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Preparation method of MWW structure molecular sieve

A molecular sieve and slurry technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of miscellaneous crystal formation, impurity accumulation, high energy consumption, etc., and achieve the effect of reducing the probability of miscellaneous crystal formation and avoiding environmental pollution

Inactive Publication Date: 2016-07-13
CHINA PETROLEUM & CHEM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, excessive reuse of the mother liquor will often lead to the accumulation of impurities, which will adversely affect the crystallization process and easily lead to the formation of miscellaneous crystals; recovery methods such as flash evaporation are high in energy consumption, and cannot completely recover the hexamethylene methylene in the wastewater. Amines, so it is not an ideal way to recover the mother liquor template

Method used

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  • Preparation method of MWW structure molecular sieve

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preparation example Construction

[0017] The present invention provides a kind of preparation method of molecular sieve of MWW structure, and this method comprises the following steps:

[0018] (1) Mix silicon source, aluminum source, alkali agent, templating agent and water, crystallize the glue solution obtained after mixing, and then cool to obtain a layered system in which the upper layer is an organic phase and the lower layer is a molecular sieve slurry, wherein , the template contains hexamethyleneimine and aniline;

[0019] (2) separating the layered system to obtain an organic phase and a molecular sieve slurry;

[0020] (3) The molecular sieve slurry is filtered, the obtained filter cake is washed, dried and roasted successively, and the obtained filtrate is distilled or rectified to reclaim the azeotrope of hexamethyleneimine and water and aniline Azeotrope with water.

[0021] In the present invention, the aluminum source can be various conventional soluble aluminum salts used in the preparation ...

Embodiment 1

[0059] This example is used to illustrate the preparation method of the molecular sieve with MWW structure of the present invention.

[0060] In the reaction unit R, dissolve a certain amount of sodium metaaluminate and sodium hydroxide in deionized water, stir until completely dissolved, then add solid silica gel, then add an appropriate amount of hexamethyleneimine and aniline, and stir evenly , the amount of the above raw materials is such that in the obtained glue, the molar ratio of sodium hydroxide, silicon source, aluminum source, HMI, AN and water is 0.18:1:0.033:0.10:0.20:15. The glue solution was crystallized at 145° C. and autogenous pressure for 72 hours at a stirring speed of 24 revolutions per minute. Then, the temperature was lowered to 20° C. with cooling water, and the stirring was stopped for 5 minutes to obtain a layered system in which the upper layer was the organic phase and the lower layer was the molecular sieve slurry.

[0061] Turn on the reaction un...

Embodiment 2

[0065] This example is used to illustrate the preparation method of the molecular sieve with MWW structure of the present invention.

[0066] According to the method of Example 1, the raw materials are mixed, crystallized and cooled in the reaction unit R, the difference is that the washing water in Example 1 is used as the water source, and the mixture recovered in the template storage tank C2 of Example 1 is used As a template, the amount of raw materials used is such that the molar ratio of sodium hydroxide, silicon source, aluminum source, HMI, AN and water in the resulting glue is 0.18:1:0.033:0.10:0.20:15.

[0067] Turn on the reaction unit R, send the molecular sieve slurry to the filter washing unit F, when the molecular sieve slurry is taken out of the organic phase, the organic phase is transported to the liquid-liquid separation container C1 through the fourth pipeline L4 to stand for phase separation, and the separated The template agent is sent to the template age...

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Abstract

The invention provides a preparation method of an MWW structure molecular sieve. The method comprises the following steps: 1, mixing a silicon source, an aluminum source, an alkali agent, a template and water, crystallizing the obtained glue solution, and cooling the crystallized glue solution to obtain a layered system with the upper layer being an organic phase and the lower layer being a molecular sieve slurry, wherein the template contains hexamethyleneimine and aniline; 2, separating the layered system to obtain the organic phase and the molecular sieve slurry; and 3, filtering the molecular sieve slurry, sequentially washing, drying and roasting the obtained filter cake, and distilling or rectifying the obtained filtrate to recover a hexamethyleneimine and water azeotrope and an aniline and water azeotrope. The method allows the superfluous template obtained after crystallization to be fully removed and recovered, and the generation probability of mixed crystals can be reduced when the template is reused; and the method can avoid environment pollution induced by hexamethyleneimine in discharged wastes.

Description

technical field [0001] The invention relates to a preparation method of molecular sieve with MWW structure. Background technique [0002] MCM-22 molecular sieve is a representative molecular sieve among MWW structure molecular sieves (MCM-22, MCM-49, MCM-56, SSZ-25, ERB-1, ITQ-1, ITQ-2 and UZM-8, etc.) , the molecular sieve has two sets of independent pore systems that are not directly connected to each other: the 10-membered ring channel with a pore size of 0.40×0.59 nm in the layer; the 12-membered ring supercage with a 0.40×0.71 The 0.54nm ten-member ring opening communicates with the outside world. The crystal surface of MCM-22 molecular sieve has some twelve-membered ring holes, which are half of the supercage, and the depth is about 0.71nm (Science, 1994, 264:1910). Therefore, in some catalytic reactions, it not only shows the characteristics of ten-membered rings, but also shows the characteristics of twelve-membered rings, and also has the characteristics of layere...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 龙立华尹文胜戴泳蔡俊华李斌周君祥沈刚廖雪强焦永东
Owner CHINA PETROLEUM & CHEM CORP
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