CN107744830B - Method for preparing Cu-based molecular sieve SCR catalyst by one-step method - Google Patents
Method for preparing Cu-based molecular sieve SCR catalyst by one-step method Download PDFInfo
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/82—Phosphates
- B01J29/84—Aluminophosphates containing other elements, e.g. metals, boron
- B01J29/85—Silicoaluminophosphates (SAPO compounds)
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- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
Abstract
The invention relates to a method for preparing a Cu-based molecular sieve SCR catalyst by a one-step method, which is characterized in that a Cu-based molecular sieve SCR catalyst is prepared by ion exchange by using an SAPO-34 molecular sieve in a molecular sieve slurry containing a template agent. The method comprises the following specific steps: firstly, ultrasonically dispersing molecular sieve slurry containing a template agent, centrifuging to obtain a solid, preparing a solution with the copper content of 0.1-1mol/L together with a copper-containing compound, adjusting the pH, stirring and heating to perform liquid phase ion exchange, then centrifuging to obtain a solid, and drying and roasting the solid at high temperature to obtain the Cu-based molecular sieve SCR catalyst. The method adopts an ion exchange method to treat the molecular sieve slurry containing the template agent, obtains the high-efficiency Cu-based molecular sieve SCR catalyst through one-time roasting, has high NOx conversion rate in a low-temperature environment, is safe and environment-friendly in the whole process, and saves energy consumption.
Description
Technical Field
The invention relates to a method for preparing a Cu-based molecular sieve SCR catalyst by a one-step method, in particular to a method for preparing a Cu-based molecular sieve catalyst for removing NOx by a diesel vehicle through SCR reaction.
Background
Nitrogen oxides (NO, NO)2、N2O, etc., abbreviated as NOx) Is one of the main atmospheric pollutants, in recent years, the country has more and more paid attention to the problem of environmental pollution, and NO is added to diesel vehiclesxEmission standards are also becoming more stringent. During the operation of the diesel engine, NO generated by the reaction of nitrogen and oxygen in the air is NOxSo that NO cannot be eliminated from the sourcexAnd (4) generating. The tail gas must be denitrated, and the Selective Catalytic Reduction (SCR) is used for treating NOxAn effective method of (1).
The SCR technology being used is classified into Urea-SCR and HC-SCR according to the difference of the reducing agent. The Urea-SCR technology has the advantages of low catalyst cost, wide active window and NOxThe conversion rate is high, the product is free from pollution, the optimal fuel economy of the diesel engine is ensured, and the SCR technology with the development potential is formed.
The SCR catalyst consists of two parts, namely a catalyst and a carrier. Among them, the honeycomb cordierite ceramic carrier has been widely used because of its stable properties and large surface area. The catalyst is used as the core of an SCR system and is mainly divided into three major categories, namely noble metal oxide, metal oxide and molecular sieve. Most of the existing vanadium-titanium catalysts are low-temperature reducibility, V metal is toxic, and the defects that the waste catalyst is easy to cause secondary pollution and the like need to be solved. However, the molecular sieve catalyst has the advantages of environmental friendliness, wide temperature window, strong thermal stability and the like, so that the molecular sieve catalyst becomes a hotspot of research.
The molecular sieve catalyst is divided into two parts of a load metal and a carrier, common carriers comprise ZSM-5, MOR, HBEA, CHA and the like, wherein the CHA type silicoaluminophosphate zeolite molecular sieve with a small pore structure has higher activity at 150 ℃ and lower N2O selectivity, which is suitable for the low-temperature SCR reaction. SAPO-34, also having the CHA-type, is more reductive at lower temperatures and produces fewer by-products than SSZ-13, and is therefore a more suitable catalyst support. Cu has higher catalytic activity as a load metal and has wide application prospect.
The molecular sieve slurry containing the template agent can be discharged only by treatment, wherein a certain amount of SAPO-34 molecular sieve is wasted by burying, the cost for producing the SAPO-34 is relatively high, and the molecular sieve in the extracted slurry achieves the aim of environmental protection while the cost is reduced. CN 103263901 a discloses a method for preparing micron-sized molecular sieve loaded copper nanoparticles, which generates copper nanoparticles on a molecular sieve carrier in situ by a liquid phase reduction method. CN 102774850A discloses a rapid preparation method of a copper-containing microporous composite molecular sieve, which adopts a molecular sieve, a copper nitrate solution and a synthetic solution to carry out hydrothermal purification synthesis. The patent CN 103007998A discloses a method for preparing a molecular sieve catalyst for catalytic decomposition and reduction of nitrous oxide, which adopts ultrasonic heating to realize rapid exchange of copper ions.
