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Method for synthesizing Cu-SAPO-34 molecular sieve, synthesized molecular sieve and application of molecular sieve

A technology of cu-sapo-34 and cu-ssz-13 is applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve catalyst, molecular sieve characteristic silicoaluminophosphate, etc., which can solve the problem of poor high temperature hydrothermal stability, affecting product yield and Crystallinity, generation of silicon islands and other issues, to achieve the effect of good catalytic performance and good catalytic performance

Active Publication Date: 2019-01-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN102259892A discloses a method for synthesizing a silicoaluminophosphate molecular sieve catalyst using a metal-amine complex as a template, which avoids the cumbersome ion exchange process, but the high-temperature hydrothermal stability of Cu-SAPO-34 synthesized in one step is relatively poor , limiting its industrial application
These works show that the copper amine complex is used as a synthetic template to easily generate silicon islands in the SAPO molecular sieve framework.
However, if in order to control the copper loading and avoid the formation of silicon islands, the dosage of copper amine complex template agent and silicon source in the system should be reduced at the same time, which will affect the product yield and crystallinity

Method used

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  • Method for synthesizing Cu-SAPO-34 molecular sieve, synthesized molecular sieve and application of molecular sieve
  • Method for synthesizing Cu-SAPO-34 molecular sieve, synthesized molecular sieve and application of molecular sieve
  • Method for synthesizing Cu-SAPO-34 molecular sieve, synthesized molecular sieve and application of molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0039] Synthesis of Cu-SSZ-13 samples as copper source. The synthesis method can refer to the literature Chem.Commun.2011, 47, 9789-9791. The molar ratios and crystallization conditions of each raw material are shown in Table 1. The specific batching process is as follows:

[0040] A certain amount of sodium aluminate (65% by weight), water, copper sulfate pentahydrate, tetraethylenepentamine (TEPA), sodium hydroxide, silica sol (31% by weight) and optional crystals were sequentially added to a 2L synthesis kettle. kind. Stir the raw material mixture evenly, then seal it, raise the temperature to 140-180°C under stirring, and crystallize by rotation for 5-24h. The solid product was centrifuged, the sample was washed with deionized water to neutrality, and after drying in the air at 120°C, the ready-to-use Cu-SSZ-13 molecular sieve sample (named Cu-13-x, x=a, b, c, d). The purpose of adding seed crystals is to reduce the particle size of the synthesized high-copper Cu-SSZ-...

Embodiment 2～8

[0044] Embodiment 2~8: the preparation of high hydrothermal stability Cu-SAPO-34 molecular sieve product

[0045] The molar ratios and crystallization conditions of each raw material are shown in Table 2. The specific batching process is as follows:

[0046] Firstly, the optional aluminum source is mixed and dissolved with water, and then the optional phosphorus source, silicon source and templating agent R are sequentially added thereto. The Cu-SSZ-13 molecular sieve sample prepared in Example 1 was added to the above mixture. After stirring evenly at room temperature, the gel was transferred to a stainless steel reactor. After the reaction kettle is put into an oven, the temperature is raised to 140-240° C. for 0.5-72 hours, and the crystallization is completed. The solid product was centrifuged, washed, and dried in air at 120° C. to obtain the molecular sieve raw powder sample. The sample is analyzed by XRD, and the peak shape presents a typical CHA structural characte...

Embodiment 9

[0049] The samples obtained in Examples 3, 5 and 7 were calcined at 650°C for 2 hours, and after removing the template, they were used for NH 3 Selective reduction to remove NO x Catalytic performance test of the reaction. The specific experimental process and conditions are as follows: after roasting, the samples were pressed into tablets and sieved, and 0.1 g of 60 to 80 mesh samples were weighed and mixed with 0.4 g of quartz sand (60 to 80 mesh), and loaded into a fixed bed reactor. Activate with nitrogen at 600°C for 40 minutes, then lower the temperature to 120°C to start the reaction, and raise the temperature to 550°C. The reaction raw material gas is: NO: 500ppm, NH 3 : 500ppm, O 2 : 5%, H 2 O: 5%, N 2 As the balance gas, the gas flow rate is 300mL / min. The reaction tail gas adopts the Tensor 27 instrument of Bruker Company to carry out online FTIR analysis, and the results are shown in Figure 6 . It can be seen that the NO conversion rate of the sample in Ex...

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Abstract

The invention relates to a method for synthesizing a Cu-SAPO-34 molecular sieve, a product and a use of the product. More specifically, the involved method comprises the synthesis of the Cu-SAPO-34 molecular sieve with a Cu-SSZ-13 molecular sieve as a Cu source, a part of silicon and aluminum sources and a crystal seed, wherein the Cu-SSZ-13 molecular sieve has high Cu content and is synthesized with a copper-amine complex as a template agent. The method not only can control the copper loading amount in an SAPO-34 molecular sieve in a certain wide range, but also can effectively control the content and distribution of silicon atoms in the molecular sieve, and has high product yield. The obtained Cu-SAPO-34 molecular sieve catalyst exhibits excellent hydrothermal stability and catalytic performance for selective reduction removal of NOx.

Description

technical field [0001] The invention belongs to the field of chemistry and chemical engineering, and relates to a molecular sieve and a preparation method thereof, in particular to a method for synthesizing Cu-SAPO-34, a product obtained by the method and an application thereof. The Cu-SAPO-34 can be used as a catalyst for nitrogen oxide elimination process. Background technique [0002] Nitrogen oxides (NOx), as one of the main air pollutants, can cause many environmental problems such as acid rain and photochemical smog, and pose serious hazards to human health. Vehicle exhaust emissions from mobile sources and factory exhaust emissions from stationary sources are the main sources of NOx. Take NH 3 Selective Catalytic Reduction of NOx or NH as Reductant 3 -SCR technology can convert it into harmless nitrogen, which plays an extremely important role in the catalytic removal of NOx. Its key core is the development of SCR catalyst. The traditional denitrification catalys...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08B01J29/85
CPCC01B37/08C01B39/54B01J29/85C01P2002/72C01P2004/03
Inventor 杨淼孙丽婧田鹏刘中民曹毅向骁桑石云曹磊
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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