Method for removing organic amine template in molecular sieve
A technology for molecular sieves and organic amines, applied in the field of removing organic amine templates in molecular sieves, can solve the problems of severe reaction conditions, increase the cost of removing organic amine templates, increase the risk of roasting operations, etc., and achieve simple operation methods, roasting The effect of short time and high crystallinity
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Embodiment 1
[0043] Weigh 2.43g of copper chloride dihydrate, add 500mL of water to form a copper chloride aqueous solution, add 1.94g of concentrated ammonia water with a mass fraction of 25% dropwise, and prepare a copper hydroxide gel.
[0044] Weigh 20g of the background sample S0 at room temperature and mix it with copper hydroxide gel, filter, wash the filter cake with deionized water several times, and dry at 110°C to obtain the intermediate sample S10 ( figure 1 ), the intermediate sample S10 was placed in a muffle furnace, and in an air atmosphere, the temperature was raised from room temperature to 350° C. over 1 hour, and the intermediate sample S11 was obtained after cooling at a constant temperature of 350° C. for 4 hours.
[0045] The thermogravimetric analysis diagram of S11 is shown in figure 2 , figure 2 It shows that the organic amine templating agent in S11 has been removed completely, which is confirmed by image 3 The disappearance of the C-H bending vibration peak...
Embodiment 2
[0049] Weigh 1.72 g of copper nitrate trihydrate, add 500 mL of water to form a copper nitrate aqueous solution, and add 0.97 g of concentrated ammonia water with a mass fraction of 25% dropwise to prepare a copper hydroxide gel.
[0050] Weigh 20g of the background sample S0, stir and mix it with copper hydroxide gel at room temperature, filter, wash the filter cake with deionized water several times, dry it at 110°C and place it in a muffle furnace. After 1 hour, the temperature was raised to 400° C., and the intermediate sample S21 was obtained after cooling at 400° C. for 4 hours.
[0051] The thermogravimetric analysis diagram of sample S21 is shown in figure 2 , figure 2 It shows that the organic amine template has been removed completely.
[0052] Grind the roasted sample S21 into powder in a quartz grinder, add 100 mL of ammonium chloride aqueous solution with a mass fraction of 10%, and adjust the pH to about 7.0 with ammonia water. Stir at room temperature for 1...
Embodiment 3
[0055] Weigh 2.43g of copper chloride dihydrate, add 20mL of water to form an aqueous solution of copper chloride, weigh 20g of the background sample S0 and mix it with aqueous solution of copper chloride at room temperature, dry it at 110°C and place it in a muffle furnace. In the atmosphere, the temperature was raised from room temperature to 350° C. over 1 hour, and fired at a constant temperature of 350° C. for 4 hours, and the intermediate sample S31 was obtained after cooling.
[0056] The thermogravimetric analysis chart of S31 is shown in figure 2 , figure 2 It shows that the organic amine template has been removed completely.
[0057] Grind S31 into powder in a quartz grinder, add 100 mL of ammonium acetate aqueous solution with a mass fraction of 10%, and adjust the pH to about 7.0 with ammonia water. Stir at room temperature for 120-180 minutes, and filter off the copper-containing residual solution. Finally, it was washed several times with deionized water, an...
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