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Kaoline-2-pyrazine carboxylic acid intercalation compound and preparation method thereof

A technology of pyrazine carboxylic acid and compound, applied in the field of new compound and preparation thereof, can solve the problems of unsatisfactory intercalation effect, time-consuming and labor-intensive and the like

Inactive Publication Date: 2016-10-12
ANQING NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the strong interaction between kaolin layers, only a few polar molecules can be intercalated directly, such as dimethyl sulfoxide, methanol, potassium acetate, formamide, etc.; Functional guest molecules can only be intercalated between kaolin layers with kaolin-dimethyl sulfoxide as precursors through long-term stirring or high-temperature melting assistance, which is time-consuming and laborious, and the intercalation effect is not ideal. Further improving the intercalation preparation method has become required

Method used

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  • Kaoline-2-pyrazine carboxylic acid intercalation compound and preparation method thereof
  • Kaoline-2-pyrazine carboxylic acid intercalation compound and preparation method thereof
  • Kaoline-2-pyrazine carboxylic acid intercalation compound and preparation method thereof

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Effect test

Embodiment 1

[0018] Example 1: Add 600ml of distilled water to 10g of kaolin raw soil, and ultrasonically clean it for 1 hour to obtain water-washed kaolin; add 5g of water-washed kaolin, 50ml of dimethyl sulfoxide and 5ml of deionized water into a 100ml round-bottomed flask, and stir at room temperature for 12 hours to obtain K- DMSO precursor; 1g of the precursor and 1g of 2-pyrazinecarboxylic acid were sealed in a 25ml stainless steel reactor, reacted at 90°C for 5 hours, added 10ml of sodium hydroxide aqueous solution, centrifuged, washed, and dried to obtain K-2-PA .

Embodiment 2

[0019] Embodiment 2: Add 600ml distilled water to 10g kaolin raw soil, and ultrasonically clean it for 2 hours to obtain water-washed kaolin; add 5g water-washed kaolin, 50ml dimethyl sulfoxide and 5ml deionized water to a 100ml round-bottomed flask, stir at room temperature for 12 hours, and obtain K- DMSO precursor; 1g of the precursor and 1g of 2-pyrazinecarboxylic acid were sealed in a 25ml stainless steel reactor, and after 8 hours of reaction at 120°C, 20ml of sodium hydroxide aqueous solution was added, centrifuged, washed, and dried to obtain K-2-PA .

Embodiment 3

[0020] Embodiment 3: Add 600ml distilled water to 10g kaolin raw soil, and ultrasonically clean it for 0.5 hours to obtain water-washed kaolin; add 5g water-washed kaolin, 50ml dimethyl sulfoxide and 5ml deionized water to a 100ml round-bottomed flask, stir at room temperature for 24 hours, and obtain K- DMSO precursor; 1g of the precursor and 1g of 2-pyrazinecarboxylic acid were sealed in a 25ml stainless steel reactor, and after 10 hours of reaction at 160°C, 15ml of sodium hydroxide aqueous solution was added, centrifuged, washed, and dried to obtain K-2-PA .

[0021] The characterization of kaolin-2-pyrazinecarboxylic acid intercalation compound of the present invention:

[0022] (1) X-ray diffraction characterization

[0023] Powder diffraction data were collected on a Bruker D8 ADVANCE diffractometer operating at a current of 40 mA and a voltage of 40 kV. Copper target X-rays using graphite monochromatization. Data collection was done using 2q / q scan mode, with contin...

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Abstract

The invention relates to a kaoline-2-pyrazine carboxylic acid intercalation compound and a preparation method thereof. The preparation method comprises steps as follows: 1) natural kaoline soil is subjected to ultrasonic cleaning for 0.5 h, and washed kaoline is obtained; 2) the washed kaoline and dimethyl sulfoxide are stirred for 12 h at the room temperature, and a precursor is prepared; 3) the precursor and 2-pyrazine carboxylic acid (in the mass ratio being 1:1) are put in a stainless steel reaction kettle, intercalation is performed under increased pressure, and the mixture reacts for 5-10 h at the temperature of 90-160 DEG C; 4) a target product is obtained through alkali liquor washing, centrifugation and drying and has a chemical formula Al2Si2O5(OH)4.(2-PA)1.11, and 2-PA is 2-pyrazine carboxylic acid. The compound has a two-dimensional lamellar structure, and interlayer 2-pyrazine carboxylic acid molecules have N,O activity coordination sites and can be applied as potential optical, electric and dielectric materials. The kaoline-2-pyrazine carboxylic acid intercalation compound adopts a simple process and is convenient to prepare.

Description

[0001] This patent application is funded by the National Natural Science Foundation of China (funding number: 21201009). technical field [0002] The invention relates to a novel compound and a preparation method thereof, in particular to a kaolin-2-pyrazine carboxylic acid intercalation compound and a preparation method thereof. Background technique [0003] Kaolin (theoretical molecular formula, Al 2 Si 2 o 5 (OH) 4 ) is a non-metallic mineral material with a layered structure, and guest molecules can enter the interlayer through intercalation to form new intercalation compounds, which are widely used in the field of organic-inorganic hybrid materials. Due to the strong interaction between kaolin layers, only a few polar molecules can be intercalated directly, such as dimethyl sulfoxide, methanol, potassium acetate, formamide, etc.; Functional guest molecules can only be intercalated between kaolin layers with kaolin-dimethyl sulfoxide as precursors through long-term s...

Claims

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Application Information

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IPC IPC(8): C01B33/44
CPCC01B33/44C01P2002/72C01P2002/82C01P2002/88
Inventor 赵顺平冯小亮朱苗苗郭玉高迎春汪婕徐衡
Owner ANQING NORMAL UNIV
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