Process for preparing a titanium-containing zeolitic material having an mww framework structure
US-2015368115-A1 · Dec 24, 2015 · US
US2022297098A1 · US · A1
| Field | Value |
|---|---|
| Publication number | US-2022297098-A1 |
| Application number | US-202117206938-A |
| Country | US |
| Kind code | A1 |
| Filing date | Mar 19, 2021 |
| Priority date | Mar 19, 2021 |
| Publication date | Sep 22, 2022 |
| Grant date | — |
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According to one or more embodiments, non-agglomerated, nano-sized ZSM-22 zeolites may be synthesized by methods comprising operating a mechanical rotation drum unit at a first temperature of from 40° C. to 60° C. and a first speed of from 200 rpm to 1000 rpm for a first time period of from 1.3 hours to 2.7 hours; operating the mechanical rotation drum unit at a second speed of from 30 rpm to 90 rpm for a second time period of from 0.05 hours to 0.4 hours; heating the mechanical rotation drum unit at a ramping temperature of from 8° C./minute to 12° C./minute to a second temperature of from 115° C. to 185° C. at the second speed; operating the mechanical rotation drum unit at the second temperature and the second speed for a third time period of from 30 hours to 90 hours; and cooling the mechanical rotation drum unit at a fourth speed of 0 rpm.
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What is claimed is: 1 . A method of synthesizing a non-agglomerated, nano-sized ZSM-22 zeolite, the method comprising: passing a silica solution and an aluminate solution into a mechanical rotation drum unit; operating the mechanical rotation drum unit at a first temperature of from 40° C. to 60° C. and a first speed of from 200 rpm to 1000 rpm for a first time period of from 1.3 hours to 2.7 hours; operating the mechanical rotation drum unit at a second speed of from 30 rpm to 90 rpm for a second time period of from 0.05 hours to 0.4 hours; heating the mechanical rotation drum unit at a ramping temperature of from 8° C./minute to 12° C./minute to a second temperature of from 115° C. to 185° C. at the second speed of from 30 rpm to 90 rpm; operating the mechanical rotation drum unit at the second temperature of from 115° C. to 185° C. and the second speed of from 30 rpm to 90 rpm for a third time period of from 30 hours to 90 hours; and cooling the mechanical rotation drum unit at a fourth speed of 0 rpm to produce the non-agglomerated, nano-sized ZSM-22 zeolite; and wherein the non-agglomerated, nano-sized ZSM-22 zeolite comprises crystals each having a length within a range of from 100 nanometers to 400 nanometers and a width within a range of from 50 nanometers to 250 nanometers. 2 . The method of claim 1 , wherein the mechanical rotation drum unit is cooled to a temperature of from 20° C. to 50° C. 3 . The method of claim 1 , further comprising drying the non-agglomerated, nano-sized ZSM-22 zeolite. 4 . The method of claim 1 , further comprising calcining the non-agglomerated, nano-sized ZSM-22 zeolite. 5 . The method of claim 1 , further comprising activating the non-agglomerated, nano-sized ZSM-22 zeolite to produce an active catalyst. 6 . The method of claim 1 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite comprises crystals each having a length within a range of from 100 nanometers to 200 nanometers and a width within a range of from 50 nanometers to 100 nanometers. 7 . The method of claim 1 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite comprises crystals each having a length within a range of from 150 nanometers to 400 nanometers and a width within a range of from 100 nanometers to 250 nanometers. 8 . The method of claim 1 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite has a silica/alumina ratio of from 25 to 100. 9 . A method of synthesizing a non-agglomerated, nano-sized ZSM-22 zeolite, the method comprising: passing a silica solution and an aluminate solution into a mechanical rotation drum unit; and operating the mechanical rotation drum unit at five stages to produce the non-agglomerated, nano-sized ZSM-22 zeolite; wherein: the first stage operates at a first mixing speed of from 200 rpm to 1000 rpm and at a first time period of from 1.3 hours to 2.7 hours; the second stage operates at a second mixing speed of from 30 rpm to 90 rpm and at a second time period of from 0.05 hours to 0.4 hours; the third stage operates at a third mixing speed of from 30 rpm to 90 rpm and at a third time period of from 0.05 hours to 0.4 hours; the fourth stage operates at a fourth mixing speed of from 30 rpm to 90 rpm and at a first time period of from 30 hours to 90 hours; and the fifth stage operates at a fifth mixing speed of 0 rpm. 10 . The method of claim 9 , wherein the first stage operates at a temperature of from 40° C. to 60° C. 11 . The method of claim 9 , wherein the second stage operates at a temperature of from 40° C. to 60° C. 12 . The method of claim 9 , wherein the fourth stage operates at a temperature of from 115° C. to 185° C. 13 . The method of claim 9 , wherein the fifth stage operates at a temperature of from 20° C. to 50° C. 14 . The method of claim 9 , wherein the third stage operates a ramping temperature of from 8° C./minute to 12° C./minute. 15 . The method of claim 9 , further comprising producing the silica solution in a silicate unit; producing the aluminate solution in an aluminate unit; and combining the silica solution and the aluminate solution prior to passing the silica solution and the aluminate solution into the mechanical rotation drum unit. 16 . The method of claim 9 , further comprising activating the non-agglomerated, nano-sized ZSM-22 zeolite to produce an active catalyst. 17 . The method of claim 9 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite comprises crystals each having a length within a range of from 100 nanometers to 400 nanometers and a width within a range of from 50 nanometers to 250 nanometers. 18 . The method of claim 17 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite comprises crystals each having a length within a range of from 100 nanometers to 200 nanometers and a width within a range of from 50 nanometers to 100 nanometers. 19 . The method of claim 17 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite comprises crystals each having a length within a range of from 150 nanometers to 400 nanometers and a width within a range of from 100 nanometers to 250 nanometers. 20 . The method of claim 9 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite has a silica/alumina ratio of from 25 to 100.
Other types characterised by their X-ray diffraction pattern and their defined composition {(C01B39/023, C01B39/026, C01B39/06 take precedence)} · CPC title
using at least one organic template directing agent · CPC title
Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof · CPC title
Nanoparticles · CPC title
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