CN113716585B - Method for preparing Cu-SSZ-13 molecular sieve by one-step method - Google Patents
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- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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Abstract
The invention discloses a synthetic method for preparing a Cu-SSZ-13 molecular sieve by a one-step method. According to the method, modified copper silica gel, an aluminum source, a template agent and an organic alkali source are adopted to form gel, a Cu-SSZ-13 molecular sieve is dynamically crystallized and hydrothermally synthesized, and an obtained molecular sieve sample shows excellent catalytic performance in an NH3-SCR reaction. The method for synthesizing the molecular sieve provided by the invention does not need ammonium exchange and copper exchange, and is used for directly synthesizing the Cu-SSZ-13 by a one-step method, and the synthesis process is simple and reliable and is easy to realize.
Description
Technical Field
The invention relates to the technical field of catalysis, in particular to a method for preparing a Cu-SSZ-13 molecular sieve by a one-step method.
Background
Nitrogen oxides (NOx) cause a series of environmental problems such as photochemical smog, acid rain, and greenhouse effect, have seriously endangered human health, and with the increase of the number of automobiles and the rapid development of industry, NOx emissions are increased, which inevitably causes serious deterioration of ecology and environment. Thus, the problem of eliminating NOx pollution is not yet sustained. Currently, the NOx-dominant control technology is NH3 selective catalytic reduction (NH 3-SCR), which is critical to the selection of catalysts with excellent performance, which will determine the success or failure of the overall catalytic reaction system.
A catalyst used in power plants and motor vehicles for denitration systems is a selective catalytic reduction (selective catalytic reduction, abbreviated as SCR) catalyst. In the SCR reaction, the SCR catalyst is capable of causing the reductant to selectively react chemically with nitrogen oxides in the flue gas at a temperature.
The common SCR catalyst is a molecular sieve with a crystal structure prepared by taking zeolite as a carrier and loading an SCR active component; the zeolite is an aluminosilicate crystalline material having a fairly regular pore size, such as beta zeolite, Y zeolite, X zeolite, faujasite, mordenite, erionite, ZSM-5, ZSM-8, ZSM-11, ZSM-12, etc., which may be exchanged with a metal such as Cu, fe, mn, ag, V, ti, co or which itself contains a portion of a metal such as Cu, fe, etc. However, the above known metal-modified zeolite catalysts can only purify nitrogen oxides in a narrow temperature range during the selective catalytic reduction of nitrogen oxides by ammonia, do not have high-activity NOx purification performance at 200 ℃ or below, have poor hydrothermal stability, and have low activity at low temperatures.
Chabazite materials, particularly SSZ-13 zeolite molecular sieves, exhibit excellent properties in catalyzing Methanol To Olefins (MTO), catalyzing NOx in automotive exhaust, separating N2/CO2, and the like.
In the prior art, the method for manufacturing the Cu-SSZ-13 molecular sieve generally adopts the following modes: adding a template agent into a silicon source and an aluminum source, stirring in the presence of alkali, performing hydrothermal synthesis, preparing a hydrogen molecular sieve, then loading copper by using copper salt, and performing treatment again to obtain the Cu-SSZ-13 molecular sieve, wherein the molecular sieve synthesized by the method has the advantages of complex process, high cost and intangibly reduced market competitiveness.
Disclosure of Invention
The invention aims to provide a method for preparing a Cu-SSZ-13 molecular sieve by a one-step method, wherein modified copper silica gel, an aluminum source, a template agent and an organic alkali source form gel, and the Cu-SSZ-13 molecular sieve is synthesized by dynamic crystallization and hydrothermal synthesis. The modified copper silica gel is mainly used as a silicon source and a copper source, ammonium exchange and copper exchange are not needed, and the synthesis process is simple and reliable and is easy to realize.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for preparing a Cu-SSZ-13 molecular sieve by a one-step method, which comprises the following steps:
step S110: mixing a template agent, modified copper silica gel and an aluminum source together in an alkaline aqueous solution, and carrying out a gelation reaction to obtain gel;
step S120: under the action of the seed crystal, the gel is crystallized to obtain a crystallized product;
step S130: and roasting the crystallized product to obtain the Cu-SSZ-13 molecular sieve.
