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Organic porous material for electronic special gas separation and purification and preparation method thereof

A technology for separation and purification of porous materials, applied in the field of organic porous materials for separation and purification of electronic special gases and its preparation, to achieve good chemical stability, inhibition of adsorption and diffusion, and high-efficiency adsorption and separation

Pending Publication Date: 2022-07-26
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of organic porous material and preparation method thereof for the separation and purification of electronic special gas, to overcome the defect that existing adsorbent technology exists, the F-POF material synthesized based on the aromatic dehalogenation reaction mechanism of the present invention is because The connection method of carbon-carbon bond shows excellent corrosion resistance. Due to its large conjugated structure and good hydrophobicity, the fluorine-containing F-POF based on carbon-carbon bond is expected to show obvious advantages in the recovery and purification of electronic special gases. The advantages

Method used

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  • Organic porous material for electronic special gas separation and purification and preparation method thereof
  • Organic porous material for electronic special gas separation and purification and preparation method thereof
  • Organic porous material for electronic special gas separation and purification and preparation method thereof

Examples

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Effect test

Embodiment 1

[0045] Step 1: In the 10L reaction kettle, weigh 1mol of tetrabromotetraphenylmethane and 2mol of 1,2,4,5 tetrafluorobenzene and add it, then add 0.1mol of palladium acetate, 0.2mol of tri-tert-butylphosphine tetrafluoroborate and 6LDMF, the materials are shaken and mixed evenly, after the nitrogen protection is completed, the temperature is set to 120 ° C, and the mixture is obtained by heating for 48 hours;

[0046] Step 2: Cool the mixture obtained in step 1 to room temperature, pour it into a material bucket, perform suction filtration on the obtained mixture, use DMF and methanol as washing solvents, and wash three times each to obtain a filter cake. Put the filter cake into a beaker containing DMF solution, rotate and stir on a magnetic stirrer for 1 h, and then perform suction filtration. The obtained product was subjected to Soxhlet extraction with ethanol reagent for 24 hours to further remove impurities, and the solid extracted by Soxhlet was vacuum-dried at 150° C. ...

Embodiment 2

[0052] Step 1: In the 10L reaction kettle, weigh 1mol of tetrabromotetraphenylmethane and 2mol of 1,2,4,5 tetrafluorobenzene and add it, then add 0.1mol of palladium acetate, 0.2mol of tri-tert-butylphosphine tetrafluoroborate With 6L nitrogen methyl pyrrolidone, the materials are shaken and mixed evenly, after nitrogen protection is completed, the temperature is set to 150 ° C, and heated for 48 hours to obtain a mixed solution;

[0053] Step 2: Cool the mixture obtained in step 1 to room temperature, pour it into a material bucket, perform suction filtration on the obtained mixture, use ethanol and methanol as washing solvents, and wash three times each to obtain a filter cake. Put the filter cake into a beaker containing DMF solution, rotate and stir on a magnetic stirrer for 1 h, and then perform suction filtration. The obtained product was subjected to Soxhlet extraction with ethanol reagent for 24 hours to further remove impurities, and the solid extracted by Soxhlet was...

Embodiment 3

[0063] Step 1: In the 10L reaction kettle, weigh 1mol of tetrabromotetraphenylmethane and 2mol of 1,2,4,5 tetrafluorobenzene and add it, then add 0.1mol of palladium acetate, 0.2mol of tri-tert-butylphosphine tetrafluoroborate and 6L nitrogen methyl pyrrolidone, the materials are shaken and mixed evenly, after nitrogen protection is completed, the temperature is set to 130 ° C, and heated for 48 hours to obtain a mixed solution;

[0064] Step 2: Cool the mixture obtained in step 1 to room temperature, pour it into a material bucket, perform suction filtration on the obtained mixture, use methanol as a rinsing solvent, and rinse three times to obtain a filter cake. Put the filter cake into a beaker containing DMF solution, rotate and stir on a magnetic stirrer for 1 h, and then perform suction filtration. The obtained product was then subjected to Soxhlet extraction with ethanol reagent for 24 hours to further remove impurities, and the solid extracted by Soxhlet was vacuum-dri...

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Abstract

The invention discloses an organic porous material for electronic special gas adsorption separation and a preparation method thereof, and a fluorine-containing organic porous framework material product connected by carbon-carbon bonds is obtained according to an aromatic hydrocarbon dehalogenation reaction principle. The material prepared by the invention has an organic nanopore structure and strong hydrophobic property, so that the material has an obvious adsorption effect on electronic special gas due to the structural characteristic.

Description

technical field [0001] The invention belongs to the field of preparation of organic porous framework materials, in particular to an organic porous material used for separation and purification of electronic special gas and a preparation method thereof. Background technique [0002] Global semiconductor market sales will reach $440 billion in 2020, a 6.8% increase from 2019, and double-digit growth of 10.9% is expected in 2021. Fluorinated electronic specialty gases (F-gases) are critical to current semiconductor manufacturing because of their unique chemical reactivity for plasma etching and cleaning, currently not replicated by other alternatives. For example, NF 3 , CF 4 and SF 6 Widely used in wafer plasma etching and chemical vapor deposition chamber plasma cleaning in the manufacture of integrated circuits, solar cells and electronic devices. Currently, in the electronic gas market, fluorine-containing electronic specialty gases account for about 30% of the total ga...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30B01D53/02
CPCB01J20/226B01J20/28011B01J20/28066B01J20/28071B01D53/02
Inventor 马和平颜童张文祥
Owner XI AN JIAOTONG UNIV
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