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Method for synthesizing silicon substrate molecular sieve by using copper amine complex as template agent

A silicon-based molecular sieve and complex technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of not being large-pore mordenite, restricting industrial application, high price, etc., and achieving low cost, simple and easy method, high cost. The effect of specific surface area

Active Publication Date: 2011-02-16
中科鸿景(宁波)环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these templates are not only expensive, but also difficult to synthesize, and require high energy to remove them in the later treatment process. These factors greatly restrict their industrial application.
[0004] For MOR zeolites, although this structure can be obtained in pure inorganic systems, the products obtained by this method are often not large-pore mordenites

Method used

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  • Method for synthesizing silicon substrate molecular sieve by using copper amine complex as template agent
  • Method for synthesizing silicon substrate molecular sieve by using copper amine complex as template agent
  • Method for synthesizing silicon substrate molecular sieve by using copper amine complex as template agent

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Experimental program
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Effect test

Embodiment 1

[0031] Embodiment 1: Preparation of CHA sample (Si / Al=8.8)

[0032] First, dissolve 0.514 grams of sodium aluminate solid in 4.722 grams of water, then add 1.149 grams of copper sulfate pentahydrate solid, and after stirring for half an hour, add 1.07 grams of tetraethylenepentamine dropwise to the above system, and then add 0.38 gram of sodium hydroxide solid, after stirring for half an hour, add 3.6 milliliters of 31.5% silica sol to the above system, after stirring for two to three hours, put it into a polytetrafluoroethylene-lined steel reactor, and react at 140 degrees Two to six days. The chemical ratio of the system is as follows: 3.41Na 2 O: 1.0Al 2 o 3 : 10SiO 2 : 200H 2 O:2.0Cu-R (wherein R:Cu=1:1). After the reaction is completed, the obtained product is fully washed with deionized water, and dried at 100 degrees for more than 12 hours.

[0033] attached figure 1 According to the XRD characterization results of the product, it can be seen that the product ha...

Embodiment 2

[0035] Embodiment 2: Preparation of CHA sample (Si / Al=20)

[0036] The addition sequence and stirring time of gel preparation are the same as in Example 1. The difference is that the solid amount of sodium aluminate is 0.129 grams, and the solid amount of sodium hydroxide is 0.45 grams. The chemical ratio of the system is: 8.7Na 2 O: 1.0Al 2 o 3 : 30SiO 2 : 200H 2 O: 6.0Cu-R (wherein R: Cu = 1: 1), react at 140 degrees for four to ten days. After the reaction is completed, the obtained product is fully washed with deionized water, and dried at 100 degrees for more than 12 hours.

[0037] attached image 3 It is the XRD characterization result of the product, and it can be known that the product is a pure phase of CHA from the XRD characteristic peak.

[0038] attached Figure 4 It is a scanning electron microscope photo of the product. From the electron microscope characterization results, it can be seen that the product is a pure phase with high crystallinity. The sh...

Embodiment 3

[0039] Embodiment 3: the preparation of MOR sample

[0040] The addition sequence and stirring time of gel preparation are the same as in Example 1. The amount of each material is respectively 0.514 grams of sodium aluminate solid, 1.149 grams of copper sulfate pentahydrate solid, 3.342 grams of deionized water, 1.07 grams of tetraethylenepentamine, 0.366 grams of sodium hydroxide, and 4.99 milliliters of 31.5% silica sol. The chemical ratio is: 3.57Na 2 O: 1.0Al 2 o 3 : 15SiO 2 : 300H 2 O: 3.0Cu-R (wherein R: Cu = 1: 1), react at 180 degrees for two to six days. After the reaction is completed, the obtained product is fully washed with deionized water, and dried at 100 degrees for more than 12 hours.

[0041] attached Figure 5 It is a scanning electron micrograph of the product, which shows that the obtained product has a high degree of crystallinity, and large spherical crystals are piled up by small rod-shaped crystals.

[0042] attached Figure 6 It is the nitrog...

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Abstract

The invention relates to a preparation method of a molecular sieve, aiming at providing a method for synthesizing a silicon substrate molecular sieve by using a copper amine complex as a template agent. The method comprises the steps of dissolving sodium metaaluminate in deionized water, adding cupric salt, dropping organic amine in the solution after stirring, stirring completely, adding sodium hydroxide solid and stirring, then adding a silica solution in the solution, stirring for 2 to 3 hours, placing in a reaction kettle, crystallizing for 3 to 20 days at 140-180 DEG C, completely washing the reaction output with deionized water after reaction, drying for 12 hours above at 80 DEG C, exchanging through ammonium nitrate and calcining for four hours at 500 DEG C, removing the template agent to obtain the final product. Compared with the CHA molecular sieve synthesized without templates, the CHA molecular sieve has higher silica alumina ratio, stability and specific surface area and has higher reaction activity in the MTO catalytic reaction. The synthesizing method has simple template agent and lower cost, and the method for removing the template is simple and easy.

Description

technical field [0001] The invention belongs to a method for preparing molecular sieves, in particular to a method for synthesizing silicon-based molecular sieves by using a copper amine complex as a template. Background technique [0002] Molecular sieves, especially silica-alumina molecular sieves, are widely used in various catalysis due to their unique pore characteristics, good adsorption performance and shape selectivity, high specific surface area, good thermal stability and hydrothermal stability. Reacting. Molecular sieve research is closely related to industry, and the development of new structures and the exploration of new synthetic routes have become the focus of researchers. The synthesis of molecular sieves is inseparable from the use of templates. Templates can be alkali metal cations such as sodium and potassium, or organic molecules such as organic quaternary ammonium salts and crown ethers. New templates are often the key factor in the development of new...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 肖丰收任利敏朱龙凤杨承广孟祥举
Owner 中科鸿景(宁波)环保科技有限公司
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