Compared with the prior art, in the preparation method of the Cu-SSZ-13 molecular sieve, the template agent, the modified copper-silicon source and the aluminum source are taken as raw materials, the raw materials are mixed together in an organic alkaline aqueous solution to carry out a gelation reaction, then the gel is subjected to a crystallization reaction under the action of a seed crystal, the crystallization product is roasted to remove the template agent and the organic base, the Cu-SSZ-13 molecular sieve is obtained, and a sample shows excellent catalytic performance in the NH3-SCR reaction. According to the process, in the preparation method of the Cu-SSZ-13 type molecular sieve, ammonium exchange and copper exchange are not needed, the Cu-SSZ-13 type molecular sieve is directly synthesized by a one-step method, and the synthesis process is simple and reliable and is easy to realize.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and do not constitute a limitation on the invention. In the drawings:
FIG. 1 is an XRD pattern of a product according to an embodiment of the invention, wherein the abscissa indicates the diffraction angle and the ordinate indicates the absorbance;
FIG. 2 is an SEM image of the product of one embodiment of the invention;
FIG. 3 is an XRD pattern of the product of example II of the invention, wherein the abscissa indicates the diffraction angle and the ordinate indicates the absorbance;
FIG. 4 is an SEM image of the product of example II;
FIG. 5 is a graph of SCR catalysis of a product in accordance with an embodiment of the present invention;
FIG. 6 is a graph of SCR catalysis of the product of example two of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The preparation method of the molecular sieve provided by the embodiment of the invention comprises the following steps:
the invention provides a method for preparing a Cu-SSZ-13 molecular sieve by a one-step method, which comprises the following steps:
step S110: mixing a template agent, modified copper silica gel and an aluminum source together in an alkaline aqueous solution, and carrying out a gelation reaction to obtain gel;
step S120: under the action of the seed crystal, the gel is crystallized to obtain a crystallized product;
step S130: and roasting the crystallized product to obtain the Cu-SSZ-13 molecular sieve.
Compared with the prior art, in the preparation method of the Cu-SSZ-13 molecular sieve, the template agent, the modified copper-silicon source and the aluminum source are taken as raw materials, the raw materials are mixed together in an organic alkaline aqueous solution to carry out a gelation reaction, then the gel is subjected to a crystallization reaction under the action of a seed crystal, the crystallization product is roasted to remove the template agent and the organic base, the Cu-SSZ-13 molecular sieve is obtained, and a sample shows excellent catalytic performance in the NH3-SCR reaction. According to the process, in the preparation method of the Cu-SSZ-13 type molecular sieve, ammonium exchange and copper exchange are not needed, the Cu-SSZ-13 type molecular sieve is directly synthesized by a one-step method, and the synthesis process is simple and reliable and is easy to realize.
The following describes each step in the preparation method of the molecular sieve provided in the embodiment of the present invention in detail.
In step S110: the molar ratio of the template agent to the silicon in the modified copper silica gel is (0.05-1): 1, preferably (0.1-0.30): 1, the mass ratio of copper atoms to silicon dioxide in the modified copper silica gel is (0.01-0.04): 1, preferably (0.02-0.035): 1. The mole ratio of the silicon dioxide of the modified copper silica gel to the aluminum oxide in the aluminum source is (5-80): 1, preferably (6-60): 1.
in addition, the molar ratio of the organic alkaline substance in the solution to the silicon in the modified copper silica gel is (0.3-0.7): 1, experiments prove that the modified copper silica gel can be fully swelled and gelled in an alkaline aqueous solution. Optionally, the mass ratio of the organic alkaline substance to water in the solution is 1: (10-100).
