Process for the production of a crystalline aluminosilicate zeolite

Claim 1

A method for making a crystalline aluminosilicate zeolite which (a) contains silicon, aluminum, sodium, and potassium in the following ratio, expressed as a molar ratio of oxides, SiO.sub.2 :(0.02-0.30)Al.sub.2 O.sub.3 :(0.05-0.30)[Na.sub.2 O+K.sub.2 O], (b) exhibits the following characteristic signals in its X-ray diffraction diagram as synthesized TABLE 1 ______________________________________ Interplanar spacings Relative intensity d[Å] I/I.sub.0 ______________________________________ 11.5 ± 0.3 strong to very strong 9.2 ± 0.2 weak 7.6 ± 0.2 weak to medium 6.6 ± 0.1 medium to strong 6.3 ± 0.1 weak 5.7 ± 0.1 weak 5.35 ± 0.1 weak 4.56 ± 0.1 weak to medium 4.32 ± 0.1 strong 4.16 ± 0.1 weak 3.81 ± 0.1 medium to strong 3.75 ± 0.1 strong to very strong 3.59 ± 0.1 strong to very strong 3.30 ± 0.1 medium 3.15 ± 0.1 medium 2.86 ± 0.1 strong to very strong 2.80 ± 0.1 weak to medium 2.67 ± 0.1 weak to medium 2.49 ± 0.1 weak to medium ______________________________________ where I O denotes the intensity of the strongest signal, which method comprises heating, in a sealed vessel, at a temperature from 80° C. to 200° C., for a time between 18 hours and 1000 hours, a reaction mixture of water and compounds of silicon, aluminum, sodium, potassium, and of an organic template agent having the following initial composition expressed as a molar ratio, SiO.sub.2 :(0.02-0.30)Al.sub.2 O.sub.3 :(0.02-0.40)Na.sub.2 O:(0.02-0.30)K.sub.2 O: (0.04-1.00) of the organic template agent (10-90)H 2 O, and then calcining the crystalline zeolite so made to destroy said organic template agent said organic template agent being provided as (i) an ammonium compound of the formula RX wherein R is an ammonium cation of the formula (HOCH 2 CH 2 ) 4 N + , (HOCH 2 CH 2 ) 3 R 1 N + , or (HOCH 2 CH 2 ) 2 R 1 R 2 N + and R 1 and R 2 , which are the same or different, are hydrogen or alkyl having up to 5 carbon atoms, and X is hydroxy, chloride, bromide, iodide, sulfate, phosphate, sulfonate, carboxylate, carbonate, or sulfite, or as (ii) a mixture of one molar part of at least one of diethanolamine and triethanolamine with from one to 10 molar parts of methanol, ethanol, propanol, butanol, ethylene glycol, 1,2-propylene glycol, dimethyl sulfate, diethyl sulfate, methyl iodide, ethyl iodide, propyl iodide, methyl p-toluenesulfonate, ethyl p-toluenesulfonate, or propyl p-toluenesulfonate.

Claim 2

A method for making a crystalline aluminosilicate zeolite which (a) contains silicon, aluminum, sodium, and potassium in the following ratio, expressed as a molar ratio of oxides, SiO.sub.2 :(0.02-0.30)Al.sub.2 O.sub.3 :(0.05-0.30)[Na.sub.2 O+K.sub.2 O], (b) exhibits the following characteristic signals in its X-ray diffraction diagram as synthesized TABLE 1 ______________________________________ Interplanar spacings Relative intensity d[Å] I/I.sub.0 ______________________________________ 11.5 ± 0.3 strong to very strong 9.2 ± 0.2 weak 7.6 ± 0.2 weak to medium 6.6 ± 0.1 medium to strong 6.3 ± 0.1 weak 5.7 ± 0.1 weak 5.35 ± 0.1 weak 4.56 ± 0.1 weak to medium 4.32 ± 0.1 strong 4.16 ± 0.1 weak 3.81 ± 0.1 medium to strong 3.75 ± 0.1 strong to very strong 3.59 ± 0.1 strong to very strong 3.30 ± 0.1 medium 3.15 ± 0.1 medium 2.86 ± 0.1 strong to very strong 2.80 ± 0.1 weak to medium 2.67 ± 0.1 weak to medium 2.49 ± 0.1 weak to medium ______________________________________ where I O denotes the intensity of the strongest signal, which method comprises heating, in a sealed vessel, at a temperature from 80° C. to 200° C., for a time between 18 hours and 1000 hours, a reaction mixture of water and compounds of silicon, aluminum, sodium, potassium, and of an organic template agent having the following initial composition expressed as a molar ratio, SiO.sub.2 :(0.02-0.30)Al.sub.2 O.sub.3 :(0.02-0.40)Na.sub.2 O:(0.02-0.30)K.sub.2 O: (0.04-1.00) of the organic template agent (10-90)H 2 O, and then calcining the crystalline zeolite so made to destroy said organic template agent said organic template agent being provided as (i) an ammonium compound of the formula RX wherein R is an ammonium cation of the formula (HOCH 2 CH 2 ) 4 N + , (HOCH 2 CH 2 ) 3 R 1 N + , or (HOCH 2 CH 2 ) 2 R 1 R 2 N + and R 1 and R 2 , which are the same or different, are hydrogen or alkyl having up to 5 carbon atoms, and X is hydroxy, chloride, bromide, iodide, sulfate, phosphate, sulfonate, carboxylate, carbonate, or sulfite, or as (ii) a mixture of one molar part of at least one of diethanolamine and triethanolamine with from one to 10 molar parts of methanol, ethanol, propanol, butanol, ethylene glycol, 1,2-propylene glycol, dimethyl sulfate, diethyl sulfate, methyl iodide, ethyl iodide, propyl iodide, methyl p-toluenesulfonate, ethyl p-toluenesulfonate, or propyl p-toluenesulfonate.