ZSM-48/Silicalite-1 composite molecular sieve and preparation method thereof

A technology of ZSM-48 and composite molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of expensive hexamethylenediamine chloride, easy carbon deposition, unfavorable long-term operation of catalyst, etc., achieve suitable pore volume, improve acid Quantity, the effect of inhibiting side effects

Active Publication Date: 2015-03-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the application process, it was found that ZSM-48 molecular sieve is very easy to deposit carbon, which is not conducive to the long-term operation of the catalyst, and the template agent hexamethylenediamine chloride used is also relatively expensive

Method used

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  • ZSM-48/Silicalite-1 composite molecular sieve and preparation method thereof
  • ZSM-48/Silicalite-1 composite molecular sieve and preparation method thereof
  • ZSM-48/Silicalite-1 composite molecular sieve and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh sodium hydroxide and sodium aluminate (Al 2 o 3 , 43wt%; Na 2 O, 38wt%) was dissolved in deionized water, and then the templating agent R (12-crown-4, content >97%) was added while stirring at a water bath temperature of 60°C, and after stirring for 0.5 hours, white carbon black was added, After stirring for 1 hour, add ZSM-48 seed crystal S, continue stirring for 2 hours, and then move to a closed stainless steel reaction kettle. Crystallized at 160°C for 6 days to obtain ZSM-48 molecular sieve with low silicon-aluminum ratio (D1-ZSM-48). See Table 1 for the specific raw material ratio and product properties.

Embodiment 2

[0026] Weigh sodium hydroxide and sodium aluminate (Al 2 o 3 , 43wt%; Na 2 O, 38wt%) was dissolved in deionized water, and then the templating agent R (12-crown-4, content >97%) was added while stirring at a water bath temperature of 60°C, and after stirring for 0.5 hours, white carbon black was added, After stirring for 1 hour, add ZSM-48 seed crystal S, continue stirring for 2 hours, and then move to a closed stainless steel reaction kettle. Crystallized at 158°C for 8 days to obtain a ZSM-48 molecular sieve (D2-ZSM-48) with a low silicon-aluminum ratio. The specific raw material ratio and product properties are shown in Table 1.

Embodiment 3

[0028] Weigh sodium hydroxide and TPABr and dissolve them in deionized water, then add D1-ZSM-48 molecular sieve while stirring at room temperature, stir for 0.5 hours, then add white carbon black, stir for 0.5 hours, then move the reaction mixture gel to an airtight In a stainless steel reaction kettle, crystallize at 140°C for 12 hours, and the crystallized product is washed, centrifuged, dried, and roasted to obtain ZSM-48 / Silicalite-1 composite molecular sieve. The specific raw material ratio and product properties are shown in Table 2.

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Abstract

The invention discloses a ZSM-48 / Silicalite-1 composite molecular sieve and a preparation method thereof, the composite molecular sieve takes the ZSM-48 molecular sieve with low silica-alumina ratio as a shell phase, and takes Silicalite-1 as a core layer, total specific surface area of the composite molecular sieve is 330-400m<2> / g, the total pore volume is 0.22-0.28ml / g, average aperture is 2.5-3.5nm, by measuring gross weight of the composite molecular sieve, the shell layer content is 10-70%; wherein, mol ratio of silicon oxide of the ZSM-48 molecular sieve with low silica-alumina ratio to alumina is 25-50. The preparation method comprises the following steps: uniformly mixing the ZSM-48 molecular sieve with low silica-alumina ratio, sodium hydroxide, a template and water, adding silicon source to prepare a reaction mixture gel system, crystallizing the reaction mixture gel, separating the crystallization products, drying, and roasting to obtain the ZSM-48 / Silicalite-1 composite molecular sieve. The composite molecular sieve has good shape-selecting performance and anti-carbon deposition capability, and has latent industrial application value in alkylation and isomerization reactions.

Description

technical field [0001] The invention relates to a composite molecular sieve and a preparation method thereof, in particular to a ZSM-48 / Silicalite-1 composite molecular sieve and a preparation method thereof. Background technique [0002] In 1983, the patent US4397827 reported the synthesis of ZSM-48 molecular sieve for the first time. ZSM-48 molecular sieve is a molecular sieve with a ten-ring pore structure with a pore size of 0.53nm×0.56nm. It is an important isomerization catalytic material. In US7482300B2 and US7625478B2, it is described that ZSM-48 molecular sieve is used in the reaction process of C10 hydroisomerization. Under the condition that the conversion rate reaches 90%, the isomer product yield reaches more than 80%, showing good isomerization structural performance. [0003] At present, the research focus of ZSM-48 molecular sieve is still on its synthesis process. The synthesis process of this molecular sieve has the following characteristics: (1) The sili...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 秦波尹泽群宋喜军刘全杰
Owner CHINA PETROLEUM & CHEM CORP
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