Method for preparing nano molecular sieve

A nano-scale molecular sieve and a synthesis method technology are applied in the field of nano-scale molecular sieve preparation, which can solve the problems of reducing water content and failing to synthesize nano-scale beta zeolite, and achieve the effect of avoiding the increase of crystal grains.

Active Publication Date: 2008-05-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method overcomes the shortcomings of the above methods, reduces the water content, and at the same time reduces the amount of template agent to a large extent, saving costs, but fails to synthesize nano-sized zeolites, and is limited to the synthesis of small-grained molecular sieves

Method used

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  • Method for preparing nano molecular sieve
  • Method for preparing nano molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] According to 0.02Al 2 o 3 : 1.0 SiO 2 : 0.08NH 4 HF 2 :0.06TMAOH:3H 2 O: 0.3C 2 h 5 The molar ratio of OH, 208g treated silica sol (200g of 408g 28wt% silica sol deep dehydration), 9.1g NH 4 HF 2 , 6.6gNaAlO 2 , 11gTMAOH, 15gH 2 O and 28gC 2 h 5 Mix OH with mechanical stirring (4000r / min) at room temperature, and continue to stir until the raw materials are evenly mixed to obtain a white sol-like silica-alumina gel. Mix 13.9g of second-line distillate oil and 0.5g of polyisobutylene triethanolamine maleate under mechanical stirring at 90°C and 4000r / min, then drop in 277.7g of silica-alumina gel, and stir until the raw materials are evenly mixed to obtain Stable hypersolubilized micelle system. Transfer to an autoclave, seal and crystallize statically at 140°C for 30 hours. The product was centrifuged, washed to neutral, dried at 110°C, calcined at 250°C for 2 hours, and then heated to 350°C for 5 hours to obtain a molecular sieve sample. Characterized by...

Embodiment 2

[0041] According to 1.0SiO2 2 : 0.02NH 4 F: 0.07 (C 2 h 5 ) 3 N:5H 2 0: The mol ratio of 0.5 ethylene glycol, 208g ethyl orthosilicate, 0.8g ammonium fluoride, 6.1g triethylamine, 54g water and 31g ethylene glycol are mixed under the mechanical stirring of 800rpm rotating speed at room temperature, and Continue to stir until the raw materials are evenly mixed to obtain white sol-like silica-alumina gel. 21.4g of the third-line distillate oil, 4.3g of polyisobutenyl diethylene glycol maleate and 4.3g of polyoxyethylene lauryl ether (10) were mixed under mechanical stirring at 90°C and 800rpm, and then slowly added 300g Silica-alumina gel, and stir until the raw materials are evenly mixed to obtain a stable supersolubilized micelle system. Transfer to an autoclave, seal and crystallize statically at 140°C for 30 hours. The product was characterized by XRD, BET and TEM after being treated as in Example 1. The characterization results show that the product Silicalite-1 is ...

Embodiment 3

[0043] According to 0.04Al 2 o 3 : 1SiO 2 :0.04KOH:0.05TPABr:2H 2 The molar ratio of O: 0.3 diethylene glycol, 120g white carbon black, 7.8g pseudo-boehmite, 2.7gTPABr, 4.5g KOH, 72gH 2 O and 63g of diethylene glycol were mixed at room temperature with mechanical stirring (rotating speed 1500rpm), and continued to stir until the raw materials were uniformly mixed to obtain white sol-like silica-alumina gel. Mix 33.8g of four-line distillate oil, 13.5g of SP-80 and 6.75g of lecithin at 90°C and 1000rpm under mechanical stirring, then slowly add 270g of silica-alumina gel and stir until the raw materials are evenly mixed to obtain a stable Hypersolubilized micellar system. Transfer to an autoclave, seal and crystallize statically at 120°C for 30 hours, calcine at 250°C for 3 hours, and then heat up to 350°C and calcine for 7 hours to obtain a molecular sieve sample. XRD, BET and TEM characterizations were carried out. The characterization results show that the product is a...

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Abstract

The invention discloses a preparation method of nanometer molecular sieve. The method is to firstly mix hydrocarbon components and surfactants evenly, then add silica gel and silica-alumina gel, and continue to stir until the raw materials are evenly mixed to obtain a super-solubilizing system of oil-in-melt, and then undergo crystallization, drying and roasting Finally, nano molecular sieves are obtained. The crystallization of the molecular sieve in the present invention is carried out in a supersolubilized micelle system of molten silica gel or silica-alumina gel in oil, and the growth of the molecular sieve crystal is limited in the nano-micelle to avoid excessive growth of the molecular sieve crystal. The surfactant and hydrocarbon components used in the method of the invention are used in small amounts and low in cost. The method has a simple process and can be used for large-scale industrial production.

Description

technical field [0001] The invention relates to a molecular sieve composition and a preparation method. In particular, it relates to a nanoscale molecular sieve preparation method. Background technique [0002] In the past ten years, the synthesis of nano-scale molecular sieves has been quite active, which is mainly due to the completely different properties of nano-scale molecular sieves and micro-scale molecular sieves. When the particle size of molecular sieve crystals is reduced from micrometer to nanometer, its mass transfer, heat transfer and other properties related to molecular sieve adsorption and catalysis will change. The nano-scale molecular sieve catalysts show better activity, selectivity and anti-coking ability in some hydrocarbon catalytic conversion reactions. The reactions that have used nano molecular sieves as catalysts so far include: hydrocracking, fluidized catalytic cracking, alkylation of benzene, oligomerization of olefins, methanol to gasoline, s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04C01B37/00B82B3/00
Inventor 王鼎聪孙万富
Owner CHINA PETROLEUM & CHEM CORP
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