Functionalization of a metal-organic framework material uio-67-4me and its functionalized products and applications
A metal-organic framework, functionalized technology, applied in chemical instruments and methods, other chemical processes, separation methods, etc., can solve the problems of limited types of MOFs and application limitations, and achieve good indoor humidity automatic regulation function, good adsorption- Desorption performance, good recyclability effect
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Embodiment 1
[0083] Example 1 Preparation of UiO-67-4Me
[0084] S1. 3,3',5,5'-tetramethyl-[1,1'-biphenyl]-4,4'-dicarboxylic acid (0.03mmol / 10.0mg), ZrCl 4 The mixed solution of (0.036mmol / 8.5mg), trifluoroacetic acid (0.67mmol / 50uL) and N,N-dimethylformamide (2mL) was put into a 10mL glass bottle, and after ultrasonic mixing, it was transferred to a 120°C oven Medium constant temperature for 48 hours;
[0085] S2. Cool the vial after the reaction in step S1 to room temperature, centrifuge and filter to obtain a solid product, and wash with N,N-dimethylformamide for 5 times to obtain UiO-67-4Me.
Embodiment 2
[0086] Example 2 Preparation of UiO-67-4Me amino / carboxyl / hydroxyl / diamino functionalized product
[0087] With UiO-67-4Me and 2-amino-[1,1'-biphenyl]-4,4'-dicarboxylic acid or 2-carboxy-[1,1'-biphenyl]-4,4'-dicarboxylic acid Or 2-hydroxy-[1,1'-biphenyl]-4,4'-dicarboxylic acid or 2,2'-diamino-[1,1'-biphenyl]-4,4'-dicarboxylic acid as raw material Preparation of UiO-67-4Me-NH separately 2 -X% (x=29, 38, 47, 59, 67), UiO-67-4Me-COOH-38%, UiO-67-4Me-OH-37%, UiO-67-4Me-2NH 2 -38% of the prepared flow diagram as in figure 1 shown.
[0088] 1. UiO-67-4Me-NH 2 - Preparation of x% (x=29, 38, 47, 59, 67)
[0089] S1. UiO-67-4Me (0.052mmol / 130.0mg) and different amounts of 2-amino-[1,1'-biphenyl]-4,4'-dicarboxylic acid (respectively 13.5mg / 0.052mmol, 17.8 mg / 0.069mmol, 21.9mg / 0.084mmol, 27.8mg / 0.107mmol, 31.5mg / 0.121mmol) and N,N-dimethylformamide (10mL) mixed solution was put into a 20mL glass bottle, after ultrasonic mixing , transferred to a constant temperature of 85°C for 24...
Embodiment 3
[0100] Example 3 Determination of specific surface area and pore volume of UiO-67-4Me amino / carboxyl / hydroxyl / diamino functionalized product
[0101] (1) Activation
[0102] S1. UiO-67-4Me-NH prepared by UiO-67-4Me and Example 2 2 -29%, UiO-67-4Me-NH 2 -38%, UiO-67-4Me-NH 2 -47%, UiO-67-4Me-NH 2 -59%, UiO-67-4Me-NH 2 -67%, UiO-67-4Me-COOH-38%, UiO-67-4Me-OH-37%, UiO-67-4Me-2NH 2 -38% solids were soaked in N,N-dimethylformamide at a ratio of 50mg:10mL for 2 days, with N,N-dimethylformamide replaced every 8 hours.
[0103] S2. Soak the solid soaked in step S1 in acetone at a ratio of 50 mg: 10 mL for 2 days, and replace the acetone every 8 hours.
[0104] S3. The solid soaked in step S2 is separated by centrifugation, and then left in the air for preliminary drying. Then vacuum heated to 100°C in a closed container and kept for 10 hours to obtain activated UiO-67-4Me, UiO-67-4Me-NH 2 -29%, UiO-67-4Me-NH 2 -38%, UiO-67-4Me-NH 2 -47%, UiO-67-4Me-NH 2 -59%, UiO-67-4Me-NH ...
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