Preparation method of kaolin-amine grafted complex

Abstract

The invention discloses a preparation method of kaolin-amine grafted complex. The preparation method comprises the following synthesis steps of: selecting 200-325 meshes of kaolin, and purifying to remove impurities; mixing the kaolin and an intercalator with a prepared intercalator solution in a mass ratio of 1:2, and directly intercalating the kaolin under a liquid condition, wherein the intercalator is selected from one or more of hydrazine hydrate, formamide, acetamide, methyl formamide, acrylamide, potassium acetate, dimethyl sulfoxide, urea and potassium chloride; repeatedly leaching the directly intercalated kaolin for ten times by liquid alcohol to prepare a kaolin-alcohol composite, wherein each leaching lasts for 10-48 hours; adding the kaolin-alcohol grated body into an amine solution under a wet condition and magnetically stirring for 40 times; and centrifuging to obtain precipitates, drying the precipitates to separate out excessive amine to obtain the kaolin-amine grafted body, wherein the interlayer distance of the kaolin-amine grafted body can be changed with the difference of intercalated amine molecule size to reach nearly 6.0nm. And the complex is of significance to nanometer research of the kaolin.

Description

technical field

[0001] The invention belongs to the field of deep processing of non-metallic mineral materials. In particular, it relates to a method for preparing kaolin organic intercalation compound with relatively large layer spacing. Background technique

[0002] Kaolinite is the first mineral in the world with a common name of origin in China. Kaolinite is mainly composed of kaolinite. It is used in plastics, rubber, cables, refractory materials, coatings, papermaking, cement, paints, inks, Indispensable mineral raw materials for various industries such as ceramics, catalysts, environmental protection, and agriculture. At present, the total output of kaolin in the world is about 40 million tons, and the application of nano-scale kaolin as a high-quality functional filler can significantly improve the application parameters of the product, and will greatly improve the utilization efficiency of kaolin raw ore under the current conditions.

[0003] The deep processing t...

Examples

Embodiment 1

[0025] Get 50g of 325 mesh white soft kaolin, its XRD pattern is shown in the attached figure 1 .Add 100ml of intercalation agent solution according to the mass ratio of 1:2. This solution is prepared from dimethyl sulfoxide and water according to the ratio of 9:1. The slurry was reacted at 60°C for 24 hours, and the precipitate obtained by centrifugation was dried at 60°C for 1 day to obtain a kaolin-dimethylsulfoxide intercalation complex with an intercalation rate of 96%. Its XRD pattern is attached figure 2 . Add 5 g of kaolin-dimethyl sulfoxide complex to 100 ml of methanol, stir magnetically at room temperature for 24 hours, centrifuge to separate the precipitate and add new methanol, repeat this 8 times, and obtain the kaolin-methanol complex, its XRD pattern See attached image 3 . After the kaolin-methanol complex was dried at room temperature, n-hexylamine was added and reacted at room temperature for one day. After centrifugation, the precipitate obtained is t...

Embodiment 2

[0027] Get 50g of 325 mesh white soft kaolin, its XRD pattern is shown in the attached figure 1 .Add 150ml of saturated urea solution, react at 60°C for 24 hours, centrifuge to obtain the precipitate and dry at 60°C for 2 days to obtain a kaolin-urea intercalation complex with an intercalation rate of 80%. Its XRD pattern is attached Figure 5 . Add 4 g of kaolin-urea intercalation complex to 100 ml of methanol, stir magnetically at room temperature for 24 hours, centrifuge to separate the precipitate and add new methanol, repeat this 8 times, and obtain the kaolin-methanol complex. See the attached XRD pattern. Figure 6. After the kaolin-methanol complex was dried at room temperature, 40 ml of n-hexylamine was added and reacted at room temperature for one day. Centrifuge, get the precipitate and continue to add 50ml dodecylamine, react at 40°C for 30 hours, centrifuge the precipitate and dry it at 40°C, the precipitate will spontaneously precipitate excess amine, that is,...