Wherein the aluminum source is one or more of aluminum sulfate, aluminum hydroxide and sodium metaaluminate. The organic alkaline substance can be one or more of ammonia water, tetramethyl ammonium hydroxide, tetraethyl ammonium hydroxide or tetrapropyl ammonium hydroxide and other quaternary amine bases. In this step, the template may be one or more of piperidinium hydroxide, amantadine hydroxide, choline chloride, etc., preferably amantadine hydroxide such as N, N-trimethyl-1-adamantylammonium hydroxide.
The modified copper silica gel is a relatively easily available raw material, a silicon source and a copper source of a reaction system can be provided simultaneously, copper atoms in the modified copper silica gel are combined with the silica gel, and the copper and the silicon are combined together to form a molecular sieve frame in the process of synthesizing the molecular sieve under the content, so that copper is well dispersed on the molecular sieve frame, copper elements are prevented from being separated from the frame, and the catalytic activity of the molecular sieve is improved.
In step S120: the seed crystal added in the crystallization reaction is commercial hydrogen type molecular sieve, and the amount of the added seed crystal is SiO in the silicon source 2 1-10% of the mass, the crystallization reaction temperature is 120-200 ℃, and the crystallization reaction time is 10-72 h;
compared with other crystal bloom methods, such as crystallization in a reaction kettle made of specific materials, the crystal bloom is carried out by adding the seed crystal such as the hydrogen molecular sieve with the content, and the like, and has the advantages of improving the reaction rate, saving the reaction time and reducing the production cost. In addition, other elements in the system are not introduced, and the performance of the molecular sieve is not affected.
In step S130: the roasting temperature is 400-650 ℃ and the roasting time is 4-30 h.
In order to describe the preparation method of the molecular sieve provided in the embodiment of the present invention in detail, a detailed description is given below in connection with the embodiment.
Example 1
The embodiment provides a method for preparing a Cu-SSZ-13 molecular sieve by a one-step method, which comprises the following steps:
embodiment one:
step S110: adding tetrapropylammonium hydroxide, modified copper silica gel, aluminum sulfate, an aqueous solution containing N, N, N-trimethyl-1-adamantylammonium hydroxide (the mass concentration is 25.0%) and deionized water into a 500mL conical flask at room temperature, and stirring for 1h at room temperature to form gel; wherein, the mol ratio of N, N, N-trimethyl-1-adamantyl ammonium hydroxide to silicon in the modified copper silica gel is 0.08:1, the mol ratio of silicon dioxide to aluminum sulfate of the modified copper silica gel is 25:1, the content of copper atomic mass ratio of the modified copper silica gel is 0.04, and the mol ratio of tetrapropylammonium hydroxide to silicon dioxide of the modified copper silica gel is 0.4:1.
Step S120: transferring the gel into a hydrothermal reaction kettle, adding seed crystals, sealing, placing the hydrothermal reaction kettle in a blast oven, reacting for 60 hours at 160 ℃, ending the reaction, cooling, filtering the reaction slurry through a sand core funnel, washing a filter cake with deionized water for two times, washing until the filter cake is neutral or slightly alkaline, and drying the filter cake at 120 ℃ for 6 hours to obtain a crystallized product; wherein the added seed crystal is 2.0% of the silica mass of the modified copper silica gel.
Step S130: the crystallized material is baked at 550 ℃ for 12 hours to obtain a powdery Cu-SSZ-13 molecular sieve, and the XRD pattern of the molecular sieve shown in figure 1 can be found: the output was CHA structure, as can be seen from the SEM images of the molecular sieves given in fig. 2: the crystal grains of the crystallized product are of a cube structure.
Further, analysis of the SCR catalyst using an X-ray fluorescence elemental analyzer revealed that: the molar ratio of silica to alumina (SAR) in the crystallized material was 22:1 copper atomic mass ratio content is 0.033.
