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A method for rapidly synthesizing ti-mww molecular sieves by rotation by seed crystal method

A technology of molecular sieve and seed crystal method, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems that the catalytic activity of Ti-MWW molecular sieve needs to be improved, is unfavorable for industrial production and application, and increases production cost, and is beneficial to industrial production and application. , The effect of short synthesis time and energy saving

Active Publication Date: 2019-03-01
HUBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The crystallization of Ti-MWW molecular sieve raw powder needs the crystallization of reaction gel under the stirring rate of 100rpm for 7 days (Chemistry Letters, 2000,774; The Journal of Physical Chemistry B, 2001,105,2897), but due to the crystallization time It is longer, which increases the production cost and is not conducive to industrial production and application
[0003] Patent 201510329456.7 discloses a method for rapidly synthesizing Ti-MWW molecular sieves. This method adopts the rotational crystallization mode, and the original powder of Ti-MWW molecular sieves can be synthesized in 63 to 90 hours. However, the crystallization time is still long, and Ti-MWW The catalytic activity of molecular sieves needs to be improved

Method used

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  • A method for rapidly synthesizing ti-mww molecular sieves by rotation by seed crystal method
  • A method for rapidly synthesizing ti-mww molecular sieves by rotation by seed crystal method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: a kind of method that the seed method rotates and synthesizes Ti-MWW molecular sieve rapidly, comprises the following steps:

[0030] 1) Mix the raw materials to make a reaction gel: firstly, the raw materials are according to the molar composition ratio: titanium source: silicon source: boron source: organic amine: water = 0.04: 1.0: 0.67: 1.5: 25.0, weighed for later use, and the organic amine is added to In water, after stirring for 0.5 hours, then add titanium source and boron source in turn and stir evenly, then add silicon source and stir thoroughly to obtain a reaction gel, wherein the titanium source is n-butyl titanate, and the silicon source is Silica, the boron source is boric acid, and the organic amine is piperidine;

[0031] 2) adding the seed crystal to the reaction gel obtained in step 1), the amount of the seed crystal added is 1% of the mass of the reaction gel, and the reaction gel containing the seed crystal is obtained, wherein the see...

Embodiment 2~10

[0036] The implementation process is the same as in Example 1 except for the following differences. Table 1 shows the raw material components and their formulations for preparing the reaction gel, and Table 2 shows the process conditions for preparing Ti-MWW molecular sieves.

[0037] Table 1

[0038]

[0039] Table 2

[0040]

Embodiment 11

[0041] Embodiment 11: Effect example

[0042] The catalytic activity of the synthesized Ti-MWW molecular sieves was evaluated by the epoxidation reaction of allyl chloride. The catalytic reaction conditions are: 0.2 grams of catalyst, 3.9 grams of acetone, 2.295 grams of allyl chloride, and 3.73 grams of hydrogen peroxide (27.3% in mass concentration). The specific process is that the catalyst, solvent and reactant are added into the double-necked flask in sequence, and the hydrogen peroxide is divided into four parts evenly under the condition of stirring, and then added into the reactor in turn within 30 minutes, and reacted at 60 ° C for 8 hours , and the results are shown in Table 3.

[0043] table 3

[0044] serial number

[0045] As can be seen from Table 3, the Ti-MWW molecular sieves obtained according to the method of rotating and rapidly synthesizing Ti-MWW molecular sieves provided by the present invention have excellent performance in the epoxidation re...

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Abstract

The invention discloses a crystal-seed method for rapidly synthesizing Ti-MWW molecular sieves through rotation. The method comprises steps as follows: firstly, crystal seeds are added to reaction gel, the reaction gel is placed in a reaction kettle, the reaction kettle is sealed and rotates along a horizontal rotating shaft for rotating ageing and rotating crystallization, and the sum of time for rotating ageing and time for rotating crystallization is larger than or equal to 48 h and smaller than or equal to 60 h. Raw powder of the Ti-MWW molecular sieves can be rapidly synthesized, the synthesis time of the Ti-MWW molecular sieves is greatly shortened, the energy consumption is greatly reduced, and the production cost is saved; besides, the method has the advantages of simplicity and easiness in operation, good repeatability and high yield.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for rapidly synthesizing Ti-MWW molecular sieves by rotating through a seed crystal method. Background technique [0002] Epoxy compounds are important intermediates in organic synthesis and are widely used in manufacturing industries such as resins, coatings, and high molecular polymers. Currently, epoxy compounds are mainly synthesized by epoxidation of alkenes. Ti-MWW molecular sieve is a titanium-silicon molecular sieve that can effectively catalyze the epoxidation of olefins. The crystallization of Ti-MWW molecular sieve raw powder needs the crystallization of reaction gel under the stirring rate of 100rpm for 7 days (Chemistry Letters, 2000,774; The Journal of Physical Chemistry B, 2001,105,2897), but due to the crystallization time It is longer, which increases the production cost and is unfavorable for industrialized production and application. [0...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08C01B39/04
CPCC01B39/04C01B39/08C01P2006/90
Inventor 周丹章天骏夏清华
Owner HUBEI UNIV