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Preparation method for rapidly synthesizing DD3R molecular sieve

A molecular sieve and mother liquor synthesis technology, applied in the chemical industry, can solve the problems of difficulty in DD3R synthesis, long synthesis time, low product yield, etc., and achieve the effects of controllable morphology, short synthesis time and uniform particle size

Active Publication Date: 2015-12-09
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the defects of the prior art and provide a preparation method for rapidly synthesizing DD3R molecular sieves, which overcomes the difficulty in synthesizing DD3R in the prior art, the synthesis time is long, the cost is expensive, the process is cumbersome, the product yield is low and the repeatability is poor Defects

Method used

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  • Preparation method for rapidly synthesizing DD3R molecular sieve
  • Preparation method for rapidly synthesizing DD3R molecular sieve
  • Preparation method for rapidly synthesizing DD3R molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1220

[0071] Example 1 Preparation of all-silicon DD3R molecular sieve by reacting at 220°C for 6 hours

[0072] Mix 5.24 grams of ethylenediamine, 1.65 grams of amantadine and 39.24 grams of water and stir for 0.5 hours, add 3.88 grams of ammonium fluorosilicate, stir for 1 hour, and put it in an oven at 220 ° C for 6 hours to react, SiO 2 :H 2 O: amantadine (Adam): ethylenediamine (EDA) = 1:100:0.5:4, after filtering and washing, DD3R molecular sieves were obtained.

[0073] figure 1 Scanning electron micrographs of DD3R molecular sieves prepared for this method. It can be seen from the figure that the DD3R molecular sieve grains are hexagonal, uniform in size, and the diagonal particle size is about 50 microns. The crystallinity is good, and the yield is calculated based on the equivalent molar number of silicon dioxide converted from the ammonium fluorosilicate added to the molecular sieve synthesis mother liquor, which can reach 50%.

[0074] figure 2 The XRD spectrum of ...

Embodiment 2220

[0075] Example 2 Preparation of all-silicon DD3R molecular sieve by reacting at 220°C for 12 hours

[0076] The difference from Example 1 is that it was placed in an oven at 220° C. for 12 hours to react. All the other steps are the same as in Example 1.

[0077] image 3 Scanning electron micrographs of DD3R molecular sieves prepared for this method. It can be seen from the figure that the particle size of DD3R molecular sieve is uniform, and the diagonal particle size of the hexagon is about 150 μm. At the same time, the crystallinity is good. Compared with the 6-hour reaction, the crystallinity is greatly improved, and the particle size increases from 50 microns to 150 microns. The yield is calculated on the basis of the equivalent moles of silicon dioxide added to the ammonium fluorosilicate synthesis mother liquor, which is close to 100%.

[0078] Figure 4 The XRD spectrum of the DD3R molecular sieve prepared by this method is consistent with the standard spectrum. ...

Embodiment 3

[0079] Example 3 Adding 0.1wt% seed crystals and reacting at 220°C for 12 hours to prepare all-silicon DD3R molecular sieves

[0080] The difference from Example 1 is that after adding 3.88 g of ammonium fluorosilicate and stirring for 1 hour, 50 mg of DD3R molecular sieve seed crystals were added, stirred for 5 minutes, and then placed in an oven at 220° C. for 12 hours. All the other steps are the same as in Example 1.

[0081] Figure 5 Scanning electron micrographs of DD3R molecular sieves prepared for this method. It can be seen from the figure that the DD3R molecular sieve crystal has a hexagonal shape, and the hexagonal diagonal particle size is about 6-15 microns. Compared with Example 2, the crystallinity is equivalent, and the crystal grain size is greatly reduced. The yield is calculated on the basis of the equivalent moles of silicon dioxide added to the ammonium fluorosilicate synthesis mother liquor, which is close to 100%.

[0082] Image 6 The XRD spectrum...

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Abstract

The invention provides a preparation method for rapidly synthesizing DD3R molecular sieve. The method comprises the following steps: 1, mixing a silicon source, adamantanamine, water and ethylene diamine to obtain a molecular sieve synthesis mother liquor, or mixing the silicon source, adamantanamine, an aluminum source, water and ethylene diamine to obtain the molecular sieve synthesis mother liquor, wherein the silicon source contains ammonium fluorosilicate; and 2, heating and reacting the molecular sieve synthesis mother liquor, filtering, and washing to obtain the DD3R molecular sieve. The preparation method adopts the silicon source containing ammonium fluorosilicate to synthesize the DD3R molecular sieve, so the preparation method has the advantages of simple and convenient operation, short synthesis time, uniform DD3R particles, controllable particle size of 4-150[mu]m, and controllable morphology. The preparation method allows the DD3R molecular sieve with good crystallization property and uniform granularity to be rapidly synthesized without adding crystal seeds.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method for rapidly synthesizing DD3R molecular sieves. Background technique [0002] Molecular sieves have uniform molecular-scale pores and are widely used in the fields of catalysis, adsorption and separation. DD3R molecular sieve (the structure code of the International Molecular Sieve Association is DDR) is a small-pore pure silicon molecular sieve with a three-dimensional pore structure. The pore size is 0.36×0.44nm, which is close to the dynamic diameter of a large number of common small molecular gases. Therefore, according to the molecular sieving effect, DD3R for the separation of small molecule mixtures, such as CO 2 -CH 4 , O 2 -N 2 , propylene-propane, water-alcohol, etc., have extremely high selectivity (Journal of Membrane Science 316 (2008) 35–45). At the same time, because DD3R molecular sieve has an all-Si skeleton structure, it has extremely h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/02
Inventor 张延风刘琛李猛林艳君白璐曾高峰孙予罕魏伟黄巍孙志强章清
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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