CN108264113B - Method for preparing high-efficiency PAFC dye water purifying agent from FCC spent catalyst - Google Patents
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Abstract
The invention relates to a method for preparing a high-efficiency PAFC dye water purifying agent from FCC spent catalyst, which comprises the following steps: firstly, carrying out hydrothermal leaching on a dried FCC spent catalyst for a period of time by using a hydrochloric acid solution; filtering and separating residues, adding a proper amount of sodium hydroxide solution into the filtrate to adjust the solution to be alkaline, separating filter residues, adding a proper amount of hydrochloric acid solution to adjust the solution to be acidic, sequentially supplementing a proper amount of ferric trichloride hexahydrate, slowly adding calcium aluminate to adjust the basicity, curing the mixture for a certain time at a certain temperature, and filtering to obtain the PAFC product. The method takes the FCC waste catalyst in the petroleum catalytic cracking industry as the raw material, changes waste into valuable according to the characteristic of higher content of residual aluminum in the FCC waste catalyst, and improves the utilization rate of aluminum resources; and the preparation condition is mild, a large amount of energy is not consumed, the aluminum recovery utilization rate is high, and the method has a good application prospect.
Description
Technical Field
The invention belongs to the technical field of environment, and mainly relates to a method for reducing, discharging and recycling FCC (fluid catalytic cracking) waste catalyst in the petroleum catalytic cracking industry.
Background
In the oil refining production process, the catalytic cracking catalyst is the catalyst with the largest consumption, more than 70% of blending components of domestic gasoline are catalytic cracking gasoline, 40% of blending components of diesel oil are from catalytic cracking, the catalytic cracking catalyst is deactivated due to toxic metals of nickel and vanadium contained in crude oil, and a large amount of waste catalytic cracking catalysts are generated every year. At present, most of the waste catalytic cracking catalysts discharged by petroleum processing plants in China are simply buried, so that a large amount of land resources are occupied, and toxic and harmful substances in the waste catalytic cracking catalysts pollute the environment and underground water resources and influence the normal life of residents. With the continuous exploitation and utilization of mineral resources, the amount of mineral raw materials is continuously reduced and the price is continuously increased, so that the treatment and comprehensive utilization of the waste catalytic cracking catalyst are urgent.
Currently, the treatment and integrated utilization of FCC spent catalyst for petroleum processing plants is still in the experimental phase. Chinese patent CN104003430A discloses a method for preparing PAC solid product by mixing a waste petroleum cracking catalyst with a mixed acid of hydrochloric acid and sulfuric acid, carrying out acidolysis at normal temperature and pressure, and then carrying out filter pressing on acidolysis solution and directly carrying out spray drying; the method has the defects of high technical requirement and high energy consumption. Chinese patent CN1049140A discloses a method for preparing inorganic high molecular hydrate (water purifying agent) by using waste catalytic cracking catalyst in oil refinery, which is to dissolve the waste catalyst directly in acid and adjust basicity with gel aluminium hydroxide to prepare aluminium chlorohydrol meeting industrial requirements. Chinese patent CN106430321A discloses a method for preparing polyaluminum ferric chloride by adjusting basicity by adding calcium aluminate under the condition of controlling a certain mass ratio by using iron-containing waste hydrochloric acid, sodium nitrate, oxygen and aluminum-containing waste hydrochloric acid; the method has the defects of complex process and high energy consumption. Chinese patent CN106044985A discloses a method for preparing polyaluminium-iron chloride by using a cinder mixture of coal gangue and pyrite as a raw material, firstly impregnating the raw material with a strong acid solution to react to obtain a solution containing iron-aluminum chloride, and then carrying out a polymerization reaction. Chinese patent CN105540778A discloses a method for preparing polyaluminum ferric chloride by using red mud and fly ash as raw materials and adopting an acid-base combination method; the method has the defects of high-temperature roasting and high activation energy consumption. Chinese patent document CN1915852A discloses a method for preparing a polyaluminium-iron chloride high-efficiency water purifying agent by using circulating fluidized bed fly ash, performing acid dissolution to obtain an aluminum-iron chloride solution, and then performing basicity adjustment.
