A catalyst loading device
By enhancing the adhesion of silicon-aluminum-phosphorus molecular sieves with reinforcing agents and using specific packing devices, the problem of uneven catalyst packing density was solved, achieving efficient and uniform catalyst packing, improving catalytic performance and reaction efficiency, and extending catalyst life.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- CHINA TIANCHEN ENGINEERING CORPORATION LTD
- Filing Date
- 2020-08-14
- Publication Date
- 2026-07-03
AI Technical Summary
During the catalyst loading process, uneven catalyst loading density leads to inconsistent pressure drop, which can easily cause physical impact and catalyst breakage, affecting experimental results and catalyst life. At the same time, existing loading technologies are difficult to achieve uniform and efficient loading of the catalyst bed.
An enhancer is used to improve the adhesion of silicon-aluminum-phosphorus molecular sieves, and the catalyst is loaded using a specific loading device. A metal rope and wheel system is used to achieve compact filling of the catalyst, ensuring uniformity and efficient loading.
The increased catalyst adhesion and packing density enhanced catalytic performance, improved reaction conversion and selectivity, extended catalyst lifespan, and prevented clogging and bridging, achieving uniform and efficient packing of the catalyst bed.
Smart Images
Figure CN115999450B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of chemical catalyst loading, specifically a catalyst loading device. Background Technology
[0002] With the increasing scale and technological advancements in catalytic reactors, the loading technology and equipment for solid catalysts have become crucial aspects of catalyst engineering development. The typical method for loading solid catalysts into a reactor involves introducing the catalyst from the reactor inlet and allowing it to fall freely. Differences in the catalyst's falling speed and loading time result in varying catalyst density. A faster falling speed or longer loading time leads to a higher density, while a slower falling speed or shorter loading time results in a lower density. Therefore, different loading methods result in different pressure drops in the catalyst bed. Furthermore, a faster falling speed can easily cause physical impacts, leading to catalyst breakage or powder formation, which inevitably affects experimental results.
[0003] The loading methods can generally be divided into ordinary loading and dense-phase loading. Ordinary loading, also known as sparse-phase loading, bag filling, or dilute-phase loading, does not require external driving force to increase the loading amount and uniformity of the catalyst. This method is simple and easy to implement, requires almost no special training for personnel, and does not require patented technology in the equipment, so it is adopted by many domestic enterprises. Dense-phase loading can increase throughput, has a low space velocity, allows for longer unit operating time, and has a high packing density, compact filling, and large loading volume, typically loading 10-25% more catalyst by weight than ordinary loading. Because the catalyst particles are regularly arranged on the reactor cross-section during the loading process, the loading density along the longitudinal and radial directions of the reactor is also very uniform. Dense-phase packing offers several advantages: reactors can be loaded with more catalyst, increasing processing capacity, extending cycle time, and improving product quality; for the same throughput, dense-phase packing results in a longer operating cycle; the catalyst bed is uniformly and densely packed, preventing bed collapse and channeling, thus avoiding localized overheating; and the radial temperature of the catalyst bed is uniform, improving reaction selectivity. Therefore, dense-phase packing shows greater promise than conventional packing.
[0004] Uneven catalyst loading can easily lead to catalyst "short circuits" or bed subsidence, resulting in uneven material and temperature distribution within the reactor, uneven contact time between the material and catalyst, and uneven reaction pressure drop, thus affecting product quality and catalyst lifespan. The core of catalyst loading technology is to achieve uniform catalyst loading during the process, improving bulk density and loading efficiency. Currently, many companies both domestically and internationally have developed proprietary loading technologies and achieved encouraging progress. However, many technical problems in catalyst loading still need to be solved.
[0005] The typical method for loading solid catalysts into a fixed-bed reactor is to introduce the catalyst from the reactor inlet and allow it to fall freely. Variations in the falling velocity and loading time result in different catalyst density levels. A faster falling velocity or longer loading time leads to a higher density, while a slower falling velocity or shorter loading time results in a lower density. Therefore, different loading methods result in different pressure drops in the catalyst bed, inevitably affecting experimental results. Furthermore, a faster falling velocity can easily cause physical impacts, leading to catalyst breakage or powder formation. Summary of the Invention
[0006] In view of this, the present invention aims to provide a catalyst loading device.
