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Synthesis method of ZSM-48 molecular sieve

A technology of ZSM-48 and synthesis method, which is applied in the field of molecular sieve synthesis technology, to achieve the effects of shortening the crystallization time, saving synthesis cost, and reducing synthesis cost

Inactive Publication Date: 2013-01-16
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the published patent, there is no introduction about the recycling of ZSM-48 mother liquor

Method used

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  • Synthesis method of ZSM-48 molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] At initial gel ratio 600SiO 2 :Al 2 o 3 :18Na 2 O:240SDA:4000H 2 O Mix the metering raw materials in order, wherein the silicon source is fumed silica, the aluminum source is aluminum sulfate octadecadecahydrate, the alkali source is sodium hydroxide, and the template agent is hexamethylenediamine. Stir fully to form a gel, and then put it into a poly In the tetrafluoroethylene-lined autoclave, the crystallization temperature was set at 160°C, and the constant temperature crystallization was carried out for 72h. The solid product was separated, the mother liquor was recovered, the solid product was washed with deionized water until it was neutral, and dried in an air atmosphere at 85°C for 24 hours to obtain the original ZSM-48 molecular sieve powder, labeled as ZSM-48-1. The X-ray diffraction analysis results are as shown in the accompanying drawings, and its relative crystallinity is determined as 100%.

Embodiment 2

[0030] The mother liquor obtained in embodiment 1 is fully utilized, and the mother liquor is analyzed to obtain SiO 2 、Al 2 o 3 , SDA, Na 2 The corresponding content of O. The synthesis steps in Example 1 were repeated to obtain ZSM-48-2. The obtained mother liquor was then analyzed, and the synthesis steps were repeated to obtain ZSM-48-3. In this way, ZSM-48-4, ZSM-48-5, and ZSM-6 are obtained. The crystallinity of all obtained ZSM-48 series molecular sieves is shown in the table below. It can be found that the ZSM-48 molecular sieve synthesized after circulating the mother liquor for six times still maintains good crystallinity, and there is no impurity phase in the product.

[0031] Table 1 The relative crystallinity of ZSM-48 molecular sieve synthesized by recovery of mother liquor

[0032] sample

Embodiment 3

[0034] At initial gel ratio 400SiO 2 :60Na 2 O:400HDA:20000H 2 O Mix the metering raw materials in order, wherein the silicon source is fumed silica, the alkali source is potassium hydroxide, the template is pentamethylenediamine, and the aluminum source is not added, fully stirred into a gel, and then loaded into a polytetrafluoroethylene In the lined high-pressure reactor, the crystallization temperature was set at 160°C, and the constant temperature crystallization was carried out for 72h. The solid product was separated, the mother liquor was recovered, the solid product was washed with deionized water until neutral, and dried in an air atmosphere at 85°C for 24 hours to obtain the original ZSM-48 molecular sieve powder, whose relative crystallinity was 104%, and still maintained good crystallization The degree shows that high-quality pure silicon ZSM-48 molecular sieves can be synthesized under the selected conditions.

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Abstract

The invention discloses a utilization method of a ZSM-48 molecular sieve and relates to the technical field of synthesis of molecular sieves. The method comprises the following steps: crystallizing the ZSM-48 molecular sieve and separating to obtain mother liquid for recycling; utilizing all or part of the mother liquid; using the mother liquid as one part of the synthesis raw materials of the ZSM-48 molecular sieve; and correspondingly replenishing fresh raw materials according to the synthesis proportioning to prepare and synthesize a gel mixture of the ZSM-48 molecular sieve for the next step of synthesis so as to recycle the mother liquid of the molecular sieve. By the utilization method of the mother liquid of the molecular sieve, the utilization ratio of a template agent in the synthesis process of the molecular sieve can be increased, the time of the crystallization in the next step is shortened due to a large amount of ZSM-48 molecular sieve microcrystal in the mother liquid, and wastewater pollution in the production process of the molecular sieve is reduced due to recycling of the mother liquid.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve synthesis, and relates to a method for utilizing ZSM-48 molecular sieve mother liquor. The mother liquor obtained after crystallization of ZSM-48 molecular sieve is reused, and a certain amount of mother liquor is put in according to the content of each component in the mother liquor. , combined with the ratio of raw materials synthesized by molecular sieves to supplement fresh raw materials, and prepare the gel mixture for synthesizing ZSM-48 molecular sieves for molecular sieve synthesis, so as to achieve the purpose of mother liquor recycling. Background technique [0002] ZSM-48 zeolite is a new type of molecular sieve with high silicon-aluminum ratio developed by Mobil Company in the United States in the early 1980s. ZSM-48 is a zeolite with orthorhombic or pseudoorthorhombic symmetry with ten-membered ring linear channels, which shows that ZSM-48 is likely to be a member of the Penta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 梁长海张淼汪镭
Owner DALIAN UNIV OF TECH
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