Catalyst loading preparation method
The method uses a computer device to pre-package catalysts into distinct bags for accurate loading in multitubular reactors, addressing crushing, pulverization, and human error issues, ensuring efficient and uniform catalyst distribution.
Patent Information
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- NIPPON KAYAKU CO LTD
- Filing Date
- 2024-11-08
- Publication Date
- 2026-05-20
AI Technical Summary
Catalyst filling in multitubular reactors faces issues such as crushing, pulverization, dust retention, catalyst shortages, on-site portioning difficulties, and human errors leading to non-uniform catalyst distribution, which are challenging to address due to discrepancies in reactor design and catalyst manufacturing timelines.
A method involving a computer device to calculate and pre-package catalysts into small, visually distinct bags with controlled air content, ensuring accurate loading into reaction tubes, minimizing human error and enabling efficient, planned catalyst distribution.
This method prevents catalyst shortages and mixing errors, enhances work efficiency, and ensures uniform catalyst loading in multitubular reactors, improving the overall catalyst filling process.
Smart Images
Figure 2026083579000001 
Figure 2026083579000002 
Figure 2026083579000003
Abstract
Description
Technical Field
[0001] The present invention relates to a preparation method for filling a catalyst into reaction tubes of a multitubular reactor.
Background Art
[0002] Catalysts used in oxidation reactions for producing unsaturated aldehydes, unsaturated carboxylic acids, and conjugated dienes are filled into thousands to tens of thousands of reaction tubes in a multitubular reactor and used. For example, Patent Document 1 discloses a method for filling a catalyst in which a tubular object is inserted and gas is released from the lower tip thereof in order to prevent the catalyst from being crushed and pulverized during filling. Also, Patent Document 2 discloses that work efficiency is improved by suppressing the retention of dust in the workplace.
Prior Art Documents
Patent Documents
[0003]
Patent Document 1
Patent Document 2
Summary of the Invention
Problems to be Solved by the Invention
[0004] At the catalyst filling site, not only problems such as the above-mentioned crushing and pulverization of the catalyst and the reduction in workability due to dust retention in the workplace occur, but various unexpected problems also occur, and countermeasures have to be taken each time. For example, a catalyst shortage may occur if the amount of catalyst ordered is insufficient for the reactor, or even if there is enough catalyst, the reactor may be a multi-tube type, requiring on-site portioning to distribute the catalyst to each reaction tube as needed. The former (catalyst shortage) is mainly caused by discrepancies between the volume and total number of reaction tubes in the drawings and the actual situation on site. However, as is clear to those skilled in the art, catalyst manufacturing generally involves multiple steps, and it typically takes several months from ordering raw materials to manufacturing, quality control, transportation, and arrival at the reactor. Therefore, it is difficult to urgently manufacture and ship catalyst even if there is a sudden shortage on-site. The latter (portioning) requires dividing several tons of catalyst into tens of thousands of bags, and securing workers and equipment, as well as ensuring uniformity of work quality, are difficult problems for catalyst reaction companies that do not normally perform such work. Furthermore, it is known to those skilled in the art that the catalyst for the oxidation reaction described above can be multi-layered to control the amount of heat generated. For this reason, it is necessary to prepare small portions of catalyst for each layer in each reaction tube, but human error by workers can lead to mix-ups in the catalyst layers, and it is not uncommon to see this happening at catalyst filling sites. This invention relates to a pre-preparation method that solves these problems, and aims to suppress unforeseen circumstances and human errors at the catalyst filling site and to achieve efficient catalyst filling. [Means for solving the problem]
[0005] The following are some of the measures to address the above issues. 1) A catalyst packing preparation method comprising packing a catalyst into a multitubular reactor containing multiple reaction tubes that produce at least one of an unsaturated aldehyde and an unsaturated carboxylic acid by an oxidation reaction using a catalyst, or a conjugated diene by an oxidative dehydrogenation reaction, In a computer device, A step of obtaining information regarding the multitubular reactor and information regarding the catalyst. The step includes outputting the required amount of the catalyst to be filled into each reaction tube, Method for preparing catalysts before filling. 2) Furthermore, the catalyst filling preparation method according to 1) above, further comprising the step of packaging ±10% by mass of the catalyst in small bags according to the required amount of the catalyst. 3) The catalyst loading preparation method according to 2) above, wherein the aforementioned small bags are of different catalyst species and are visually distinct small bags. 4) The catalyst filling preparation method according to 2) or 3) above, wherein in the step of packaging the catalyst into individual bags, the amount of air contained in each individual bag is 25% or less of the total volume of the individual bags. 5) A method for loading a catalyst, wherein the catalyst, which has been divided into smaller portions by the catalyst loading preparation method described in 2) or 3) above, is loaded into the reaction tubes of a multi-tube reactor. [Effects of the Invention]
