Metal organic framework adsorbent as well as preparation method and application thereof

A metal-organic framework and metal-organic framework technology are applied in the field of metal-organic framework adsorbents and their preparation, which can solve the problem of low selectivity, and achieve the effects of large adsorption capacity, high-efficiency separation selectivity, and strong adsorption effect.

Active Publication Date: 2015-04-08
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these new MOF materials have a high adsorption capacity for alkenes and alkanes, they also have the problem of low selectivity.

Method used

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  • Metal organic framework adsorbent as well as preparation method and application thereof
  • Metal organic framework adsorbent as well as preparation method and application thereof
  • Metal organic framework adsorbent as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) MIL-101(Cr)-SO 3 Preparation of H: 4g chromium nitrate nonahydrate, 5.4g sodium monosulfonate terephthalic acid, 60g deionized water and 0.6g hydrofluoric acid (~40wt%) (ratio: 1mmol: 2mmol: 6g: 0.06g) Add it into the reaction kettle, stir it evenly with ultrasonic waves, and then react at 190°C for 24 hours to obtain ((Cr))-MIL-101-SO 3 H. The initially synthesized MOF was washed with deionized water and ethanol for 2 to 3 times respectively, centrifuged, filtered, and finally vacuum-dried at 120°C for 12 hours to obtain the purified MIL-101(Cr)-SO 3 H, the specific surface area is 1856m 2 / g, the pore volume is 1.35cm 3 / g. Unless otherwise specified, the following examples are MIL-101(Cr)-SO synthesized by this method 3 H.

[0042] (2) Adsorbent MIL-101(Cr)-SO 3 The preparation of Ag: get the purified MIL-101(Cr)-SO in 250mg step (1) 3 H was added to the container. Then add 20ml of AgBF at a concentration of 40mg / ml 4 In the solution of acetonitrile / wat...

Embodiment 2

[0045] Adsorbent MIL-101(Cr)-SO 3 The preparation of Ag: get the purified MIL-101(Cr)-SO in 250mg embodiment 1 step (1) 3 H was added to the container, and then 20ml, 40mg / ml AgNO 3 in a solution of acetonitrile / water (volume ratio 1:1). Stir in the dark for 6 hours, centrifuge, remove the supernatant, and vacuum-dry at 120°C for 12 hours to obtain MIL-101(Cr)-SO with a loading of Ag(I) of 17.6wt%. 3 Ag.

[0046] At 30°C and 100kPa, the adsorption capacity of the adsorbent for ethylene is 2.15mmol / g, and the adsorption capacity for ethane is 1.48mmol / g. AgNO can be found 3 No AgBF as active ingredient 4 The effect is good, so the next experiments all use AgBF 4 as an active ingredient.

Embodiment 3

[0048] Adsorbent MIL-101(Cr)-SO 3 The preparation of Ag: get the purified MIL-101(Cr)-SO in 250mg example 1 step (1) 3 Add H into the container, then add 20ml, 40mg / ml AgBF 4 in a solution of acetonitrile / water (volume ratio 1:1). Stir in the dark for 12 hours, centrifuge, remove the supernatant, and dry in vacuum at 120°C for 12 hours to obtain MIL-101(Cr)-SO with a loading of Ag(I) of 24.8wt%. 3 Ag.

[0049] At 30°C and 100kPa, the adsorption capacity of the adsorbent to ethylene is 2.43mmol / g, and the adsorption capacity to ethane is 1.37mmol / g, calculated by IAST C 2 h 4 / C 2 h 6 (1:1) separation selectivity is 12.

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Abstract

The invention discloses a metal organic framework adsorbent. A sulfonic acid funtionalized metal organic framework material MIL-101(Cr)-SO3H serves as a carrier, Ag(I) serves as an active ingredient, the active ingredient is loaded to the carrier by virtue of an ion exchange reaction, and the loading capacity is 10-40wt% based on the total amount of the adsorbent. The invention also discloses a method for preparing the metal organic framework adsorbent. The method comprises the following steps: preparing the MIL-101(Cr)-SO3H, mixing the MIL-101(Cr)-SO3H with solution of Ag(I), carrying out an ion exchange reaction, thereby obtaining the adsorbent MIL-101(Cr)-SO3H Ag. The preparation process is simple, the conditions are mild, and the prepared adsorbent can realize high-selectivity separation on olefin / alkane mixed gas and has good industrial application prospects in the deep desulfurization aspect of fuel oil.

Description

technical field [0001] The invention relates to the technical field of adsorption materials, in particular to a metal organic framework adsorbent and its preparation method and application. Background technique [0002] The separation of olefins and alkanes is an important separation process in the petrochemical industry, among which the separation of ethylene-ethane and propylene-propane is the most representative. In olefins plants, cryogenic rectification has traditionally been used to separate olefins-alkanes. Although rectification is a very mature process, it consumes a lot of energy. Researchers have been working hard to find an efficient, energy-saving, and low-cost method to replace low-temperature distillation. The adsorption method is due to its high efficiency, energy saving, and low cost. Advantages, it is currently recognized as one of the methods most likely to replace cryogenic separation. [0003] The key to the adsorption separation of alkenes and alkanes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30C10G25/06
CPCB01J20/223B01J20/3085B01J2220/4812C10G25/06C10G2300/202
Inventor 鲍宗必任其龙常刚刚黄敏慧苏宝根邢华斌杨亦文张治国杨启炜
Owner ZHEJIANG UNIV
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