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Preparation method of modified metal organic framework material for adsorbing and separating BTEX in C8 aromatic hydrocarbon

A metal-organic framework, adsorption separation technology, applied in the direction of adsorption purification/separation, organic chemistry, selective adsorption, etc., can solve the problems of low selectivity and small adsorption capacity

Pending Publication Date: 2021-09-28
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved in the present invention is to provide a preparation for the problem that the current adsorption material has a small adsorption capacity and low selectivity for BTEX (BTEX including benzene, toluene, ethylbenzene and xylene) in C8 aromatics. The method is simple, and the alkylating agent is a synthetic method of modifying the metal-organic framework material with a quaternary ammonium salt cationic surfactant of an alkyl halide, and the prepared adsorption material has a higher adsorption capacity and selective separation effect on BTEX in C8 aromatics

Method used

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  • Preparation method of modified metal organic framework material for adsorbing and separating BTEX in C8 aromatic hydrocarbon
  • Preparation method of modified metal organic framework material for adsorbing and separating BTEX in C8 aromatic hydrocarbon
  • Preparation method of modified metal organic framework material for adsorbing and separating BTEX in C8 aromatic hydrocarbon

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Embodiment 1

[0029] [According to molar ratio Cu(NO 3 ) 2 ·3H 2 O:H 3 BTC:CTAB:DMSO=9:5:0.2:1130] to synthesize Cu 3 (BTC) 2 (H 2 O) 3 (CTAB):

[0030] Add H to the beaker 3 BTC (0.1051g, 0.5mmol) and DMSO 8mL, stirred and dissolved 3 ) 2 ·3H 2 O (0.2174g, 0.9mmol) was mixed and sonicated for 10min until all the solids were dissolved to form a homogeneous solution. CTAB (0.0073g, 0.02mmol) was added to the reaction kettle in advance. Transfer the homogeneous solution after ultrasound to a polytetrafluoroethylene-lined stainless steel reaction kettle, and crystallize at 120°C for 24 hours. After cooling, filter the blue-green powder at the bottom of the kettle, wash with ethanol, and put it in Dry in a drying oven at a constant temperature of 80°C for 24 hours to obtain Cu 3 (BTC) 2 (H 2 O) 3 (CTAB), the addition amount of CTAB among the embodiment 1 is 0.08wt%.

Embodiment 2

[0032] [According to molar ratio Cu(NO 3 ) 2 ·3H 2 O:H 3 BTC:CTAB:DMSO=9:5:0.4:1130] to synthesize Cu 3 (BTC) 2 (H 2 O) 3 (CTAB):

[0033]Add H to the beaker 3 BTC (0.1051g, 0.5mmol) and DMSO 8mL, stirred and dissolved 3 ) 2 ·3H 2 O (0.2174g, 0.9mmol) was mixed and sonicated for 10min until all the solids were dissolved to form a homogeneous solution. CTAB (0.01462g, 0.04mmol) was added to the reaction kettle in advance. Transfer the homogeneous solution after ultrasound to a polytetrafluoroethylene-lined stainless steel reaction kettle, and crystallize at 120°C for 24 hours. After cooling, filter the blue-green powder at the bottom of the kettle, wash with ethanol, and put it in Dry in a drying oven at a constant temperature of 80°C for 24 hours to obtain Cu 3 (BTC) 2 (H 2 O) 3 (CTAB), the CTAB addition amount is 0.16wt% among the embodiment 2.

Embodiment 3

[0035] [According to molar ratio Cu(NO 3 ) 2 ·3H 2 O:H 3 BTC:CTAB:DMSO=9:5:0.6:1130] to synthesize Cu 3 (BTC) 2 (H 2 O) 3 (CTAB):

[0036] Add H to the beaker 3 BTC (0.1051g, 0.5mmol) and DMSO 8mL, stirred and dissolved 3 ) 2 ·3H 2 O (0.2174g, 0.9mmol) was mixed and sonicated for 10min until all the solids were dissolved to form a homogeneous solution. CTAB (0.02195g, 0.06mmol) was added to the reaction kettle in advance. Transfer the homogeneous solution after ultrasound to a polytetrafluoroethylene-lined stainless steel reaction kettle, and crystallize at 120°C for 24 hours. After cooling, filter the blue-green powder at the bottom of the kettle, wash with ethanol, and put it in Dry in a drying oven at a constant temperature of 80°C for 24 hours to obtain Cu 3 (BTC) 2 (H 2 O) 3 (CTAB), the CTAB addition amount is 0.24wt% among the embodiment 3.

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Abstract

The invention relates to a preparation method of a modified metal organic framework material for adsorbing and separating BTEX in C8 aromatic hydrocarbon, the preparation method comprises the following steps: introducing a quaternary ammonium salt type cationic surface active agent into synthesis of the metal organic framework material, dissolving metal copper salt and trimesic acid ligand into an organic solvent, mixing, and carrying out ultrasonic treatment; and adding quaternary ammonium salt cationic surfactants with different molar ratios, reacting the obtained mixed solution in a hydrothermal environment, carrying out suction filtration on the obtained blue-green crystal, washing, and drying to obtain the modified metal organic framework material. The highest static saturation adsorption capacity of the metal organic framework material modified by the quaternary ammonium salt cationic surface active agent to p-xylene in C8 aromatic hydrocarbon can reach 456mg / g, the separation coefficient of para-position and ortho-position xylene isomers is higher than 10.0, the adsorption capacity and the separation selectivity are 1.5-2 times of those of most MOFs materials, and the metal organic framework material is an excellent material for replacing a commercial zeolite molecular sieve adsorbent.

Description

technical field [0001] The invention relates to the technical field of adsorption separation, in particular to a preparation method of a modified metal organic framework material used for adsorbing BTEX in C8 aromatic hydrocarbons. Background technique [0002] C8 aromatics are mainly composed of by-products such as BTEX (toluene, ethylbenzene, xylene, etc.) produced by the catalytic reforming process of crude oil. Wherein EB (ethylbenzene) usually exists as xylene isomer impurity. The xylene isomers are para-xylene (PX), ortho-xylene (OX) and meta-xylene (MX). Among the isomers, PX is the most valuable intermediate and an indispensable raw material for the synthesis of polyethylene terephthalate (PET) and polybutylene terephthalate (PBT). OX is mainly used in the production of phthalic anhydride, and MX is mainly used in the production of isophthalic acid. Due to the value of the individual isomers, efficient separation of xylene isomers from ethylbenzene is a key focus ...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30B01D15/08C07C7/12C07C15/08
CPCB01J20/226B01D15/08C07C7/12C07C15/08
Inventor 陈乐张楠李秀娟张致慧何明阳陈群
Owner CHANGZHOU UNIV
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