Disclosure of Invention
The invention aims to solve the problems that: on the basis of improving the utilization rate of aluminum, heavy metals in the waste catalyst are removed by an acid-base combination method, and the method for recycling and preparing the PAFC from the FCC waste catalyst with excellent water purification effect is provided, so that the defects of low aluminum utilization rate, excessive heavy metal content and poor water purification effect existing in the conventional method for preparing the PAFC by utilizing the FCC waste catalyst are overcome.
The technical scheme adopted by the invention is as follows:
the invention provides a method for preparing a high-efficiency PAFC dye water purifying agent from an FCC spent catalyst, which comprises the following steps:
(1) taking a plurality of FCC waste catalysts, drying at 80-120 ℃ for 10h, weighing 5g of dried FCC waste catalysts, placing in a hydrothermal kettle, adding a hydrochloric acid solution with the mass fraction of 15-30% according to the solid-to-liquid ratio of 1 (4.5-5.5), heating to 120-200 ℃ at the heating rate of 5 ℃/min for hydrothermal time of 1.5-2.5h, and filtering and separating residues to obtain a leaching solution;
(2) dropwise adding 0.1-0.5mol/L sodium hydroxide solution into the leachate to adjust the pH value to 9-12, filtering and separating filter residues to obtain a filtrate, and then supplementing 0.1-0.5mol/L hydrochloric acid solution into the filtrate to adjust the pH value to acidity to obtain a solution after impurity removal;
(3) and (3) stirring the solution at the speed of 150-.
In the step (2), the acidic pH value is 0.5-1.5.
In the step (3), the oil bath temperature is 60-90 ℃.
In the step (3), the addition amount of the ferric trichloride hexahydrate is 0.49-4.45 g.
In the step (3), the curing temperature of the solution is 60-90 ℃, and the curing time is 1.5-3 h.
The PAFC prepared by the method has the salinity of 37.62-72.40% and the content of alumina of 6.32-6.89%.
Compared with the prior art, the invention has the following main advantages:
(1) the leaching rate of the aluminum is greatly improved under the mild hydrothermal condition, so that the utilization rate of the aluminum is improved (see the leaching rate of the PAFC dissolving process in the table 5 compared with other processes);
(2) the acid-base combination method removes heavy metal ions in the waste catalyst, and solves the problem of heavy metal ion residue in the water treatment process (see the ICP element analysis result of PAFC in Table 2, which can reflect the problem that the content of heavy metal ions reaches the standard);
(3) the PAFC is prepared by taking the FCC waste catalyst generated by a petroleum processing plant as a raw material, so that the emission of the FCC waste catalyst can be reduced, waste can be changed into valuable, domestic sewage is treated, and the PAFC has important environmental protection and economic significance.
Drawings
FIG. 1 is a flow diagram of a process for preparing a high efficiency PAFC dye water purifier from FCC spent catalyst.
Detailed Description
The present invention will be further described with reference to the following examples and accompanying drawings, which are merely illustrative of preferred embodiments of the present invention, and are not intended to limit the present invention.
Example 1:
taking a plurality of FCC waste catalysts, drying at 80-120 ℃ for 10h, weighing 5g of the dried FCC waste catalysts, placing in a hydrothermal kettle, adding hydrochloric acid solution with the mass fraction of 20% according to the solid-to-liquid ratio of 1:5, heating to 200 ℃, carrying out hydrothermal treatment for 2h, and filtering and separating residues to obtain a leaching solution. The leaching rate of aluminum is 89.6% detected by a back titration method of a copper sulfate standard solution in GB 14563-2008.
Dropwise adding 0.5mol/L sodium hydroxide solution into the leachate to adjust the pH value to 10, filtering and separating filter residues to obtain a filtrate, and supplementing a proper amount of 0.5mol/L hydrochloric acid solution into the filtrate to adjust the pH value to 1.5 to obtain a solution after impurity removal; stirring the solution at 200r/min, keeping the oil bath temperature at 90 ℃, supplementing 0.49g of ferric trichloride hexahydrate according to the mass ratio of Al to Fe of 9, curing for 3 hours to obtain a suspension, and naturally cooling, standing, filtering and separating the suspension to obtain a PAFC product. The basicity of the obtained liquid PAFC is 72.40% detected by a [ national standard ] GB22627-2008 copper sulfate standard solution titration method, and the alumina content of the obtained liquid PAC is 6.89% detected by a potassium fluoride masking method.
