IPC분류정보
국가/구분 |
United States(US) Patent
등록
|
국제특허분류(IPC7판) |
|
출원번호 |
US-0014853
(2001-12-14)
|
우선권정보 |
IT-MI00A2772 (2000-12-21) |
§371/§102 date |
20030930
(20030930)
|
발명자
/ 주소 |
- Carati, Angela
- Pazzuconi, Giannino
- Perego, Carlo
- Cappellazzo, Oscar
- Girotti, Gianni
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출원인 / 주소 |
- Eni S.p.A.
- Enichem S.p.A.
- Enitecnologie S.p.A.
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대리인 / 주소 |
Oblon, Spviak, McClelland, Maier &
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인용정보 |
피인용 횟수 :
0 인용 특허 :
4 |
초록
▼
According to a particular aspect of the invention, the crystalline phase is separated in a mixture with oxides which can be used as ligands. Said oxides can be generated by the reagents of the zeolite preparation reagent mixture, not transformed into crystalline phase during the synthesis hydrotherm
According to a particular aspect of the invention, the crystalline phase is separated in a mixture with oxides which can be used as ligands. Said oxides can be generated by the reagents of the zeolite preparation reagent mixture, not transformed into crystalline phase during the synthesis hydrothermal treatment, or they can be added to the suspension of crystals before the separation treatment, or again they can be generated by precursors suitably added to the crystallization slurry.
대표청구항
▼
1. A method for separating zeolite crystals from an aqueous medium, comprising:(a) preparing an aqueous alkaline mother liquor containing, as reagents for zeolite preparation, a silica source, optionally alumina and/or other metal oxide sources and/or an organic templating agent; (b) hydrothermally
1. A method for separating zeolite crystals from an aqueous medium, comprising:(a) preparing an aqueous alkaline mother liquor containing, as reagents for zeolite preparation, a silica source, optionally alumina and/or other metal oxide sources and/or an organic templating agent; (b) hydrothermally treating said mother liquor thereby obtaining a suspension containing: - zeolite crystals, reagents of the zeolite preparation not transformed into zeolitic crystalline phase during the hydrothermal treatment and optionally oxides generated by them, optionally organic templating agent and optionally product generated by the decomposition of said sources of silica and alumina; (c) treating the zeolite crystal containing suspension with an acid until the suspension attains a pH ranging from 3-8; and (d) filtering or decanting the resulting mixture to isolate the zeolite crystals in mixture with oxides generated by said reagents of the zeolite preparation not transformed into zeolitic crystalline phase. 2. The process according to claim 1, which further comprises:in step (c) treating the suspension with said acid and with a material selected from the group consisting of a clay, an oxide and a precursor of an oxide which generates the oxide by hydrolysis; and in step (d) filtering or decanting the resulting mixture to isolate said zeolite crystals in a mixture with the oxide. 3. The process according to claim 2, wherein said oxide is selected from the group consisting of silica, silica-alumina and alumina.4. The process according to claim 2, wherein said precursor of an oxide is selected from the group consisting of aluminum acetylacetonate, alkylaluminates, alkylsilicates and combinations thereof.5. The method according to claim 2, wherein the content of said oxide in the separated zeolite product ranges from 1 to 50% by weight based on the amount of zeolite.6. The process according to claim 1, wherein said acid of step (c) is an acid precursor which is capable of simultaneously generating an acid and a binder by hydrolysis.7. The process according to claim 6, wherein said precursor which simultaneously generates acid and said oxide is selected from the group consisting of Al(NO3)3, Al2(SO4)3, silicic acid, silicon or aluminum halides and Al(CH3COO)3.8. The method according to claim 6, wherein the content of said oxide in the separated zeolite product ranges from 1 to 50 % by weight based on the amount of zeolite.9. The process according to claim 1, wherein said pH ranges from 3 to 6.10. The process according to claim 1, wherein said acid is selected from the group consisting of acetic acid, hydrochloric acid, nitric acid, formic acid, propionic acid and oxalic acid.11. The method according to claim 1, wherein the content of said oxide in the separated zeolite product ranges from 1 to 50 % by weight based on the amount of zeolite.12. A method for separating zeolite crystals from an aqueous medium, comprising:(a) preparing an aqueous alkaline mother liquor containing alumina and silica precursors and optionally an organic templating agent; (b) hydrothermally treating said mother liquor thereby obtaining a suspension containing zeolite crystals, silicates or amorphous silica aluminate and optionally (i) organic templating agent and product generated by decomposition of the organic templating agent and optionally (ii) alcohol derived by the decomposition of said silica and alumina precursors; (c) treating the alkaline zeolite crystal containing suspension with an acid until the suspension attains a pH ranging from 3-8; and (d) filtering or decanting the resulting mixture to isolate the zeolite crystals. 13. A process for preparing zeolite catalysts in acid or ammonia form, which comprises:(a) preparing an aqueous alkaline mother liquor containing, as reagents for zeolite preparation, a silica source, optionally alumina and/or other metal oxide sources and/or an organic templating agent; (b) hydrothermally treating said mother liquor thereby obtaining a suspension containing: - zeolite crystals, reagents of the zeolite preparation not transformed into zeolitic crystalline phase during the hydrothermal treatment and optionally oxides generated by them, optionally organic templating agent and optionally product generated by the decomposition of said sources of silica and alumina; (c) treating the suspension of zeolite crystals in the crystallization mother liquor containing the crystals with an aqueous acid solution to change the pH to a pH ranging from 3-8; (d) filtering or decanting the resulting mixture to separate the zeolite crystals in mixture with oxides generated by said reagents of the zeolite preparation not transformed into zeolitic crystalline phase; (e) drying the crystals; (f) calcining the crystals; (g) effecting an ion exchange in the zeolite crystals in an aqueous solution containing an acid or ammonium salt; (h) filtering or decanting the ion exchange zeolite crystals and subjecting the crystals to washing; (i) drying the crystals; and (j) calcining the crystals to remove ammonium ion therefrom in the event said ion exchange is conducted with ammonium salt and the acid form of the zeolite catalyst is required. 