Nanometer A type molecular sieve preparation method

A molecular sieve and nanotechnology, applied in the field of preparation of A-type molecular sieves, can solve problems such as expensive equipment, harsh reaction conditions, and difficult industrialization, and achieve significant economic benefits, excellent performance, and low cost

Inactive Publication Date: 2004-11-10
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional hydrothermal synthesis method can usually only obtain micron and submicron A-type molecular sieves, such as A-type molecular sieves with a particle size of 500nm, but cannot obtain molecular sieves with a particle size of 0.1-100nm
[0005] Zhou Zhou, Pan Weixiong, etc. in the article "Synthesis of Nano-4A Molecular Sieves" published in "Natural Gas Chemical Industry" on June 4, 2001, involved the synthesis method of nano-4A molecular sieves. The method uses ethyl silicate as the silicon source, isopropyl Aluminum alkoxide is the aluminum source, and the superfine oxide powder is prepared by the sol-gel supercritical drying method, and an appropriate amount of NaoH solution is added to synthesize nano-4A molecular sieves in an autoclave. The reaction synthesis method is complicated, the required equipment is expensive, and the reaction conditions are harsh. , the industrialization is difficult; the reaction time is long, the energy consumption is large, and the cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A kind of preparation method of nano-type A molecular sieve, select silicon: the silicon source and aluminum source that aluminum molar ratio is 2: 1, and add 5mol / L by the ratio of total solid weight of silicon source aluminum source: NaoH solution=1:8 The NaoH solution comprises the following steps: silicon source, aluminum source plus NaoH solution, combined with ultrasonic and microwave treatment for 100 minutes, controlled temperature at 98°C for crystallization, cooling and filtering, washing to PH=7-10, washing process The NaoH mother liquor is recovered and returned to the original process for reuse.

[0032] The nano-type A molecular sieve is obtained after post-treatment.

[0033] In the process of combined ultrasonic and microwave processing, the ultrasonic technical parameters are frequency 50KHz, power 1000 watts; microwave technical parameters frequency is 2000MHz, power 1000 watts.

[0034] The silicon source and the aluminum source are specifically sele...

Embodiment 2

[0038] A kind of preparation method of nano-type A molecular sieve, select the silicon source and the aluminum source that silicon: aluminum molar ratio is 2: 1, and add 10mol / L by the ratio of total solid weight of silicon source aluminum source: NaoH solution=1:8 The NaoH solution comprises the following steps: silicon source, aluminum source plus NaoH solution, combined ultrasonic and microwave treatment for 100 minutes, controlled temperature at 98°C for crystallization, cooling, filtering, washing to PH=7-10, washing process The NaoH mother liquor in the process is recovered and returned to the original process for reuse.

[0039] All the other are with embodiment 1. It is proved to be a 4A product by infrared spectrum detection and x-ray diffraction crystal phase analysis, and only a 4A product with a particle size of 140nm can be obtained. The high concentration of NaoH solution is not conducive to the formation of small particle nanometer 4A products.

Embodiment 3

[0041]A preparation method of nano-type A molecular sieves is obtained by selecting kaolin produced in Jingdezhen, Jiangxi Province with a silicon:aluminum molar ratio of 2:1, crushing and calcining at 800° C. for 5 hours. Silicon source, aluminum source and NaoH solution are combined with ultrasonic and microwave pretreatment, the time of combined pretreatment is 80 minutes, and the temperature is controlled at 60°C; ultrasonic technical parameters are frequency 60KHz, power 1500 watts; microwave technical parameter frequency is 1000MHz , power 400 watts.

[0042] After ultrasonic and microwave combined pretreatment, the crystallization temperature does not need to be too high, and the nano-type A molecular sieve can be obtained at 90°C. All the other are with embodiment 1.

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PUM

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Abstract

The invention relates to a process for preparing nano A type molecular sieve, including 3A, 4A and 5A molecular sieves, wherein silicon source and aluminum source are selected according the mol ratio of silicon : aluminum = 2:1, and 3-7 mol/L NaOH solution is added by the proportion of total solid weight of silicon and aluminum source : NaOH = 1:5-12, the process comprises the steps of, adding NaOH solution into silicon and aluminum sources, carrying out ultrasonic and microwave combination treatment for 10-150 minutes, controlling the temperature between 90-100 deg. C, filtering, scouring till pH=7-10, post-treating to obtain the nano A type amolecular sieve.

Description

technical field [0001] The invention relates to a preparation method of A-type molecular sieve, in particular to a preparation method of nanometer A-type molecular sieve. Background technique [0002] Ordinary 4A zeolite molecular sieve has good surface adsorption capacity, its calcium exchange capacity is 5 times that of sodium tripolyphosphate (STPP), and it has anti-redeposition properties, which can provide a deposition surface for oils and dyes, and can avoid stains on fabrics Redeposition also has good thermal stability and dispersion performance, does not pollute the environment, is non-toxic and non-irritating to the human body. It is the preferred agent to replace STPP as hard water softener in synthetic detergents. Using 4A zeolite molecular sieves as detergent additives is an effective method for countries to produce low-phosphorus or phosphorus-free washing powder to solve environmental pollution problems such as excessive phosphorous in detergent wastewater and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/14
Inventor 钟起玲章磊
Owner JIANGXI NORMAL UNIV
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