Example 2:
taking a plurality of FCC waste catalysts, drying at 80-120 ℃ for 10h, weighing 5g of the dried FCC waste catalysts, placing in a hydrothermal kettle, adding hydrochloric acid solution with the mass fraction of 20% according to the solid-to-liquid ratio of 1:5, heating to 200 ℃, performing hydrothermal for 2h, and filtering and separating residues to obtain a leaching solution. The leaching rate of aluminum is 89.6 percent detected by a back titration method of a copper sulfate standard solution in GB 14563-2008;
dropwise adding 0.5mol/L sodium hydroxide solution into the leachate to adjust the pH value to 10, filtering and separating filter residues to obtain a filtrate, and supplementing a proper amount of 0.5mol/L hydrochloric acid solution into the filtrate to adjust the pH value to 0.5 to obtain a solution after impurity removal; stirring the solution at 200r/min, keeping the oil bath temperature at 60 ℃, supplementing 4.45g of ferric trichloride hexahydrate according to the mass ratio of Al to Fe of 1, curing for 1.5 hours to obtain a suspension, and naturally cooling, standing, filtering and separating the suspension to obtain a PAFC product. The basicity of the obtained liquid PAFC is 37.62% detected by a [ national standard ] GB22627-2008 copper sulfate standard solution titration method, and the alumina content of the obtained liquid PAC is 6.32% detected by a potassium fluoride masking method.
Example 3:
taking a plurality of FCC waste catalysts, drying at 80-120 ℃ for 10h, weighing 5g of the dried FCC waste catalysts, placing in a hydrothermal kettle, adding hydrochloric acid solution with the mass fraction of 20% according to the solid-to-liquid ratio of 1:5, heating to 200 ℃, performing hydrothermal for 2h, and filtering and separating residues to obtain a leaching solution. The leaching rate of aluminum is 89.6% detected by a back titration method of a copper sulfate standard solution in GB 14563-2008.
Dropwise adding 0.5mol/L sodium hydroxide solution into the leachate to adjust the pH value to 10, filtering and separating filter residues to obtain a filtrate, and supplementing a proper amount of 0.5mol/L hydrochloric acid solution into the filtrate to adjust the pH value to 1.5 to obtain a solution after impurity removal; and (3) stirring the solution at 200r/min, keeping the oil bath temperature at 60 ℃, supplementing 0.74g of ferric trichloride hexahydrate according to the mass ratio of Al to Fe of 6, curing for 3 hours to obtain a suspension, and naturally cooling, standing, filtering and separating the suspension to obtain a PAFC product. The basicity of the obtained liquid PAFC is 52.41% detected by a [ national standard ] GB22627-2008 copper sulfate standard solution titration method, and the alumina content of the obtained liquid PAC is 6.42% detected by a potassium fluoride masking method.
Example 4:
taking a plurality of FCC waste catalysts, drying at 80-120 ℃ for 10h, weighing 5g of the dried FCC waste catalysts, placing in a hydrothermal kettle, adding hydrochloric acid solution with the mass fraction of 20% according to the solid-to-liquid ratio of 1:5, heating to 200 ℃, performing hydrothermal for 2h, and filtering and separating residues to obtain a leaching solution. The leaching rate of aluminum is 89.6 percent detected by a back titration method of a copper sulfate standard solution in GB 14563-2008;
dropwise adding 0.5mol/L sodium hydroxide solution into the leachate to adjust the pH value to 10, filtering and separating filter residues to obtain a filtrate, and supplementing a proper amount of 0.5mol/L hydrochloric acid solution into the filtrate to adjust the pH value to 1.0 to obtain a solution after impurity removal; and (3) stirring the solution at 200r/min, keeping the oil bath temperature at 70 ℃, supplementing 0.49g of ferric trichloride hexahydrate according to the mass ratio of Al to Fe of 9, curing for 2 hours to obtain a suspension, and naturally cooling, standing, filtering and separating the suspension to obtain a PAFC product. The basicity of the obtained liquid PAFC is 61.20% detected by a [ national standard ] GB22627-2008 copper sulfate standard solution titration method, and the alumina content of the obtained liquid PAC is 6.49% detected by a potassium fluoride masking method.