[0007] To achieve the above objectives, the technical solution of the present invention is implemented as follows:
[0008] An enhancer for improving the adhesion of catalyst-supported silica-alumino-phosphorus molecular sieves comprises a main agent, an auxiliary agent, and an additive, with a mass ratio of main agent: auxiliary agent: additive = (81-90): (8-18): 1. The main agent includes sol, ammonia, acid, and desalinated water, with a mass ratio of (70-84): (15-26): 1: (100-500). The auxiliary agents include polyvinyl alcohol, carboxymethyl cellulose, and dextrin, with a mass ratio of (20-30): (40-50): (20-40). The additives mainly include cyanate ester and alkylphenol polyoxyethylene ether, with a mass ratio of (90-95): (5-10).
[0009] Preferably, the sol is an aluminum sol or a silica sol, and the acid is hydrochloric acid or nitric acid.
[0010] Preferably, the dextrin is replaced with guar gum powder, and the alkylphenol polyoxyethylene ether is replaced with dioctyl phthalate or vinyl acetate resin.
[0011] A method for synthesizing the above-mentioned reinforcing agent includes the following steps: Step A1: Select a 304 stainless steel reaction vessel A, put in an appropriate amount of deionized water, heat the reaction vessel A to 30-60℃ and keep it warm, and then add each substance according to the order and proportion of each component of the main agent. After each substance is added, it needs to be stirred for 10-30 minutes. After all substances are added, it is kept stirring.
[0012] Step A2: Select 304 stainless steel reaction vessel B, maintain the temperature at 20-40℃, and mix all components in the additive evenly.
[0013] Step A3: Add the already well-stirred additive from reaction vessel B to reaction vessel A which is being stirred, and continue stirring for 2-4 hours;
[0014] Step A4: Select 304 stainless steel reaction vessel C, maintain the temperature at 20-40℃, add each component of the additive, stir for 10-20 minutes, then add it to reaction vessel A which was stirred in step A3, maintain the temperature at 20-50℃, and continue stirring the slurry in reaction vessel A for 1-4 hours to prepare the reinforcing agent.
[0015] A method for preparing a catalyst with a high content of silica-alumina-phosphorus molecular sieve using the above-mentioned reinforcing agent includes the following steps: Step B1: Select cordierite ceramic honeycomb as a carrier, soak it in dilute nitric acid for 0.5-3 hours, then take it out, remove the excess dilute nitric acid from the pores of the cordierite ceramic honeycomb carrier, and then dry and calcine it.
[0016] Step B2: Soak the cordierite ceramic honeycomb carrier treated in step B1 in the prepared reinforcing agent for 1-3 hours, then take it out, remove the excess slurry in the channels of the cordierite ceramic honeycomb carrier, and then dry and calcine it.
[0017] Step B3: The cordierite ceramic honeycomb carrier treated in step B2 is placed in the reaction slurry prepared by silica-alumina-phosphorus molecular sieve for synthesis. During the reaction, the silica-alumina-phosphorus molecular sieve generated will adhere to the surface and pores of the cordierite ceramic honeycomb carrier. After the reaction is completed, the cordierite ceramic honeycomb carrier is removed, excess slurry in the pores is removed, and then it is dried and calcined to obtain a monolithic catalyst with a high silica-alumina-phosphorus molecular sieve content.
[0018] Furthermore, the preparation method of the reaction slurry for preparing the silica-alumina-phosphorus molecular sieve in step B3 includes the following steps: stirring and mixing silica sol, boehmite, phosphoric acid, triethylamine and demineralized water at 10-40℃ to obtain the initial slurry of silica-alumina-phosphorus molecular sieve, and then hydrothermally crystallizing the slurry at a temperature of 120-220℃ for 48-72h, with the ratio of silica sol, boehmite, phosphoric acid, triethylamine and demineralized water being (0.1-2):1:(0.5-2):(0.5-4):(100-200).
[0019] A loading device for catalysts prepared by the above method includes a furnace body, a base, a conveyor, a metal rope, a main wheel axle, and auxiliary wheel axles. The base is placed inside the furnace body via a pluggable mechanism. The bottom of the furnace body has an upward-facing slot around its perimeter, the center of the base protrudes downwards, and the edge of the base has a downward-facing slot that interlocks with the upward-facing slots on the bottom of the furnace body. Two main wheel axles are located on the outer side of the upper part of the furnace body and are arranged vertically. Two auxiliary wheel axles are also provided, each hinged to a shaft. The shaft is hinged to the inner wall of the furnace body, and the inner wall of the furnace body has corresponding... The inner groove is used to place the shaft and auxiliary wheel shaft. In its natural state, the auxiliary wheel shaft is laid down to a horizontal position due to the limit of the lower end face of the inner groove. When the bottom support is lifted from bottom to top, the bottom support drives the shaft and auxiliary wheel shaft to flip upward and be embedded in the inner groove. The two auxiliary wheel shafts are located on opposite sides near the bottom of the furnace body. The metal rope is wound around one main wheel shaft, the two auxiliary wheel shafts and the other main wheel shaft in sequence. The loop of the metal rope is gradually conveyed from one main wheel shaft to the other main wheel shaft. The conveyor is located at the upper edge of the furnace body. The metal rope is provided with barbs at equal intervals.
[0020] A method of using the above-mentioned filling device includes the following steps: Step C1: Use wooden sticks to bind the cloth to clean the inside of the furnace body, remove the impurities inside the furnace body, and then air dry for 4 to 8 hours to keep the inside of the furnace body completely dry.
[0021] Step C2: Place the base plate at the bottom of the furnace body and secure it in the slot at the bottom of the furnace body, ensuring that the two are in close contact without any gaps;
[0022] Step C3: Initially, the metal ropes are all wound around one of the main axles, so that the other end of the metal rope is connected to the other main axle;
[0023] Step C4: The catalyst is conveyed into the furnace body by the conveyor. The metal rope is gradually and completely wrapped around the other main shaft. Through the transmission of the metal rope, the barbs gradually eliminate the gaps between the catalysts, making the catalyst filling more compact.
[0024] Step C5: Remove the metal rope and conveyor, and firmly connect the upper part of the furnace body to the reaction system to complete the overall catalyst loading operation;
[0025] Step C6: After the reaction, separate the reaction system, put a collection bag on the upper part of the furnace body, and when unloading the catalyst from the furnace body, introduce compressed air from the bottom of the furnace body upwards, the bottom support rises, and the entire catalyst enters the collection bag along the upper part of the furnace body.
[0026] Furthermore, the linear speed of the main wheel shaft rotation is 0.3 to 0.6 times the conveyor speed.
[0027] Furthermore, the overall catalyst loading height is 80-95% of the furnace height.
[0028] Compared with the prior art, the reinforcing agent for enhancing the adhesion ability of catalyst-supported silica-aluminophosphorus molecular sieves and the loading device suitable for the catalyst described in this invention have the following advantages: The reinforcing agent can enable more silica-aluminophosphorus molecular sieves to adhere to the cordierite support. Under normal circumstances, the mass of silica-aluminophosphorus molecular sieves attached to the cordierite support using silica sol is 15-21%, while after using this reinforcing agent, the mass of silica-aluminophosphorus molecular sieves attached to the cordierite support can reach 20-30%, thereby greatly improving the overall catalytic performance of the catalyst for the reaction. At the same time, it can also improve the overall conversion rate and selectivity of the catalyst, and extend the service life of the overall catalyst.
[0029] By using this loading device to load the entire catalyst, the overall catalyst loading amount can be increased by 20-40%, thereby achieving a basically uniform catalyst resistance inside the furnace tube and preventing blockages and bridging. After loading using this device, the reactants undergo a uniform chemical reaction inside the furnace tube, and the service life of the furnace tube can also be extended. This device has a high degree of automation and is easy to implement industrially. Attached Figure Description
[0030] The accompanying drawings, which form part of this invention, are used to provide a further understanding of the invention. The illustrative embodiments of the invention and their descriptions are used to explain the invention and do not constitute an undue limitation of the invention. In the drawings:
[0031] Figure 1 This is a schematic diagram of the filling device of the present invention;
[0032] Figure 2 for Figure 1 An enlarged schematic diagram of part A in the middle;
[0033] Explanation of reference numerals in the attached figures:
[0034] 1-Main wheel shaft; 2-Furnace body; 3-Auxiliary wheel shaft; 4-Bottom support; 5-Metal rope; 6-Barbs; 7-Conveyor; 8-Inner groove; 9-Shaft. Detailed Implementation
[0035] It should be noted that, unless otherwise specified, the embodiments and features described in the present invention can be combined with each other.
