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A kind of molecular sieve with MWW structure and its synthesis method
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A synthesis method and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problem that the effect of composite template agent is irreplaceable
Active Publication Date: 2018-07-31
CHINA PETROLEUM & CHEM CORP +1
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This significantly expands the scope of templates used in molecular sieves with MWW structures, but hexamethyleneimine is still the most commonly used template for the synthesis of molecular sieves with MWW structures, and its role in composite templates is irreplaceable
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[0032] The present invention further provides the above-mentioned synthetic method with MWW structure molecular sieve, it is characterized in that comprising the following steps:
[0033] (1) Mix silicon source, alkali source and deionized water to obtain molar composition: OH - / SiO 2 =0.05~0.5,H 2 O / SiO 2 = 10-60 mixture A, the mixture A is treated at a temperature of 80-120°C under hydrothermal crystallization conditions for 5-24 hours;
[0034] (2) Mix the product of step (1) with aluminum source, alkali source, template agent and deionized water to obtain mixture B, and crystallize it under hydrothermal conditions to obtain guiding glue, wherein the template The agent is a template agent that can be used to synthesize molecular sieves with MWW structure;
[0035] (3) Mix the guide gel with silicon source, aluminum source, alkali source, template agent and optional deionized water to obtain mixture C, crystallize under hydrothermal conditions and recover the product. ...
Embodiment 1
[0065] This example illustrates the synthetic method and product provided by the invention.
[0066] (1) Mix Hailing silica gel, sodium hydroxide, and deionized water evenly to obtain a molar ratio of 0.10NaOH:SiO 2 : 15H 2 Mixture A of O was placed in a crystallization tank at 100°C for 8 hours.
[0067] (2) Mix the product of (1) with sodium metaaluminate, hexamethyleneimine, sodium hydroxide and water to obtain a molar ratio: 0.18NaOH:SiO 2 : 0.04Al 2 o 3 :0.30HMI: 30H 2 Mixture B of O was stirred and crystallized in a closed crystallization tank at a temperature of 145°C under autogenous pressure at a stirring speed of 30 rpm for 40 hours, and then cooled to room temperature to obtain a directing agent. Detect the XRD spectrum of this directing agent, without any MWW structure characteristic diffraction peaks.
[0068] (3) Continue to add Hailing silica gel, sodium metaaluminate, sodium hydroxide, and hexamethyleneimine to the guide agent to obtain a molar ratio of 0...
Embodiment 2
[0077] This example illustrates the synthetic method and product provided by the invention.
[0078] With embodiment 1, the difference is that Hailing silica gel in (1) is replaced by white carbon black.
[0079] Get the sample, number A2.
[0080] The XRD diffraction pattern of sample A1 shows MCM-22 molecular sieve; the relative crystallinity is 103%, and the BJH curve shows that the nitrogen desorption at 3.8nm is 0.14cm 3 / g; SEM morphology presents sheet-like irregular accumulation ( figure 2 -A2).
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Abstract
The invention discloses a molecular sieve with MWW structure, which is characterized in that the nitrogen adsorption-desorption BJH curve of the molecular sieve shows that the nitrogen desorption amount at 3.8±0.5nm is 0.01-0.15cm3 / g, and the SEM morphology presents slices irregular accumulation. A kind of synthetic method with MWW structure molecular sieve is characterized in that comprising the following steps: (1) silicon source, alkali source and deionized water are mixed to obtain molar composition: OH- / SiO2=0.05~0.5, H2O / SiO2= 10-60 of the mixture A, the mixture A is treated at a temperature of 80-120 ° C under hydrothermal crystallization conditions for 5-24 hours; (2) the product of step (1) is then mixed with an aluminum source, an alkali source, and a template agent and deionized water are mixed uniformly to obtain mixture B, and it is crystallized under hydrothermal conditions to obtain a guiding glue, wherein the template agent is a template agent that can be used to synthesize molecular sieves with a MWW structure; (3) guide the glue Mix well with silicon source, aluminum source, alkali source, templating agent and optional deionized water to obtain mixture C, crystallize under hydrothermal conditions and recover the product.
Description
technical field [0001] The invention relates to a molecular sieve with MWW structure and a synthesis method thereof. Background technique [0002] Molecular sieves with MWW structure include molecular sieves such as MCM-22, MCM-49, MCM-36, MCM-56, ITQ-1 and ITQ-2. In 1990, Mobil Corporation first used hexamethyleneimine as a template to hydrothermally synthesize MCM-22 molecular sieve (US, 4954325, 1990), and first analyzed its structure in 1994, and named it MWW structure molecular sieve. Therefore, layered molecular sieves with MWW topology are also called MCM-22 family molecular sieves. [0003] Molecular sieves with MWW structure have two sets of independent channels that do not intersect each other: the elliptical 10MR two-dimensional sinusoidal channel with a pore diameter of 0.40×0.59nm in the layer; the 12MR supercage with a pore size of 0.40×0.54nm The 10MR opening of the supercage communicates with the outside world; in addition, some 12MR holes are distributed o...
Claims
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