CN115430413A - Preparation method of kaolin-based metal trapping agent - Google Patents
Preparation method of kaolin-based metal trapping agent Download PDFInfo
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- CN115430413A CN115430413A CN202211046671.2A CN202211046671A CN115430413A CN 115430413 A CN115430413 A CN 115430413A CN 202211046671 A CN202211046671 A CN 202211046671A CN 115430413 A CN115430413 A CN 115430413A
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- kaolin
- roasting
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- 239000005995 Aluminium silicate Substances 0.000 title claims abstract description 45
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 235000012211 aluminium silicate Nutrition 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 12
- 239000002184 metal Substances 0.000 title claims abstract description 12
- 239000004005 microsphere Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 10
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000004537 pulping Methods 0.000 claims abstract description 6
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 5
- 150000001450 anions Chemical class 0.000 claims abstract description 4
- 150000001768 cations Chemical class 0.000 claims abstract description 4
- 238000005507 spraying Methods 0.000 claims abstract description 3
- 230000032683 aging Effects 0.000 claims description 12
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000008025 crystallization Effects 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 4
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- 125000000129 anionic group Chemical group 0.000 claims description 4
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 4
- 125000002091 cationic group Chemical group 0.000 claims description 2
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims description 2
- 239000011654 magnesium acetate Substances 0.000 claims description 2
- 235000011285 magnesium acetate Nutrition 0.000 claims description 2
- 229940069446 magnesium acetate Drugs 0.000 claims description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 2
- 159000000003 magnesium salts Chemical class 0.000 claims description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 2
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 24
- 238000003756 stirring Methods 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000002808 molecular sieve Substances 0.000 description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 5
- 239000004115 Sodium Silicate Substances 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910052911 sodium silicate Inorganic materials 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000004523 catalytic cracking Methods 0.000 description 2
- 239000002734 clay mineral Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
-
- B01J35/51—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G11/00—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils
- C10G11/02—Catalytic cracking, in the absence of hydrogen, of hydrocarbon oils characterised by the catalyst used
- C10G11/04—Oxides
Abstract
The invention discloses a preparation method of a kaolin-based metal trapping agent, which comprises the steps of pulping kaolin and water glass, spraying the mixture into microspheres, and roasting the microspheres; will contain Mg 2+ The cation solution is marked as B and the anion solution is marked as C, and the cation solution and the anion solution are simultaneously added into kaolin microspheres, aged for a period of time, crystallized, washed and roasted to obtain the kaolin-based metal trapping agent. The metal trapping agent prepared by the method has good wear resistance and specific surface, and strong metal pollution resistance.
Description
The technical field is as follows:
the invention relates to a preparation method of a kaolin-based metal trapping agent, belonging to the field of catalytic cracking auxiliaries.
Background art:
kaolin is a white clay mainly composed of minerals of the kaolinite group, and mainly comprises clay minerals and non-clay minerals. In the aspects of synthesizing zeolite, developing other novel materials and producing chemical products as raw materials, kaolin is often required to be subjected to high-temperature treatment in advance, and the physical and chemical properties of the kaolin are changed due to the change of a crystal structure after calcination, so that the kaolin has more excellent properties, and a plurality of patent reports are provided for the treatment and use of the kaolin.
The patent CN109453783A discloses a preparation method of a kaolin-based composite molecular sieve membrane, which comprises the steps of mixing kaolin and sodium carbonate, then carrying out high-temperature activation and alkali activation treatment to obtain active kaolin, pressing the kaolin into a tablet, placing the tablet in a muffle furnace for calcination to obtain a load substrate, and then loading ZSM-5 and SAPO-34 molecular sieve membranes.
Patent CN102674384A discloses a preparation method of a hydrotalcite-like-kaolin composite material, which comprises heating kaolin raw powder or spray-molded microspheres to a high temperature for roasting; dissolving urea and soluble divalent inorganic salt in deionized water, adding calcined kaolin, stirring at room temperature, heating for crystallization, washing with deionized water, filtering, and drying.
Patent CN102583432A discloses a method for synthesizing a nano-scale Y-type molecular sieve by intercalation stripping of coal-series kaolin, which comprises mixing coal-series kaolin with an organic intercalation agent solution to obtain a coal-series kaolin-organic intercalation compound; then roasting at 550-1100 ℃ to obtain nano kaolin powder; preparing a directing agent by using sodium hydroxide, a silicon source, an aluminum source and water, uniformly mixing coal series kaolin powder, the sodium hydroxide, the silicon source and the water to prepare a gel reactant, then adding the directing agent into the gel reactant, uniformly stirring the mixture, and then aging and crystallizing the mixture; and filtering, washing and drying after crystallization to prepare the nano-scale Y-shaped molecular sieve.