[0036] In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicating orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, are only for the convenience of describing the invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the invention. Furthermore, the terms "first," "second," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined with "first," "second," etc., may explicitly or implicitly include one or more of that feature. In the description of this invention, unless otherwise stated, "a plurality of" means two or more.
[0037] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art will understand the specific meaning of the above terms in this invention based on the specific circumstances.
[0038] The present invention will now be described in detail with reference to the accompanying drawings and embodiments.
[0039] Example 1
[0040] An enhancer for improving the adhesion of catalyst-supported silica-alumino-phosphorus molecular sieves comprises a main agent, an auxiliary agent, and an additive, with a mass ratio of main agent: auxiliary agent: additive = 81:8:1. The main agent includes aluminum sol, ammonia, hydrochloric acid, and demineralized water, with a mass ratio of 70:15:1:100. The auxiliary agent includes polyvinyl alcohol, carboxymethyl cellulose, and dextrin, with a mass ratio of 20:40:20. The additive mainly includes cyanate ester and alkylphenol polyoxyethylene ether, with a mass ratio of 90:5.
[0041] A method for synthesizing the above-mentioned reinforcing agent includes the following steps: Step A1: Select a 304 stainless steel reaction vessel A, put in an appropriate amount of deionized water, heat the reaction vessel A to 30°C and keep it warm, and then add each substance according to the order and proportion of each component of the main agent. Each substance needs to be stirred for 10 minutes after it is added. After all the substances are added, it is kept stirring.
[0042] Step A2: Select 304 stainless steel reaction vessel B, maintain the temperature at 20℃, and add the components of the additive and mix them evenly.
[0043] Step A3: Add the already stirred additive from reaction vessel B to reaction vessel A which is being stirred, and continue stirring for 2 hours;
[0044] Step A4: Select 304 stainless steel reaction vessel C, maintain the temperature at 20℃, add all components of the additive, stir for 10 minutes, then add to reaction vessel A which was stirred in step A3, maintain the temperature at 20℃, and continue stirring the slurry in reaction vessel A for 1 hour to prepare the reinforcing agent.
[0045] A method for preparing a catalyst with a high content of silica-alumina-phosphorus molecular sieve using the above-mentioned reinforcing agent includes the following steps: Step B1: Select cordierite ceramic honeycomb as a carrier, soak it in dilute nitric acid for 0.5 h, then take it out, remove the excess dilute nitric acid from the pores of the cordierite ceramic honeycomb carrier, and then dry and calcine it.
[0046] Step B2: Soak the cordierite ceramic honeycomb carrier treated in step B1 in the prepared reinforcing agent for 1 hour, then take it out, remove the excess slurry in the channels of the cordierite ceramic honeycomb carrier, and then dry and calcine it.
[0047] Step B3: The cordierite ceramic honeycomb carrier treated in step B2 is placed in the reaction slurry prepared by silica-alumina-phosphorus molecular sieve for synthesis. During the reaction, the silica-alumina-phosphorus molecular sieve generated will adhere to the surface and pores of the cordierite ceramic honeycomb carrier. After the reaction is completed, the cordierite ceramic honeycomb carrier is removed, excess slurry in the pores is removed, and then it is dried and calcined to obtain a monolithic catalyst with a high silica-alumina-phosphorus molecular sieve content.
[0048] The preparation method of the reaction slurry for preparing the silica-alumina-phosphorus molecular sieve in step B3 includes the following steps: stirring and mixing silica sol, boehmite, phosphoric acid, triethylamine and demineralized water at 10-40℃ to obtain the initial slurry of silica-alumina-phosphorus molecular sieve, and then hydrothermally crystallizing the slurry at a temperature of 120℃ for 48 hours, with the ratio of silica sol, boehmite, phosphoric acid, triethylamine and demineralized water being 0.1:1:0.5:0.5:100.
[0049] Example 2
[0050] An enhancer for improving the adhesion of catalyst-supported silica-alumino-phosphorus molecular sieves comprises a main agent, an auxiliary agent, and an additive, with a mass ratio of main agent: auxiliary agent: additive = 90:18:1. The main agent includes silica sol, ammonia, nitric acid, and demineralized water, with a mass ratio of 84:26:1:500. The auxiliary agent includes polyvinyl alcohol, carboxymethyl cellulose, and guar gum powder, with a mass ratio of 30:50:40. The additive mainly includes cyanate ester and alkylphenol polyoxyethylene ether, with a mass ratio of 95:10.
