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Nano-scale ultra-fine analcime preparation method

Analcime and nano-scale technology, applied in the field of molecular sieve synthesis, can solve the problems of large alkali consumption, large particle size, serious pollution, etc., and achieve the effect of low cost

Active Publication Date: 2017-05-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The analcite crystal grains obtained by this method can reach nanoscale, but the particle size is still relatively large, and when fly ash is used as raw material, the pretreatment process needs to consume a large amount of alkali, the corrosion and pollution are serious, and the entire preparation process is also relatively cumbersome.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0035] At room temperature, mix water, sodium hydroxide, silica sol, and N-methylpyrrolidine according to a certain ratio, then heat in sealed water at 90°C for 24 hours, cool to room temperature, and then add the spare sodium metaaluminate powder to the above solution in, and stir well. The final material ratio satisfies: Al 2 o 3 / SiO 2 =30, N-Methylpyrrolidine / SiO 2 =0.15,OH - / SiO 2 =0.75,H 2 O / SiO 2 =40. Afterwards, the above mixture was ultrasonically (1.0 KW / L) and magnetically stirred at 40°C for 3 hours, and then placed in a reaction kettle for crystallization at 175°C for 120 hours. The obtained product was washed with distilled water, dried at 120°C, and then calcined at 550°C for 5 hours. It is confirmed to be analcime by XRD detection, observed by scanning electron microscope, it is spherical shape, the grain size is about 30nm, belongs to the nanoscale range, and the specific surface area is 270m 2 / g.

Embodiment 2

[0037] At room temperature, mix water, sodium hydroxide, silica sol, and N-methylpyrrolidine according to a certain ratio, then heat in airtight water at 100°C for 24 hours, cool to room temperature, and then add the spare sodium metaaluminate powder to the above solution in, and stir well. The final material ratio satisfies: Al 2 o 3 / SiO 2 =40, N-Methylpyrrolidine / SiO 2 =0.20,OH - / SiO 2 =0.8,H 2 O / SiO 2 =60. Afterwards, the above mixture was ultrasonically stirred (0.5 KW / L) at 60°C for 3 hours, and then placed in a reaction kettle for crystallization at 180°C for 140 hours. The obtained product was washed with distilled water, dried at 120°C, and then calcined at 550°C for 5 hours. The product was confirmed to be analcime by XRD detection, observed by scanning electron microscope, it was spherical shape, the grain size was about 35nm, belonging to the nanoscale range, and the specific surface area was 212m 2 / g.

Embodiment 3

[0039]At room temperature, mix water, sodium hydroxide, silica sol, and N-methylpyrrolidine according to a certain ratio, then heat in sealed water at 120°C for 6 hours, cool to room temperature, and then add aluminum isopropoxide powder to the above solution, and stir well. The final material ratio satisfies: Al 2 o 3 / SiO 2 =60, N-Methylpyrrolidine / SiO 2 =0.25,OH - / SiO 2 =0.9,H 2 O / SiO 2 =80. Afterwards, the above mixture was ultrasonically (2.0 KW / L) and magnetically stirred at 50°C for 3 hours, and then placed in a reactor for crystallization at 180°C for 140 hours. The obtained product was washed with distilled water, dried at 120°C, and then calcined at 550°C for 5 hours. The product was confirmed to be analcime by XRD detection, observed by scanning electron microscope, it was in spherical shape, the grain size was about 18nm, it belonged to ultra-fine nanometer range, and the specific surface area was 380m 2 / g.

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Abstract

The present invention discloses a nano-scale ultra-fine analcime preparation method, wherein an alkali source, a silicon source, an aluminum source, water and N-methylpyrrolidine are adopted as reaction raw materials and crystallization is performed for 5-200 h under autogenous pressure and 140-200 DEG C hydrothermal condition to obtain the small grain nanometer analcime. According to the present invention, the obtained nano-scale ultra-fine analcime has characteristics of simple process, pure crystal phase, high crystallinity, large specific surface, low cost and the like, and has wide application prospects in ion adsorption and purification.

Description

technical field [0001] The invention relates to a preparation method of nano-scale ultrafine analcime, which belongs to the technical field of molecular sieve synthesis. Background technique [0002] Analcime has a unique internal structure and crystal chemical properties, and has special properties in catalysis, adsorption, ion exchange, etc. As one of the zeolite minerals, analcime has a very broad field of development and utilization, and has a large potential market value. However, the natural analcite mineral has the disadvantages of high impurity content, difficult purification, and large crystal grains. The artificially synthesized analcite perfect crystal is more universal and controllable. [0003] (Journal of the American Chemical Society 2007, 129, 13305-13312) reported the preparation of cubic tetragonal trioctahedral analcite crystals by hydrothermal method. In the preparation process of this method, a surfactant needs to be added, the raw materials are expens...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02B82Y30/00
Inventor 杨卫亚凌凤香王少军沈智奇季洪海王丽华郭长友
Owner CHINA PETROLEUM & CHEM CORP
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