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Synthesis method of mesoporous-microporous Cr-MIL-101 carrier capable of realizing synchronous immobilizing of phosphotungstic acid

A synthesis method and phosphotungstic acid technology, applied in the field of materials, can solve problems such as limiting the application of PTA, and achieve the effects of simple preparation process and high material yield

Active Publication Date: 2018-12-04
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can only be applied to the catalytic conversion of small molecules such as hexanol and cyclopentene, while macromolecules such as cellulose and starch are difficult to enter into the pores of MOFs and fully contact with the catalytic center of PTA, which limits the application of PTA.

Method used

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  • Synthesis method of mesoporous-microporous Cr-MIL-101 carrier capable of realizing synchronous immobilizing of phosphotungstic acid
  • Synthesis method of mesoporous-microporous Cr-MIL-101 carrier capable of realizing synchronous immobilizing of phosphotungstic acid
  • Synthesis method of mesoporous-microporous Cr-MIL-101 carrier capable of realizing synchronous immobilizing of phosphotungstic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The meso-micro-double-porous Cr-MIL-101 material with simultaneous immobilization of phosphotungstic acid was prepared by the following method: 45 mL distilled water, 6.0 mmol Cr(NO 3 ) 3 ∙9H 2 O, 0.3 mmol PTA, 6.0 mmol 2-aminoterephthalic acid, and 1.8 mmol CTAB were stirred evenly at room temperature, then added to a 100 mL polytetrafluoroethylene reactor, heated at 150 °C for 12 h, cooled to room temperature, and then used The solid obtained after repeated washing and centrifugation with DMF and ethanol was vacuum-dried at 80 °C for 16 h, and the obtained solid was the meso-microbiporous Cr-MIL-101 material with synchronously immobilized phosphotungstic acid.

Embodiment 2

[0022] The meso-micro-double-porous Cr-MIL-101 material with simultaneous immobilization of phosphotungstic acid was prepared by the following method: 45 mL distilled water, 6.0 mmol Cr(NO 3 ) 3 ∙9H 2 O, 0.3 mmol PTA, 6.0 mmol 2-aminoterephthalic acid, and 3.6 mmol CTAB were stirred evenly at room temperature, then added to a 100 mL polytetrafluoroethylene reactor, heated at 150 °C for 12 h, cooled to room temperature, and then used The solid obtained after repeated washing and centrifugation with DMF and ethanol was vacuum-dried at 80 °C for 16 h, and the obtained solid was the meso-microbiporous Cr-MIL-101 material with synchronously immobilized phosphotungstic acid.

[0023] The pore size distribution figure of embodiment 1~2 gained material is as follows figure 1 with figure 2 As shown, it can be seen that the products added with CTAB all have a meso-micro biporous structure, wherein the material pore size distribution obtained in Examples 1~2 is 1.1~46 nm, and the mes...

Embodiment 3

[0029] The application of the meso-micro-double-porous Cr-MIL-101 material that simultaneously immobilizes phosphotungstic acid includes the following steps: adding 0.12 g of the meso-micro-double-porous Cr-MIL-101 that simultaneously immobilizes phosphotungstic acid to 10 mL of distilled water material or pure PTAx g with the same amount of PTA immobilized in the meso-micro-biporous Cr-MIL-101 material of 0.12 g synchronously immobilized phosphotungstic acid, and 0.04 g microcrystalline cellulose was added at the same time, and kept at a constant temperature of 180 °C Heated and stirred continuously for 11 h, and centrifuged after the reaction. The solid residue precipitated at the bottom of the centrifuge tube after centrifugation is the large-pore metal-organic framework material of immobilized PTA used to catalyze the hydrolysis of microcrystalline cellulose after the reaction, which can be washed with distilled water and dried at 80 °C for 16 h. reuse.

[0030] Cr 3+ : ...

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Abstract

The invention discloses a synthesis method of a mesoporous-microporous Cr-MIL-101 carrier capable of realizing synchronous immobilizing of phosphotungstic acid. The synthesis method comprises following steps: distilled water, 2-aminoterephthalic acid, Cr(NO3)3-9H2O, PTA, and CTAB are mixed to be uniform using magnetic stirring, an obtained mixture is heated for 10 to 14h at a constant temperatureof 130 to 170 DEG C, an obtained product is cooled to room temperature through natural cooling, and is subjected to centrifugation; an obtained solid substance is washed repeatedly with DMF and ethanol until the supernatant of centrifugation is transparent, and the solid substance is subjected to vacuum drying for 15.95 to 16.05h at 78 to 82 DEG C so as to obtain the mesoporous-microporous Cr-MIL-101 carrier capable of realizing synchronous immobilizing of phosphotungstic acid. The synthesis method is simple; yield is high; the synthesis method is convenient for large scale production; no organic solution or alkaline solution is added as a solvent in synthesis process; the obtained PTA@MIL-101(Cr)-NH2 is excellent in water stability and heat stability.

Description

technical field [0001] The invention belongs to the field of materials, and in particular relates to a synthesis method of a meso-micro-double hole Cr-MIL-101 carrier which simultaneously immobilizes phosphotungstic acid. Background technique [0002] As a solid acid catalyst with strong oxidizing properties and strong electronegativity, PTA has broad application prospects, and its immobilization is the key to solving the difficulties in its recovery and reuse. Without affecting the catalytic performance of PTA, the existing solid-phase PTA formed by immobilization such as hydrogen zeolite and MOFs has a microporous structure with channels less than 2nm. It can only be applied to the catalytic conversion of small molecules such as hexanol and cyclopentene, while macromolecules such as cellulose and starch are difficult to enter the MOFs pores and fully contact with the PTA catalytic center, which limits the application of PTA. The present invention proposes a method for syn...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J27/188B01J35/10C13K1/02
CPCC13K1/02B01J27/188B01J31/1691B01J2531/0241B01J2531/62B01J35/643B01J35/695B01J35/647
Inventor 王艳万金泉郝金蕾马邕文
Owner SOUTH CHINA UNIV OF TECH
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