300 order, abrasive dust, removal of impurities, obtain the coal gangue powder of activation 1000 ℃ of roastings by naturally cooling;
2) alkali soaks desiliconization: the coal gangue powder of above-mentioned activation is placed in leacher, and adding at twice massfraction is that 22% sodium hydroxide solution carries out alkali and soaks, and adds for the first time the 50-80% of total amount, and the alkali time of soaking is 30 ~ 40 minutes; Add for the second time remaining sodium hydroxide solution, the alkali time of soaking is 20 ~ 30 minutes.Total consumption of sodium hydroxide is according to Na
2O:SiO
2=1.1 mass ratio calculates, react complete after, filtration obtains sodium silicate solution and alkali soaks slag.
3) preparation white carbon black:
A, add in the above-mentioned sodium silicate solution polyoxyethylene glycol and Sodium hexametaphosphate 99 according to the mixing solutions of 1:1 proportional arrangement, addition is 0.7% of sodium silicate solution quality, passes into to contain CO
2Gas carry out carbonating and process, carbonation reaction finishes when the pH of solution is 6.5, filters to get orthosilicic acid precipitated filter cakes and sodium carbonate filtrate; The described CO that contains
2Gas in CO
2Volumetric concentration be 30-60%, 50 ~ 80 ℃ of the starting temperatures of carbonation reaction, pressure is 0.25 ~ 0.4Mpa, terminal temperature is 40 ~ 50 ℃.
B, the orthosilicic acid precipitated filter cakes is carried out ageing, roasting, pulverizing make white carbon black.
4) preparation pseudo-boehmite:
A, with step 2) alkali that makes soaks slag and sodium carbonate and Wingdale according to mass ratio: Ca/Si=2, puts into alkali after Na/Al=1 mixes and melts device, obtains grog in 1 hour at 1350 ℃ of lower sintering; What produce in sintering process contains CO
2Gas recovery make carbonating and use;
B, the clinker cooling to 600 of sintering processes ℃ is melted device from alkali take out, achieve from efflorescence, will carry out shrend, filtration from the powder of efflorescence, obtain NaAlO
2Thick liquid and calcium silicate slag, described NaAlO
2Thick liquid obtains NaAlO after rare lime milk solution deep desilication
2Seminal fluid; The temperature of shrend is controlled at 20 ℃, and the time is controlled at 30 ~ 60min, and the condition of deep desilication is: lime milk solution concentration is 10%, and total consumption of calcium hydroxide is according to Ca
2O:SiO
2=1.0 mol ratio is calculated, and the deep desilication time is 5 minutes.
C, described seminal fluid become Al by distilled water diluting
2O
3Concentration is/rare NaAlO of L
2Solution is with above-mentioned rare NaAlO
2After solution is heated to, add the expanding agent that accounts for solution total amount 0.2wt%, described expanding agent be in gac, polyvinyl alcohol, polyacrylamide, Mierocrystalline cellulose, urea and starch one or more, and pass into and contain CO
2Volumetric concentration is 35% gas, carry out carbonating plastic reaction 75 minutes under the stirring velocity of 800-2000r/min, then reacting slurry is continued to be warming up to 90 ℃, glue is incubated aging 6 hours, filtration obtains glue and filtrate, glue is through washing, dry, pulverizing gained powder, and detecting through X-ray diffraction analysis is the pseudo-boehmite powder, and X-ray diffraction analysis figure and Fig. 1 are similar.
After testing, the aluminum oxide in coal gangue and silicon-dioxide utilization ratio are respectively 97.3%, 95.1%, and sodium carbonate, carbonic acid gas, water circuit rate of utilization are all over 94%.The particle diameter that obtains the pseudo-boehmite powder is 35 ~ 50nm, and specific surface area is 341m
2/ g, pore volume are 1.84ml/g; The white carbon black particle diameter is 15 ~ 25nm, and the purity of white carbon black is 98.0%, and specific surface area is 346m
2/ g.
Claims (14)
1. a method of utilizing coal gangue to prepare the pseudo-boehmite co-producing white carbon black, is characterized in that, comprises the following steps:
1) the coal gangue powder of preparation activation: with cooling after coal gangue fragmentation, abrasive dust, roasting, the coal gangue powder that obtains activating;
2) alkali soaks desiliconization: the coal gangue powder of above-mentioned activation is leached with sodium hydroxide solution, and filtration obtains sodium silicate solution and alkali soaks slag;
3) preparation white carbon black comprises:
A, add dispersion agent in described sodium silicate solution, and pass into and contain CO
2Gas carry out carbonating and process, carbonation reaction finishes when the pH of solution is 4 ~ 7, filters, and obtains orthosilicic acid precipitated filter cakes and filtrate;
B, described orthosilicic acid precipitated filter cakes is carried out ageing, roasting, pulverize and obtain white carbon black;
4) preparation pseudo-boehmite comprises:
A, with step 2) alkali that makes soak slag and mix with sodium carbonate and Wingdale after sintering, obtain grog, what produce in sintering process contains CO
2Gas recovery make carbonating and use;
Then b, cooling described grog obtain NaAlO after shrend, filtration
2Thick liquid and calcium silicate slag, described NaAlO
2Thick liquid obtains NaAlO after with the lime milk solution deep desilication
2Seminal fluid;
C, the described NaAlO of use distilled water diluting
2Seminal fluid obtains NaAlO
2Solution is to NaAlO
2Pass in solution and contain CO
2Gas carry out carbonating plastic reaction, after the plastic reaction is completed, reacting slurry is carried out burin-in process, then filter and obtain glue and filtrate, glue obtains pulverous pseudo-boehmite through washing, dry, pulverization process.
