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Nano MFI/MOR eutectic molecular sieve and synthesis method of nano Ti-MFI/MOR eutectic molecular sieve

A synthesis method and molecular sieve technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolite, etc. low cost effect

Active Publication Date: 2022-02-11
格润科技(大连)有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above-mentioned patented technologies and articles are only researched on a single TS-1 titanium silicalite molecular sieve or a single Ti-MOR titanium silicalite molecular sieve
However, there are few studies on the synthesis method and catalytic performance of eutectic Ti-MFI / MOR molecular sieves with both MFI and MOR topological structures, especially nano-Ti-MFI / MOR eutectic molecular sieves.

Method used

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  • Nano MFI/MOR eutectic molecular sieve and synthesis method of nano Ti-MFI/MOR eutectic molecular sieve
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1: synthetic MFI / MOR eutectic molecular sieve

[0039] Step (1): Synthesis of Zeolite Seed Crystals

[0040] Add 290g of deionized water and 210g of tetrapropyl ammonium hydroxide (25wt%) into a plastic beaker in turn, and after stirring evenly, add 150g of tetraethyl orthosilicate under stirring, then stir and age at room temperature for 3 hours to obtain mixture 1, mixture 1 The initial material composition is SiO 2 :TPAOH:H 2 O=1:0.36:35 (molar ratio); the mixture 1 was transferred to a hydrothermal synthesis kettle, and crystallized at 140° C. for 10 h to obtain zeolite seed crystals.

[0041] Step (2): Synthesis of MFI / MOR co-crystal molecular sieves

[0042] Add 462g of deionized water and 44.0g of sodium hydroxide into the plastic beaker in turn, after stirring evenly, add 18.0g of sodium aluminate under stirring state, after stirring until clarified, add 420g of silica sol (30wt%), the sol composition is SiO 2 : NaO 2 :Al 2 o 3 :H 2 O=1:0.3:0....

Embodiment 2

[0043] Embodiment 2 synthesizes Ti-MFI / MOR zeolite molecular sieve

[0044] Take 10 g of the MFI / MOR eutectic molecular sieve synthesized in Example 1, reflux for 10 h in an aqueous solution of nitric acid (6 ml / L) with a solid-to-liquid ratio of 1:10, filter and wash until neutral, and dry at 80 ° C for 12 h to obtain dealuminated Sample: Place the sample in a quartz reaction tube, dehydrate and activate it at 400°C for 2h under a nitrogen atmosphere, then treat it with TiCl steam for 4h, then blow it with nitrogen for 1h, cool to room temperature, wash with deionized water, and dry at 110°C 12h, get the Ti-MFI / MOR eutectic molecular sieve sample, marked as 1#, 1# sample XRD peak figure 1 , which is the eutectic topological structure of MFI and MOR; see the SEM photo figure 2 , showing that the obtained Ti-MFI / MOR zeolite molecular sieve particle size is 80-160nm, and the silicon-titanium ratio is 41 according to XRF analysis.

Embodiment 3

[0045] Embodiment 3 synthesis Ti-MFI / MOR zeolite molecular sieve

[0046] The raw materials and synthesis steps are the same as in Example 2, except that the crystallization temperature in the step (1) of synthesizing the MFI / MOR eutectic molecular sieve is changed to 130°C to obtain a Ti-MFI / MOR zeolite molecular sieve sample, marked as 2 #. According to XRD test and analysis, the crystal phase is MFI / MOR eutectic molecular sieve; after SEM characterization, the particle size of Ti-MFI / MOR zeolite molecular sieve is 60-110nm, and the silicon-titanium ratio is 38 according to XRF analysis.

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Abstract

The invention relates to a synthesis method of a nano MFI / MOR eutectic molecular sieve and a nano Ti-MFI / MOR eutectic molecular sieve. The synthesis method of the nano MFI / MOR eutectic molecular sieve comprises the following steps: (1) mixing a silicon source, a template agent and water, aging and carrying out hydrothermal crystallization to obtain zeolite seed crystals; and (2) mixing a silicon source, an aluminum source, an alkali source and water to form sol, adding the zeolite seed crystals, aging, carrying out hydrothermal crystallization, and carrying out solid-liquid separation, washing, drying and roasting on mother liquor after crystallization to obtain the nano MFI / MOR eutectic molecular sieve; subjecting the nano MFI / MOR eutectic molecular sieve to acid pickling, water washing, drying and roasting so as to obtain an aluminium-removed nano MFI / MOR eutectic molecular sieve; and carrying out gas-solid phase isomorphous substitution on the aluminium-removed nano MFI / MOR eutectic molecular sieve and titanium tetrachloride to obtain the nano Ti-MFI / MOR eutectic molecular sieve. The nano Ti-MFI / MOR eutectic molecular sieve synthesized by the method disclosed by the invention is low in cost and small in grain size (60-190 nm), shows excellent catalytic performance in the reaction of catalyzing ammoxidation of cyclohexanone to prepare cyclohexanone-oxime and hydroxylation of phenol to prepare benzenediol, and has great industrial application potential.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve synthesis, and in particular relates to a method for synthesizing a nanometer MFI / MOR eutectic molecular sieve and a nanometer Ti-MFI / MOR eutectic molecular sieve. Background technique [0002] Titanium silicalite molecular sieve (TS-1) is a molecular sieve containing titanium (Ti) heteroatoms. In 1983, US Patent 4410501 reported its synthesis method for the first time. The Ti atoms on the TS-1 zeolite molecular sieve replace the silicon or aluminum atoms in the zeolite molecular sieve framework to form a four-coordinate titanium framework, which makes the TS-1 zeolite molecular sieve have excellent selective oxidation activity. The oxidation system composed of TS-1 zeolite molecular sieve and hydrogen peroxide shows good application prospects in the oxidation of olefins, hydroxylation of aromatic hydrocarbons, ammoxidation of ketones, partial oxidation of alkanes and selective oxidation o...

Claims

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Application Information

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IPC IPC(8): C01B39/02
CPCC01B39/023C01P2002/72C01P2004/03Y02P20/52
Inventor 马楠
Owner 格润科技(大连)有限责任公司
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