A kind of method for preparing hierarchically porous titanium silicon ts-1 molecular sieve

A TS-1 and molecular sieve technology, which is applied in the direction of molecular sieve compounds, molecular sieve catalysts, and metal phosphates with molecular sieve characteristics, can solve the problems of difficult control conditions, poor experimental repeatability, cumbersome operation, etc., and achieve the effect of preventing precipitation

Active Publication Date: 2021-12-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Claims
  • Application Information

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Problems solved by technology

However, the method is cumbersome to operate, the conditions are not easy to control, and the repeatability of the experiment is poor. Moreover, due to the difference in the hydrolysis rate of the silicon source and the titanium source, a large amount of non-framework titanium is formed, which affects the catalytic performance of the TS-1 molecular sieve.

Method used

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  • A kind of method for preparing hierarchically porous titanium silicon ts-1 molecular sieve
  • A kind of method for preparing hierarchically porous titanium silicon ts-1 molecular sieve
  • A kind of method for preparing hierarchically porous titanium silicon ts-1 molecular sieve

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Experimental program
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Embodiment approach

[0139] According to one embodiment of the present application, the method for preparing the hierarchically porous TS-1 molecular sieve is as follows:

[0140] a) Mix titanate-based polyester polyol with organic base template, silicon source, water, etc. according to a certain ratio to obtain a gel mixture. Preferably, the gel mixture has the following molar ratio:

[0141] TiO 2 / SiO 2 =0.005~0.1;

[0142] Organic base template / SiO 2 =0.01~10;

[0143] h 2 O / SiO 2 =5~500;

[0144] The silicon content in the silicon source is SiO 2 In terms of moles, the titanium content in titanic acid polyester polyol is calculated as TiO 2 The number of moles; the content of the organic base template is based on the number of moles of N atoms.

[0145] b) subjecting the gel mixture obtained in step a) to an aging process, which can be omitted or carried out under stirring or static conditions, the aging temperature is 0-120°C, and the time is 0-100 hours;

[0146] c) Put the gel mi...

Embodiment 1

[0157] The types and molar amounts of each raw material, crystallization temperature and time, XRD crystal form and external specific surface results are shown in Table 1 below.

[0158] In Example 1, the specific batching process is as follows: add 6.76g tetrapropylammonium hydroxide (25wt.%) aqueous solution, 1g white carbon black, 10g water to 0.14g ethylene glycol titanate polyester, mix well, and stir at room temperature 2 hours, and then transferred to a stainless steel autoclave. At this time, the molar ratio of each component of the synthesis system is 0.05[Ti(OCH 2 CH 2 O) 2 ] 20 :SiO2 2 :0.5TPAOH:50H 2 O. The autoclave was sealed and placed in an oven at a constant temperature of 170°C for crystallization under autogenous pressure for 2 days. After the crystallization, the solid product was centrifuged, washed with deionized water until neutral, and dried in air at 110°C to obtain a multi-order pore TS-1 molecular sieve. Get the sample of this former powder a...

Embodiment 2-13

[0165] Specific ingredients, materials, reaction conditions and analysis results are shown in Table 1 below. The synthesis process is similar to Example 1. Other analysis results of the product are shown in Table 1 below.

[0166] Table 1 Raw material composition and crystallization conditions of Examples 2-13

[0167]

[0168]

[0169] In Table 1, R is selected from the group formed by the loss of x hydrogen atoms in hydrocarbon compounds, ethyl, propyl, butyl, polyethylene glycol, terephthalyl, etc., x is 2-6 between.

[0170] The crystallization in Examples 1 to 13 is static crystallization.

[0171] Wherein, the preparation method of the titanate-based polyester polyol in Example 2 to Example 13 is the same as the preparation method of the titanate glycol polyester in Example 1, the difference is that 5g of ethylene glycol is replaced by 6.1 g 1,3-propanediol, 5g glycerol, 7.2g 1,4-butanediol, 9.5g 1,6-hexanediol, 11.1g terephthalenediol, 9.3g 1,4-cyclohexanediol, ...

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Abstract

The present application discloses a method for preparing a hierarchically porous titanium-silicon TS‑1 molecular sieve, using titanate-based polyester polyol as a titanium source. In the method described, titanium is attached to the polymer, which makes titanium more difficult to hydrolyze and prevents TiO 2 Precipitation to reduce the generation of non-skeletal titanium; and titanate-based polyester polyols can also be used as a mesoporous template in the synthesis process while being used as a titanium source. The application of TS‑1 molecular sieve in the field of catalysis plays an important role in promoting.

Description

technical field [0001] The application relates to a method for preparing a hierarchically porous titanium-silicon TS-1 molecular sieve, which belongs to the field of molecular sieve preparation. Background technique [0002] TS-1 molecular sieve is a microporous molecular sieve with MFI topology, due to the presence of tetrahedral Ti in its framework structure 4+ center, thus for H 2 o 2 Participated in the selective oxidation of organic matter has a good catalytic effect, such as epoxidation of olefins, hydroxylation of phenols, ammoximation of ketones, oxidation of alkanes and other selective oxidation reactions. The catalytic oxidation process of TS-1 molecular sieve has no pollution, and the reaction conditions are mild, which overcomes the shortcomings of serious pollution and lengthy reaction process in the traditional process. [0003] There are two main factors affecting the activity and stability of TS-1: one is the content of molecular sieve framework titanium a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/00B01J29/89B01J35/10
CPCC01B37/002B01J29/89B01J35/1061B01J37/0018C01P2006/16C01P2004/62B01J2229/32
Inventor 袁丹华邢嘉成徐云鹏刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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