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A kind of preparation method of hierarchical porous ts-1 molecular sieve

A TS-1, multi-stage pore technology, applied in molecular sieve compounds, molecular sieve catalysts, molecular sieve characteristic metal phosphates, etc., to prevent precipitation and narrow pore size distribution.

Active Publication Date: 2021-05-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the soft template method such as Zhou Xinggui (CN103357432A) utilizes polyether type Pluronic F127 as a mesoporous template agent, and the xerogel method synthesizes mesoporous nanometer TS-1 molecular sieve; Zhang Shufen (CN102910643A) utilizes hexadecyltrimethylammonium bromide Introducing mesoporous channels into titanium-silicon molecular sieves as mesoporous templating agent; wherein the hard template method such as Chen Lihua et al. TS-1 nanocrystals were grown within the channel, and the hard template was removed to prepare a hierarchical TS-1 molecular sieve; Li Gang et al. (CN101962195A) used cheap sugar instead of porous carbon material as a macroporous-mesoporous template. During the process of heat-treating the TS-1 molecular sieve synthetic sol of sugar, the sugar is heated, carbonized and dehydrated to form a hard template directly, and a multi-level pore TS-1 molecular sieve is obtained, but the activity and stability of the TS-1 molecular sieve need to be improved.

Method used

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  • A kind of preparation method of hierarchical porous ts-1 molecular sieve
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  • A kind of preparation method of hierarchical porous ts-1 molecular sieve

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Experimental program
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Embodiment approach

[0134] According to one embodiment of the present application, the method for preparing the hierarchically porous TS-1 molecular sieve is as follows:

[0135] a) Add silicate, titanate and polyols into a three-necked flask and mix evenly, carry out transesterification reaction under stirring, connect to a distillation device, protect with nitrogen, the reaction temperature is between 80-180°C, and the reaction time is between After 2 to 10 hours, the conversion rate of the transesterification reaction is between 60% and 80%.

[0136] b) Connect the device after the reaction in step a) to a water pump or an oil pump for vacuum distillation to make the transesterification reaction more complete. The vacuum degree of the control system is 0.01-5KPa, the reaction temperature is between 170-230°C, and the reaction time is between After 0.5-5 hours, the conversion rate of the transesterification reaction is greater than 90%, and the silicon-titanium ester polymer is obtained.

[01...

Embodiment 1

[0162] The specific batching process is as follows: add 5g tetraethyl titanate, 0.29g tetraethyl titanate and 10g polyethylene glycol 200 into the three-necked flask and mix evenly, carry out the transesterification reaction under stirring, connect the distillation device, and pass nitrogen gas Protection, heating up to 175°C, reaction time 5 hours, the conversion rate of the transesterification reaction is 75%, connected to a water pump for vacuum distillation to make the transesterification reaction more complete, control the vacuum degree of the system at 3KPa, the reaction temperature is 200°C, the reaction After 1 hour, the conversion rate of the transesterification reaction was 92%, and the silicon-titanium polyethylene glycol ester polymer was obtained. The obtained silicon-titanium polyethylene glycol ester polymer was mixed with 8g tetrapropylammonium hydroxide (25wt.% aqueous solution) and 12g water, stirred and aged at room temperature for 2 hours, and then transferr...

Embodiment 2

[0164] The specific batching process is as follows: add 5g tetraethyl titanate, 0.05g tetraethyl titanate and 3.13g ethylene glycol into the three-necked flask and mix evenly, carry out transesterification reaction under stirring, connect the distillation device, and pass nitrogen protection , the temperature was raised to 100°C, the reaction time was 5 hours, and the conversion rate of the transesterification reaction was 70%. Connected to a water pump for vacuum distillation to make the transesterification reaction more complete, the vacuum degree of the control system was at 3KPa, the reaction temperature was 170°C, and the reaction time was After 1 hour, the conversion rate of the transesterification reaction was 90%, and the silicon-titanium glycol ester polymer was obtained. The obtained silicon-titanium glycol ester polymer was mixed with 2g tetrapropylammonium hydroxide (25%wt. aqueous solution) and 3g water, stirred and aged at room temperature for 2 hours, and then tr...

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Abstract

The present application discloses a preparation method of a multi-level porous TS-1 molecular sieve. The multi-level porous TS-1 molecular sieve is obtained by using a silicon-titanium ester polymer as a titanium silicon source. In the method, silicon and titanium are evenly connected on the same polymer, and the hydrolysis rate is equivalent during hydrolysis, which can prevent TiO 2 Precipitation, reducing the generation of non-skeleton titanium; and the new silicon titanium ester polymer as silicon source and titanium source, can also be used as a mesoporous template in the synthesis process, the obtained TS-1 molecular sieve has mesoporous structure with a narrow pore size distribution.

Description

technical field [0001] The application relates to a method for preparing a multi-stage porous 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 framework titanium and non-framework titanium in the mol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/00B01J29/89B01J35/10
CPCC01B37/002B01J29/89B01J37/0018C01P2006/16C01P2004/62B01J2229/32B01J35/647
Inventor 袁丹华邢嘉成徐云鹏刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI