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Ti-MWW molecular sieve and preparation method and application thereof

A technology of molecular sieves and titanium-silicon molecular sieves, applied in the direction of molecular sieve catalysts, molecular sieves and base exchange compounds, chemical instruments and methods, etc., can solve problems such as suitable hydrophilicity, inability to prepare skeleton titanium, low hydrophilicity of skeleton titanium content, etc. Achieve the effect of suitable hydrophilicity, effective regulation of repairing hydrophilicity, and high content of titanium in the skeleton

Active Publication Date: 2022-01-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] One of the technical problems to be solved by the present invention is to solve the problem of low titanium content and strong hydrophilicity in the framework of Ti-MWW molecular sieve, and provide a Ti-MWW molecular sieve with the advantages of high framework titanium content and suitable hydrophilicity
[0007] The second technical problem to be solved by the present invention is to solve the problem that the prior art cannot prepare Ti-MWW molecular sieves with high skeleton titanium content and suitable hydrophilicity, and provide a new preparation method of Ti-MWW molecular sieves

Method used

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  • Ti-MWW molecular sieve and preparation method and application thereof
  • Ti-MWW molecular sieve and preparation method and application thereof

Examples

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Embodiment 1

[0045] Molar ratio SiO 2 :B 2 o 3 : piperidine: water 1: 0.6: 1.5: 20. The corresponding amount of water, piperidine, boric acid and 60 grams of fumed silica were evenly mixed to form a gel, and dynamic hydrothermal crystallization was carried out at 50 rpm and 170 °C for 5 days. Centrifuge, wash, and dry at 80°C for 12 hours to obtain a B-MWW molecular sieve precursor. Then mix the B-MWW molecular sieve precursor with 2mol / L nitric acid solution at a mass ratio of 1:20, and then add tetra-n-butyl titanate to make the molar ratio of the B-MWW molecular sieve precursor to 0.06:1. Treat at 80°C for 24 hours to replenish titanium, centrifuge, wash, dry at 80°C for 12 hours, and calcine at 550°C in an air atmosphere for 10 hours to obtain a titanium-silicon molecular sieve with MWW structure. Then mix the MWW structure titanium-silicon molecular sieve with the nitric acid solution with a pH value of 1 at a mass ratio of 1:100, treat it at 160°C for 6 days, centrifuge, wash, dry...

Embodiment 2

[0047] Molar ratio SiO 2 :B 2 o 3 : Hexamethyleneimine: Water is 1: 0.8: 1.8: 50 Mix the corresponding amount of water, hexamethyleneimine, sodium tetraborate and 200 grams of silica sol with a mass fraction of 30% evenly, at 50rpm, Dynamic hydrothermal crystallization at 170°C for 5 days, centrifugation, washing, and drying at 80°C for 12 hours to obtain the B-MWW molecular sieve precursor. Then mix the B-MWW molecular sieve precursor with 2mol / L nitric acid solution at a mass ratio of 1:20, and then add tetra-n-butyl titanate to make the molar ratio of the B-MWW molecular sieve precursor to 0.06:1. Treat at 80°C for 24 hours to replenish titanium, centrifuge, wash, dry at 80°C for 12 hours, and calcine at 550°C in an air atmosphere for 10 hours to obtain a titanium-silicon molecular sieve with MWW structure. Then mix the MWW structure titanium-silicon molecular sieve with the nitric acid solution with a pH value of 1 at a mass ratio of 1:100, treat it at 160°C for 6 days,...

Embodiment 3

[0049] Molar ratio SiO 2 :B 2 o 3 : piperidine: water 1: 0.4: 1.0: 20. The corresponding amount of water, piperidine, boric acid and 60 grams of fumed silica were evenly mixed into a gel, and dynamic hydrothermal crystallization was carried out at 50 rpm and 170 °C for 5 days. Centrifuge, wash, and dry at 80°C for 12 hours to obtain a B-MWW molecular sieve precursor. Then mix the B-MWW molecular sieve precursor with 2mol / L nitric acid solution at a mass ratio of 1:20, and then add tetra-n-butyl titanate to make the molar ratio of the B-MWW molecular sieve precursor to 0.06:1. Treat at 80°C for 24 hours to replenish titanium, centrifuge, wash, dry at 80°C for 12 hours, and calcine at 550°C in an air atmosphere for 10 hours to obtain a titanium-silicon molecular sieve with MWW structure. Then mix the MWW structure titanium-silicon molecular sieve with the nitric acid solution with a pH value of 1 at a mass ratio of 1:100, treat it at 160°C for 6 days, centrifuge, wash, dry at...

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Abstract

The invention discloses a Ti-MWW molecular sieve as well as a preparation method and application thereof. According to the Ti-MWW molecular sieve, the molar fraction of titanium is 1.0%-3.0%, and the molar fraction of boron is 0.1%-1.0%; water adsorption capacity is 0.003 to 0.030 mL / g; diffraction peaks appear in an X-ray diffraction pattern when the value of 2 theta is 7.2 + / - 0.09 degrees, 8.0 + / - 0.10 degrees, 9.6 + / - 0.07 degrees, 14.4 + / - 0.07 degrees, 22.7 + / - 0.15 degrees and 26.1 + / - 0.12 degrees; and a strong absorption peak of 215 + / - 5 nm belonging to framework titanium appears in an ultraviolet visible spectrogram. The Ti-MWW molecular sieve provided by the invention has the advantages of high titanium content, proper hydrophilicity and good catalytic oxidation performance, and can be used in the industrial production process of epoxide.

Description

technical field [0001] The invention relates to a Ti-MWW molecular sieve and its preparation method and application, belonging to the field of molecular sieve inorganic materials. Background technique [0002] The discovery of titanium-silicon molecular sieve TS-1 is an important milestone in the field of molecular sieves, which expanded the catalytic application of molecular sieves from the field of acid-base catalysis to the field of selective oxidation catalysis (US4410501). With hydrogen peroxide as the oxidant, TS-1 molecular sieve can catalyze the selective oxidation of many organic substrates under mild conditions, some of which, such as propylene epoxidation, have achieved large-scale industrial applications. However, TS-1 molecular sieves showed lower activity in the catalytic oxidation of macromolecules due to the diffusion-limited effect of ten-membered ring micropores (0.5–0.55 nm). To solve this problem, researchers have developed Ti-MWW titanium-silicon molecu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/46C01B39/12C08F8/08C08F10/00B01J29/89C07D301/12C07D303/04C07D303/08
CPCC01B39/46C01B39/12C08F8/08B01J29/89C07D301/12C07D303/04C07D303/08C01P2002/72C01P2002/84C08F10/00Y02P20/52
Inventor 金少青杨为民沈震浩孙洪敏何俊琳
Owner CHINA PETROLEUM & CHEM CORP
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