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Core-shell type molecular sieve microsphere as well as preparation method and application thereof

A technology of molecular sieve and core-shell type, which is applied in the field of core-shell type molecular sieve microsphere materials and its preparation, can solve the problems of increasing product production cycle, increasing preparation cost, complicated process, etc., and achieves low cost, high selective adsorption capacity, and preparation The effect of simple method

Inactive Publication Date: 2015-04-08
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the above method prepares a binder-free zeolite material, the steps are cumbersome and the process is complicated, which increases the production cycle of the product and increases the preparation cost

Method used

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  • Core-shell type molecular sieve microsphere as well as preparation method and application thereof
  • Core-shell type molecular sieve microsphere as well as preparation method and application thereof
  • Core-shell type molecular sieve microsphere as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Add 8.3g of 30% silica sol to 28.57g of deionized water, then add 1.0g of chitosan, and add 1.6g of 36% acetic acid drop by drop to the above solution under stirring, and stir evenly , forming a viscous chitosan silica solution, the molar ratio of the silicon solution is 0.0004CS:0.3HAc:1.4SiO 2 :54H 2 O. Add 5.68g of sodium hydroxide to 83.8g of deionized water. After fully dissolving, add 2.24g of sodium aluminate and stir until clear to form an aluminum solution. The molar ratio of the aluminum solution is 3Na 2 O:2Al 2 o 3 :34H 2 O. The silicon solution was added dropwise to the aluminum solution at a mass ratio of 0.9:1 to form dispersed gel beads. After the dropwise addition, immerse the balls and aluminum solution at room temperature for 8 hours, then heat the balls together with the aluminum solution in an oven at 70°C for 12 hours, wash the obtained microspheres to pH = 7, and then dry them at 60°C for 7 hours , to obtain NaA / NaX / chitosan composite micro...

Embodiment 2

[0033] Add 10.9g of 30% silica sol to 35.3g of deionized water, then add 2.0g of chitosan, and add 1.82g of 36% acetic acid drop by drop to the above solution under stirring, and stir evenly , the molar ratio of silicon solution is 0.0008CS:0.5HAc:2.5SiO 2 :90H 2 O. Add 6.05g of sodium hydroxide to 40.8g of deionized water. After fully dissolving, add 18.6g of sodium aluminate and stir until clear to form an aluminum solution. The molar ratio of the aluminum solution is 5Na 2 O:3Al 2 o 3 :60H 2 O. The silicon solution was added dropwise to the aluminum solution at a mass ratio of 0.8:1 to form gel beads. After the dropwise addition, the balls and the aluminum solution were immersed for 23 hours at room temperature, and then the balls and the aluminum solution were placed in an oven at 100° C. for 4 hours under hydrothermal heating, and the obtained microspheres were fully washed to pH=8. The microspheres were dried at 80° C. for 4 hours to obtain NaA / NaX / chitosan compos...

Embodiment 3

[0035] According to the same long-film synthesis solution preparation method and long-film method as in Example 1, sample Q2 was added to the long-film synthesis solution at a mass ratio of 1:20, crystallized at 100°C for 5h, and carried out two secondary membrane. The obtained core-shell molecular sieve microspheres are denoted as Q4, and the electron microscope image of sample Q4 is shown in Figure 4 As shown, the shell thickness is 3.8 μm, and the surface intergrowth is better than that of sample Q2. The XRD pattern of sample Q3 is as follows Figure 10 As shown, there are A-type and X-type characteristic peaks, and the X-type peak intensity is higher than that of A.

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Abstract

The invention relates to a core-shell type molecular sieve microsphere as well as a preparation method and application thereof. The core-shell type molecular sieve microsphere is characterized by having the structure that an A type molecular sieve serves as a shell, and an A-X type molecular sieve serve as a core. The preparation method of the core-shell type molecular sieve microsphere comprises the following steps of: preparing a NaA-NaX type molecular sieve composite microsphere in advance, then growing a layer of NaA type molecular sieve film on the surface of the NaA-NaX type molecular sieve composite microsphere to form a Na-ion type core-shell molecular sieve microsphere, and exchanging ions by using a K ion solution and a Ca ion solution to form a K-Ca type core-shell molecular sieve microsphere. The core-shell type molecular sieve microsphere prepared by adopting the preparation method contains no binder, has high mechanical strength and is suitable for separating a CO2-CH4 mixture, a CO2-N2 mixture and a CH4-N2 mixture. The preparation method of the core-shell type molecular sieve microsphere is simple and is suitable for industrial production.

Description

technical field [0001] The present invention relates to a core-shell type molecular sieve microsphere material and its preparation method and application, in particular to a composite microsphere with NaA and NaX mixed crystal forms prepared by this method in one step, and a compound microsphere with type A The molecular sieve is a dense shell, and the A and X molecular sieves are the core-shell molecular sieve microspheres. Mainly used for adsorption and separation of gases, increasing CO 2 and CH 4 , N 2 Separation factor for two-component gases. Background technique [0002] The greenhouse effect produced by carbon dioxide emissions is a worrying global environmental problem, and the vast majority of CO 2 The emissions are produced by fossil combustion, how to efficiently separate and capture CO from flue gas 2 It is of great significance to reduce greenhouse gas emissions. In addition, CO 2 It is also the main impurity gas in natural gas and biogas, CO 2 The pres...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/28B01J20/18B01D53/02
CPCB01D53/02B01J20/18B01J20/28021B01D2253/1085B01D2257/504B01D2257/7025B01D2256/10B01D2257/102B01D2256/245B01D2256/22B01J2220/4806B01J2220/42B01J2220/4812Y02C20/20Y02C20/40
Inventor 张利雄于爽曾昌凤王重庆
Owner NANJING UNIV OF TECH