Patent CN103641132A discloses a method for synthesizing SAPO-34 molecular sieve by using kaolin, which can greatly reduce cost and improve product quality.
The invention content is as follows:
the invention aims to provide a preparation method of a kaolin-based metal trapping agent. The technical route adopted is as follows:
(1) Pulping kaolin and water glass according to a certain proportion, spraying, granulating and roasting, and recording as A.
(2) Preparation of a composition containing Mg 2+ The cationic solution of (a) is denoted as B; an anionic solution was prepared and noted C.
(3) And adding the solution B and the solution C into the solution A at the same time, aging for a period of time, crystallizing, washing and roasting to obtain the title compound.
The preparation method provided by the invention is characterized in that the ratio of the dry basis of the water glass in the step (1) to the total dry basis of the title compound is (0.1-0.3): 1.
in the step (1) of the preparation method provided by the invention, the kaolin is added with water and fully stirred for not less than 3 hours, and the dry-based solid content of kaolin slurry is 15-30%.
In the step (1) of the preparation method provided by the invention, the kaolin microspheres are roasted to 600-900 ℃, preferably 700-800 ℃.
In the preparation method provided by the invention, in the step (2), mg is contained 2+ The cation solution of (2) may be a soluble magnesium salt such as magnesium chloride, magnesium nitrate, magnesium sulfate, magnesium acetate, etc. The anionic solution may be OH-containing - 、CO 3 2- 、HCO 3 - One or more kinds of anion solution.
In the step (3) of the preparation method provided by the invention, the solution B contains Mg 2+ Is added in an amount corresponding to Al in A 3+ The ratio of the amounts is 2 to 5, preferably 3 to 4, and solution B is added to solution A simultaneously with solution C, controlling the pH to 9 to 11, preferably 9 to 10.
In the step (3), the aging temperature is 50-70 ℃, the aging time is 4-12 h, the crystallization temperature is 80-100 ℃, and the crystallization time is 6-24 h.
In the step (3), the roasting temperature is 750-850 ℃, and the roasting time is 1-3 h.
Compared with the prior art, the invention has the following innovation points or advantages:
(1) The roasted kaolin microspheres are used as a carrier, most of Al can participate in the reaction, magnesium-aluminum hydrotalcite is formed on the surfaces of the microspheres, and the treated spinel microspheres have better wear resistance and can meet the use requirement of a catalytic cracking device; meanwhile, as a plurality of active components are dispersed on the surface of the microsphere, the metal pollution resistance is also stronger.
(2) More additional value is added for the treatment and use of the kaolin, and more economic benefits are generated.
The specific implementation mode is as follows:
reference will now be made in detail to the present embodiments of the invention, with the understanding that the present disclosure is to be considered an exemplification of the invention and is not intended to limit the invention to that as illustrated.
Example 1:
(1) Adding water into 90 parts of kaolin with dry mass, fully stirring for 5 hours until the dry solid content of kaolin slurry is 25%, then adding 10 parts of sodium silicate with dry mass, mixing, pulping, spray drying to form balls, roasting kaolin microspheres at the roasting condition of 750 ℃/3 hours, and recording the roasted microspheres as A 1 ;
(2) Preparation of MgCl 2 (Mg 2+ =7 wt%) solution is denoted as B 1 (ii) a The NaOH solution (NaOH =20 wt%) was prepared and noted C 1 。
(3) According to n (Mg) 2+ )/n(Al 3+ ) =3 addition of solution B 1 While adding C 1 Adjusting the pH value of the solution and the slurry to 9.5-10.5, stirring uniformly, aging at 60 ℃ for 6h, continuing heating for crystallization, crystallizing at 90 ℃ for 12h, washing to be neutral, drying, and roasting at 800 ℃ for 2h. Thus, example 1 was obtained.
Example 2:
(1) Adding 80 parts of kaolin of dry mass into water, fully stirring for 5 hours until the dry solid content of kaolin slurry is 25%, adding 20 parts of sodium silicate of dry mass, mixing, pulping, spray-drying to form balls, roasting the kaolin microspheres under the roasting condition of 750 ℃/3 hours, and recording the roasted microspheres as A 2 ;
(2) Preparation of MgCl 2 (Mg 2+ =8 wt%) solution is denoted B 2 (ii) a Prepare NaOH solution (NaOH =25 wt%) and record C 2 。
(3) According to n (Mg) 2+ )/n(Al 3+ ) =3.5 Add solution B 2 While adding C 2 Solutions ofAdjusting the pH value of the slurry to 9.5-10.5, stirring uniformly, aging at 50 ℃ for 12h, continuing heating for crystallization, crystallizing at 100 ℃ for 8h, washing to be neutral, drying, and roasting at 750 ℃ for 2h. Thus, example 2 was obtained.