The method for preparing the copper-based molecular sieve catalyst has the characteristics of expensive raw materials, high preparation cost, harsh required conditions and difficult realization of industrialization. In addition, the number of production steps is large, and the difficulty in using the produced catalyst in diesel vehicles has been a factor that limits the development thereof.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for preparing a Cu-based molecular sieve SCR catalyst in a one-step method.
The technical scheme of the invention is as follows: the Cu-based molecular sieve SCR catalyst is prepared by using molecular sieve slurry containing a template agent, Cu is loaded on an SAPO-34 molecular sieve by adopting an ion exchange method, and components recovered from waste membrane preparation liquid are utilizedThe sub-sieve achieves the effect of recycling. Cu can be made by ion exchange method2+Uniformly dispersing to obtain the catalyst with higher activity and conversion rate, and meeting the requirement of practical application.
The specific technical scheme of the invention is as follows: the method for preparing the Cu-based molecular sieve SCR catalyst by the one-step method is characterized by comprising the following steps of: copper is treated by a liquid phase ion exchange method by using SAPO-34 molecular sieve slurry containing a template agent and Cu2+The copper is uniformly loaded on the molecular sieve, the mass fraction of the copper reaches 0.4-10.0%, and the high-efficiency SCR catalyst is obtained by one-time roasting.
Further, the method for preparing the Cu-based molecular sieve SCR catalyst by the one-step method comprises the following specific steps:
a) adding deionized water into the SAPO-34 molecular sieve synthesis kettle liquid to ensure that the mass solid content is 2-15%, and ultrasonically dispersing to obtain a suspension;
b) carrying out centrifugal separation on the suspension obtained in the step a) to obtain a solid;
c) adding deionized water into the solid obtained in the step b) to obtain a suspension with the solid content of 5-15 wt%;
d) weighing a copper salt compound, adding the suspension obtained in the step c), controlling the copper content to be 0.1-1mol/L, and uniformly stirring to obtain a suspension;
e) adding alkali into the suspension obtained in the step d), and adjusting the pH to 4-6 while stirring;
f) stirring and heating the suspension obtained in the step e) at a high speed, and carrying out liquid phase ion exchange;
g) carrying out centrifugal separation on the suspension obtained in the step f);
h) and g) dehydrating, drying, grinding and roasting the solid obtained in the step g) to obtain the Cu-based molecular sieve SCR catalyst.
Preferably, the ultrasonic power in the step (a) is 30-80kHz, and the ultrasonic time is 0.5-3 h. Preferably, the centrifugation rates in steps (b) and (g) are 8000-12000r/min and the centrifugation time is 3-30 min.
Preferably, in step (e), the base is ammonia or tetramethylammonium hydroxide.
Preferably, the stirring rate in the step (f) is 150-350 r/min; heating at 50-90 deg.C for 1.5-6 hr.
Preferably, the drying temperature in the step (h) is 100-130 ℃, and the drying is carried out for 1-5 hours; the roasting temperature is 400-800 ℃, and the roasting time is 2-6 hours.
The preferable synthetic SAPO-34 molecular sieve kettle liquid is kettle liquid for preparing SAPO-34 molecular sieve by hydrothermal reaction, kettle liquid for preparing SAPO-34 molecular sieve by solid phase reaction, kettle liquid for preparing SAPO-34 molecular sieve by gas phase reaction or kettle liquid for producing SAPO-34 molecular sieve membrane, wherein the kettle liquid contains template agent. The type of the template agent comprises one or more of tetramethylammonium hydroxide, tetraethylammonium hydroxide, di-n-propylamine or triethylamine.
Preferably, the copper salt compound is copper sulfate, copper nitrate, copper chloride, copper acetate or copper oxide. More preferably: copper sulfate, copper nitrate, copper chloride, copper acetate, and copper oxide.
Has the advantages that:
the preparation process of the project is simple, the large-scale industrial production of the SCR catalyst is facilitated, the molecular sieve slurry containing the template agent is adopted for preparation, the cost is low, and the preparation period is short. The prepared catalyst has high stability and can be used for a long time.
Drawings
FIG. 1 is an XRD pattern of the Cu-SAPO-34 materials of examples 1-6 after calcination;
FIG. 2 is an SEM image of Cu-SAPO-34 materials of examples 1-5 after calcination;
FIG. 3 is a TPR graph of Cu-SAPO-34 materials of examples 2, 4, 8, 10 after calcination;
FIG. 4 is a graph of SCR performance of the Cu-SAPO-34 materials of examples 1-4 after calcination.
