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Mcm-41 molecular sieve containing bea type zeolite structural unit and its preparation method

A technology of MCM-41 and structural units, applied in the field of MCM-41 molecular sieves and its preparation, can solve the problems of poor hydrothermal stability and single pore size of mesoporous materials

Active Publication Date: 2017-01-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] One of the technical problems to be solved by the present invention is that the mesoporous materials synthesized in the prior art have a single pore size and poor hydrothermal stability. A new MCM-41 molecular sieve containing BEA-type zeolite structural units is provided

Method used

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  • Mcm-41 molecular sieve containing bea type zeolite structural unit and its preparation method
  • Mcm-41 molecular sieve containing bea type zeolite structural unit and its preparation method
  • Mcm-41 molecular sieve containing bea type zeolite structural unit and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0024] Add 0.7 g Beta zeolite powder into 10 ml, 0.2 mol / L hydrochloric acid solution, stir at 50°C for 1 h, then add CTAB, OP-10, silica gel powder, aluminum sulfate, hydrochloric acid and deionized water to the solution to make the reaction mixture The molar ratio of SiO 2 / Al 2 o 3 = 40:1, CTAB / SiO 2 =0.25:1, CTAB / OP-10=7:1, H + / SiO 2 = 1.9:1,H 2 O / SiO 2 = 160:1, another W Beta / W SiO2 (g / g) = 0.7, stirred at 30°C for 2h, put it into a closed container, and crystallized at 100°C for 48h under autogenous pressure. The crystallized product was taken out after cooling, washed with water, filtered, and dried. Calcined at 550°C for 1h in a nitrogen atmosphere and 550°C in an air atmosphere for 5h, the molar composition of SiO 2 :Al 2 o 3 =40 MCM-41 molecular sieve containing BEA-type zeolite structural units, the specific surface area is 833 m 2 / g, pore volume 1.1 cm 3 / g, average pore size 5.6nm, the XRD diffraction pattern of this material is figure 1 , t...

Embodiment 2

[0026] Add 0.7 g Beta zeolite powder into 10 ml, 0.2 mol / L hydrochloric acid solution, stir at 50°C for 1 h, then add CTAB, OP-10, silica gel powder, aluminum sulfate, hydrochloric acid and deionized water to the solution to make the reaction mixture The molar ratio of SiO 2 / Al 2 o 3 = 20:1, CTAB / SiO 2 =0.25:1, CTAB / OP-10=7:1, H + / SiO 2 = 1.9:1,H 2 O / SiO2 = 160:1, another W Beta / W SiO2 (g / g) = 0.7, stirred at 30°C for 2h, put it into a closed container, and crystallized at 100°C for 48h under autogenous pressure. The crystallized product was taken out after cooling, washed with water, filtered, and dried. Calcined at 550°C for 1h in a nitrogen atmosphere and 550°C in an air atmosphere for 5h, the molar composition of SiO 2 :Al 2 o 3 =20 MCM-41 molecular sieve containing BEA type zeolite structural unit, specific surface area is 810 m 2 / g, pore volume 1.0 cm 3 / g, average pore diameter 5nm, the XRD diffraction pattern of this material is figure 2 .

Embodiment 3

[0028] Add 0.7 g Beta zeolite powder into 10 ml, 0.2 mol / L hydrochloric acid solution, stir at 50 °C for 1 h, then add CTAB, OP-10, silica gel powder, hydrochloric acid and deionized water to the solution to make the molar distribution of the reaction mixture than SiO 2 / Al 2 o 3 = ∞: 1, CTAB / SiO 2 =0.25:1, CTAB / OP-10=7:1, H + / SiO 2 = 1.9:1,H 2 O / SiO 2 = 160:1, another W Beta / W SiO2 (g / g) = 0.7, stirred at 30°C for 2h, put it into a closed container, and crystallized at 100°C for 48h under autogenous pressure. The crystallized product was taken out after cooling, washed with water, filtered, and dried. Calcined at 550°C for 1h in a nitrogen atmosphere and 550°C in an air atmosphere for 5h, the molar composition of SiO 2 :Al 2 o 3 =∞ MCM-41 molecular sieve containing BEA-type zeolite structural units, with a specific surface area of ​​860 m 2 / g, pore volume 1.2 cm 3 / g, average pore diameter 6nm, this material XRD collection of patterns and scanning electr...

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Abstract

The invention relates to an MCM-41 molecular sieve containing a BEA type zeolite structure unit and a preparation method of the MCM-41 molecular sieve. The MCM-41 molecular sieve is mainly used for solving the problem that a mesoporous material synthesized by using the prior art is single in aperture and poor in hydrothermal stability. According to the MCM-41 molecular sieve and the method disclosed by the invention, the MCM-41 molecular sieve containing the BEA type zeolite structure unit is prepared in an acidic system by adopting an S<+>S0X<->I<+> route assembling method, wherein the proportion of a BEA type zeolite phase can be adjusted, a synthesized porous material consists of components with the following molar relationships: nSiO2 and Al2O3, n is equal to 40 to infinity, and an XRD diffraction spectrum has characteristic diffraction peaks when 2theta is equal to 2.14+ / -0.04, 3.9+ / -0.5, 7.79+ / -0.03 or 22.38+ / -0.03. By adopting the technical scheme, the problem that the mesoporous material synthesized by using the prior art is single in aperture and poor in hydrothermal stability can be relatively well solved; and the material disclosed by the invention can be applied to the industrial production of catalysis and adsorption separation.

Description

technical field [0001] The invention relates to an MCM-41 molecular sieve containing a BEA type zeolite structural unit and a preparation method thereof. Background technique [0002] The hydrocracking catalyst developed with molecular sieve materials as the carrier is the mainstream and direction of hydrocracking technology research and development. The molecular sieves currently used are mainly microporous molecular sieves such as ZSM-5, Y and Beta. Performance plays an important role. However, as the oil becomes heavier, the narrow pore size of the microporous molecular sieve limits its application. Although the pore can be enlarged after the super-stabilization secondary treatment, the pore size is not uniform. In 1992, the appearance of mesoporous molecular sieve, its large specific surface area, uniform mesoporous pore size and high thermal stability, brought dawn to the lightening reaction of heavy oil. However, the weak acidity and low hydrothermal stability caused...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/46C01B39/48
Inventor 李旭光孔德金郑均林陈燕
Owner CHINA PETROLEUM & CHEM CORP