Example 3:
(1) Adding 70 parts of kaolin of dry mass into water, fully stirring for 5 hours until the dry solid content of kaolin slurry is 25%, then adding 30 parts of sodium silicate of dry mass, mixing, pulping, spray drying to form balls, roasting kaolin microspheres under the roasting condition of 700 ℃/3 hours, and recording the roasted microspheres as A 3 ;
(2) Preparation of MgCl 2 (Mg 2+ =10 wt%) solution is denoted B 3 (ii) a The NaOH solution (NaOH =30 wt%) was prepared and noted C 3 。
(3) According to n (Mg) 2+ )/n(Al 3+ ) =3.5 Add solution B 3 While adding C 3 Adjusting the pH value of the solution and the slurry to 9.5-10.5, uniformly stirring, aging at 50 ℃ for 12h, continuously heating for crystallization, crystallizing at 100 ℃ for 8h, washing to be neutral, drying, and roasting at 800 ℃ for 2h to obtain the solution of the embodiment 3.
The performance evaluation of the examples was carried out by using an ACE evaluation device manufactured by KTI of America, and AIC-308 of our company was selected as an evaluation main agent, 5% of examples 1, 2 and 3 were added to each sample, and the mixture was mixed uniformly and contaminated by immersion of metal V, the contamination amount of V being 6000ppm. Before performance evaluation, the catalyst samples impregnated with the metals need to be subjected to steam aging deactivation treatment, wherein the aging conditions are 760 ℃/10h and 100% steam. The evaluation data are shown in table 1 below, and from the evaluation data, several samples in the examples have good metal-trapping ability.
Claims (8)
1. A preparation method of a kaolin-based metal trapping agent comprises the following specific steps:
(1) Pulping kaolin and water glass according to a certain proportion, spraying, granulating and roasting, and marking as A.
(2) Preparation of a composition containing Mg 2+ The cationic solution of (1) is denoted as B; an anionic solution was prepared and noted C.
(3) And adding the solution B and the solution C into the solution A at the same time, aging for a period of time, crystallizing, washing and roasting to obtain the title compound.
2. The method of claim 1, wherein: in the step (1), the dry basis ratio of the water glass to the total dry basis of the title compound is 0.1-0.3: 1.
3. the method of claim 1, wherein: in the step (1), the kaolin is added with water and fully stirred for not less than 3 hours, and the dry-basis solid content of kaolin slurry is 15-30%.
4. The method of claim 1, wherein: in the step (1), the kaolin microspheres are roasted to 600-900 ℃, preferably 700-800 ℃.
5. The method of claim 1, wherein: in the step (2), mg is contained 2+ The cation solution of (2) may be a soluble magnesium salt such as magnesium chloride, magnesium nitrate, magnesium sulfate, magnesium acetate, etc. The anionic solution may be OH-containing - 、CO 3 2- 、HCO 3 - One or more kinds of anion solution.
6. The method of claim 1, wherein: in the step (2), mg solution B 2+ Is added in an amount corresponding to Al in A 3+ The ratio of the amounts is 2 to 5, preferably 3 to 4, and solution B is added to solution A simultaneously with solution C, controlling the pH to 9 to 11, preferably 9 to 10.
7. The method of claim 1, wherein: in the step (3), the aging temperature is 50-70 ℃, the aging time is 4-12 h, the crystallization temperature is 80-100 ℃, and the crystallization time is 6-24 h.
8. The method of claim 1, wherein: in the step (3), the roasting temperature is 750-850 ℃, and the roasting time is 1-3 h.
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US4847225A (en) * | 1984-10-05 | 1989-07-11 | W. R. Grace & Co.-Conn. | Catalysts and catalyst supports |
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US5300469A (en) * | 1992-12-08 | 1994-04-05 | Engelhard Corporation | Composition for passivating vanadium in catalytic cracking and preparation thereof |
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CN102674384A (en) * | 2011-03-17 | 2012-09-19 | 华东师范大学 | Hydrotalcite like compound-kaolin composite material and preparation method thereof |
CN103785428A (en) * | 2012-10-29 | 2014-05-14 | 中国石油化工股份有限公司 | Metal chelating agent, preparation method and application thereof, and catalytic cracking method |
CN106378203A (en) * | 2016-08-12 | 2017-02-08 | 青岛惠城环保科技股份有限公司 | Preparation method for metal capturing agent |
CN114425453A (en) * | 2020-09-25 | 2022-05-03 | 中国石油化工股份有限公司 | Catalytic cracking multifunctional metal trapping agent and preparation method thereof |
CN114713267A (en) * | 2021-01-06 | 2022-07-08 | 中国石油天然气股份有限公司 | Catalyst for improving catalytic cracking gasoline yield and preparation method thereof |
-
2022
- 2022-08-30 CN CN202211046671.2A patent/CN115430413A/en not_active Withdrawn
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Title |
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Application publication date: 20221206 |