Preparation method of silanization-modified molecular sieve

A molecular sieve and silanization technology, which is applied in chemical instruments and methods, molecular sieves and alkali exchange compounds, inorganic chemistry, etc., can solve the problems of difficult internal modification of molecular sieves, low silanization degree, and low silanization efficiency. Effects of reduced static and dynamic water adsorption, high degree of silanization, and improved hydrophobicity

Active Publication Date: 2015-04-01
杭州富阳奥玛德科技有限公司
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Problems solved by technology

[0004] In order to solve the problems of low silanization degree, low silanization efficiency, difficult internal modification of molecular sieve channels and high c

Method used

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  • Preparation method of silanization-modified molecular sieve
  • Preparation method of silanization-modified molecular sieve
  • Preparation method of silanization-modified molecular sieve

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Example Embodiment

[0022] A preparation method of silylated modified molecular sieve. The molecular sieve is placed in an aqueous solution and organic acid and organic base are alternately added for pretreatment. The pretreated molecular sieve, accelerator and silylation reagent dissolved in organic solvent are silanized The reaction to obtain a silanized modified molecular sieve specifically includes the following steps:

[0023] Molecular sieve pretreatment: place the molecular sieve in an aqueous solution, alternately add organic acids and organic bases, adjust the pH value to swing between 4-10 and change 2-12 times, and treat both the acidic side and the alkaline side at room temperature for 10-120 Minutes; Wash the molecular sieve after acid-base treatment, and dry it at 40-120°C for 1-10 hours, and quickly transfer to drying equipment for later use after cooling.

[0024] Molecular sieve silanization: dissolve the silylation reagent in an organic solvent and transfer it to the reactor, add the...

Example Embodiment

[0045] Example 1

[0046] Pretreatment of molecular sieve: place the synthesized HMS molecular sieve in an aqueous solution, alternately add acetic acid and carbonamide, adjust the pH value to swing between 4 and 10 for 5 times, and treat both the acid side and the alkaline side at room temperature for 60 minutes ; Then washed and transferred to a vacuum drying box, dried at 90 ℃ for 6 hours, after cooling, quickly transferred to the drying box for later use.

[0047] Silanization of molecular sieve: Dissolve 26.3 mL of trimethylchlorosilane in 606 mL of ether to prepare a solution with a mass fraction of 5%, and transfer it to a tank reactor; add 15.1 g of pretreated HMS molecular sieve and triethylamine 5.8mL, the molar ratio of trimethylchlorosilane to molecular sieve and accelerator is 1:1.2:0.2, stirring uniformly; nitrogen gas is introduced to ensure that the air is exhausted and the air is quickly sealed, and then the temperature is 90℃, the pressure is 1.5MPa, and the stirr...

Example Embodiment

[0048] Example 2

[0049] Pretreatment of molecular sieve: place the synthesized HMS molecular sieve in an aqueous solution, alternately add acetic acid and carbonamide, adjust the pH value to swing between 4-10 and change twice, and treat both the acid side and the alkaline side at room temperature for 10 minutes ; Then washed and transferred to a vacuum drying box, dried at 40 ℃ for 1 hour, after cooling, quickly transferred to the drying box for later use.

[0050] Silanization of molecular sieve: Dissolve 26.3 mL of trimethylchlorosilane in 765 mL of ether to prepare a solution with a mass fraction of 4%, and transfer it to a tank reactor; add 12.6 g of pretreated HMS molecular sieve and triethylamine to it 2.9mL, the molar ratio of trimethylchlorosilane to molecular sieve and accelerator is 1:1:0.1, and stir evenly; nitrogen gas is introduced to ensure that the air is exhausted and the air is quickly sealed, and then the temperature is 30℃, the pressure is 0.5MPa, and the stir...

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Abstract

The invention belongs to the field of synthesis and application of molecular sieves, and discloses a preparation method of a silanization-modified molecular sieve. The method comprises the following steps: transferring a molecular sieve subjected to acid-alkali alternate treatment, an accelerator and a silanization reagent dissolved in an organic solvent into a reactor, carrying out silanization modification on the molecular sieve in a nitrogen protective sealed environment under the conditions of certain temperature and high pressure, filtering, washing, and drying to obtain the silanization-modified molecular sieve. The preparation method disclosed by the invention can effectively enhance the silanization efficiency, does not have great influence on the pore structure of the molecular sieve, and has the advantages of low cost, simple technique and high silanization degree.

Description

technical field [0001] The invention relates to the field of synthesis and application of molecular sieves, in particular to a preparation method of silanized modified molecular sieves. Background technique [0002] Molecular sieve is a kind of inorganic porous material, which has the advantages of large specific surface area, uniform pore structure and adjustable pore size. Most of the pore walls of molecular sieves such as HMS, MCM-41, and SBA-15 are in an amorphous state. In the air, the Si-O-Si on the surface will also undergo hydrolysis reaction at room temperature, resulting in the slow disintegration of the pore structure, and the surface of the molecular sieve is rich in a large number of silanol groups, and has strong hydrophilicity, which seriously affects the catalytic performance of the molecular sieve. , it is difficult to meet the requirements of industrial catalytic processes; another example is that ZSM-5 molecular sieve has a structure of high-silicon three-...

Claims

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Application Information

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IPC IPC(8): C01B39/00C01B39/38
Inventor 王广建韩亚飞王芳
Owner 杭州富阳奥玛德科技有限公司
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