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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 cost in the existing molecular sieve silanization modification technology, the present invention provides a preparation method of silanization modified molecular sieve

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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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preparation example Construction

[0022] A method for preparing silanized modified molecular sieves. The molecular sieves are placed in an aqueous solution and organic acids and organic bases are alternately added for pretreatment, and the pretreated molecular sieves, accelerators and silylating agents dissolved in organic solvents are silanized Reaction, makes the molecular sieve of silanization modification, specifically comprises the following steps:

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

[0024] Molecular sieve silanization: Dissolve the silylating agent in an organic solvent, transfer it to the reactor, a...

Embodiment 1

[0046] Molecular sieve pretreatment: put the synthesized HMS molecular sieve in aqueous solution, add acetic acid and carbonamide alternately, adjust the pH value to swing between 4-10 and change 5 times, and treat both the acid side and the alkaline side at room temperature for 60 minutes Then wash and transfer to a vacuum drying oven, dry at 90°C for 6 hours, and quickly transfer to a drying oven for use after cooling.

[0047] Silanization of molecular sieves: Dissolve 26.3mL of trimethylchlorosilane in 606mL of ether to prepare a solution with a mass fraction of 5%, and transfer it to a tank reactor; 5.8mL, the molar ratio of trimethylchlorosilane to molecular sieve and accelerator is 1:1.2:0.2, stir evenly; pass nitrogen gas to ensure that the air is exhausted and seal it quickly, and then at a temperature of 90°C, a pressure of 1.5MPa, and a stirring speed Under the condition of 200r / min, the constant temperature reaction was carried out for 5 hours. Cool to room temper...

Embodiment 2

[0049] Molecular sieve pretreatment: put the synthesized HMS molecular sieve in aqueous solution, add acetic acid and carbonamide alternately, adjust the pH value between 4-10 and swing twice, and treat both the acidic side and the alkaline side at room temperature for 10 minutes ; Then wash and transfer to a vacuum drying oven, dry at 40°C for 1 hour, and quickly transfer to a drying oven for use after cooling.

[0050] Silanization of molecular sieves: Dissolve 26.3mL of trimethylchlorosilane in 765mL of ether to prepare a solution with a mass fraction of 4%, and transfer it to a tank reactor; pretreated HMS molecular sieves 12.6g and triethylamine 2.9mL, the molar ratio of trimethylchlorosilane to molecular sieve and accelerator is 1:1:0.1, stir evenly; pass in nitrogen gas to ensure that the air is exhausted and seal it quickly, and then at a temperature of 30°C, a pressure of 0.5MPa, and a stirring speed Under the condition of 100r / min, constant temperature reaction for 1...

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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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