[0051] A method for synthesizing the above-mentioned reinforcing agent includes the following steps: Step A1: Select a 304 stainless steel reaction vessel A, put in an appropriate amount of deionized water, heat the reaction vessel A to 60°C and keep it warm, and then add each substance according to the order and proportion of each component of the main agent. Each substance needs to be stirred for 30 minutes after it is added. After all the substances are added, it is kept stirring.
[0052] Step A2: Select 304 stainless steel reaction vessel B, maintain the temperature at 40℃, and add the auxiliary agent and mix all components evenly;
[0053] Step A3: Add the already well-stirred additive from reaction vessel B to reaction vessel A which is being stirred, and continue stirring for 4 hours;
[0054] Step A4: Select 304 stainless steel reaction vessel C, maintain the temperature at 40℃, add all components of the additive, stir for 20 minutes, then add to reaction vessel A which was stirred in step A3, maintain the temperature at 50℃, and continue stirring the slurry in reaction vessel A for 4 hours to prepare the reinforcing agent.
[0055] A method for preparing a catalyst with a high content of silica-alumino-phosphorus molecular sieve using the above-mentioned reinforcing agent includes the following steps: Step B1: Select cordierite ceramic honeycomb as a carrier, soak it in dilute nitric acid for 3 hours, then take it out, remove the excess dilute nitric acid from the pores of the cordierite ceramic honeycomb carrier, and then dry and calcine it.
[0056] Step B2: Soak the cordierite ceramic honeycomb carrier treated in step B1 in the prepared reinforcing agent for 3 hours, then take it out, remove the excess slurry in the channels of the cordierite ceramic honeycomb carrier, and then dry and calcine it.
[0057] Step B3: The cordierite ceramic honeycomb carrier treated in step B2 is placed in the reaction slurry prepared by silica-alumina-phosphorus molecular sieve for synthesis. During the reaction, the silica-alumina-phosphorus molecular sieve generated will adhere to the surface and pores of the cordierite ceramic honeycomb carrier. After the reaction is completed, the cordierite ceramic honeycomb carrier is removed, excess slurry in the pores is removed, and then it is dried and calcined to obtain a monolithic catalyst with a high silica-alumina-phosphorus molecular sieve content.
[0058] The preparation method of the reaction slurry for preparing the silica-alumina-phosphorus molecular sieve in step B3 includes the following steps: stirring and mixing silica sol, boehmite, phosphoric acid, triethylamine and demineralized water at 40°C to obtain the initial slurry of silica-alumina-phosphorus molecular sieve, and then hydrothermally crystallizing the slurry at a temperature of 220°C for 72 hours, with the ratio of silica sol, boehmite, phosphoric acid, triethylamine and demineralized water being 2:1:2:4:200.
[0059] Example 3
[0060] An enhancer for improving the adhesion of catalyst-supported silica-alumino-phosphorus molecular sieves comprises a main agent, an auxiliary agent, and additives, with a mass ratio of main agent: auxiliary agent: additives = 85:12:1. The main agent includes aluminum sol, ammonia, nitric acid, and demineralized water, with a mass ratio of 75:20:1:200. The auxiliary agent includes polyvinyl alcohol, carboxymethyl cellulose, and dextrin, with a mass ratio of 25:45:30. The additives mainly include cyanate ester and dioctyl phthalate, with a mass ratio of 92:8.
[0061] A method for synthesizing the above-mentioned reinforcing agent includes the following steps: Step A1: Select a 304 stainless steel reaction vessel A, put in an appropriate amount of deionized water, heat the reaction vessel A to 45°C and keep it warm, and then add each substance according to the order and proportion of each component of the main agent. Each substance needs to be stirred for 20 minutes after it is added. After all the substances are added, it is kept stirring.
[0062] Step A2: Select 304 stainless steel reaction vessel B, maintain the temperature at 30℃, and add the auxiliary agent and mix all components evenly;
[0063] Step A3: Add the already stirred additive from reaction vessel B to reaction vessel A which is being stirred, and continue stirring for 3 hours;
[0064] Step A4: Select 304 stainless steel reaction vessel C, maintain the temperature at 30℃, add all components of the additive, stir for 15 minutes, then add to reaction vessel A which was stirred in step A3, maintain the temperature at 30℃, and continue stirring the slurry in reaction vessel A for 2 hours to prepare the reinforcing agent.
