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Method for preparing beta-molecular sieve from oil shale waste

A technology of β molecular sieve and oil shale slag, which is applied in the field of in-situ crystallization to synthesize β molecular sieve, which can solve the problems of ineffective use of aluminum elements, large energy consumption, and high requirements for containers, and achieve low cost, large external area, and diffusion long range short effect

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the aluminum element in oil shale slag has not been effectively utilized, and NaOH is contained in the second calcination activation, NaOH is very corrosive, and the requirements for containers are also high.
[0008] CN101723397A provides a method for preparing 13X zeolite molecular sieve with oil shale ash residue. The method pulverizes the ash residue, calcines at high temperature, and then dissolves aluminum and silicon elements with acid and alkali respectively to prepare sodium metaaluminate solution and water Glass solution; then use sodium metaaluminate solution and water glass solution as raw materials to synthesize 13X zeolite molecular sieve; Alkaline solid residues are generated during the solution process, and the treatment of alkaline solid residues is not mentioned, which will pollute the environment

Method used

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  • Method for preparing beta-molecular sieve from oil shale waste
  • Method for preparing beta-molecular sieve from oil shale waste

Examples

Experimental program
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Effect test

Embodiment 1

[0053] Using oil shale slag as raw material, according to the liquid-solid ratio of 10mL / g, the oil shale slag was mixed 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, crushed to 7 μm, and roasted at 800 °C in a muffle furnace at a heating rate of 5 °C / min for 4 h to obtain Activate oil shale residue.

Embodiment 2

[0055] Using oil shale slag as raw material, according to the liquid-solid ratio of 10mL / g, put oil shale slag in a mixed alkali solution composed of NaOH, KOH, and TEAOH (the mass fractions of NaOH, KOH, and TEAOH in the alkali solution are respectively 10% , 5% and 5%) at 50°C for 2 h, washed, dried, crushed to 10 μm, and roasted in a muffle furnace at 850°C for 2 h at a heating rate of 10°C / min to obtain activated oil shale slag.

Embodiment 3

[0057] Soak 20 g of the activated oil shale slag of Example 1 in 40 mL of tetraethylammonium hydroxide with a weight concentration of 25 wt % at 60° C. for 5 h. Then put 1.0g of sodium hydroxide, 0.3g of sodium chloride, 1.0g of potassium chloride, 20mL of distilled water, 30mL of tetraethylammonium hydroxide with a concentration of 25wt%, and 25g of white carbon black into a beaker and stir at 70°C. 4h 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 β molecular sieve in the product is 80%, and the crystal grain of molecular sieve reaches 80~120nm. The single-pot yield reaches more than 70wt%.

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Abstract

The invention discloses a method for preparing a beta-molecular sieve from oil shale waste. The method comprises the following steps: (1) performing alkaline treatment on the oil shale waste, roasting, and adding the roasted product into a template water solution to be soaked; (2) adding a silicon source, an aluminium source, alkali, water and a template into a material obtained in the step (1), and mixing to obtain a gel material; (3) performing hydrothermal crystallization on the gel material obtained in the step (2), washing and drying to obtain the product, namely the beta-molecular sieve. According to the method, the oil shale waste which is low in cost is used as a synthetic raw material, so that the purpose that the beta-molecular sieve is synthetized at low cost is realized, and the method has a wide application range in the field of synthesis of the molecular sieve.

Description

technical field [0001] The invention belongs to molecular sieve and its preparation technology. Specifically, it relates to a method for synthesizing a β molecular sieve through in-situ crystallization by using oil shale slag to provide all or part of the aluminum source and part of the silicon source required for the synthesis of a β molecular sieve. 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 with high water content, the amount of template agent is 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 production. US5164170 adopts mixed template agent (q...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48B01J29/78
Inventor 徐志扬凌凤香王少军
Owner CHINA PETROLEUM & CHEM CORP
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