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Method for functionalizing porous metal-organic framework materials, solid acid catalyst using same, and method for evaporating alcohol using the solid acid catalyst

A porous metal and organic framework technology, applied in organic chemistry, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., can solve problems such as high operating costs and uneconomical

Inactive Publication Date: 2012-10-24
KOREA RES INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] However, the method of maintaining the reactor at a vacuum or high pressure is not only uneconomical in terms of reactor composition, but also has very high operating costs. Therefore, it is necessary to provide a simpler alcohol dehydration reaction process that does not use High or reduced pressure without removal of by-product water

Method used

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  • Method for functionalizing porous metal-organic framework materials, solid acid catalyst using same, and method for evaporating alcohol using the solid acid catalyst
  • Method for functionalizing porous metal-organic framework materials, solid acid catalyst using same, and method for evaporating alcohol using the solid acid catalyst
  • Method for functionalizing porous metal-organic framework materials, solid acid catalyst using same, and method for evaporating alcohol using the solid acid catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0091] Embodiment 1 (functionalization of MIL-101 (Cr))

[0092] MIL-101(Cr)-AS was synthesized (Crystal Growth Design, 10, 1860, 2010 (Crystal Growth Design, 10, 1860, 2010)), and then 0.3 g of MIL-101(Cr) was added to a glass test tube using the material -AS, then add 20ml of DMF to make a suspension. After heating to 70° C., the suspension in the test tube was irradiated with ultrasonic waves for 60 minutes by using an ultrasonic generator (VC ×750, Sonic & materials). After cooling, the solid was collected by filtration and dried at 100° C. for 5 hours to obtain 0.25 g of refined MIL-101(Cr). 0.3g of MIL-101 (Cr) collected through 2 refinements was dried and cooled at 150°C under a vacuum condition of 0.8 pressure, and then 0.096g (1.25mmol) of cysteamine was added to 30ml of In ethanol, it was heated to reflux at 80°C for 8 hours. It was then filtered and dried to obtain 0.3 g of MIL-101(Cr) (referred to as MIL-101(Cr)-SH). Use 0.4g of MIL-101(Cr)-SH synthesized by th...

Embodiment 2

[0094] Embodiment 2 (using MIL-101 (Cr)-SO 3 Dehydration reaction of sorbitol in H)

[0095] Using the MIL-101(Cr)-SO obtained in Example 1 3 The H catalyst carried out the dehydration reaction of sorbitol. 10g of sorbitol and 0.2g of MIL-101(Cr)-SO 3 The H catalyst was added into a microwave reactor, and then reacted at 180° C. for 3 hours in a microwave oven (MARS-5, CEM Company). After the reaction, cooling was performed, the reactor was opened, and the solid catalyst was separated by filtration at high temperature. The obtained product was then dried at 110° C. to remove water. The composition of the product was analyzed using Acme 9000HPLC of Younglin Company equipped with RI detector and Asahipak NH2P-504E (No. N712004) column. The reaction conditions and results are briefly recorded in Table 1.

[0096] The dehydration conversion rate was 100%, and the yield of obtained isosorbide was 49.6%.

Embodiment 3

[0097] Embodiment 3 (using MIL-101 (Cr)-SO 3 H dehydration reaction of 2-butanol)

[0098] Using the MIL-101(Cr)-SO of 0.1g obtained in Example 1 3 H catalyst, carried out the dehydration reaction of 2-butanol with gas phase. The space velocity of the reactants is 1h -1 , the catalyst is dehydrated at 300°C, and the reaction temperature is 275°C. Such as image 3 As shown, it was confirmed by GC that butenes can be easily obtained by the dehydration reaction, and the catalyst performance can be stably maintained for more than 4 hours.

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Abstract

The present invention relates to a method for functionalizing porous metal-organic framework materials which have a large surface area and molecular- or nano-scale pores, and which can thus be used for an absorbent, gas storage, a sensor, a membrane, a functional thin film, a catalyst, a catalyst carrier, and the like, to a method for preparing a solid acid catalyst using same, and to a method for evaporating alcohol using the catalyst.

Description

technical field [0001] The present invention relates to a method for functionalizing porous metal-organic frameworks, and in more detail, involves activating porous metal-organic frameworks to generate unsaturated coordination sites and simultaneously containing Elements and sulfhydryl (-SH) compounds are coordinated and bonded to prepare functionalized porous metal-organic frameworks, and then oxidized sulfhydryls are converted into sulfonic acid groups (-SO 3 H), thereby obtaining the technology of solid acid catalyst. [0002] In addition, the present invention also relates to a method for dehydrating alcohol by using the solid acid catalyst obtained above and various catalysts. Background technique [0003] Porous metal-organic framework materials can be defined as porous organic-inorganic polymer compounds formed by the combination of central metal ions and organic ligands, which means that both organic and inorganic substances are included in the framework structure, ...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J37/00B01J35/10C07D493/04C07C11/08C07C1/24
CPCB01J31/226C07D493/04B01J20/226C07C1/24B01J31/2239B01J31/1691B01J31/1805B01J2531/62B01J2531/842B01J2531/31B01J2540/32C07C11/08
Inventor 黄镇秀张钟山丹尼斯・库马尔・米斯拉姜仁中祖拜尔・哈萨那祖木・阿贝丁・卡恩郑成和
Owner KOREA RES INST OF CHEM TECH
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