Method for preparing kaolin intercalation compound

A technology of intercalation compound and kaolin, which is applied in the direction of silicon compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of easy methanol release, long reaction cycle, unstable kaolin/methanol intercalation complex, etc., to achieve The effect of high intercalation rate and short preparation process time

Inactive Publication Date: 2015-11-25
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Abstract
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Problems solved by technology

[0008] The above method has successfully prepared the imidazolium ionic liquid intercalated kaolin complex, but there are many shortcomings: first, the reaction steps are more complicated, second, the reaction cycle is long, and third, the kaolin / methanol intercalation complex is not very stable. , Methanol is easy to come out in high temperature or high humidity environment. Fourth, it is difficult for the above method to insert the ionic liquid with a high melting point into the kaolin layer.

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  • Method for preparing kaolin intercalation compound
  • Method for preparing kaolin intercalation compound
  • Method for preparing kaolin intercalation compound

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preparation example Construction

[0028] The preparation process of kaolin intercalation compound of the present invention is as follows:

[0029] According to the ratio of monochloroacetic acid to 1-methylimidazole molar ratio of 1:1, put monochloroacetic acid to melt at 70-80°C, add 1-methylimidazole and react for 4-6 hours to obtain a reddish-brown viscous liquid ; Wash with absolute ethanol until the lower layer is a white solid and the upper layer is a colorless transparent liquid, the white solid is taken out and dried to obtain an ionic liquid 1-carboxymethyl-3-methylimidazolium chloride salt; set aside.

[0030] Mix kaolin: dimethyl sulfoxide: distilled water according to 15g: 60-80mL: 5-15mL, heat and stir at 25-75°C for 48-72 hours; centrifuge, wash and dry to obtain kaolin / dimethyl sulfoxide-based intercalation complex; the interlayer distance d(001) increases from 0.72nm to 1.12nm, and the intercalation rate is about 92%. It is ready for use.

[0031] The X-ray powder crystal diffraction pattern o...

Embodiment 1

[0033] Weigh 0.5 g of the spare kaolin / dimethyl sulfoxide intercalation complex and mix with 1 g of 1-carboxymethyl-3-methylimidazolium chloride salt, grind and mix with a mortar.

[0034] The ground mixture was placed in an autoclave, protected by nitrogen gas, and heated in a 210°C drying oven for 4 hours.

[0035] The reaction product was washed repeatedly with dimethyl sulfoxide to remove the residue of 1-carboxymethyl-3-methylimidazolium chloride salt, and then washed with absolute ethanol for 3-4 times and centrifuged.

[0036] The obtained reaction product was dried in a vacuum oven at 80°C.

[0037] The X-ray powder crystal diffraction pattern of kaolin / 1-carboxymethyl-3 methylimidazolium chloride salt intercalation complex in the present embodiment is as follows image 3 , it can be seen from the figure that the interlayer spacing of kaolin increases from 0.71nm to 1.36nm, and the diffraction peak intensity of the intercalation complex is relatively strong, indicatin...

Embodiment 2

[0039] Weigh 0.5 g of the spare kaolin / dimethyl sulfoxide intercalation complex and mix with 1.5 g of 1-carboxymethyl-3-methylimidazolium chloride salt, grind and mix with a mortar.

[0040] The ground mixture was placed in an autoclave, protected by nitrogen gas, and heated in a 210°C drying oven for 4 hours.

[0041] The reaction product was washed repeatedly with dimethyl sulfoxide to remove the residue of 1-carboxymethyl-3-methylimidazolium chloride salt, and then washed with absolute ethanol for 3-4 times and centrifuged.

[0042] The obtained reaction product was dried in a vacuum oven at 80°C.

[0043]The X-ray powder crystal diffraction pattern of the present embodiment kaolin / 1-carboxymethyl-3 methylimidazolium chloride salt intercalation complex is as follows Figure 4 , the (001) interlayer spacing is 1.35nm, and the intercalation rate reaches 84.00%.

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Abstract

The invention discloses a method for preparing a kaolin intercalation compound. Kaolin, dimethyl sulfoxide and distilled water are mixed, and are heated and stirred for 48-72 hours at the temperature of 25 DEG C to 75 DEG C; centrifugal separation, washing and drying are carried out to obtain a kaolin / dimethyl sulfoxide intercalation compound; the obtained kaolin / dimethyl sulfoxide intercalation compound and 1-carboxymethyl-3 methylimidazole chlorine salt are mixed and heated in the environment of 190 DEG C to 210 DEG C under inert gas shielding, and cooling is carried out after heat preservation is carried out for 4-12 h; 1-carboxymethyl-3 methylimidazole chlorine salt is removed through washing of dimethyl sulfoxide, then washing is carried out through absolute ethyl alcohol, centrifugal separation and drying are carried out, and the kaolin / 1- carboxymethyl-3 methylimidazole chlorine salt intercalation compound is obtained. According to the method, imidazole ionic liquid can enter an interlayer of the kaolin in an intercalation mode only through a two-step method, and therefore the preparation process is short in time and high in intercalation efficiency.

Description

technical field [0001] The invention relates to the field of deep processing of kaolin materials, in particular to a preparation method of a kaolin intercalation compound. Background technique [0002] Kaolin is a common clay mineral, which is widely used in papermaking, coating, ceramics, building materials, refractory materials, petrochemical industry, agriculture, cutting-edge defense technology and other fields. The main component of kaolin in nature is kaolinite, which is a typical layered silicate mineral, and the interlayer distance d(001) is about 0.72nm. As a 1:1 layered clay mineral, kaolin is widely used in organic-inorganic composite materials. In recent years, the research on kaolin intercalation has been more active. The intercalation of kaolin with organic matter can significantly increase the interlayer spacing of kaolin, and make kaolin composite materials have the physical and chemical properties of kaolin and organic matter. Therefore, it is widely used i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/44
Inventor 朱小燕朱志超雷新荣严春杰陈洁渝吴红丹曾萍
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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