Example 5:
taking a plurality of FCC waste catalysts, drying at 80-120 ℃ for 10h, weighing 5g of the dried FCC waste catalysts, placing in a hydrothermal kettle, adding hydrochloric acid solution with the mass fraction of 20% according to the solid-to-liquid ratio of 1:5, heating to 200 ℃, performing hydrothermal for 2h, and filtering and separating residues to obtain a leaching solution. The aluminum leaching rate detected by the counter titration method of the copper sulfate standard solution in GB14563-2008 is 89.6%.
Dropwise adding 0.5mol/L sodium hydroxide solution into the leachate to adjust the pH value to 10, filtering and separating filter residues to obtain a filtrate, and supplementing a proper amount of 0.5mol/L hydrochloric acid solution into the filtrate to adjust the pH value to 0.5 to obtain a solution after impurity removal; and (3) stirring the solution at 200r/min, keeping the oil bath temperature at 90 ℃, supplementing 1.125g of ferric trichloride hexahydrate according to the mass ratio of Al to Fe of 4, curing for 1.5 hours to obtain a suspension, and naturally cooling, standing, filtering and separating the suspension to obtain a PAFC product. The basicity of the obtained liquid PAFC is 66.10% detected by a [ national standard ] GB22627-2008 copper sulfate standard solution titration method, and the alumina content of the obtained liquid PAC is 6.54% detected by a potassium fluoride masking method.
Example 6:
taking a plurality of FCC waste catalysts, drying at 80-120 ℃ for 10h, weighing 5g of the dried FCC waste catalysts, placing in a hydrothermal kettle, adding hydrochloric acid solution with the mass fraction of 20% according to the solid-to-liquid ratio of 1:5, heating to 200 ℃, performing hydrothermal for 2h, and filtering and separating residues to obtain a leaching solution. The leaching rate of aluminum is 89.6% detected by a back titration method of a copper sulfate standard solution in GB 14563-2008.
Dropwise adding 0.5mol/L sodium hydroxide solution into the leachate to adjust the pH value to 10, filtering and separating filter residues to obtain a filtrate, and supplementing a proper amount of 0.5mol/L hydrochloric acid solution into the filtrate to adjust the pH value to 1.5 to obtain a solution after impurity removal; and (3) stirring the solution at 200r/min, keeping the oil bath temperature at 80 ℃, supplementing 0.89g of ferric trichloride hexahydrate according to the mass ratio of Al to Fe of 5, curing for 2 hours to obtain a suspension, and naturally cooling, standing, filtering and separating the suspension to obtain a PAFC product. The basicity of the obtained liquid PAFC is 68.24% detected by a [ national standard ] GB22627-2008 copper sulfate standard solution titration method, and the alumina content of the obtained liquid PAC is 6.78% detected by a potassium fluoride masking method.
TABLE 1 XRF data Table for FCC spent catalyst
(Note: FCC spent catalyst from Shandong)
TABLE 2 table of comparative index and national standard data for PAFC prepared in example 1
| Index name | National standard liquid PAFC | Self-made liquid PAFC |
| Alumina (with Al)2O3Meter) of the mass fraction ═ mass fraction | 6.0 | 6.89 |
| Degree of basicity/%) | 30-95 | 72.40 |
| pH value (10g/L aqueous solution) | 2.0-4.0 | 3.0 |
| Arsenic (As) mass fraction/% < ═ mass fraction | 0.0005 | 0.00026 |
| Lead (A), (B) and (C)Pb) Mass fraction/% < ═ of | 0.002 | 0.00016 |
TABLE 3-1 ICP analysis of PAFC product prepared in example 1
Tables 3-2 ICP analysis of the PAFC product prepared in example 1
TABLE 4 comparison of the indices of the examples with the national standard data
| Index name | Alumina content (%) | Degree of basicity (%) |
| National standard | ＞＝6.0 | 30-95 |
| Example 1 | 6.89 | 72.40 |
| Example 2 | 6.32 | 37.62 |
| Example 3 | 6.42 | 52.41 |
| Example 4 | 6.49 | 61.20 |
| Example 5 | 6.54 | 66.10 |
| Example 6 | 6.78 | 68.24 |
TABLE 5 comparison of the aluminum dissolution rates in example 1 and the prior art
| Index (I) | Aluminum leaching rate (%) |
| Prior art technique | 10-30 |
| Example 1 | 89.6 |
Note that: the method for measuring the aluminum leaching rate is described in GB14563-2008 kaolin and the test method thereof.