Second embodiment
Step S110: adding tetraethylammonium hydroxide, modified copper silica gel, aluminum hydroxide, an aqueous solution containing N, N, N-trimethyl-1-adamantylammonium hydroxide (the mass concentration is 25.0%) and deionized water into a 500mL conical flask at room temperature, and stirring for 1h at room temperature to form gel; wherein the molar ratio of the N, N, N-trimethyl-1-adamantyl ammonium hydroxide to the silicon in the modified copper silica gel is 0.16:1, the molar ratio of the silicon in the modified copper silica gel to the aluminum oxide in the aluminum hydroxide is 30:1, the copper atomic mass ratio content of the modified copper silica gel is 0.020, and the molar ratio of the tetraethyl ammonium hydroxide to the silicon dioxide of the modified copper silica gel is 0.3:1
Step S120: transferring the gel into a hydrothermal reaction kettle, adding seed crystals, sealing, placing the hydrothermal reaction kettle in a blast oven, reacting for 36 hours at 180 ℃, ending the reaction, cooling, filtering the reaction slurry through a sand core funnel, washing a filter cake with deionized water for two times, washing until the filter cake is neutral or slightly alkaline, and drying the filter cake at 180 ℃ for 4 hours to obtain a crystallized product; wherein the added seed crystal is 1.0% of the silica mass of the modified copper silica gel.
Step S130: the crystallized material was calcined at 530 c for 16 hours to obtain a powdery Cu-SSZ-13 molecular sieve, as can be seen from the XRD pattern of the molecular sieve shown in fig. 3: the output was CHA structure, as can be seen from the SEM images of the molecular sieves given in fig. 4: the crystal grains of the crystallized product are of a cube structure.
Further, analysis of the SCR catalyst using an X-ray fluorescence elemental analyzer revealed that: the molar ratio of silica to alumina (SAR) in the crystallized material was 27:1 copper atomic mass ratio content is 0.022.
The SCR catalysts prepared in the first and second examples were subjected to activity test on a catalyst activity evaluation device under the following conditions: the temperature is 100-650 ℃, the reaction gas is simulated motor vehicle tail gas, NO and NH3 are 500ppm of 10% O2,5% H2O, and the balance N2, the activity test results are shown in figures 5 and 6, and the catalyst has wide operation window and excellent catalytic performance as can be seen from figures 5 and 6.
In the description of the above embodiments, particular features, structures, materials, or characteristics may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (3)
1. The preparation method of the Cu-SSZ-13 molecular sieve is characterized by comprising the following steps of:
step S110: mixing a template agent, modified copper silica gel and an aluminum source together in an alkaline aqueous solution, and carrying out gelation reaction to obtain gel, wherein the mass ratio of copper atoms in the modified copper silica gel to silicon dioxide is (0.02-0.035): 1, the template agent is at least one of piperidinium hydroxide, amantadine hydroxide or choline chloride, and the mole ratio of the template agent to silicon in the modified copper silica gel is (0.1-0.3): 1, the mole ratio of silicon dioxide in the modified copper silica gel to aluminum oxide in the aluminum source is (6-60): 1, the molar ratio of organic alkaline substances in the alkaline aqueous solution to silicon in the modified copper silica gel is (0.3-0.7): 1, a step of;
step S120: under the action of seed crystal, the gel is crystallized to obtain crystallized product, the seed crystal added in the crystallization reaction is hydrogen molecular sieve, and the amount of the added seed crystal is SiO in the silicon source 2 1-10% of the mass, the crystallization reaction temperature is 120-200 ℃, and the crystallization reaction time is 10-72 h;
step S130: and roasting the crystallized product to obtain the Cu-SSZ-13 molecular sieve.
2. The method of claim 1, wherein the organic alkaline material in the aqueous alkaline solution is at least one of tetramethylammonium hydroxide, tetraethylammonium hydroxide, or tetrapropylammonium hydroxide.
3. The method according to any one of claims 1 to 2, wherein in step S130, the firing temperature is 400 ℃ to 650 ℃ and the firing time is 4h to 30h.
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| CN106238092A (en) * | 2016-07-13 | 2016-12-21 | 无锡威孚环保催化剂有限公司 | The method of one-step synthesis method Cu SSZ 13 molecular sieve catalyst |
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| CN111704145A (en) * | 2020-06-05 | 2020-09-25 | 浙江天地环保科技股份有限公司 | Method for in-situ synthesis of nano hydrogen type Cu-SSZ-13 molecular sieve |
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