Microporous crystals and synthesis schemes
View Patent ↗Novel zeolites are produced by combining a polar solute, a silicon or phosphorous source, and a structure directing agent. Surfactants and a hydrophobic solvent are added to the previously mixed three species and shaken to disperse the surfactants. The reverse microemulsion is stirred overnight, at about room temperature and then iced for five to ten minutes. A metal source is added vigorously shaken for about two minutes. The mixture is then aged for about two hours at about room temperature. A mineralizer is added and the resultant mixture aged for about two hours at about room temperature. The mixture is heated to about 180° C., for a suitable time period. The final novel product is then isolated.
1. An AlPO 4 -5 zeotype microporous crystalline species produced in a hydrothermal process comprising the steps:
a) mixing water, phosphorous acid, and a structure directing agent to produce a first mixture;
b) mixing cetyl pyridinium chloride, n-butanol, and toluene to produce a second mixture;
c) combining said first and said second mixtures to produce a reverse microemulsion;
d) stirring said reverse microemulsion for a first period and time at a first temperature;
e) adding aluminum triisopropoxide to said stirred reverse microemulsion;
f) aging said aluminum triisopropoxide containing reverse microemulsion for a second period of time at a second temperature;
g) adding hydrofluoric acid to said aged aluminum triisopropoxide containing reverse microemulsion;
h) aging said hydrofluoric acid containing and aluminum triisopropoxide contain reverse microemulsion for a third period of time at a third temperature;
i) transferring said reverse microemulsion to a suitable heating vessel; and
j) heating said transferred reverse microemulsion to a temperature of between about 100° C. and 220° C. for a selected period of time.
2. An AlPO 4 -5 zeotype microporous crystalline species produced according to claim 1 , wherein said structure directing agent contains an amine functional group.
3. An AlPO 4 -5 zeotype microporous crystalline species produced according to claim 1 , wherein said structure directing agent is triethylamine.
4. An AlPO 4 -5 zeotype microporous crystalline species produced according to claim 1 , wherein said temperature is between about 140° C. and 200° C.
5. An AlPO 4 -5 zeotype microporous crystalline species produced according to claim 1 , wherein said temperature is approximately 180° C.
6. An AlPO 4 -5 zeotype microporous crystalline species produced according to claim 1 , wherein said selected period of time is about five to seven hours with conventional heating and about 15 to 20 minutes with microwave heating.
7. An AlPO 4 -5 zeotype microporous crystalline species produced according to claim 1 , wherein said structure directing agent contains an amine functional group.
8. An AlPO 4 -5 zeotype microporous crystalline species produced according to claim 1 , wherein said structure directing agent is triethylamine.
9. An AlPO 4 -5 zeotype microporous crystalline species produced in a hydrothermal process comprising the steps:
a) mixing water, phosphorous acid, and triethylamine to produce a first mixture;
b) mixing cetyl pyridinium chloride, n-butanol, and toluene to produce a second mixture;
c) combining said first and said second mixtures to produce a reverse microemulsion;
d) stirring said reverse microemulsion for overnight at room temperature;
e) adding aluminum triisopropoxide to said stirred reverse microemulsion;
f) aging said aluminum triisopropoxide containing reverse microemulsion for one to three hours at room temperature;
g) adding hydrofluoric acid to said aged aluminum triisopropoxide containing reverse microemulsion;
h) aging said hydrofluoric acid containing and aluminum triisopropoxide contain reverse microemulsion for one to three hours at room temperature;
i) transferring said reverse microemulsion to a suitable heating vessel; and
j) heating said transferred reverse microemulsion to a temperature of between about 100° C. and 220° C. for a selected period of time.
10. An AlPO 4 -5 zeotype microporous crystalline species produced according to claim 9 , wherein said temperature is between about 140° C. and 200° C.
11. An AlPO 4 -5 zeotype microporous crystalline species produced according to claim 9 , wherein said temperature is approximately 180° C.
12. An AlPO 4 -5 zeotype microporous crystalline species produced according to claim 9 , wherein said selected period of time is about five to seven hours with conventional heating and about 15 to 20 minutes with microwave heating.
13. A zeotype microporous crystalline fiber structure comprising AlPO 4 -5 with linear micropores running approximately parallel to a long axis of said fiber.