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Method for synthesizing new titanium-silicone metapore molecular sieve

A technology of mesoporous molecular sieve and synthesis method, which is applied in the field of synthesis of new titanium-silicon mesoporous molecular sieves, can solve problems such as poor structural order and application limitations, and avoid TiO2 precipitation and generation of TiO2 impurity phases. simple effect

Inactive Publication Date: 2003-07-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
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Problems solved by technology

Ti-SBA-15 can only be synthesized under the condition of microwave heating, and its disadvantages are: its application is limited, and its structural order is not good enough (document 2: Newalkar, B.L, et al., Chem. , Mater., 2001, 13, 552)
There is no report on the preparation of Ti-SBA-15 material by hydrothermal synthesis, a general method for synthesizing molecular sieves

Method used

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  • Method for synthesizing new titanium-silicone metapore molecular sieve
  • Method for synthesizing new titanium-silicone metapore molecular sieve
  • Method for synthesizing new titanium-silicone metapore molecular sieve

Examples

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example 1

[0034] 2 g of P123 (EO 20 PO 70 EO 20 ) surfactant was dissolved in 75ml of HCl solution with pH 1.0, stirred at 35-45°C for 5 hours, then added with molar ratio SiO 2 / F - 35 NH 4 F, add 7 g of methyl orthosilicate and TiO under vigorous stirring 2 / SiO 2 The isopropyl titanium mixture with a molar ratio of 1% was continuously stirred at high speed for 15 hours, and then the resulting gel was transferred to an oven at 60° C. and kept at least 24 hours. The white crystalline solid product is separated from the mother liquor, washed with deionized water until neutral, and dried under an air atmosphere below 100°C for 10 hours, and finally sintered at 500°C for 10 hours to obtain Ti- with a titanium content of 1.0%. SBA-15 mesoporous molecular sieve material. Wherein the titanium content is 1.0% the sample 1# XRD crystallographic pattern is as follows figure 1 Shown, ultraviolet-visible absorption spectrum (UV-vis) see figure 2 As can be seen from the figure, the three...

example 2

[0036] Change the HCl solution of pH 1.0 in Example 1 to the solution of pH 2.0, and other conditions and processes remain unchanged, and the titanium-containing-SBA-15 mesoporous molecular sieve material can also be obtained. Wherein the titanium content is 1.0% the sample 2# XRD crystalline pattern pattern such as image 3 Shown, UV-vis absorption spectrum see Figure 4 Although the sample still has three low-angle diffraction peaks, it shows that the obtained sample is a high-quality SBA-15 structure material, but in the UV-vis spectrum, it can be found that the tailing phenomenon of the absorption band of sample 2# at 210nm is very Seriously, this shows that not only some Ti 4+ into the framework of the sample, and there is a large amount of non-framework TiO 2 exist.

example 3

[0038] Change the HCl solution of pH 1.0 in Example 1 to the HCl solution of 1M concentration, and other conditions and processes remain unchanged, and Ti-SBA-15 mesoporous molecular sieve materials containing titanium can also be obtained. Wherein the titanium content is 1.0% the sample 3# XRD crystalline pattern pattern as image 3 shown by image 3It can be seen that the obtained material is a high-quality SBA-15 structure, and at the same time, from the UV-vis spectrum Figure 4 It can be seen that no non-framework titanium species were found in sample 3#, and most titanium should exist in the form of framework titanium.

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Abstract

The synthesis method of titanium-silicon metaporous molecular sieve uses non-ionic surfactant P123 as template agent, uses F(-1) as catalyst and utilizes silicon source and titanium source to make synthesis under the acid condition, and its preparation process includes the following steps: (1). using template agent and making it into acid solution, stirring for 5-24 hr, at 35-80 deg.c; (2). adding fluoride and stirring for above 5 hr.; (3) mixing silicon source and titanium source, adding them and continuously stirring for 12-48 hr, and obtaining primary gel product; (4) crystallizing said product for above 12 hr. at 40-100 deg.c and (5) precipitation, separation, washing, drying and roasting for above 5 hr. at 450-800 deg.C so as to obtain the invented product.

Description

technical field [0001] The invention relates to a heteroatom mesoporous molecular sieve, in particular to a synthesis method of a novel titanium-silicon mesoporous molecular sieve. Background technique [0002] Titanium-silicon mesoporous molecular sieves are widely used in the selective oxidation of large-volume organic compounds to prepare fine chemicals. The active center is generally considered to be the tetrahedral coordinated titanium that exists in isolation in the isomorphic substitution of silicon in the framework. Titanium species present outside the framework are irrelevant. So far, titanium-containing mesoporous molecular sieves, such as Ti-MCM-41, Ti-MCM-48, Ti-HMS and Ti-MSU, have been successfully synthesized. As for SBA-15, a very important member of mesoporous molecular sieves, there are very few reports on its element substitution due to the need for hydrothermal treatment under strong acidic conditions. This pure silicon oxide SAB-15 material is generall...

Claims

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Application Information

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IPC IPC(8): B01J29/89C01B39/08
Inventor 李灿张文华应品良
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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