CN108328638B - method for preparing ammonium aluminum sulfate from FCC spent catalyst - Google Patents
method for preparing ammonium aluminum sulfate from FCC spent catalyst Download PDFInfo
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- CN108328638B CN108328638B CN201810253731.5A CN201810253731A CN108328638B CN 108328638 B CN108328638 B CN 108328638B CN 201810253731 A CN201810253731 A CN 201810253731A CN 108328638 B CN108328638 B CN 108328638B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/74—Sulfates
- C01F7/76—Double salts, i.e. compounds containing, besides aluminium and sulfate ions, only other cations, e.g. alums
- C01F7/762—Ammonium or alkali metal aluminium sulfates
- C01F7/765—Ammonium aluminium sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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Abstract
The invention discloses a method for preparing aluminum ammonium sulfate from FCC spent catalyst, which comprises the steps of sieving the FCC spent catalyst, drying, mixing with quantitative sulfuric acid solution, stirring for hours, drying the mixture obtained after stirring in a drying oven, adding quantitative distilled water into the dried product, stirring, performing suction filtration, adding a proper amount of concentrated ammonia water into the filtrate, adjusting the pH value of the concentrated ammonia water to obtain suspension, stirring the suspension at room temperature, performing suction filtration, washing the filter cake with a small amount of distilled water, and drying the obtained filter cake to obtain the aluminum ammonium sulfate.
Description
Technical Field
The invention relates to preparation of aluminum ammonium sulfate, in particular to methods for preparing aluminum ammonium sulfate from FCC spent catalyst.
Background
Most of oil refineries use the small particle Y-type molecular sieve catalyst loaded with a small amount of rare earth metal as the catalyst used in the catalytic cracking process for refining crude oil, and after hours of use, the catalyst is polluted by heavy metals to reduce the activity of the catalyst, thus the comprehensive economic index is deteriorated, so that the catalyst with reduced activity needs to be periodically discharged from the system, and the discharged part is called FCC waste catalyst.
The invention discloses a method for preparing ammonium alum by using solid waste generated in aluminum product pretreatment as a raw material and sequentially performing pulping, crude aluminum sulfate liquid preparation, aluminum sulfate crude liquid sedimentation, aluminum ammonium sulfate crude liquid preparation, cooling crystallization and water washing and air drying, wherein the method has multiple operation steps and a complex process.
Disclosure of Invention
The technical problem to be solved by the invention is to provide methods for preparing aluminum ammonium sulfate from FCC spent catalyst, and the method has the excellent characteristics of simple process, mild preparation conditions, low heavy metal content of the prepared aluminum ammonium sulfate and the like.
The invention adopts the following technical scheme for solving the technical problems:
the method for preparing the ammonium aluminum sulfate from the FCC spent catalyst comprises the following steps:
(1) sieving a plurality of FCC spent catalysts with a 100-mesh sieve, drying at 105 ℃ for 10h, weighing 3g of dried FCC spent catalysts, placing in a beaker, adding quantitative acid liquor, stirring at room temperature at the rotation speed of 180-;
(2) feeding the slurry into an oven, and drying at for periods;
(3) mixing the dried substance with quantitative distilled water, stirring at room temperature at the rotation speed of 200-;
(4) slowly adding an appropriate amount of alkali liquor into the filtrate while stirring, and adjusting the pH value of the alkali liquor to obtain a suspension; stirring the suspension at the rotation speed of 150-.
In the step (1), the acid solution is a sulfuric acid solution, and the mass fraction of the sulfuric acid solution is 25-35%.
In the step (1), the volume of the acid solution is 20 ml.
In the step (2), the drying temperature of the slurry is 150 ℃.
In the method, the drying time of the slurry is 3-5 h.
In the step (3), the volume of the distilled water is 20 ml.
In the step (4), the alkali liquor is concentrated ammonia water, and the mass fraction of the alkali liquor is 26.5%.
In the step (4), the pH value is in the range of 1.4-2.0.
The content of heavy metal impurities in the aluminum ammonium sulfate prepared by the method is less than or equal to 0.2 wt%.