2. method according to claim 1, step 1), the granularity of powder is the 50-300 order, and the temperature range of roasting is 700-1050 ℃, and the time of roasting is 30 ~ 60 minutes.
3. be the described coal gangue powder of 5-25% sodium hydroxide solution leaching 30 ~ 90 minutes with massfraction under 80 ~ 100 ℃ of conditions method according to claim 1, step 2), total consumption of sodium hydroxide is according to Na
2O:SiO
2=1.0 ~ 1.2 mol ratio is calculated.
4. be that 10% ~ 20% sodium hydroxide solution leaches described coal gangue powder 50 ~ 70 minutes with massfraction method according to claim 3, step 2).
5. the dispersion agent method according to claim 1, step 3-a) is selected from one or more in Sodium hexametaphosphate 99, polyoxyethylene glycol, sodium lauryl sulphate, polyvinyl alcohol and trolamine.
6. the quality of the dispersion agent that adds method according to claim 1 or 5, step 3-a) is 0.5 ~ 5% of sodium silicate solution, the described CO that contains
2Gas in CO
2Volumetric concentration be not less than 15%, 50 ~ 95 ℃ of the starting temperatures of carbonation reaction, pressure is 0.25 ~ 0.4Mpa, terminal temperature is 40 ~ 60 ℃, carbonation reaction finishes when the pH of solution is 6.
7. pass into method according to claim 6, step 3-a) and contain CO
2Volumetric concentration is that 30 ~ 60% gas carries out carbonating and processes.
8. method according to claim 1, step 3-b), the ageing in ageing tank of orthosilicic acid precipitated filter cakes was filtered after 6 ~ 9 hours, and dewater under 200 ~ 250 ℃ of conditions, then 500 ~ 650 ℃ of roastings 1 hour, pulverize and namely get white carbon black.
9. method according to claim 1, step 4-a), alkali is soaked slag and sodium carbonate and Wingdale according to mol ratio: Ca/Si=2 ~ 3, mix Na/Al=1 ~ 1.2, carries out sintering under 1000 ~ 1350 ℃, and sintering time is controlled to be 0.5 ~ 1 hour.
10. method according to claim 1, step 4-b), the temperature of shrend is controlled at 20 ℃-30 ℃, and the time is controlled at 30 ~ 60min, and the condition of deep desilication is: lime milk solution concentration is 5 ~ 25wt%, and total consumption of calcium hydroxide is according to Ca
2O:SiO
2=0.8 ~ 1.2 mol ratio is calculated, and the deep desilication time is 3 ~ 10 minutes.
11. method according to claim 1, step 4-c) in to NaAlO
2Pass in solution and contain CO
2Volumetric concentration is that 30 ~ 50% gas carries out the carbonating plastic, and the plastic reaction conditions is temperature: 20 ~ 45 ℃, and the time: 45 ~ 90 minutes.
12. according to claim 1 or 11 described methods, step 4-c) in, to NaAlO
2After adding the expanding agent that accounts for described solution total amount 0.1-0.5wt% in solution, under the stirring velocity of 800-2000r/min, pass into and contain CO
2Volumetric concentration is that 30 ~ 50% gas carries out the carbonating plastic, and the plastic reaction conditions is temperature: 20 ~ 45 ℃, the time: 45 ~ 90 minutes, described expanding agent was one or more in gac, polyvinyl alcohol, polyacrylamide, Mierocrystalline cellulose, urea and starch.
13. according to claim 1 or 11 described methods, step 4-c) after in, the plastic reaction is completed, described reacting slurry is warmed up to 60 ~ 100 ℃, is incubated aging 2 ~ 6 hours.
14. according to claim 1-13 described methods of any one, step 2) in, sodium hydroxide solution adds the described coal gangue powder of leaching at twice, the massfraction of sodium hydroxide solution is 15 ~ 20%, the quality that adds for the first time sodium hydroxide is the 50-80% of sodium hydroxide total amount, and alkali time of soaking is 30 ~ 40 minutes for the first time; The sodium hydroxide that adds for the second time residual mass, alkali time of soaking is 20 ~ 30 minutes for the second time.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941725A (en) * | 2009-07-10 | 2011-01-12 | 同方环境股份有限公司 | Method for extracting aluminum oxide from coal gangue and co-producing active calcium silicate |
| CN101966999A (en) * | 2010-11-11 | 2011-02-09 | 中国地质大学（北京） | Method for extracting aluminum oxide and white carbon black through two-step alkaline leaching method by adopting high-alumina fly ash |
-
2013
- 2013-01-08 CN CN201310006059.7A patent/CN103145161B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101941725A (en) * | 2009-07-10 | 2011-01-12 | 同方环境股份有限公司 | Method for extracting aluminum oxide from coal gangue and co-producing active calcium silicate |
| CN101966999A (en) * | 2010-11-11 | 2011-02-09 | 中国地质大学（北京） | Method for extracting aluminum oxide and white carbon black through two-step alkaline leaching method by adopting high-alumina fly ash |
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