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ZSM-12 molecular sieve with special crystal orientation as well as preparation method thereof

A technology of crystal orientation and molecular sieve, applied in the direction of ZSM-12 crystalline aluminosilicate zeolite, organic chemistry, crystalline aluminosilicate zeolite, etc., can solve the problem of inability to control the crystal orientation of ZSM-12 molecular sieve, and improve the conversion rate. Effect

Inactive Publication Date: 2015-03-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] One of the technical problems to be solved by the present invention is that the method for preparing ZSM-12 molecular sieve in the prior art cannot control the crystal orientation of ZSM-12 molecular sieve, and a new ZSM-12 molecular sieve with specific crystal orientation is provided

Method used

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  • ZSM-12 molecular sieve with special crystal orientation as well as preparation method thereof
  • ZSM-12 molecular sieve with special crystal orientation as well as preparation method thereof
  • ZSM-12 molecular sieve with special crystal orientation as well as preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. Stir 3.283ml of water glass and 11.866ml of water first, then add 4.802ml of 23.08% MTEABr solution and stir evenly, then add 2.779ml of 7.41% nonahydrate aluminum nitrate solution, and add 0.271ml of 30% sulfuric acid under strong stirring solution, forming a mixture with the following molar composition: SiO2 / Al 2 o 3 =60, OH / SiO 2 =0.3, Na 2 O / (MTEA) 2 O=1.5, H 2 O / OH=225.

[0027] 2. Pour the sample into a polytetrafluoroethylene-lined reactor and crystallize at 160 oC for 156 hours.

[0028] 3. The above product is cooled, filtered, washed and dried to obtain a product sample.

[0029] The results of the XRD pattern of the product are shown in the appendix of the instruction manual. figure 1 : Its XRD pattern shows ZSM-12 topological structure, and the relative intensity of characteristic peaks is B / A=1.7, C / A=0.8.

[0030]

Embodiment 2

[0032] 1. First, stir 4.894ml of 40% TEABr solution and 3.709ml of water evenly, add 0.14g of sodium metaaluminate and stir until the solid dissolves, then add 13.461ml of 30% silica sol, and stir well to form a mixture with the following molar composition: SiO 2 / Al 2 o 3 =120, OH / SiO 2 =0.1, TEA + / SiO 2 =0.125,H 2 O / SiO 2 =13.

[0033] 2. Pour the sample into a polytetrafluoroethylene-lined reactor and crystallize at 160 oC for 120 hours.

[0034] 3. The above product is cooled, filtered, washed and dried to obtain a product sample.

[0035] The XRD of the product is shown in the attached manual figure 2 : Its XRD pattern shows ZSM-12 topological structure, and the relative intensity of characteristic peaks is B / A=1.5, C / A=4.5.

[0036]

Embodiment 3

[0038] 1. First, stir 10.380 ml of 25% TEAOH solution and 0.485 ml of water evenly, add 0.128 g of sodium metaaluminate and stir until the solid dissolves, then add 12.076 ml of 30% silica sol, and stir well to form the following mixture with molar composition: SiO 2 / Al 2 o 3 =116, OH / SiO 2 =0.245,TEA + / SiO 2 =0.245,H 2 O / SiO 2 =14.

[0039] 2. Pour the sample into a polytetrafluoroethylene-lined reactor and crystallize at 160 oC for 132 hours.

[0040] 3. The above product is cooled, filtered, washed and dried to obtain a product sample.

[0041] The XRD of the product is shown in the attached manual image 3 : Its XRD pattern shows ZSM-12 topological structure, and the relative intensity of characteristic peaks is B / A=1.4, C / A=1.4.

[0042]

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Abstract

The invention relates to a ZSM-12 molecular sieve with special crystal orientation as well as a preparation method thereof, and mainly solves the problem in the prior art that crystal orientation of the ZSM-12 molecular sieve cannot be controlled. According to the technical scheme, the ZSM-12 molecular sieve with special crystal orientation comprises SiO2 / Al2O3 which is smaller than 360, three characteristic diffraction peaks appear at 2theta: A=7.6+ / -0.2, B=20.9+ / -0.2 and C=22.6+ / -0.2 on an XRD (X-Ray Diffraction) spectrum of the ZSM-12 molecular sieve; the corresponding crystal faces are respectively (0, 0, 2), (3, 0, 0) and (0, 0, 6), the molecular sieve is preferably oriented in at least one of the three crystal face directions, and the relative intensity range is B / A=0.2-10 and C / A=0.1-10. The technical scheme well solves the technical problem, and the prepared molecular sieve can be used for various catalytic processes.

Description

technical field [0001] The invention relates to a ZSM-12 molecular sieve with specific crystal orientation and a preparation method thereof. Background technique [0002] ZSM-12 molecular sieve is a kind of high silica zeolite, which has one-dimensional linear non-intersecting channels composed of twelve-membered rings. Its channel size between medium-pore and large-pore molecular sieves can effectively realize the selection of most organic molecules. Shape catalytic conversion, ZSM-12 molecular sieve has good geothermal stability, unique pore structure and adjustable acidity. Good catalytic activity, product selectivity and catalytic stability. [0003] U.S. Patent No. 3,832,449 first disclosed the synthesis of ZSM-12 molecular sieves using tetramethylammonium or tetraethylammonium as a template. US4452769, US4537758 and literature (S. Ernst, P.A. Jacobs, J.A. Martens, J. Weitkamp, ​​Synthesis of zeolite ZSM-12 in the system (MTEA) 2 O-Na 2 O-SiO 2 -Al 2 o 3 -H 2 O,...

Claims

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Application Information

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IPC IPC(8): C01B39/42C07C15/08
Inventor 冯刚连迎迎孔德金祁晓岚
Owner CHINA PETROLEUM & CHEM CORP
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