Compared with the prior art, the invention has the advantages that:
(1) by adopting a new low-temperature dissolution process, the energy consumption for dissolving the aluminum element in the FCC spent catalyst is reduced, the operation period is shortened, and the efficiency for preparing the aluminum ammonium sulfate is improved.
(2) The aluminum ammonium sulfate with higher purity is prepared by using the FCC waste catalyst as the raw material, so that the emission of the FCC catalyst is reduced, waste is changed into valuable, and the economic benefit of the raw material is improved.
Drawings
FIG. 1 is an XRD pattern of the synthesized products of examples 1-5 and a standard XRD pattern of aluminum ammonium sulfate.
Detailed Description
The present invention will be further described with reference to the following examples and accompanying drawings, which are included merely for purposes of illustration and are not intended to limit the scope of the invention.
Example 1:
sieving FCC spent catalyst with 100 mesh sieve, oven drying at 105 deg.C for 10 hr, weighing 3g dry FCC spent catalyst, placing in a beaker, adding 20ml 35 wt% H2SO4The solution was stirred at room temperature at 180r/min for 1 h. The stirred slurry was sent to an oven and dried at 150 ℃ for 4 h. Then, the dried product was mixed with 20ml of distilled water, stirred at room temperature at a rotation speed of 300r/min for 1 hour, and filtered by suction to obtain a filtrate. Slowly adding a proper amount of 26.5 wt% concentrated ammonia water into the filtrate while stirring, adjusting the pH of the filtrate to 2, stirring the obtained suspension at the rotating speed of 200r/min for 1h at room temperature, and obtaining a filter cake after suction filtration and washing by a small amount of distilled water. And drying the filter cake at 60 ℃ for 1h to obtain an aluminum ammonium sulfate product.
The total mass of the obtained aluminum ammonium sulfate product is 6.3115g, and the heavy metal content is 0.14 wt%.
Example 2:
sieving FCC spent catalyst with 100 mesh sieve, oven drying at 105 deg.C for 10 hr, weighing 3g dry FCC spent catalyst, placing in a beaker, adding 20ml 25 wt% H2SO4The solution was stirred at room temperature for 1h at 210 r/min. The stirred slurry was sent to an oven and dried at 150 ℃ for 4 h. Then, the dried product was mixed with 20ml of distilled water, stirred at room temperature at a rotation speed of 200r/min for 1 hour, and filtered by suction to obtain a filtrate. Slowly adding a proper amount of 26.5 wt% concentrated ammonia water into the filtrate while stirring, adjusting the pH of the filtrate to 2, stirring the obtained suspension at the rotating speed of 200r/min for 1h at room temperature, carrying out suction filtration, washing with a small amount of distilled water, and drying the filter cake at 60 ℃ for 1h to obtain an aluminum ammonium sulfate product. The total mass of the obtained aluminum ammonium sulfate product is 4.6841g, and the heavy metal content is 0.14 wt%.
Example 3:
sieving FCC spent catalyst with 100 mesh sieve, oven drying at 105 deg.C for 10 hr, weighing 3g dry FCC spent catalyst, placing in a beaker, adding 20ml 30 wt% H2SO4Stirring the solution at room temperature at 240r/min for 1h, drying the slurry at 150 deg.C for 3h, mixing the dried product with quantitative distilled water, stirring at 250r/min for 1h, vacuum filtering to obtain filtrate, and adding the filtrate into the filtrateSlowly adding a proper amount of concentrated ammonia water with the concentration of 26.5 wt% while stirring, adjusting the pH of the filtrate to 1.4, stirring the obtained suspension at the rotating speed of 150r/min for 1h at room temperature, carrying out suction filtration, washing with a small amount of distilled water, and drying the filter cake at the temperature of 60 ℃ for 1h to obtain an aluminum ammonium sulfate product. The total mass of the obtained aluminum ammonium sulfate product is 4.5847g, and the heavy metal content is 0.09 wt%.
