Mesoporous ternary composite material and corresponding method of preparation

Abstract

Mesoporous ternary composite materials and a corresponding preparation method are described herein. The method includes the following steps: (1) adding hydrochloric acid and acetic acid into an ethanol solution to prepare a dissolving system; (2) adding a surfactant into the dissolving system and fully stirring for dissolution; (3) adding copper nitrate, manganese nitrate solution and tetrabutyl titanate into the mixed liquid obtained from step (2) and evenly stirring; (4) transferring the mixture obtained from step (3) into petri dishes and obtaining transparent films after drying; and (5) calcinating the transparent films to obtain mesoporous ternary composite materials. The materials prepared are ordered mesoporous materials with high specific surface areas and high dispersion degree of every component.

Claims

1. A method for preparing mesoporous ternary composite materials, comprising the following steps: (a) adding hydrochloric acid and acetic acid into an ethanol solution to prepare a dissolving system; (b) adding a surfactant into the dissolving system and fully stirring for dissolution; (c) adding copper nitrate, manganese nitrate solution and tetrabutyl titanate into the mixed liquid obtained from step (b) and evenly stirring; (d) transferring the mixture obtained from step (c) into petri dishes and obtaining transparent films after drying; and (e) calcinating the transparent films to obtain mesoporous ternary composite materials.

2. The method according to claim 1, wherein in the step (a) the concentrations of the hydrochloric acid and the acetic acid in the dissolving system are 30 to 50 g/L and 60 to 100 g/L, respectively.

3. The method according to claim 1, wherein in the step (b), the surfactant comprises a polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer, and the mass ratio of surfactant to ethanol is 1:10 to 1:20.

4. The method according to claim 3, wherein in the step (c), the copper nitrate, the manganese nitrate solution and the tetrabutyl titanate are added at element mole ratio of Cu:Mn:Ti =(1-5):(1-5):(40-48) and then vigorously stirring at the temperature of 40 C. for 1 to 3 h with the rotating speed at 300 to 500 r/min; wherein, the mass ratio of the tetrabutyl titanate to surfactant is 1:1 to 3:1.

5. The method according to claim 1, wherein in the step (d), the mixture is placed under conditions at a temperature of 40 C. and a relative humidity of 40 to 60%, and stands for 12 to 24 h for volatilization.

6. The method according to claim 1, wherein in the step (e), calcinating is conducted at 350 to 350 C. for 5 h.

7. The method of claim 1, wherein the surfactant comprises a polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer having the molecular formula (ethylene oxide).sub.106(propylene oxide).sub.70(ethylene oxide).sub.106.

Description

DETAILED DESCRIPTION OF THE INVENTION

(1) Further illustration of the present invention is made in connection with the following examples.

EXAMPLE 1

(2) Adding appropriate amount of hydrochloric acid and acetic acid into an ethanol solution to prepare a dissolving system; wherein the concentrations of the hydrochloric acid and the acetic acid are 50 g/L and 100 g/L, respectively.

(3) Adding a surfactant F127 into the dissolving system and fully stirring for dissolution; wherein, the mass ratio of F127 to ethanol is 1:20. (3), adding copper nitrate, manganese nitrate solution and tetrabutyl titanate at element mole ratio of Cu:Mn:Ti=1:1:48 into the mixed liquid obtained from step (2), wherein the mass ratio of the tetrabutyl titanate to F127 is 3:1, and then vigorously stirring at the temperature of 40 C. for 1 h with the rotating speed at 500 r/min.

(4) Transferring the mixture obtained from step (3) into petri dishes, placing it under conditions at a temperature of 40 C. and a relative humidity of 40% and letting it stand for 12 h for volatilization and then drying at a temperature of 65 C. for 24 h.

(5) Calcinating the acquired transparent films at 350 C. for 5 h to obtain the mesoporous ternary composite materials.