[0065] A method for preparing a catalyst with a high content of silica-alumino-phosphorus molecular sieve using the above-mentioned reinforcing agent includes the following steps: Step B1: Select cordierite ceramic honeycomb as a carrier, soak it in dilute nitric acid for 2 hours, then take it out, remove the excess dilute nitric acid from the pores of the cordierite ceramic honeycomb carrier, and then dry and calcine it.
[0066] Step B2: Soak the cordierite ceramic honeycomb carrier treated in step B1 in the prepared reinforcing agent for 2 hours, then take it out, remove the excess slurry in the channels of the cordierite ceramic honeycomb carrier, and then dry and calcine it.
[0067] Step B3: The cordierite ceramic honeycomb carrier treated in step B2 is placed in the reaction slurry prepared by silica-alumina-phosphorus molecular sieve for synthesis. During the reaction, the silica-alumina-phosphorus molecular sieve generated will adhere to the surface and pores of the cordierite ceramic honeycomb carrier. After the reaction is completed, the cordierite ceramic honeycomb carrier is removed, excess slurry in the pores is removed, and then it is dried and calcined to obtain a monolithic catalyst with a high silica-alumina-phosphorus molecular sieve content.
[0068] The preparation method of the reaction slurry for preparing the silica-alumina-phosphorus molecular sieve in step B3 includes the following steps: stirring and mixing silica sol, boehmite, phosphoric acid, triethylamine and demineralized water at 20°C to obtain the initial slurry of silica-alumina-phosphorus molecular sieve, and then hydrothermally crystallizing the slurry at a temperature of 160°C for 72 hours, with the ratio of silica sol, boehmite, phosphoric acid, triethylamine and demineralized water being 1:1:1.5:2:150.
[0069] Example 4
[0070] An enhancer for improving the adhesion of catalyst-supported silica-alumino-phosphorus molecular sieves comprises a main agent, an auxiliary agent, and an additive, with a mass ratio of main agent: auxiliary agent: additive = 90:15:1. The main agent includes silica sol, ammonia, hydrochloric acid, and demineralized water, with a mass ratio of 84:20:1:100. The auxiliary agent includes polyvinyl alcohol, carboxymethyl cellulose, and guar gum powder, with a mass ratio of 25:40:35. The additive mainly includes cyanate ester and vinyl acetate resin, with a mass ratio of 90:5.
[0071] A method for synthesizing the above-mentioned reinforcing agent includes the following steps: Step A1: Select a 304 stainless steel reaction vessel A, put in an appropriate amount of deionized water, heat the reaction vessel A to 60°C and keep it warm, and then add each substance according to the order and proportion of each component of the main agent. Each substance needs to be stirred for 10 minutes after it is added. After all the substances are added, it is kept stirring.
[0072] Step A2: Select 304 stainless steel reaction vessel B, maintain the temperature at 40℃, and add the auxiliary agent and mix all components evenly;
[0073] Step A3: Add the already stirred additive from reaction vessel B to reaction vessel A which is being stirred, and continue stirring for 2 hours;
[0074] Step A4: Select 304 stainless steel reaction vessel C, maintain the temperature at 30℃, add all components of the additive, stir for 15 minutes, then add to reaction vessel A which was stirred in step A3, maintain the temperature at 50℃, and continue stirring the slurry in reaction vessel A for 3 hours to prepare the reinforcing agent.
[0075] A method for preparing a catalyst with a high content of silica-alumina-phosphorus molecular sieve using the above-mentioned reinforcing agent includes the following steps: Step B1: Select cordierite ceramic honeycomb as a carrier, soak it in dilute nitric acid for 1 hour, then take it out, remove the excess dilute nitric acid from the pores of the cordierite ceramic honeycomb carrier, and then dry and calcine it.
[0076] Step B2: Soak the cordierite ceramic honeycomb carrier treated in step B1 in the prepared reinforcing agent for 1 hour, then take it out, remove the excess slurry in the channels of the cordierite ceramic honeycomb carrier, and then dry and calcine it.