Claims (6)
1. A method for preparing a high-efficiency PAFC dye water purifying agent from FCC spent catalyst is characterized by comprising the following steps:
(1) taking a plurality of FCC waste catalysts, drying at 80-120 ℃ for 10h, weighing 5g of dried FCC waste catalysts, placing in a hydrothermal kettle, adding a hydrochloric acid solution with the mass fraction of 15-30% according to the solid-to-liquid ratio of 1 (4.5-5.5), heating to 120-200 ℃ at the heating rate of 5 ℃/min for hydrothermal time of 1.5-2.5h, and filtering and separating residues to obtain a leaching solution;
(2) dropwise adding 0.1-0.5mol/L sodium hydroxide solution into the leachate to adjust the pH value to 9-12, filtering and separating filter residues to obtain a filtrate, and then supplementing 0.1-0.5mol/L hydrochloric acid solution into the filtrate to adjust the pH value to acidity to obtain a solution after impurity removal;
(3) and (3) stirring the solution at the speed of 150-.
2. The method for preparing a high efficiency PAFC dye water purifying agent from FCC spent catalyst according to claim 1, wherein in the step (2), the pH is adjusted to be acidic, and the specific pH value thereof is 0.5-1.5.
3. The method for preparing a high efficiency PAFC dye water purifier from FCC spent catalyst according to claim 1, wherein in step (3), the oil bath temperature is 60-90 ℃.
4. The method for preparing a high efficiency PAFC dye water purifying agent from FCC spent catalyst according to claim 1, wherein in step (3), the ferric chloride hexahydrate is added in an amount of 0.49-4.45 g.
5. The method for preparing a high efficiency PAFC dye water purifying agent from FCC spent catalyst according to claim 1, wherein in the step (3), the aging temperature is 60-90 ℃ and the aging time is 1.5-3 h.
6. A PAFC according to any one of claims 1 to 5, characterised in that it has a basicity in the range 37.62-72.40% and an alumina content in the range 6.32-6.89%.
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| US4017584A (en) * | 1975-05-06 | 1977-04-12 | Societa' Italiana Resine S.I.R.. S.p.A. | Process for the recovery of aluminum trichloride |
| CN1288086C (en) * | 2005-03-29 | 2006-12-06 | 煤炭科学研究总院抚顺分院 | Method for preparing polyaluminium chloride through catalyst of deposed molecular sieve |
| CN101591032B (en) * | 2009-06-29 | 2011-12-07 | 同济大学 | Method for preparing modified polyaluminium chloride flocculating agent by waste molecular sieve |
| MX2012000567A (en) * | 2012-01-11 | 2013-07-15 | Ricardo Elizondo Elizondo | Process for the manufacture of aluminum chloride and polymeric salts of aluminum such as: aluminum polychloride, aluminum chlorhydroxide and aluminum sesquichlorohydrate having a wide range of basicities and concentrations, under normal conditions of pressure and temperature. |
| CN103964482B (en) * | 2014-05-16 | 2016-09-28 | 山西大学 | A kind of method that gangue silicon aluminum carbon works in coordination with utilization |
| CN106241843A (en) * | 2016-07-19 | 2016-12-21 | 武汉理工大学 | A kind of method that aluminium hydroxide is prepared in polyaluminium waste slag of aluminum acid system recovery |
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