(6) The mesoporous ternary composite materials have particle sizes at 5 to 8 mm, the specific surface area is equal to 300 m.sup.2/g, pore volume is greater than 0.3 mL/g; the mesoporous ternary composite materials comprise 2% of CuO, 2% of MnO.sub.x and 96% of TiO.sub.2 in molar ratio, wherein the MnO.sub.x is MnO.sub.2 and Mn.sub.2O.sub.3.

EXAMPLE 2

(7) Adding appropriate amount of hydrochloric acid and acetic acid into an ethanol solution to prepare a dissolving system; wherein the concentrations of the hydrochloric acid and the acetic acid are 30 g/L and 60 g/L, respectively.

(8) Adding appropriate amount of the surfactant F127 into the dissolving system and fully stirring for dissolution; wherein, the mass ratio of F127 to ethanol is 1:10.

(9) Adding copper nitrate, manganese nitrate solution and tetrabutyl titanate at element mole ratio of Cu:Mn:Ti=5:5:40 into the mixed liquid obtained from step (2), wherein the mass ratio of the tetrabutyl titanate to F127 is 1:1 and then vigorously stirring at the temperature of 40 C. for 3 h with the rotating speed at 300 r/min.

(10) Transferring the mixture obtained from step (3) into petri dishes, placing it under conditions at a temperature of 40 C. and a relative humidity of 60% and letting it stand for 24 h for volatilization and then drying at a temperature of 65 C. for 48 h.

(11) Calcinating the acquired transparent films at 450 C. for 5 h to obtain the mesoporous ternary composite materials.

(12) The mesoporous ternary composite materials have particle sizes at 5 to 8 mm, the specific surface area is equal to 200 m.sup.2/g, pore volume is greater than 0.3 mL/g; the mesoporous ternary composite materials comprise 10% of CuO, 10% of MnO.sub.x and 80% of TiO.sub.2 in molar ratio, wherein the MnO.sub.x is MnO.sub.2 and Mn.sub.2O.sub.3.

EXAMPLE 3

(13) Adding appropriate amount of hydrochloric acid and acetic acid into an ethanol solution to prepare a dissolving system; wherein the concentrations of the hydrochloric acid and the acetic acid are 40 g/L and 80 g/L, respectively.

(14) Adding appropriate amount of the surfactant F127 into the dissolving system and fully stirring for dissolution; wherein, the mass ratio of F127 to ethanol is 1:15.

(15) Adding copper nitrate, manganese nitrate solution and tetrabutyl titanate at element mole ratio of Cu:Mn:Ti=5:5:90 into the mixed liquid obtained from step (2), wherein the mass ratio of the tetrabutyl titanate to F127 is 2:1 and then vigorously stirring at the temperature of 40 C. for 2 h with the rotating speed at 400 r/min.

(16) Transferring the mixture obtained from step (3) into petri dishes, placing it under conditions at a temperature of 40 C. and a relative humidity of 50% and letting it stand for 24 h for volatilization and then drying at a temperature of 65 C. for 48 h.

(17) Calcinating the acquired transparent films at 550 C. for 5 h to obtain the mesoporous ternary composite materials.

(18) The mesoporous ternary composite materials have particle sizes at 5 to 8 mm, the specific surface area is equal to 260 m.sup.2/g, pore volume is greater than 0.3 mL/g; the mesoporous ternary composite materials comprise 5% of CuO, 5% of MnO.sub.x and 90% of TiO.sub.2 in molar ratio, wherein the MnO.sub.x is MnO.sub.2 and Mn.sub.2O.sub.3.

(19) The above descriptions of examples are conducive for ordinary technicians of the present technical field to understand and exploit the invention. It is obvious that persons skilled in the art of the present field can easily make various amendments to the above examples and apply the general principle illustrated in here into other examples without the effort of inventive work. Therefore, the present invention is not confined to examples herein. Any improvements and modifications conducted by persons skilled in the art of the present field according to the instructions of the present invention and without going beyond the scope of the present invention shall be included in the extent of protection of the present invention.