Preparation method of small-crystalline-grain ZSM-22 (Zeolite Socony Mobil-22) molecular sieve

A technology of ZSM-22 and molecular sieve, which is applied in the field of TON topological structure, can solve the problems of increased catalyst activity, organic solvent and acid-base solution increase waste liquid treatment process and difficulty, and high treatment cost, so as to achieve high catalytic activity and good catalytic application Prospects, low-cost effects

Active Publication Date: 2016-05-11
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although these three methods can effectively prepare mesoporous-microporous zeolite molecular sieves, the use of organic solvents and acid-base solutions greatly increases the process and difficulty of waste liquid treatment, making the treatment cost high. In addition, ultrason

Method used

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  • Preparation method of small-crystalline-grain ZSM-22 (Zeolite Socony Mobil-22) molecular sieve
  • Preparation method of small-crystalline-grain ZSM-22 (Zeolite Socony Mobil-22) molecular sieve
  • Preparation method of small-crystalline-grain ZSM-22 (Zeolite Socony Mobil-22) molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0027] First, mix the raw materials uniformly according to the following molar ratio, silica sol (in the form of SiO 2 In terms of): aluminum sulfate (as Al 2 o 3 Total): 1,6-hexanediamine: potassium hydroxide: deionized water = 1: 0.011: 0.005: 0.29: 40. Then, add 0.5g activated carbon (with SiO 2 The mass ratio is 0.06:1), adding ZSM-22 powder (addition amount is 10% of SiO2 mass). Stir well. Finally, the mixed raw materials were transferred to a stainless steel reaction kettle, and dynamically crystallized at 160°C for 48 hours. The product was filtered, washed, dried, and roasted at 550°C for 16 hours to obtain ZSM-22 molecular sieve with small grains, the grain length was ~200nm, and the product The XRD and SEM spectra are shown in figure 2 .

Embodiment 2-8

[0029] The specific proportions of ingredients and crystallization conditions are shown in Table 1, and the specific preparation process is the same as in Example 1. Wherein, the seed crystal added in embodiment 2 is the stock solution containing ZSM-22 seed crystal, and the addition amount is SiO 2 0.1% of mass. The seed crystal added in embodiment 3 is the original powder of ZSM-22, and the addition amount is SiO 2 10% of the mass. Examples 4-9, no seed crystals were added.

Embodiment 4-9

[0029] The specific proportions of ingredients and crystallization conditions are shown in Table 1, and the specific preparation process is the same as in Example 1. Wherein, the seed crystal added in embodiment 2 is the stock solution containing ZSM-22 seed crystal, and the addition amount is SiO 2 0.1% of mass. The seed crystal added in embodiment 3 is the original powder of ZSM-22, and the addition amount is SiO 2 10% of the mass. Examples 4-9, no seed crystals were added.

[0030] The synthetic samples were analyzed by XRD, and the data results were compared with figure 1 close, indicating that the synthesized product is a high-purity ZSM-22 molecular sieve. SEM analysis of the synthesized samples shows that the products are all small-grained molecular sieves with a length ≦220nm.

[0031] Table 1 Molecular sieve synthesis ingredients and crystallization, roasting conditions

[0032]

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Abstract

The invention discloses a preparation method of a small-crystalline-grain ZSM-22 (Zeolite Socony Mobil-22) molecular sieve. The preparation method comprises the following steps of uniformly mixing a silicon source, a aluminum source, an alkali source, a templating agent and deionized water, to form an initial gel mixture, and then adding one or several of active carbon, graphite, graphene, black carbon, a starch microsphere, chitosan and a polylactic acid microsphere into the initial gel mixture, uniformly agitating an obtained mixture, and then crystallizing the agitated mixture, filtering to separate a solid product, washing the solid product to be neutral by using the deionized water, and drying and roasting the washed solid product, to obtain the small-crystalline-grain ZSM-22 molecular sieve. The preparation method has the advantages that the activity of a catalyst is high; the large-scale industrial production can be realized; the operation charge is low.

Description

[0001] Field [0002] The invention relates to a preparation method of a small-grain ZSM-22 silicon-aluminum molecular sieve. Background technique [0003] ZSM-22 molecular sieve is a microporous, high-silicon molecular sieve developed by Mobil Corporation of the United States in the late 1980s, which belongs to the TON topology. It only has one-dimensional channels opened by ten-membered rings, the size of the pores is 0.44nm×0.55nm, the size of the pores is relatively small, and there is no intersecting pores. Because ZSM-22 molecular sieve has a relatively suitable pore structure and acidic properties, it has good catalytic performance in the isomerization reaction of n-paraffins, and has been obtained in the petrochemical field, especially in the isomerization dewaxing of lubricating oil base oils. widely used. [0004] The main component of wax in lubricating base oil is long-chain normal alkanes with high melting point, which has high pour point and poor low temperatur...

Claims

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Application Information

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IPC IPC(8): C01B39/04B82Y30/00
CPCC01B39/04C01P2002/72C01P2004/03C01P2004/62C01P2004/64
Inventor 李德宝郗宏娟侯博林明桂贾丽涛
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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