[0077] Step B3: The cordierite ceramic honeycomb carrier treated in step B2 is placed in the reaction slurry prepared by silica-alumina-phosphorus molecular sieve for synthesis. During the reaction, the silica-alumina-phosphorus molecular sieve generated will adhere to the surface and pores of the cordierite ceramic honeycomb carrier. After the reaction is completed, the cordierite ceramic honeycomb carrier is removed, excess slurry in the pores is removed, and then it is dried and calcined to obtain a monolithic catalyst with a high silica-alumina-phosphorus molecular sieve content.
[0078] The preparation method of the reaction slurry for preparing the silica-alumina-phosphorus molecular sieve in step B3 includes the following steps: silica sol, boehmite, phosphoric acid, triethylamine and demineralized water are stirred and mixed at 40°C to obtain the initial slurry of silica-alumina-phosphorus molecular sieve. Then the slurry is hydrothermally crystallized at a temperature of 220°C for 72 hours. The ratio of silica sol, boehmite, phosphoric acid, triethylamine and demineralized water is 2:1:0.5:0.5:150.
[0079] Example 5
[0080] like Figure 1-2As shown, a loading device suitable for catalysts prepared by the above method includes a furnace body 2, a base 4, a conveyor 7, a metal rope 5, a main wheel axle 1, and auxiliary wheel axles 3. The base 4 is placed inside the furnace body 2 by a pluggable method. The bottom of the furnace body 2 has an upward-facing slot around its perimeter, and the center of the base 4 protrudes downward. The edge of the base 4 has a downward-facing slot that interlocks with the upward-facing slots at the bottom of the furnace body 2. The main wheel axle 1 is located on the outer side above the furnace body 2. There are two main wheel axles 1, arranged vertically. There are two auxiliary wheel axles 3, which are hinged to shafts 9. The shafts 9 are hinged to the inner wall of the furnace body 2. The inner wall of the furnace body 2 is provided with corresponding supports for the shafts 9 and... The auxiliary wheel shaft 3 is placed in the embedded groove 8. In its natural state, the shaft 9 is laid down to a horizontal position due to the limitation of the lower end face of the embedded groove 8. When the bottom support 4 is lifted from bottom to top, the bottom support 4 drives the shaft 9 and the auxiliary wheel shaft 3 to flip upward and be embedded in the embedded groove 8. The two auxiliary wheel shafts 3 are located on opposite sides near the bottom of the furnace body 2. The metal rope 5 is wound around one main wheel shaft 1, the two auxiliary wheel shafts 3 and the other main wheel shaft 1 in sequence. The loop of the metal rope 5 is gradually conveyed from one main wheel shaft 1 to the other main wheel shaft 1. The conveyor 7 is located at the upper edge of the furnace body 2 and is used to convey the catalyst into the furnace body 2. The metal rope 5 is provided with barbs 6 at equal intervals.
[0081] A method of using the above-mentioned filling device includes the following steps: Step C1: Use wooden sticks to bind the cloth to clean the inside of the furnace body 2, remove the impurities inside the furnace body 2, and then air dry for 4 to 8 hours to keep the inside of the furnace body 2 completely dry.
[0082] Step C2: Place the base 4 at the bottom of the furnace body 2 and make it fit into the slot at the bottom of the furnace body 2, ensuring that the two are in close contact without any gaps;
[0083] Step C3: Initially, all metal ropes 5 are wound around one of the main wheel shafts 1, so that the other end of the metal rope 5 is connected to the other main wheel shaft 1;
[0084] Step C4: The catalyst is conveyed into the furnace body 2 by the conveyor 7. The metal rope 5 is gradually wrapped around the other main wheel shaft 1. Through the transmission of the metal rope 5, its barbs 6 gradually eliminate the gaps between the catalysts, making the catalyst filling more compact.
[0085] Step C5: Remove the metal rope 5 and the conveyor 7, and firmly connect the upper end of the furnace body 2 to the reaction system to complete the overall catalyst loading operation.
[0086] Step C6: After the reaction, separate the reaction system, put a collection bag on the upper end of the furnace body 2, and when unloading the catalyst from the furnace body 2, introduce compressed air from the bottom outside the furnace body 2 upwards, the bottom support 4 rises, and the entire catalyst enters the collection bag along the upper end of the furnace body 2.
[0087] Metal rope 5 is made of iron wire, and its length is approximately 6.4-9.5 times the height of furnace body 2. The linear speed of the main wheel shaft 1 is 0.3-0.6 times the conveying speed of conveyor 7. The overall catalyst filling height is 80-95% of the height of furnace body 2.
