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Method for direct hydrothermal synthesis of chabasite with intermediate silica-alumina ratio

A technology for hydrothermal synthesis and aluminosilicate zeolite, which is applied in the directions of crystalline aluminosilicate zeolite, chemical instruments and methods, molecular sieve catalysts, etc. handy effect

Active Publication Date: 2016-11-23
北方稀土华凯高科技河北有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Although the synthesis of the above-mentioned K-G, D and R-type molecular sieves does not use an organic template, it is carried out in a highly alkaline hydrogel system, and its crystallization process is controlled by kinetics. The chemical composition, volume, stirring rate and other parameters of the raw materials And related factors such as mass transfer and heat transfer are very sensitive, and it is difficult to scale up production

Method used

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  • Method for direct hydrothermal synthesis of chabasite with intermediate silica-alumina ratio
  • Method for direct hydrothermal synthesis of chabasite with intermediate silica-alumina ratio
  • Method for direct hydrothermal synthesis of chabasite with intermediate silica-alumina ratio

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Embodiment 1

[0028] 8.0 grams of sodium hydroxide, 13.2 grams of potassium hydroxide (85%) and 150 grams of deionized water were prepared into a solution, and 6.2 grams of ammonium oxalate was added and stirred to dissolve. Put in 2.7 grams of aluminum powder to dissolve. After the solution temperature is down to room temperature, add 24.0 grams of white carbon black, stir to obtain hydrogel, the molar ratio of the material for synthesizing hydrogel is 0.5AOxa (ammonium oxalate): 2.0Na 2 O:2.0K 2 O: Al 2 o 3 :8SiO2 2 : 150H 2 O. It was left to stand at room temperature for 2 hours, then transferred to a Teflon-lined stainless steel sealed kettle, heated to 110°C, and left to stand for 2 days. Then cool to room temperature, open the sealed kettle, pour off the supernatant, recover the white solid, and wash it three times with clear water. The resulting white powder was dried at 80°C.

[0029] attached Picture 1-1 It is the powder X-ray diffraction pattern of the product obtained i...

Embodiment 2

[0032] Dissolve 4.0 grams of sodium hydroxide and 19.7 grams of 85% potassium hydroxide in 45.0 grams of deionized water, add 4.6 grams of ammonium acetate, and add 6.66 grams of aluminum sulfate octadecahydrate to dissolve. Then slowly add 60.0 grams of 40% silica sol while stirring, stir to obtain hydrogel, the molar ratio of the material for synthesizing hydrogel is 6.0AAc (ammonium acetate): 10.0Na 2 O:30.0K 2 O: Al 2 o 3 :80SiO2 2 : 800H 2 O. After standing at room temperature for 12 hours, the aged mixture was sealed in a Teflon-lined stainless steel kettle, heated to 150 °C, and allowed to stand for 5 days. Cool to room temperature, open the sealed kettle, pour off the supernatant, recover the white solid, and wash with water three times. The resulting white powder was dried at 80°C.

[0033] attached Figure 1-2 It is the powder X-ray diffraction pattern of the product obtained in this embodiment, and it can be known that the product is a zeolite molecular siev...

Embodiment 3

[0035]Dissolve 2.65 grams of potassium hydroxide in 12.0 grams of deionized water, add 0.8 grams of ammonium bicarbonate, and add 0.82 grams of sodium metaaluminate to dissolve. Slowly add 7.5 grams of 40% silica sol under stirring, stir to obtain hydrogel, the molar ratio of the material for synthesizing hydrogel is 2.0AHC (ammonium bicarbonate): 1.0Na 2 O:4.0K 2 O: Al 2 o 3 :10SiO2 2 :190H 2 O. After the mixture was stirred evenly, without aging, it was directly transferred to a stainless steel kettle with a Teflon liner, heated to 100 degrees Celsius, allowed to stand for 3 days, then cooled to room temperature, the sealed kettle was opened, and the supernatant liquid was poured out. The white solid was recovered and washed three times with water. The resulting white powder was dried at 80°C.

[0036] attached Figure 1-3 It is the powder X-ray diffraction pattern of the product obtained in this embodiment, and it can be known that the product is a zeolite molecular...

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Abstract

The invention provides a method for direct hydrothermal synthesis of chabasite with an intermediate silica-alumina ratio. The method is characterized by comprising the steps that in a reaction for synthesizing the chabasite under the hydrothermal condition, no organic template is added, no chabasite seed crystal is added, alkalescent inorganic salt is added, and an aluminosilicate zeolite molecular sieve with a chabasite structure is obtained; reacting matter for preparing hydrogel is prepared from, by molar ratio, 1-20 parts of Na2O, 2-30 parts of K2O, 0.05-8.0 parts of alkalescent inorganic salt, 1 part of Al2O3, 8-80 parts of SiO2 and 150-800 parts of H2O. According to the method, the zeolite molecular sieve with the chabasite structure can be synthesized stably without using template or fluorochemicals or seed crystals.

Description

technical field [0001] The invention belongs to the field of preparation of zeolite molecular sieves, in particular to a method for synthesizing zeolite molecular sieves with a chabazite structure. Background technique [0002] Chabazite has a CHA crystal structure and belongs to the trigonal crystal system. The unit cell parameters are: a=13.7 angstroms, c=14.8 angstroms. In the structure, aluminum-oxygen tetrahedrons and silicon-oxygen tetrahedrons are strictly alternately connected, and the skeleton is staggered by double six-membered rings. A cage structure is formed, and the pore diameter of the eight-membered ring channel in the a and b directions is 3.8 angstroms×3.8 angstroms. Chabazite with a low silicon-aluminum ratio can be used as a gas adsorbent, and has adsorption properties for nitrogen, oxygen, and argon. The SSZ-13 and synthetic chabazite with medium and high silicon-aluminum ratio can be used as the raw material of the catalyst, and can be used as the acti...

Claims

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Application Information

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IPC IPC(8): C01B39/02B01J29/70
CPCB01J29/7015C01B39/02C01P2002/72C01P2002/88
Inventor 杨晓波赵向云肖剑鸣
Owner 北方稀土华凯高科技河北有限公司
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