Embodiment 3

[0029] Take 20g of 325 mesh white soft kaolin, add 150ml of methylformamide solution (the ratio of methylformamide to water is about 8:1), react at room temperature for 30 hours, centrifuge to obtain the precipitate and dry it at 60°C for 2 days to get A kaolin-methylformamide intercalation composite with an intercalation rate of 75%. Add 5 g of kaolin-methylformamide intercalation complex to 100 ml of methanol, stir magnetically at room temperature for 24 hours, centrifuge to separate the precipitate and add new methanol, and repeat this 6 times to obtain kaolin-methanol complex. Dodecylamine was added to the kaolin-methanol complex, and magnetically stirred at 40°C for 24 hours. After centrifugation, the precipitate obtained is the kaolin-laurylamine grafting complex.

technical field

[0001] The invention belongs to the field of deep processing of non-metallic mineral materials. In particular, it relates to a method for preparing kaolin organic intercalation compound with relatively large layer spacing. Background technique

[0002] Kaolinite is the first mineral in the world with a common name of origin in China. Kaolinite is mainly composed of kaolinite. It is used in plastics, rubber, cables, refractory materials, coatings, papermaking, cement, paints, inks, Indispensable mineral raw materials for various industries such as ceramics, catalysts, environmental protection, and agriculture. At present, the total output of kaolin in the world is about 40 million tons, and the application of nano-scale kaolin as a high-quality functional filler can significantly improve the application parameters of the product, and will greatly improve the utilization efficiency of kaolin raw ore under the current conditions.

[0003] The deep processing t...

Examples

Embodiment 1

[0025] Get 50g of 325 mesh white soft kaolin, its XRD pattern is shown in the attached figure 1 .Add 100ml of intercalation agent solution according to the mass ratio of 1:2. This solution is prepared from dimethyl sulfoxide and water according to the ratio of 9:1. The slurry was reacted at 60°C for 24 hours, and the precipitate obtained by centrifugation was dried at 60°C for 1 day to obtain a kaolin-dimethylsulfoxide intercalation complex with an intercalation rate of 96%. Its XRD pattern is attached figure 2 . Add 5 g of kaolin-dimethyl sulfoxide complex to 100 ml of methanol, stir magnetically at room temperature for 24 hours, centrifuge to separate the precipitate and add new methanol, repeat this 8 times, and obtain the kaolin-methanol complex, its XRD pattern See attached image 3 . After the kaolin-methanol complex was dried at room temperature, n-hexylamine was added and reacted at room temperature for one day. After centrifugation, the precipitate obtained is t...

Embodiment 2

[0027] Get 50g of 325 mesh white soft kaolin, its XRD pattern is shown in the attached figure 1 .Add 150ml of saturated urea solution, react at 60°C for 24 hours, centrifuge to obtain the precipitate and dry at 60°C for 2 days to obtain a kaolin-urea intercalation complex with an intercalation rate of 80%. Its XRD pattern is attached Figure 5 . Add 4 g of kaolin-urea intercalation complex to 100 ml of methanol, stir magnetically at room temperature for 24 hours, centrifuge to separate the precipitate and add new methanol, repeat this 8 times, and obtain the kaolin-methanol complex. See the attached XRD pattern. Figure 6. After the kaolin-methanol complex was dried at room temperature, 40 ml of n-hexylamine was added and reacted at room temperature for one day. Centrifuge, get the precipitate and continue to add 50ml dodecylamine, react at 40°C for 30 hours, centrifuge the precipitate and dry it at 40°C, the precipitate will spontaneously precipitate excess amine, that is,...

Embodiment 3

[0029] Take 20g of 325 mesh white soft kaolin, add 150ml of methylformamide solution (the ratio of methylformamide to water is about 8:1), react at room temperature for 30 hours, centrifuge to obtain the precipitate and dry it at 60°C for 2 days to get A kaolin-methylformamide intercalation composite with an intercalation rate of 75%. Add 5 g of kaolin-methylformamide intercalation complex to 100 ml of methanol, stir magnetically at room temperature for 24 hours, centrifuge to separate the precipitate and add new methanol, and repeat this 6 times to obtain kaolin-methanol complex. Dodecylamine was added to the kaolin-methanol complex, and magnetically stirred at 40°C for 24 hours. After centrifugation, the precipitate obtained is the kaolin-laurylamine grafting complex.

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