[0088] The two main shafts 1 rotate in opposite directions; that is, when the lower main shaft 1 rotates counterclockwise, the upper main shaft 1 rotates clockwise. The metal rope 5 is distributed in a loop within the furnace body 2. The metal rope 5 extends from one main shaft 1, then extends from one side of the furnace body 2 to the bottom, then flips upwards and extends out of the furnace body 2, before wrapping around the other main shaft 1. The metal rope 5 has a node every 10-20 cm. Each node has 6-10 barbs (6) approximately 1-2 cm long. The metal rope 5 is made of carbon fiber and is relatively soft. The barbs (6) are made of high-quality 40#-45# medium carbon steel and are very hard.
[0089] The diameter of the integral catalyst suitable for this loading device is 1 / 10 or less of the furnace tube diameter.
[0090] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
Claims
1. A catalyst loading device, characterized in that: The furnace includes a furnace body (2), a base (4), a conveyor (7), a metal rope (5), a main wheel axle (1), and an auxiliary wheel axle (3). The base (4) is placed inside the furnace body (2) in a pluggable manner. The bottom of the furnace body (2) has an upward-facing slot around its perimeter. The center of the base (4) protrudes downward, and the edge of the base (4) has a downward-facing slot that plugs into the upward-facing slot at the bottom of the furnace body (2). The main wheel axle (1) is located on the outer side above the furnace body (2). There are two main wheel axles (1) arranged vertically. There are two auxiliary wheel axles (3). The auxiliary wheel axles (3) are hinged to a shaft (9). The shaft (9) is hinged to the inner wall of the furnace body (2). The inner wall of the furnace body (2) is provided with corresponding supports for the shaft (9) and the auxiliary wheel axles (3). The embedded groove (8) is placed in the natural state. Due to the limitation of the lower end face of the embedded groove (8), the shaft (9) is laid down to a horizontal state. When the bottom support (4) is lifted from bottom to top, the bottom support (4) drives the shaft (9) and the auxiliary wheel shaft (3) to flip upward and be embedded in the embedded groove (8). The two auxiliary wheel shafts (3) are located on opposite sides near the bottom of the furnace body (2). The metal rope (5) is wound around one main wheel shaft (1), the two auxiliary wheel shafts (3) and the other main wheel shaft (1) in sequence. The loop of the metal rope (5) is gradually conveyed from one main wheel shaft (1) to the other main wheel shaft (1). The conveyor (7) is located at the upper edge of the furnace body (2). The metal rope (5) is provided with barbs (6) at equal intervals.
2. A method of using the loading device of claim 1, characterized in that: The steps include the following: Step C1: Use wooden sticks to bind the cloth to clean the inside of the furnace body (2), remove the impurities inside the furnace body (2), and then air dry for 4 to 8 hours to keep the inside of the furnace body (2) completely dry. Step C2: Place the base (4) at the bottom of the furnace body (2) and make it fit into the slot at the bottom of the furnace body (2), ensuring that the two are in close contact without any gaps; Step C3: Initially, all the metal ropes (5) are wound around one of the main axles (1), so that the other end of the metal ropes (5) is connected to the other main axle (1); Step C4: The catalyst is conveyed into the furnace body (2) by the conveyor (7). The metal rope (5) is gradually wrapped completely from one main shaft (1) to another main shaft (1). Through the transmission of the metal rope (5), its barbs (6) gradually eliminate the gaps between the catalysts, making the catalyst filling more compact. Step C5: Remove the metal rope (5) and the conveyor (7), and connect the upper end of the furnace body (2) and the reaction system tightly to complete the overall catalyst loading operation; Step C6: After the reaction, separate the reaction system, put a collection bag on the upper end of the furnace body (2), and when unloading the catalyst in the furnace body (2), introduce compressed air upward from the bottom outside the furnace body (2), the bottom support (4) rises, and the entire catalyst enters the collection bag along the upper end of the furnace body (2).
3. The method of use according to claim 2, characterized in that: The linear speed of the main wheel shaft (1) is 0.3 to 0.6 times the conveying speed of the conveyor (7).
4. The method of use according to claim 2, characterized in that: The overall catalyst loading height is 80-95% of the furnace body (2) height.