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A kind of square β molecular sieve and preparation method thereof

A beta molecular sieve and square technology, which is applied in the field of in-situ crystallization and synthesis of square beta molecular sieve, can solve the problems of aluminum loss, little activation of silicon oxide, environmental pollution of waste acid liquid, etc., and achieves loose framework, low cost, and reduction of raw materials. cost effect

Active Publication Date: 2015-10-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, soaking in acid will cause a large amount of loss of aluminum and has little activation effect on silicon oxide, and how to deal with the soaked acid solution has not been elaborated, a large amount of waste acid solution will pollute the environment, and the patent does not have The morphology of the β molecular sieve synthesized by this method is described. After analysis, the morphology of the β molecular sieve synthesized by this method is the same as that of the β molecular sieve synthesized by the general method, that is, the conventional ellipsoidal particles

Method used

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  • A kind of square β molecular sieve and preparation method thereof
  • A kind of square β molecular sieve and preparation method thereof
  • A kind of square β molecular sieve and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0056] Using commercially available montmorillonite as raw material, take the purified montmorillonite, and mix the montmorillonite with NaOH, K 2 CO 3 , TEAOH mixed alkali solution (NaOH, K in the alkali solution 2 CO 3 , TEAOH mass fractions were 15%, 10% and 5%) at room temperature for 1 h, washed, dried, pulverized to 7 μm, and baked in a muffle furnace at 700 °C for 4 h at a heating rate of 5 °C / min. Prepared activated montmorillonite.

Embodiment 2

[0058] Using commercially available montmorillonite as raw material, take the purified montmorillonite, and mix the montmorillonite in a mixed alkali solution composed of NaOH, KOH, and TEAOH (NaOH, KOH, TEAOH in the alkali solution The mass fractions were 10%, 5% and 5% respectively) at 50 °C for 2 h, washed, dried, pulverized to 10 μm, and baked at 850 °C in a muffle furnace at a heating rate of 10 °C / min for 2 h. Get activated montmorillonite.

Embodiment 3

[0060] 30 g of activated montmorillonite in Example 1 was soaked in 60 mL of tetraethylammonium hydroxide with a weight concentration of 25 wt% at 60 °C for 5 h. Then 1.5 g of sodium hydroxide, 0.5 g of sodium chloride, 1.5 g of potassium chloride, 30 mL of distilled water, 40 mL of tetraethylammonium hydroxide with a concentration of 25 wt%, 30 g of white carbon black, and 70 Stirred at ℃ for 4 h to make the mixture gel. The gel was transferred to a stainless steel reactor for static crystallization at 140 °C for 48 h. After the crystallization is completed, cool, filter and separate from the mother liquor, wash and dry the filter cake to obtain a crystallized product. According to X-ray measurement, its phase belongs to β molecular sieve, the relative crystallinity of square β molecular sieve in the product is 80%, and the crystal grain of molecular sieve reaches 80~120 nm. The single-pot yield reached over 70 wt%.

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Abstract

The invention relates to a square beta molecular sieve and a preparing method thereof. According to the method, cheaper natural mineral montmorillonoid with wider raw material source is adopted as a synthesis raw material, so that the purpose of low-cost synthesis of square beta molecular sieves is realized. Crystalline grains of the square beta molecular sieve are mostly and basically cuboid, and accordingly the beta molecular sieve with the form is outstanding in diffusion performance.

Description

technical field [0001] The invention belongs to molecular sieve and its preparation technology. Specifically, it relates to a method for synthesizing square β molecular sieves through in-situ crystallization by using natural mineral montmorillonite to provide all or part of the aluminum source and part of the silicon source required for the synthesis of square β molecular sieves. Background technique [0002] β molecular sieve was first synthesized in 1967 by Wadlinger of Mobil Corporation of the United States by the classic hydrothermal crystallization method (US3308069). Since the silicon source used is silica sol, which has a large water content, the dosage of template agent is relatively large, resulting in high production cost of β molecular sieve. At the same time, due to the large volume of the entire reaction solution and the long crystallization time, problems such as low production efficiency are brought about, which are unfavorable for large-scale industrial prod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/48
Inventor 徐志扬凌凤香
Owner CHINA PETROLEUM & CHEM CORP
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