Method for greenly synthesizing Ti-Si molecular sieve

A titanium-silicon molecular sieve and green synthesis technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problem of not involving the recycling of small crystal TS-1 mother liquor, so as to reduce the use of raw materials, reduce costs, and stabilize product quality Effect

Active Publication Date: 2012-06-20
DALIAN UNIV OF TECH
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  • Abstract
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Problems solved by technology

The patent pointed out that the seed crystal and its crystallization mother liquor are used

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] (a) Get 340ml deionized water and join in 147g silica sol (30%wt), after stirring for 10 minutes, 21g tetrapropylammonium bromide is added in the glue solution, continue to stir for 20 minutes, make raw material silicon solution; Tetrabutyl titanate and acetylacetone (ACAC) were mixed at a mass ratio of 1:0.8, and stirred for 15 minutes to obtain a raw titanium solution; 9.7 ml of the prepared raw titanium solution was added to the raw silicon solution, and after stirring for 30 minutes, , add 34g of n-butylamine mineralizer, continue to stir for 25 minutes to get a uniform gel; its composition is SiO 2:TiO 2 :TPABr:ACAC:NBA:H 2 O=50:1:5.3:3.1:31.6:167, then the resulting gel was added to a 2L stainless steel reactor, and the crystallization was completed under autogenous pressure and 170°C for 96 hours; the crystallized product was separated from the solid substance by centrifugation and mother liquor, the mother liquor is collected for later use. The solid was wash...

Embodiment 2

[0085] Repeat Example 1, but the reaction mixture is loaded into 2L stainless steel sealed kettle with stirring device, then the product obtained proves to be a titanium silicon molecular sieve through X-ray diffraction analysis, and its relative crystallinity is respectively 90%, and the product yield is 96%.

Embodiment 3

[0087] Repeat Example 1, but change the distillation temperature to 80°C, 85°C, and 95°C in turn, and the obtained product is proved to be a titanium-silicon molecular sieve through X-ray diffraction analysis, and its relative crystallinity is 90%, 99%, and 91% respectively , and the product yields were 95%, 92% and 89% respectively.

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Abstract

The invention discloses a method for greenly synthesizing Ti-Si molecular sieves in a low-cost raw material system, which belongs to the field of zeolite molecular sieve material preparation. The method is characterized in that: firstly preparing Ti-Si gel, then preparing Ti-Si molecular sieves, separating a template and an organic alkali from a filtrate, and recycling mother liquor to prepare TS-1 zeolite molecular sieves. The key of the method is separation and testing of organic components in recycled molecular sieve crystallization mother liquor, analyzing concentrations of template ion TPA+ and n-butylamine respectively, and accurately calculating content of each substance so as to precisely perform dosing. By separating the template and an alkaline mineralizer in the mother liquor, testing accurate contents of the template and the alkaline mineralizer, and recycling the mother liquor, thereby making gel composition be stable and product quality be stable in mother liquor recycling and overcoming blindness of mother liquor recycling in the previous technology. The Ti-Si molecular sieves synthesized by the inventive method save raw material, reduce cost, and eliminate pollution of mother liquor after molecular sieve crystallization to environment.

Description

technical field [0001] The invention belongs to the field of preparation of zeolite molecular sieve materials, and relates to a preparation method of titanium-silicon molecular sieve (TS-1) with MFI structure. Background technique [0002] Titanium-silicon molecular sieve (TS-1) is a new heteroatom molecular sieve material developed in the 1980s. It is a molecular sieve with MFI topology and titanium atoms in the framework. The catalytic system composed of titanium-silicon molecular sieve and dilute hydrogen peroxide is widely used in the field of selective oxidation, and has excellent low-temperature selective oxidation reaction performance. The use of TS-1 in the oxidation reaction of organic matter avoids the problems of complex oxidation process and environmental pollution. It has the incomparable advantages of energy saving, economy and environmental friendliness in traditional oxidation systems, and lays the foundation for the development of environmentally friendly p...

Claims

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Application Information

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IPC IPC(8): C01B39/08
Inventor 郭洪臣赵晓月李海龙
Owner DALIAN UNIV OF TECH
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