Detailed Description
Example 1:
taking SAPO-34 molecular sieve membrane preparation kettle liquid, preparing molecular sieve slurry containing a template agent with the solid content of 2 wt%, carrying out ultrasonic dispersion for 0.5h, carrying out ultrasonic power of 30kHz and centrifugal separation at the rotating speed of 8000r/min for 3min to obtain a solid, adding deionized water into the solid, and preparing into 5wt% suspension of about 200 ml. Adding copper nitrate to prepare 0.1mol/L solution, stirring uniformly, and adjusting the pH value to 4.0 by using ammonia water. And heating and stirring the suspension at the stirring speed of 150r/min, the heating temperature of 50 ℃ and the heating time of 1.5 hours. And centrifugally separating the obtained suspension at 8000r/min for 3min to obtain solid, dehydrating and drying at 100 deg.C for 1 hr, grinding to a certain particle size, and calcining at 400 deg.C for 2 hr.
Example 2:
preparing SAPO-34 kettle liquid through hydrothermal reaction, preparing molecular sieve slurry containing a template agent and having a solid content of 15wt%, performing ultrasonic dispersion for 3 hours, performing ultrasonic power of 80kHz, performing centrifugal separation for 30 minutes at a rotating speed of 12000r/min to obtain a solid, and adding deionized water into the solid to prepare a 15wt% suspension of about 200 ml. Copper nitrate was added to make a 1mol/L solution and stirred well, and the pH was adjusted to 4.4 with ammonia. And heating and stirring the suspension at the stirring speed of 350r/min and the heating temperature of 90 ℃ for 6 hours. And centrifugally separating the obtained suspension at the rotating speed of 12000r/min for 30min, dehydrating and drying the obtained solid at the drying temperature of 130 ℃ for 5 hours, grinding the solid to a certain particle size, roasting the solid at high temperature at the roasting temperature of 800 ℃ for 6 hours.
Example 3:
preparing SAPO-34 kettle liquid by hydrothermal reaction, preparing molecular sieve slurry containing a template agent with the solid content of 10 wt%, performing ultrasonic dispersion for 2 hours, performing ultrasonic power of 50kHz and centrifugal separation at the rotating speed of 10000r/min for 10min to obtain solid, and adding deionized water into the solid to prepare about 200ml of 10 wt% suspension. Copper nitrate was added to make a 0.5mol/L solution and stirred well, and the pH was adjusted to 4.8 with ammonia. And heating and stirring the suspension at the stirring speed of 150r/min, the heating temperature of 50 ℃ and the heating time of 1.5 hours. And centrifugally separating the obtained suspension at a rotating speed of 8000r/min for 3min, dehydrating and drying the obtained solid at a drying temperature of 110 ℃ for 2 hours, grinding the solid to a certain particle size, roasting at a high temperature of 550 ℃ for 4 hours.
Example 4:
preparing SAPO-34 kettle liquid by hydrothermal reaction, preparing molecular sieve slurry containing a template agent with the solid content of 10 wt%, performing ultrasonic dispersion for 2 hours, performing ultrasonic power of 50kHz and centrifugal separation at the rotating speed of 10000r/min for 30 minutes to obtain solid, and adding deionized water into the solid to prepare about 200ml of 10 wt% suspension. Copper nitrate was added to make a 0.5mol/L solution and stirred well, and the pH was adjusted to 5.2 with ammonia. And heating and stirring the suspension at the stirring speed of 150r/min, the heating temperature of 50 ℃ and the heating time of 1.5 hours. And centrifugally separating the obtained suspension at 10000r/min for 10min, dehydrating and drying the obtained solid at the drying temperature of 110 ℃ for 2h, grinding the solid to a certain particle size, roasting the solid at high temperature at the roasting temperature of 550 ℃ for 4 h.
Example 5:
preparing SAPO-34 kettle liquid by hydrothermal reaction, preparing molecular sieve slurry containing a template agent with the solid content of 10 wt%, performing ultrasonic dispersion for 2 hours, performing ultrasonic power of 50kHz and centrifugal separation at the rotating speed of 10000r/min for 30 minutes to obtain solid, and adding deionized water into the solid to prepare about 200ml of 10 wt% suspension. Copper nitrate was added to make a 0.5mol/L solution and stirred well, and the pH was adjusted to 5.6 with ammonia. And heating and stirring the suspension at the stirring speed of 150r/min, the heating temperature of 50 ℃ and the heating time of 1.5 hours. And centrifugally separating the obtained suspension at 10000r/min for 10min, dehydrating and drying the obtained solid at the drying temperature of 110 ℃ for 2h, grinding the solid to a certain particle size, roasting the solid at high temperature at the roasting temperature of 550 ℃ for 4 h.
