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1. WO2020109292 - MECHANOCHEMICAL ACTIVATION IN ZEOLITE SYNTHESIS

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[ EN ]

Claims

1. A process for the preparation of a zeolitic material comprising YO2 and X2O3 in its framework structure, wherein Y stands for a tetravalent element and X stands for a trivalent el ement, wherein said process comprises:

(i) preparing a mixture comprising one or more sources of YO2, one or more sources of X2O3, and H2O;

(ii) grinding and/or mixing the mixture prepared in (i), wherein the energy intake of the mixture during the grinding and/or mixing procedure is in the range of from 5 to 2,000 kJ/kg of the mixture;

(iii) heating the mixture obtained in (ii) at a temperature in the range of from 80 to 300 °C for crystallizing a zeolitic material comprising YO2 and X2O3 in its framework structure from the mixture;

wherein the mixture prepared in (i) contains from 100 to 1 ,500 wt.-% of H2O based on 100 wt.-% of the one or more sources of YO2, calculated as YO2, contained in the mixture prepared in (i) and heated in (iii).

2. The process of claim 1 , wherein the 27AI MAS NMR of the mixture obtained in (ii), after drying thereof at 110°C, comprises:

a first peak (P1 ) in the range of from 25 to 75 ppm; and

one or more peaks (PX) in the range of from -20 to 25 ppm;

wherein the relative 27AI solid-state NMR intensity integral within the range of 75 to 25 ppm (Ii) and within the range of 25 to -20 ppm (I2) of the zeolitic material offer a ratio of the integration values I2 : (h + I2) comprised in the range of from 5 to 75%.

3. The process of claim 1 or 2, wherein grinding and/or mixing in (ii) is carried out in a mill selected from the group consisting of a stirred media mill, a planetary ball mill, a ball mill, a roller mill, a kneader, a high shear mixer, and a mix muller.

4. The process of any of claims 1 to 3, wherein Y is selected from the group consisting of Si, Sn, Ti, Zr, Ge, and mixtures of two or more thereof.

5. The process of any of claims 1 to 4, wherein X is selected from the group consisting of Al, B, In, Ga, and combinations of two or more thereof.

6. The process of any of claims 1 to 5, wherein the mixture prepared in (i) further contains one or more structure directing agents.

7. The process of claim 6, wherein the one or more structure directing agents comprises one or more tetraalkylammonium cation R1R2R3R4N+-containing compounds, wherein R1 , R2, and R3 independently from one another stand for alkyl, and wherein R4 stands for ada- mantyl and/or benzyl.

8. The process of claim 6, wherein the one or more structure directing agents comprises one or more tetraalkylammonium cation R1R2R3R4N+-containing compounds, wherein R1 , R2, and R3 independently from one another stand for alkyl, and wherein R4 stands for cycloalkyl.

9. The process of claim 6, wherein the one or more structure directing agents comprises one or more tetraalkylammonium cation selected from the group consisting of V,/V-di(Ci- C4)alkyl-3,5-di(Ci-C4)alkylpyrrolidinium, A/, V-di(Ci-C4)alkyl-3,5-di(Ci-C4)alkylpiperidinium, /V,/\Adi(Ci-C4)alkyl-3,5-di(Ci-C4)alkylhexahydroazepinium, and mixtures of two or more thereof.

10. The process of any of claims 1 to 9, wherein heating in (iii) is conducted as a continuous process.

11. The process of claim 10, wherein heating in (iii) comprises continuously feeding the mixture obtained in (ii) into a continuous flow reactor at a liquid hourly space velocity in the range of from 0.3 to 20 lv1 for a duration of at least 1 h, and crystallizing the zeolitic material comprising YO2 and X2O3 in its framework structure from the mixture in the continuous flow reactor, wherein the mixture is heated to a temperature in the range of from 80 to 300°C.

12. The process of any of claims 1 to 11 , wherein the mixture prepared in (i) and heated in (iii) further comprises seed crystals, wherein the amount of the seed crystals contained in the mixture prepared in (i) and heated in (iii) preferably ranges from 1 to 30 wt.-% based on 100 wt.-% of the one or more sources of YO2, calculated as YO2.

13. The process of claim 12, wherein the seed crystals contained in the mixture prepared in (i) and heated in (iii) comprise one or more zeolitic materials, wherein the one or more zeolit ic materials preferably have a framework structure type selected from the group consisting of AEI, BEA, BEC, CHA, EUO, FAU, FER, HEU, ITH, ITW, LEV, MEL, MFI, MOR, MTN, MWW, and TON, including mixed structures of two or more thereof.

14. A zeolitic material comprising YO2 and X2O3 in its framework structure obtainable and/or obtained according to the process of any of claims 1 to 13.

15. The zeolitic material of claim 14, wherein the zeolitic material has a CHA-type framework structure.

16. Use of the zeolitic material according to claim 14 or 15 as a molecular sieve, as an adsor bent, for ion-exchange, as a catalyst or a precursor thereof, and/or as a catalyst support or a precursor thereof.