Synthesis method of Nu-6(1) molecular sieve

A molecular sieve, nu-6 technology, applied in the field of synthesis of Nu-6 molecular sieves, can solve the problems of long production cycle and heavy labor, and achieve the effects of reduced content, large application potential, and uniform crystal size

Inactive Publication Date: 2016-11-09
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above-mentioned shortcoming of the prior art, the object of the present invention is to provide a kind of synthetic method of Nu-6 (1) molecular sieve, to overcome the large amount of manpower in the prior art, the defect of long production cycle

Method used

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  • Synthesis method of Nu-6(1) molecular sieve
  • Synthesis method of Nu-6(1) molecular sieve
  • Synthesis method of Nu-6(1) molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] The molar ratio of synthesized Nu-6(1) is: 0.278Na 2 O:1SiO 2 :0.02Al 2 O 3 :0.13 4,4’-Bipyridine:0.5H 2 O, add 1wt% seed crystals, statically crystallize, and react at 135°C for 72 hours to prepare Nu-6(1) molecular sieve.

[0049] 1) Mix 0.912 g of 4,4'-bipyridine and 5.040 g of absolute ethanol to obtain solution A, 10.158 g of sodium silicate solution and 5.960 g of deionized water to obtain solution B, 0.310 g of aluminum sulfate, and 12.110 g of deionized water. Mix water and 0.760 g of concentrated sulfuric acid to obtain C solution, and stir for 2 hours;

[0050] 2) Add solution B dropwise to solution A prepared in step 1), stir for 1 hour, then add solution C dropwise to the mixed solution of A and B, after aging at room temperature for 24 hours, add 27 mg of Nu-6(1) Seed crystal.

[0051] Dry the mother liquor in step 2) at 80°C for 24 hours, and grind into powder;

[0052] 3) Pour the powder into a polytetrafluoroethylene reactor, add 0.522 g of deionized water, sti...

Embodiment 2

[0058] The molar ratio of synthesized Nu-6(1) is: 0.278Na 2 O:1SiO 2 :0.02Al 2 O 3 :0.065 4,4’-Bipyridine:0.5H 2 O, adding 5wt% seed crystals, static crystallization, and reacting at 135°C for 72 hours to prepare Nu-6(1) molecular sieve.

[0059] The difference from Example 1 is that in step 1), 0.458 g of 4,4'-bipyridine is added to solution A; in step 2), 135 mg of Nu-6(1) seed crystal is added; in step 4), 0.478 is added G deionized water, add acid to adjust the pH to 1.0. The remaining steps and parameters are the same as in Example 1.

[0060] Figure 7 This is a scanning electron micrograph of Nu-6(1) molecular sieve. Nu-6(1) molecular sieve crystals are about 1 micron flaky crystals with relatively uniform crystal size. Compared with the traditional Nu-6(1) synthesis method, the ratio of water to silicon decreased from 30 to 0.5, and the ratio of silicon to template decreased from 0.13 to 0.065. The conditions of hydrothermal synthesis were changed from dynamic crystallizat...

Embodiment 3

[0063] The molar ratio of synthesized Nu-6(1) is: 0.278Na 2 O:1SiO 2 :0.02Al 2 O 3 :0.065 4,4’-Bipyridine:3H 2 O, add 1wt% seed crystals, statically crystallize, and react at 135°C for 72 hours to prepare Nu-6(1) molecular sieve.

[0064] The difference from Example 1 is that in step 1), 0.458 g of 4,4'-bipyridine is added to solution A; in step 4), 1.632 g of deionized water is added, and acid is added to adjust the pH to 11.0. The remaining steps and parameters are the same as in Example 1.

[0065] Picture 9 This is a scanning electron micrograph of Nu-6(1) molecular sieve. Nu-6(1) molecular sieve crystals are about 1 micron flaky crystals with relatively uniform crystal size. Compared with the traditional Nu-6(1) synthesis method, while the ratio of water to silicon is reduced from 30 to 3, the ratio of silicon to template is reduced from 0.13 to 0.065. The conditions of hydrothermal synthesis are changed from dynamic crystallization and reaction for 96 hours. The improvement...

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Abstract

The invention discloses a method for synthesizing a Nu-6(1) molecular sieve. The method comprises the following steps that 1, a mother solution is prepared, wherein a template agent and ethyl alcohol are mixed to obtain a solution A, a silicon source, an alkali source and water are mixed to obtain a solution B, an aluminum source, water and acid with a pH value regulating effect are mixed to obtain a solution C, the solution B is dropwise added into the solution A, the solution C is dropwise added into the mixed solution of the solution A and the solution B, aging is conducted, and seed crystals are added to obtain the mother solution; 2, the mother solution obtained in the step 1 is dried and ground into powder; 3, the powder and water are mixed, and the Nu-6(1) molecular sieve is synthesized through crystallization. According to the technical scheme, the content of the water and the template agent in the raw materials is greatly decreased, so that raw material cost and environmental pollution are greatly reduced, and the green chemistry requirement is met.

Description

Technical field [0001] The invention relates to a method for synthesizing molecular sieve, in particular to a method for synthesizing Nu-6(1) molecular sieve. Background technique [0002] Molecular sieves are aluminosilicate crystal materials with regular microporous structure, which can be widely used in the fields of catalysis, adsorption and separation. [0003] Nu-6(1) is a molecular sieve with a layered structure, composed of [SiO 4 ] And [SiO 3 The OH] tetrahedron forms each layer, and the structure-directing agent 4,4'-bipyridine molecule is located in the middle of the sandwich. After calcining to remove 4,4'-bipyridine, Nu-6(1) is transformed into Nu-6(2) molecular sieve with NSI type framework structure. Nu-6(2) molecular sieve can be used as a catalyst for disproportionation and isomerization reactions, and due to its smaller pore size and flake growth properties, Nu-6(2) hybrid membrane is used for H 2 Selective osmosis. [0004] Corma et al. obtained Nu-6(1) molecular...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
CPCC01B39/04C01P2002/72C01P2002/86C01P2004/03C01P2004/20C01P2004/61
Inventor 王宜慧张延风李猛白璐常娜南贵珍胡登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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