Example 6:
preparing SAPO-34 kettle liquid by hydrothermal reaction, preparing molecular sieve slurry containing a template agent with the solid content of 10 wt%, performing ultrasonic dispersion for 2 hours, performing ultrasonic power of 50kHz and centrifugal separation at the rotating speed of 10000r/min for 30 minutes to obtain solid, and adding deionized water into the solid to prepare about 200ml of 10 wt% suspension. Copper nitrate was added to make a 0.5mol/L solution and stirred well, and the pH was adjusted to 6.0 with tetramethylammonium hydroxide. And heating and stirring the suspension at the stirring speed of 150r/min, the heating temperature of 50 ℃ and the heating time of 1.5 hours. And centrifugally separating the obtained suspension at 10000r/min for 10min, dehydrating and drying the obtained solid at the drying temperature of 110 ℃ for 2h, grinding the solid to a certain particle size, roasting the solid at high temperature at the roasting temperature of 550 ℃ for 4 h.
Examples 7 to 10:
taking SAPO-34 kettle liquid prepared by solid phase reaction, preparing molecular sieve slurry containing a template agent with the solid content of 10 wt%, performing ultrasonic dispersion for 2h, performing ultrasonic power of 50kHz, performing centrifugal separation for 30min at the rotating speed of 10000r/min to obtain solid, and adding deionized water into the solid to prepare about 200ml of suspension liquid with the solid content of 10 wt%. Copper sulfate, copper acetate, copper chloride and copper oxide are respectively added to prepare 0.5mol/L solution and are stirred evenly, and ammonia water is used for respectively adjusting the pH value to 6.0. And heating and stirring the suspension at the stirring speed of 150r/min, the heating temperature of 50 ℃ and the heating time of 1.5 hours. And centrifugally separating the obtained suspension at 10000r/min for 10min, dehydrating and drying the obtained solid at the drying temperature of 110 ℃ for 2h, grinding the solid to a certain particle size, roasting the solid at high temperature at the roasting temperature of 550 ℃ for 4 h.
Examples 11 to 13:
taking gas phase reaction to prepare SAPO-34 kettle liquid, preparing molecular sieve slurry containing a template agent with the solid content of 10 wt%, performing ultrasonic dispersion for 2h, performing ultrasonic power of 50kHz, performing centrifugal separation for 30min at the rotating speed of 10000r/min to obtain solid, and adding deionized water into the solid to prepare 10 wt% suspension of about 200 ml. Adding copper nitrate to prepare 0.4,0.6 and 0.8mol/L solutions respectively, stirring uniformly, and adjusting the pH value to 6.0 by using ammonia water respectively. And heating and stirring the suspension at the stirring speed of 150r/min, the heating temperature of 50 ℃ and the heating time of 1.5 hours. And centrifugally separating the obtained suspension at 10000r/min for 10min, dehydrating and drying the obtained solid at the drying temperature of 110 ℃ for 2h, grinding the solid to a certain particle size, roasting the solid at high temperature at the roasting temperature of 550 ℃ for 4 h.
The samples synthesized in examples 1-6 were further characterized by XRD, SEM, ICP and BET.
FIG. 1 shows XRD of the Cu-SAPO-34 materials of examples 1-5 after calcination to confirm the structure and crystallinity of the ion-exchanged SAPO-34.
Table 1 shows the ICP and BET of the Cu-SAPO-34 materials of examples 1-6 after calcination to confirm the SAPO-34 copper loading and microstructure after ion exchange.
Table 1: ICP and BET results at different pH conditions
Table 2 shows the ICP results for the Cu-SAPO-34 materials of examples 7-15 after calcination to confirm the SAPO-34 copper loading after ion exchange.
Table 2: ICP results under different preparation conditions
| Cu mass fraction (%) | |
| Example 7 | 2.64 |
| Example 8 | 2.34 |
| Example 9 | 2.57 |
| Example 10 | 2.08 |
| Example 11 | 1.27 |
| Example 12 | 6.38 |
| Example 13 | 9.24 |
FIG. 2 shows SEM of the Cu-SAPO-34 materials of examples 1-5 after calcination to confirm the microstructure of the SAPO-34 after ion exchange, the above chart indicating that too high a pH is not suitable for ion exchange
The samples synthesized in examples 2, 4, 8, 10 were tested for their reducing properties by TPR
FIG. 3 shows TPR of Cu-SAPO-34 materials of examples 2, 4, 8, 10 after calcination to confirm the ability of the ion-exchanged SAPO-34 temperature programmed reduction to consume hydrogen. Experiments show that the higher the content of Cu element is, the stronger the reduction performance is.
