Preparation method of DNL-1 molecular sieve

A technology of aluminum phosphate molecular sieve and deionized water, which is applied in the field of molecular sieves, can solve the problems of high price of ionic liquids, difficult to achieve purity, and reduced thermal stability, and achieve the effect of commercially available raw materials, simple methods, and easy operation

Active Publication Date: 2019-04-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ionic liquid used in this preparation method, because ionic liquid easily absorbs the moisture in the air, some ionic liquid can react (as bmic) with water after absorbing water, its performance (as wide electrochemical window, thermal conductivity) of the ionic liquid that does not react Stability) will also be greatly reduced due to water absorption, so it can only be tested in an inert gas environment, and its practical application ability is also greatly reduced
And the price of ionic liquid is high and its purity is limited by the preparation process, it is difficult to achieve the ideal value, and once mixed with impurities, it is easy to affect the performance of the prepared material

Method used

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  • Preparation method of DNL-1 molecular sieve
  • Preparation method of DNL-1 molecular sieve
  • Preparation method of DNL-1 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] The pseudo-boehmite (Al 2 O 3 The mass percentage is 77%, aluminum source) and diethylethanolamine (the mass percentage is 99%, R1) are mixed and stirred, and then phosphoric acid (H 3 PO 4 Add 85% by mass, phosphorus source) drop by drop, stir evenly, then add water, hydrofluoric acid (40% by mass HF) and butyltrimethylammonium chloride (R2), stir evenly to make Gel, transfer the gel to the stainless steel reactor. After putting the reactor into the oven, program the temperature to 200°C for dynamic crystallization for 48 hours. After the crystallization is completed, the solid product is centrifuged, washed, and dried in air at 100° C. to obtain the original molecular sieve powder sample. The sample was analyzed by XRD (the results are shown in Table 2), and the XRD diffraction data shows that the sample is DNL-1 molecular sieve; the electron micrograph of the sample is shown in figure 1 .

[0055] The static crystallization in the embodiment is to put the reactor direc...

Embodiment 2-19

[0065] The specific ingredient ratio and crystallization conditions are shown in Table 1, and the specific ingredient process is the same as in Example 1.

[0066] The prepared samples were subjected to XRD analysis, and the data results were close to Table 2, that is, the peak position and shape were the same, and the relative kurtosis of the peak fluctuated within ±10% depending on the preparation conditions, indicating that the prepared product had the characteristics of DNL-1 structure.

experiment example 20

[0068] The sample obtained in Example 1 was baked in air at 550°C for 8 hours, and then subjected to XRD analysis. The results are shown in Table 3. The XRD diffraction patterns of the sample before and after baking are shown in figure 2 . The diffraction pattern shows that the positions and shapes of the diffraction peaks are approximately the same before and after the sample is calcined, indicating that the calcined product has the characteristics of aluminum phosphate molecular sieve DNL-1 structure, and also that the prepared aluminum phosphate molecular sieve DNL-1 sample has good thermal stability.

[0069] Table 3 XRD results

[0070]

[0071]

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Abstract

The invention discloses a preparation method of a DNL-1 molecular sieve. The method comprises the following steps: 1) mixing an aluminum source, a phosphorus source, R1, R2, hydrofluoric acid and deionized water to obtain a primary mixture; 2) crystallizing the obtained primary mixture for 0.5-96 h at the temperature of 150-220 DEG C to obtain an aluminum phosphate molecular sieve, wherein the molar ratio of Al2O3, P2O5, R1, R2, HF and H2O in the primary mixture is 1: 0.5: 1.5: 5-20: 0.1-1.5: 0.1-2: 8-40; R1 is diethylethanol or triethanolamine; and R2 is selected from one or more of butyl trimethyl ammonium chloride, tetramethyl ammonium chloride, diethylamine and choline chloride. The preparation method of the aluminum phosphate molecular sieve DNL-1 is simple, and is simple and convenient to operate and low in cost, raw materials are commercial and easily obtained, and thus, the aluminum phosphate molecular sieve DNL-1 is suitable for being produced industrially.

Description

Technical field [0001] The invention belongs to the field of molecular sieves, and specifically relates to the preparation of aluminum phosphate molecular sieve DNL-1. Background technique [0002] Molecular sieves are widely used in the fields of catalysis, adsorption and ion exchange due to their regular pore structure and unique surface properties. The pore size of molecular sieve is an important characteristic parameter of molecular sieve materials. The pore size of most molecular sieve materials is smaller than It greatly limits their ability to catalyze, adsorb and separate organic macromolecules. Artificial preparation of super-large pore molecular sieves is a way to solve this problem. At present, the super-large pore molecular sieves that have been successfully prepared include VPI-5, AlPO 4 -8. Gallium phosphate molecular sieve Cloverite and several silicon-based molecular sieves, etc. [0003] -CLO structure is an ultra-large microporous structure with a 20-membered ri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/04
CPCC01B37/04C01B39/54C01P2002/72C01P2004/03C01P2006/12C01P2006/14
Inventor 孙丽婧田鹏刘中民杨淼刘琳
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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