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Preparation method of ZSM-48 molecular sieve with low silica-alumina ratio

A low-silicon-aluminum ratio, molecular sieve technology, applied in the direction of molecular sieve catalysts, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc., can solve the problems of expensive template agents, long crystallization time, etc., to shorten the crystallization time, improve Isomer selectivity, effective removal effect

Active Publication Date: 2019-10-18
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] At present, the synthesis technology of ZSM-48 molecular sieve still has the problem that the crystallization time is too long, and the synthesis of ZSM-48 with low silicon-aluminum ratio must use expensive templates.

Method used

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  • Preparation method of ZSM-48 molecular sieve with low silica-alumina ratio
  • Preparation method of ZSM-48 molecular sieve with low silica-alumina ratio
  • Preparation method of ZSM-48 molecular sieve with low silica-alumina ratio

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Weigh 2.72g of aluminum sulfate and 0.1g of sodium hydroxide, add to 30g of deionized water, stir well, add dropwise a solution of 2.1g of tetraethylammonium hydroxide, 1.3g of cyclohexylamine and 3.6g of deionized water, Stir for 1 hour, add 18 g of silica sol (solid content 41%) dropwise, stir for 2 hours to obtain a sol, transfer the mixed sol to a pressure melting bomb with a polytetrafluoroethylene liner, rotate at a speed of 10 rpm, and crystallize for 48 hours, the crystallization temperature was 140°C, and it was roasted at 550°C for 8 hours. The obtained crystallized product was analyzed by XDR to be ZSM-48 molecular sieve with a relative crystallinity of 98%.

[0064] SiO 2 / Al 2 o 3 = 30;

[0065] Templating agent / SiO 2 = 0.2;

[0066] Na 2 O / SiO 2 =0.01;

[0067] h 2 O / SiO 2 =20;

Embodiment 2

[0069] Weigh 0.49g of sodium aluminate and 0.48g of sodium hydroxide, add them to 150g of deionized water, stir evenly, add dropwise a solution of 0.25g of hexamethylammonium chloride, 5.4g of dimethylamine and 12g of deionized water, and stir for 1 hour , add 18g of white carbon black drop by drop, stir for 2 hours to obtain a sol, transfer the mixed sol to a PTFE-lined pressure melting bomb, rotate at a speed of 20 rpm, crystallize for 60 hours, and the crystallization temperature is 150°C , roasted at 560°C for 8 hours, and the obtained crystallized product was analyzed by XDR to be ZSM-48 molecular sieve, with a relative crystallinity of 99%, code Z2, and the properties of the product are shown in Table 1.

[0070] SiO 2 / Al 2 o 3 = 50;

[0071] Templating agent / SiO 2 =0.4;

[0072] Na 2 O / SiO 2 =0.02;

[0073] h 2 O / SiO 2 = 30;

Embodiment 3

[0075] Weigh 0.32g of aluminum nitrate and 1.0g of potassium hydroxide, add to 50g of deionized water, stir evenly, add dropwise a solution of 0.2g of hexamethylammonium bromide, 77.5g of di-n-propylamine and 12.3g of deionized water, and stir for 1 hour , add 18g tetraethyl orthosilicate dropwise, stir for 2h to get the sol, transfer the mixed sol to the pressure melting bomb lined with polytetrafluoroethylene, rotate at a speed of 30 rpm, crystallize for 60 hours, and the crystallization temperature is Calcined at 160°C and 570°C for 8 hours, the obtained crystallized product was analyzed by XDR to be ZSM-48 molecular sieve, with a relative crystallinity of 100%, code number Z3, and the properties of the product are shown in Table 1.

[0076] SiO 2 / Al 2 o 3 = 101;

[0077] Templating agent / SiO 2 = 2.5;

[0078] Na 2 O / SiO 2 = 0.1;

[0079] h 2 O / SiO 2 =40

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Abstract

The invention provides a preparation method of a ZSM-48 molecular sieve with low silica-alumina ratio. The method utilizes a dual template agent to synthesize the ZSM-48 molecular sieve with low silica-alumina ratio at low cost, compared with the existing preparation method of ZSM-48 molecular sieve with low silica-alumina ratio, by adopting the dual template agent, the method shortens the crystallization time while lowering the template agent cost, efficiently synthesizes the pure phase ZSM-48 molecular sieve with high crystallinity and low silica-alumina ratio, at the same time achieves easier and effective removal of the template, increases the specific surface area, pore volume, pore diameter and acid content of the molecular sieve, can realize more effective hydroisomerization reaction, and improves the isomerization selectivity. The molecular sieve has high application value and prospect in the hydroisomerization dewaxing field.

Description

technical field [0001] The invention relates to a low-cost and high-efficiency preparation method for synthesizing low-silicon-aluminum ratio ZSM-48 molecular sieves. It belongs to the technical field of catalysts. Background technique [0002] In 1981, Schlenker first discovered the fibrous rod-shaped ZSM-48 molecular sieve. The ZSM-48 molecular sieve is a molecular sieve with a one-dimensional ten-ring channel structure, and the pore size is 0.56nm×0.56nm. Raul proposed that ZSM-48 molecular sieve is not the name of a material, but represents a series of materials with similar pore structures. Experiments have found that the pore structure of molecular sieves is disordered and contains at least nine topological structures. The suitable pore structure and acidity of ZSM-48 molecular sieve make it have good isomerization selectivity in the hydroisomerization of long-chain alkanes, and can be used to prepare lubricating oil isomerization dewaxing catalysts in the reaction of...

Claims

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Application Information

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IPC IPC(8): C01B39/48B01J29/70B01J35/10
CPCC01B39/48B01J29/703C01P2006/12C01P2006/14C01P2006/16B01J35/633B01J35/647B01J35/615
Inventor 于宏悦江路明李梦晨孟祥彬高善彬崔岩刘彦峰迟克彬王晓化沈宜泓沈雨歌路明霄
Owner PETROCHINA CO LTD
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