Example 4:
sieving FCC spent catalyst with 100 mesh sieve, oven drying at 105 deg.C for 10 hr, weighing 3g dry FCC spent catalyst, placing in a beaker, adding 20ml 35 wt% H2SO4The solution was stirred at room temperature for 1h at 210 r/min. The stirred slurry was sent to an oven and dried at 150 ℃ for 3 h. Then, the dried product was mixed with 20ml of distilled water, stirred at room temperature at a rotation speed of 200r/min for 1 hour, and filtered by suction to obtain a filtrate. Slowly adding a proper amount of 26.5 wt% concentrated ammonia water into the filtrate while stirring, adjusting the pH of the filtrate to 1.4, stirring the obtained suspension at the rotating speed of 200r/min for 1h at room temperature, carrying out suction filtration, washing with a small amount of water, and drying the filter cake at 60 ℃ for 1h to obtain an aluminum ammonium sulfate product. The total mass of the obtained aluminum ammonium sulfate product is 5.4011g, and the heavy metal content is 0.12 wt%.
Example 5:
sieving FCC spent catalyst with 100 mesh sieve, oven drying at 105 deg.C for 10 hr, weighing 3g dry FCC spent catalyst, placing in a beaker, adding 20ml 30 wt% H2SO4The solution was stirred at room temperature for 1h at 240 r/min. The stirred slurry was sent to an oven and dried at 150 ℃ for 5 h. Then, the dried product was mixed with 20ml of distilled water, stirred at room temperature at a rotation speed of 300r/min for 1 hour, and filtered by suction to obtain a filtrate. Slowly adding a proper amount of concentrated ammonia water with the concentration of 26.5 wt% into the filtrate while stirring, adjusting the pH of the filtrate to 1.7, stirring the obtained suspension at the rotation speed of 150r/min for 1h at room temperature, carrying out suction filtration, washing with a small amount of distilled water, and drying the filter cake for 1h at the temperature of 60 ℃ to obtain an aluminum ammonium sulfate product. The total mass of the obtained aluminum ammonium sulfate product is 5.8506g, and the heavy metal content is 0.11 wt%.
The XRF data for the product FCC spent catalyst of examples 1-5 above are shown in table 1.
Because the aluminum ammonium sulfate is easily decomposed by heating and is not suitable for XRF detection, the impurity content of the aluminum ammonium sulfate is detected by ICP-AES. The results of ICP-AES measurements for the products of examples 1-5 above are shown in Table 2.
TABLE 1 XRF data for FCC spent catalyst
TABLE 2 ICP-AES assay results for the products of examples 1-5
Claims (8)
1, process for preparing ammonium aluminum sulfate from FCC spent catalyst, characterized by the steps of:
(1) sieving a plurality of FCC spent catalysts with a 100-mesh sieve, drying at 105 ℃ for 10h, weighing 3g of dried FCC spent catalysts, placing in a beaker, adding quantitative acid liquor, stirring at room temperature at the rotation speed of 180-;
(2) feeding the slurry into an oven, and drying at for periods;
(3) mixing the dried substance with quantitative distilled water, stirring at room temperature at the rotation speed of 200-;
(4) slowly adding an appropriate amount of alkali liquor into the filtrate while stirring, and adjusting the pH value of the alkali liquor to obtain a suspension; stirring the suspension at the rotation speed of 150-.
2. The method according to claim 1, wherein in the step (1), the acid solution is a sulfuric acid solution, and the mass fraction of the sulfuric acid solution is 25-35%.
3. A process according to claim 2, characterized in that the volume of acid is 20 ml.
4. The method according to claim 1, wherein in the step (2), the drying temperature of the slurry is 150 ℃.
5. The method according to claim 4, characterized in that the drying time of the slurry is 3-5 h.
6. The method according to claim 1, wherein in the step (3), the volume of the distilled water is 20 ml.
7. The method according to claim 1, wherein in the step (4), the alkali solution is concentrated ammonia water, and the mass fraction of the alkali solution is 26.5%.
8. The method according to claim 1, wherein in step (4), the pH value is in the range of 1.4 to 2.0.
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