14. The process according to claim 13, wherein in step (c), said suspension is treated with a material selected from the group consisting of clay, an oxide and an oxide precursor that generates an oxide by hydrolysis.15. The process according to claim 13, wherein said acid in step (c) is added in the form of a precursor which generates said acid and an oxide by hydrolysis.16. A process for preparing zeolitic catalysts in acid form, which comprises:(a) preparing an aqueous alkaline mother liquor containing, as reagents for zeolite preparation, a silica source, optionally alumina and/or other metal oxide sources and/or an organic templating agent; (b) hydrothermally treating said mother liquor thereby obtaining a suspension containing: - zeolite crystals, reagents of the zeolite preparation not transformed into zeolitic crystalline phase during the hydrothermal treatment and optionally oxides generated by them, optionally organic templating agent and optionally product generated by the decompostion of said sources of silica and alumina; (c) treating the alkaline suspension of zeolite crystals in the mother liquor with an acid until the suspension attain a pH ranging from 3 to 8 ; (d) filtering or decanting the resulting mixture to isolate the zeolite crystals; in mixture with oxides generated by said reagents of the zeolite preparation not transformed into zeolitic crystalline phase; (e) exchanging the zeolite with an aqueous solution containing an acid or ammonium salt; (f) filtering or decanting the zeolite crystals to effect separation thereof; (g) drying the zeolite crystals; and (h) calcining the crystals to remove templating agent and ammonium ion in the event ion exchange reaction is conducted with an ammonium salt, the zeolite product having a tridimensional large or extra-large pore system. 17. The process according to claim 16, wherein step (c), said suspension is treated with a material selected from the group consisting of clay, an oxide and an oxide precursor that generates an oxide by hydrolysis.18. The process according to claim 16, wherein said acid in step (c) is added in the form of a precursor which generates said acid and an oxide by hydolysis.19. A process for preparing zeolitic catalysts in extruded form, which comprises:(a) preparing an aqueous alkaline mother liquor containing, as reagents for zeolite preparation, a silica source, optionally alumina and/or other metal oxide source and/or an organic templating agent; (b) hydrothermally treating said mother liquor thereby obtaining a suspension containing: - zeolite crystals, reagents of the zeolite preparation not transformed into zeolitic crystalline phase during the hydrothermal treatment and optionally oxides generated by them, optionally organic templating agent and optionally product generated by the decomposition of said sources of silica and alumina; (c) treating the suspension of zeolite crystals in the crystallization mother liquor containing the crystals with an aqueous acid solution to change the pH to a pH ranging from 3-8; (d) filtering or decanting the resulting mixture to separate the zeolite crystals in mixture with oxides generated by said reagents of the zeolite preparation not transformed into zeolitic crystalline phase; (e) drying the crystals; (f) calcining the crystals; (g) effecting an ion exchange in the zeolite crystals in an aqueous solution containing an acid or ammonium salt; (h) filtering or decanting the ion exchange zeolite crystals and subjecting the crystals to washing; (i) drying the crystals; and (j) calcining the crystals to remove ammonium ion therefrom in the event said ion exchange is conducted with ammonium salt and the acid form of the zeolite catalyst is required; and (k) extruding the crystals, optionally, in a mixture with a binder. 20. A process for preparing zeolitic catalyst in extruded form, which comprises:(a) preparing an aqueous alkaline mother liquor containing, as reagents for zeolite preparation, a silica source, optionally alumina and/or other metal oxide sources and/or an organic templating agent; (b) hydrothermally treating said mother liquor thereby obtaining a suspension containing: - zeolite crystals, reagents of the zeolite preparation not transformed into zeolitic crystalline phase during the hydrothermal treatment and optionally oxides generated by them, optionally organic templating agent and optionally product generated by the decomposition of said sources of silica and alumina; (c) treating the alkaline suspension of zeolite crystals in the mother liquor with an acid until the suspension attains a pH ranging from 3 to 8; (d) filtering or decanting the resulting mixture to isolate the zeolite crystals in mixture with oxides generated by said reagents of the zeolite preparation not transformed into zeolitic crystalline phase; (e) exchanging the zeolite with an aqueous solution containing an acid or ammonium salt; (f) filtering or decanting the zeolite crystals to effect separation thereof; (g) drying the zeolite crystals; and (h) calcining the crystals to remove residual templating agent and ammonium ion in the event the ion exchange reaction is conducted with an ammonium salt, the zeolite product having a tridimensional large or extra-large pore system; and (i) extruding the crystals, optionally, in a mixture with a binder.
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