Time effective method for preparing ferrierite

Claim 1

A time effective method of manufacture of sodium ferrierite which comprises crystallizing an aqueous mixture at hydrothermal crystallizing conditions of from about 100° to about 400° C. over a period of time greater than 10 hours and less than 20 hours to form a crystalline sodium ferrierite, said aqueous mixture comprising a sodium compound, one or more aluminum compounds, a silicon compound and one nitrogen compound selected from the group consisting of piperidine, piperazine, pyridine, 4-picoline-N-oxide and 4-picoline, wherein the mole ratios of both the sodium compound and aluminum compound, in relation to the silicon compound, calculated on the basis of the oxide forms of said sodium compound, aluminum compound and silicon compound, are equal to the presence of 1.6 to 3.4 moles of sodium oxide per 25 moles of said silicon oxide and 0.7 to 1.6 moles of said aluminum oxide per 25 moles of said silicon oxide, and wherein water is present in a molar ratio of 5-500 moles of water per mole of said silicon oxide and said nitrogen compound is present in a molar ratio of 0.05 to 1.0 moles of said nitrogen compound per mole of said silicon oxide and where the mole ratio of sodium oxide to aluminum oxide is greater than 1, and calcining said crystalline sodium ferrierite.

Claim 8

A method of preparing a hydrogen ferrierite which comprises crystallizing over a period of time of greater than 10 hours and less than 20 hours, at hydrothermal crystallization conditions, an aqueous mixture comprising: i. one or more compounds of sodium (MX); ii. one or more compounds of aluminum (AlX); iii. one or more compounds of silicon (SiX); iv. a nitrogen compound selected from the group consisting of piperidine, piperazine, pyridine, 4-picoline-N-oxide and 4-picoline represented by (RN); and v. water; wherein the mole ratio of said components is equal to: (a) water to (SiX) of 5 to 500; (b) (RN) to (SiX) of 0.05 to 1.0; (c) (MX) per 25 moles of (SiX) of 1.6 to 3.4; and (d) (AlX) per 25 moles of (SiX) of 0.7 to 1.6; and wherein the quantities of (MX) and (AlX) are calculated on the basis of their oxide form regardless of the form of said compounds added to said aqueous mixture, calcining said crystalline mixture, to prepare a crystallized sodium ferrierite catalyst precursor and treating said catalyst precursor in the presence of an ion exchange means to exchange said sodium ions with hydrogen ions and to thereby prepare said hydrogen ferrierite.

Claim 9

A method of preparing a hydrogen ferrierite which comprises crystallizing over a period of time of greater than 10 hours and less than 20 hours, at hydrothermal crystallization conditions, an aqueous mixture comprising: i. one or more compounds of sodium (MX); ii. one or more compounds of aluminum (AlX); iii. one or more compounds of silicon (SiX); iv. a nitrogen compound selected from the group consisting of piperidine, piperazine, pyridine, 4-picoline-N-oxide and 4-picoline represented by (RN); and v. water; wherein the mole ratio of said components is equal to: (a) water to (SiX) of 5 to 500; (b) (RN) to (SiX) of 0.05 to 1.0; (c) (MX) per 25 moles of (SiX) of 1.6 to 3.4; and (d) (AlX) per 25 moles of (SiX) of 0.7 to 1.6; and wherein the quantities of (MX) and (AlX) are calculated on the basis of their oxide form regardless of the form of said compounds added to said aqueous mixture, calcining said crystalline mixture, to prepare a crystallized sodium ferrierite catalyst precursor and treating said catalyst precursor in the presence of an ion exchange means to exchange said sodium ions with hydrogen ions and to thereby prepare said hydrogen ferrierite.

Claim 14

A method of manufacture of a sodium ferrierite catalyst precursor which comprises: (a) forming an admixture of compounds in an aqueous solvent of one or more compounds of sodium, one or more compounds of aluminum, one or more compounds of silicon and piperadine wherein the molar ratio of said silicon, aluminum and sodium compounds when calculated on the basis for the oxide for is equal to: i. 1.6 to 3.4 moles of sodium oxide per 25 moles of said silicon oxide; ii. 0.7 to 1.6 moles of said aluminum oxide per mole of 25 moles of said silicon oxide; iii. 125 to 12,500 moles of water per 25 moles of silicon oxide; iv. 1.25 to 25 moles of said piperidine per 25 moles of said silicon oxide; and v. a ratio of sodium oxide to aluminum oxide of greater than 1; (b) crystallizing said aqueous admixture to form a sodium ferrierite at hydrothermal treatment conditions including a temperature of from 100° to 400° C. and a period of time greater than 10 hours and less than 20 hours; (c) removing said crystallized sodium ferrierite from the residuum mother liquor of said crystallization step (b); and (d) calcining said crystalline material in air to remove occluded amine.

Claim 15

A method of manufacture of a sodium ferrierite catalyst precursor which comprises: (a) forming an admixture of compounds in an aqueous solvent of one or more compounds of sodium, one or more compounds of aluminum, one or more compounds of silicon and piperadine wherein the molar ratio of said silicon, aluminum and sodium compounds when calculated on the basis for the oxide for is equal to: i. 1.6 to 3.4 moles of sodium oxide per 25 moles of said silicon oxide; ii. 0.7 to 1.6 moles of said aluminum oxide per mole of 25 moles of said silicon oxide; iii. 125 to 12,500 moles of water per 25 moles of silicon oxide; iv. 1.25 to 25 moles of said piperidine per 25 moles of said silicon oxide; and v. a ratio of sodium oxide to aluminum oxide of greater than 1; (b) crystallizing said aqueous admixture to form a sodium ferrierite at hydrothermal treatment conditions including a temperature of from 100° to 400° C. and a period of time greater than 10 hours and less than 20 hours; (c) removing said crystallized sodium ferrierite from the residuum mother liquor of said crystallization step (b); and (d) calcining said crystalline material in air to remove occluded amine.