The sample synthesized in example 4 was subjected to catalytic testing of SCR for NOx reduction
The SCR test was performed in a fixed bed quartz tube reactor having a diameter of 2 cm and a length of 50 cm. The catalyst was pelletized into 0.25-0.42 mm pellets between experimental runs. Added to the catalytic layer of the reactor, heated to 550 ℃ (see reaction conditions in "table 3") and held under a nitrogen atmosphere for 1 hour. After which the feed is carried out. Using NH3SCR of NO is performed as a reducing agent. The reaction results are shown in FIG. 4.
The samples synthesized in the examples 7-13 pass the SCR test, and the conversion rate of nitrogen oxides exceeds more than 80% in the temperature range of 250 ℃ and 350 ℃, and have good SCR activity.
Table 3: SCR test conditions
| Total gas flow rate (L/h) | 30 |
| Catalyst loading (mL) | 2 |
| NO concentration (ppm) | 1000 |
| NH3 concentration (ppm) | 1000 |
| O2 concentration (%) | 3 |
| Temperature range of measurement (. degree. C.) | 150-450 |
Claims (5)
1. The method for preparing the Cu-based molecular sieve SCR catalyst by the one-step method is characterized by comprising the following steps of: copper is treated by a liquid phase ion exchange method by using SAPO-34 molecular sieve slurry containing a template agent and Cu2+The Cu-based molecular sieve SCR catalyst is uniformly loaded on a molecular sieve, the mass fraction of copper reaches 0.4-10.0%, and the Cu-based molecular sieve SCR catalyst is obtained by primary roasting; the method comprises the following specific steps:
a) adding deionized water into the SAPO-34 molecular sieve synthesis kettle liquid to ensure that the mass solid content is 2-15%, and ultrasonically dispersing to obtain a suspension; wherein the synthesized SAPO-34 molecular sieve kettle liquid is kettle liquid for preparing SAPO-34 molecular sieve by hydrothermal reaction, kettle liquid for preparing SAPO-34 molecular sieve by solid phase reaction, kettle liquid for preparing SAPO-34 molecular sieve by gas phase reaction or kettle liquid for producing SAPO-34 molecular sieve membrane;
b) carrying out centrifugal separation on the suspension obtained in the step a) to obtain a solid;
c) adding deionized water into the solid obtained in the step b) to obtain a suspension with the solid content of 5-15 wt%;
d) weighing a copper salt compound, adding the suspension obtained in the step c), controlling the copper content to be 0.1-1mol/L, and uniformly stirring to obtain a suspension;
e) adding alkali into the suspension obtained in the step d), and adjusting the pH to 4-6 while stirring; wherein the alkali is ammonia water or tetramethyl ammonium hydroxide;
f) stirring and heating the suspension obtained in the step e) at a high speed, and carrying out liquid phase ion exchange; wherein the stirring speed is 150-350 r/min; heating at 50-90 deg.C for 1.5-6 hr;
g) carrying out centrifugal separation on the suspension obtained in the step f);
h) and g) dehydrating, drying, grinding and roasting the solid obtained in the step g) to obtain the Cu-based molecular sieve SCR catalyst.
2. The method according to claim 1, wherein the ultrasonic power in step (a) is 30-80kHz and the ultrasonic time is 0.5-3 h.
3. The method as claimed in claim 1, wherein the centrifugation rates in steps (b) and (g) are 8000-12000r/min and the centrifugation time is 3-30 min.
4. The method as claimed in claim 1, wherein the drying temperature in step (h) is 100 ℃ and 130 ℃, and the drying time is 1-5 hours; the roasting temperature is 400-800 ℃, and the roasting time is 2-6 hours.
5. The method according to claim 1, wherein the copper salt compound is a sulfate of copper, a nitrate of copper, a chloride of copper or an acetate of copper.
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| Copper Ion-Exchanged SAPO-34 as a Thermostable Catalyst for Selective Reduction of NO with C3H6;Tatsumi Ishihara等;《JOURNAL OF CATALYSIS》;19971231;第169卷;第93-102页 * |
| Fabrication of Gold Nanoparticles in Confined Spaces using Solid-Phase Reduction: Significant Enhancement of Dispersion Degree and Catalytic Activity;Zhi-Min Xing等;《Chemical Engineering Science》;20161017;第158卷;第216-226页 * |
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