Hierarchical zeolites and preparation method therefor
View Patent ↗The present invention relates to a method for preparing hierarchical zeolites, including the steps of preparing a first mixture solution including a structure-directing agent, an alumina precursor and a pH controller; preparing a second mixture solution by injecting a silica precursor into the first mixture solution; preparing an aqueous solution including a surfactant; preparing a third mixture solution by injecting the aqueous solution into the second mixture solution; and drying and heat-treating the third mixture solution. According to the present invention, hierarchical zeolites having a uniform morphology can be prepared, and thus hierarchical zeolites having improved activity are provided.
1. A method for preparing a hierarchical zeolite, comprising:
preparing a first mixture solution containing a structure-directing agent having a carbon number of C10 or less and an ammonium functional group, an alumina precursor, and a pH adjusting material;
adding a silica precursor to the first mixture solution to prepare a second mixture solution;
preparing an aqueous solution containing a surfactant having a carbon number of C11 or more and an ammonium function group;
adding the aqueous solution to the second mixture solution to prepare a third mixture solution; and
hydrothermal reaction and drying of the third mixture solution,
wherein the structure-directing agent is added in a molar ratio of 1/120 to 1/50, relative to an amount of silica,
wherein the surfactant is added in a molar ratio of 1/200 to 1/50, relative to an amount of silica,
wherein a concentration of the surfactant in the aqueous solution is 77 mmol/L to 360 mmol/L, and
wherein the hierarchical zeolite is ZSM-48.
2. The method of claim 1 , wherein the structure-directing agent is at least one selected from the group consisting of tetramethylammonium bromide, tetramethylammonium chloride, tetramethylammonium hydroxide, tetraethylammonium bromide, tetraethylammonium chloride, tetraethylammonium hydroxide, tetraethylammonium tetrafluoroborate, hexamethonium chloride, and hexamethonium bromide.
3. The method of claim 1 , wherein the surfactant is at least one selected from the group consisting of cetyltrimethylammonium bromide, cetyltrimethylammonium chloride, and cetylpyridinium chloride.
4. The method of claim 1 , wherein the preparing a third mixture solution comprises adding the aqueous solution to the second mixture solution in a dropwise manner.
5. The method of claim 1 , wherein the method is performed, without containing a seed.
6. The method of claim 1 ,
wherein the structure-directing agent is at least one selected from the group consisting of hexamethonium chloride and hexamethonium bromide;
wherein the surfactant is at least one selected from the group consisting of cetyltrimethylammonium chloride, cetyltrimethylammonium bromide, and cetylpyridinium chloride;
wherein the structure-directing agent is added in a molar ratio of 1/120 to 1/50, relative to an amount of silica;
wherein the surfactant is added in a molar ratio of 1/200 to 1/50, relative to an amount of silica; and
wherein a concentration of the surfactant in the aqueous solution is 77 mmol/L to 360 mmol/L.