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Preparation method of kaolin nanotubes

A technology of kaolin nanotubes and kaolin, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of cumbersome and complicated processes, low economic benefits, cumbersome processes, etc., and achieve simple and efficient processes , large economic value, and the effect of uniform pipe diameter distribution

Inactive Publication Date: 2019-08-23
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation technology of kaolin nanotubes mostly adopts the process of intercalation-exfoliation for multi-step operation. For example, Chinese patent CN102602951A reports a preparation method of kaolin nanotubes. After mixing, heating and mechanical stirring for 20-30 hours, mix with methanol and react with mechanical stirring at room temperature for 48-72 hours, then mix with methanol solution of quaternary ammonium salt surfactant, and react with mechanical stirring for 10-30 hours at room temperature , and finally calcined at high temperature for 4-6 hours, plus the washing and drying of each step, it took nearly a week
This method is not only relatively cumbersome, but also takes a long time, consumes a lot of energy, and has low economic benefits.
Another example is the preparation method of kaolin nanotubes reported by Chinese patent CN104386702A. In the preparation process, the method needs to repeatedly heat up, keep warm, and cool down. The reagents used include urea, triethanolamine, methyl iodide ethanol solution, sodium cetylsulfonate aqueous solution, etc. , where multiple high-temperature treatment parts need to be heated to 90-170°C, the process is also cumbersome and complicated, and the energy consumption is large

Method used

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  • Preparation method of kaolin nanotubes
  • Preparation method of kaolin nanotubes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation method of this kaolin nanotube is as follows:

[0015] A. Select ordinary flaky kaolin as raw material, add 10g of kaolin into the intercalation agent N-methylformamide, prepare a slurry containing 1g of kaolin per milliliter of intercalation agent, and put it into a ball mill (Nanjing Boyuntong Instrument Technology Co., Ltd. , model: GB-80, the same below) in the ball mill for 1min, and dried to obtain powder.

[0016] B. Get 5g of the powder obtained in step A and mix it with 50mL of methanol, put it into a ball mill and mill it for 30min, and centrifuge to remove the solvent to obtain the kaolin grafted with methoxy on the surface;

[0017] C. Add 0.5 g of methoxy-grafted kaolin to 20 ml of methanol solution with a concentration of 1 mol / L cetyltrimethylammonium chloride, put it into a ball mill and mill it for 8 hours, and then wash it with ethanol into the washing liquid Add water until there is no foam, then dry, and heat up to 600°C for 5 hours ...

Embodiment 2

[0020] The preparation method of this kaolin nanotube is as follows:

[0021] A. Choose ordinary flaky kaolin as raw material, add 10g of kaolin to the intercalation agent pyridine, prepare a slurry containing 0.5g of kaolin per milliliter of intercalation agent, put it into a ball mill and mill for 10 minutes, and dry to obtain a powder. Ball mill manufacturer: Nanjing Boyuntong Instrument Technology Co., Ltd., model: GB-80;

[0022] B. Mix 5 g of the powder obtained in step A with 10 mL of ethanol, put it into a ball mill and mill it for 2 hours, and centrifuge to remove the solvent to obtain surface ethoxy grafted kaolin;

[0023] C. Add 1g of ethoxy-grafted kaolin to 20ml of methanol solution with a concentration of 1.2mol / L cetyltrimethylammonium bromide, put it into a ball mill and mill it for 24h, and then wash it with ethanol into the washing liquid Add water until there is no foam, then dry, and heat up to 600°C for 4 hours at a constant temperature at a heating rate...

Embodiment 3

[0026] The preparation method of this kaolin nanotube is as follows:

[0027] A. Choose ordinary flaky kaolin as raw material, add 10g of kaolin to the intercalation agent dimethyl sulfoxide, prepare a slurry containing 0.7g of kaolin per milliliter of intercalation agent, put it into a ball mill and mill for 1 hour, and dry to obtain a powder. Ball mill manufacturer: Nanjing Boyuntong Instrument Technology Co., Ltd., model: GB-80;

[0028] B. Get 5g of the powder obtained in step A and mix it with 20mL of methanol, put it into a ball mill and mill it for 10h, and centrifuge to remove the solvent to obtain surface methoxy grafted kaolin;

[0029] C. Add 0.5 g of methoxy-grafted kaolin to 20 ml of methanol solution with a concentration of 1.5 mol / L cetyltrimethylammonium chloride, put it into a ball mill and mill it for 18 hours, and then wash it with ethanol to the washing liquid Add water until there is no foam, then dry, heat up to 500°C at a constant temperature for 5 hour...

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Abstract

The invention discloses a preparation method of kaolin nanotubes. The preparation method comprises the following steps: flaky kaolin and an intercalating agent (such as N-methylformamide) are mixed, then are ball-milled in a high-energy ball mill for 1 min to 24 h, and are dried; the obtained mixture and a solvent (such as methanol) are mixed, and then are ball-milled in the high-energy ball millfor 1 min to 24 h to carry out a surface grafting reaction; the obtained reaction product and a structure inducing agent (such as a quaternary ammonium salt surfactant) are mixed, and are ball-milledin the high-energy ball mill for 1 min to 24 h; and finally the obtained mixture is dried and calcined to obtain the kaolin nanotubes. The preparation method converts kaolin with a flaky crystal structure into kaolin with a tubular crystal structure in a short time and a high efficiency, breaks the bottleneck restricting a processing and preparation technology of a kaolin-based catalyst carrier material, and achieves the purposes of high efficiency and low energy consumption.

Description

technical field [0001] The invention relates to a preparation method of kaolin nanotubes. Background technique [0002] Kaolin is a general term for clay or rock mainly composed of kaolinite minerals. It is widely distributed in my country and has large reserves. It is currently widely used in ceramic industry, refractory material industry, chemical industry, light industry, and in aerospace industry. It also shows its unique effect. An important application of kaolin in the chemical industry is as a catalyst support material. Domestic refineries generally use fluid catalytic cracking (FCC) process to process heavy oil to produce gasoline, diesel and low-carbon olefins. The key technology is the catalyst, and the kaolin-based carrier is crucial to the performance of the catalytic cracking catalyst. The microstructure (pores, micromorphology, etc.), particle size distribution, and surface acidity of kaolin all have important effects on the performance of catalytic materials....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/44B82Y30/00B82Y40/00
CPCC01B33/44B82Y30/00B82Y40/00C01P2004/64C01P2004/13C01P2006/12
Inventor 郭学锋郭佳冯杰张豫李慕鸿陈善勇郝盼盼毕菲菲陈庆亮严咏丁维平
Owner NANJING UNIV
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