The method of dredging of boron aluminum molecules to sieve holes
A technology of boroaluminate and molecular sieve, which is applied in the direction of molecular sieve compounds, molecular sieve catalysts, molecular sieves and alkali exchange compounds, etc., can solve the problems of pore blockage, small specific surface area, and influence on the catalytic activity of PKU-n series materials, and achieve reproducibility High performance, increased specific surface area, and easy operation
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Embodiment 1
[0026] Example 1: Synthesis of Cr-PKU-1
[0027] (1) Weigh 200mg Cr (NO 3 ) 3 ·9H 2 O and 1575mg Al (NO 3 ) 3 ·9H 2 O is placed in the polytetrafluoroethylene lining of the hydrothermal kettle, and 0.3 mL of concentrated nitric acid is added to it, placed in a vacuum oven at 60 °C for reaction for 0.5 h, naturally cooled, and taken out;
[0028] (2) Weigh 6g H 3 BO 3 was added to the reaction mixture obtained in the previous step, and was placed in an oven for hydrothermal reaction at 190° C. for 2 hours again;
[0029] (3) The mixture obtained after the reaction is placed in deionized water, and placed on a magnetic stirrer and stirred for 20 min, and the supernatant is removed after natural sedimentation, and washed and sedimented with deionized water more than 3 times, and placed in a vacuum drying oven Cr-PKU-1 can be obtained by medium drying.
[0030] The SEM photo of the Cr-PKU-1 synthesized in Example 1 is as follows figure 1 As can be seen from the photos, t...
Embodiment 2
[0036] Example 2: Cleaning Cr-PKU-1
[0037] (1) 40 mg of Cr-PKU-1 synthesized in Example 1 was weighed and fully ground for 10 min, then dropped into 15 mL of organic solvent, placed in a round-bottomed flask and connected to a reflux device, and maintained at a constant temperature of 60 °C in an oil bath for 5 hours;
[0038] (2) sedimentation of the mixture passing through the constant temperature oil bath in the step (1), removing the supernatant, throwing in the same organic solvent as the step (1) again, repeating the cleaning 5 times, then placing the sediment in a vacuum oven and drying at 80°C The cleaned sample of Cr-PKU-1 can be obtained.
[0039] Wash with three organic solvents under the same conditions. The three organic solvents are a mixed solution of acetonitrile and ethylene glycol with a volume ratio of 6:1 and a mixed solution of acetonitrile and glycerol with a volume ratio of 6:1. , a mixed solution with a volume ratio of acetonitrile and 1,4-dioxane of...
Embodiment 3
[0041] Example 3: BET testing
[0042] (1) Weigh 100 mg of Cr-PKU-1 before and after cleaning, and place them in sample tubes respectively;
[0043] (2) The above-mentioned sample tube is degassed at 150°C for 2 hours under vacuum conditions to remove impurities adsorbed on the surface of the sample, such as water, oil, etc.;
[0044] (3) Flush the degassed sample tube containing Cr-PKU-1 into N 2 , and then connect it to the physical adsorption instrument for testing to obtain the specific surface area data of the sample.
[0045] The BET curves of Cr-PKU-1 before and after cleaning are as follows Figure 4 As shown in Table 1, the specific surface area is shown in Table 1, from which it can be seen that the specific surface area of Cr-PKU-1 after cleaning with the mixed solution of acetonitrile and 1,4-dioxane is the largest, and the increase is nearly 7 times of the original.
[0046] Table 1 Specific surface area of Cr-PKU-1
[0047] sample Specific surf...
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