[0006] According to the present invention, when loading catalysts into the reaction tubes of a multi-tube reactor, it is possible to avoid sudden shortages of catalyst and cumbersome small-portion work at the loading site, enabling efficient and planned catalyst loading. Furthermore, by changing the appearance of the small-portion bags for each type of catalyst, it is possible to avoid mixing up the catalysts to be loaded at the loading site and achieve planned catalyst loading. [Brief explanation of the drawing]
[0007] [Figure 1] This is a schematic plan view showing a multitubular reactor according to an embodiment, and also shows an example in which the multitubular reactor is spatially divided into three sections. [Figure 2] This is a schematic diagram showing the catalyst layers packed into a single reaction tube. [Figure 3] This figure shows a flowchart of the method according to the embodiment. [Figure 4] This diagram shows small bags filled with catalyst. [Modes for carrying out the invention]
[0008] The present invention relates to a method for preparing in advance for catalyst filling in a multi-tubular reactor, comprising: acquiring, by a computer device, information on the multi-tubular reactor and information on the catalyst, and calculating a required amount of the catalyst to be filled in each reaction tube. The method for preparing in advance for catalyst filling is related thereto.
[0009] [Computer device] The computer device used in the present invention is a computer device including a microprocessor such as a CPU (Central Processing Unit), a memory such as a ROM (Read Only Memory), a RAM (Random Access Memory), a flash memory, and a bus. The computer device may execute at least part of the method according to the present embodiment by a program recorded in a memory included in the computer device or a recording medium readable by the computer device. In the present embodiment, a program for causing the computer device to execute at least part of the method described later, and a recording medium recording the program are also presented. Note that the computer device that can be used in the present embodiment is not limited to this mode. For example, a cloud computing system connected via a network or the like may be used as the computer device for the method of the present disclosure.
[0010] [Step of acquiring information on the multi-tubular reactor and information on the catalyst] The method for preparing in advance for catalyst filling of the present invention includes a step of acquiring information on the multi-tubular reactor and information on the catalyst.
[0011] [Information on the multi-tubular reactor] Information on the multi-tubular reactor (hereinafter referred to as reaction tube information) means information on the number of reaction tubes, the inner diameter of the reaction tubes, and other information on the reaction tubes necessary for knowing the total amount of catalyst required for filling. In a reactor generally equipped with several thousand to tens of thousands of reaction tubes, it is not practical to obtain all the reaction tube information. Generally, the information of one to several reaction tubes is regarded as the information of the whole reactor without any special processing. More specifically, the reaction tube information includes the inner diameter of the reaction tube, the outer diameter of the reaction tube, the thickness of the reaction tube, and further, for measuring the temperature distribution inside the reaction tube, the information regarding the inner diameter of the reaction tube, the outer diameter of the reaction tube, the thickness of the reaction tube, and the information regarding the measuring device for the temperature distribution inside the reaction tube [specifically, the outer diameter and length of the measuring instrument (e.g., thermocouple), the information regarding the temperature measurement points, the dimensions and specifications of the control device of the measuring instrument, and further, the information regarding the outer diameter, length, and specifications of the equipment for enclosing the measuring instrument (e.g., the temperature sheath for enclosing the thermocouple as the measuring instrument)]. More broadly, the reaction tube information shall also include the information regarding the filling length of each catalyst layer as the filling design value. FIG. 1 is a schematic plan view showing a multitubular reactor 10 targeted by the method according to the present embodiment. The multitubular reactor 10 shown in FIG. 1 is cylindrical. In FIG. 1, three sections A, B, and C divided every 120° based on the center when the multitubular reactor 10 is viewed in plan are shown. A part of the plurality of reaction tubes 20 included in section A is surrounded by a dashed line and shown. Although a plurality of reaction tubes 20 are also provided outside the dashed line in section A and in sections B and C, illustration of those reaction tubes 20 is omitted. The multitubular reactor 10 produces at least one of a target unsaturated aldehyde, unsaturated carboxylic acid, and conjugated diene according to the catalyst to be filled, the raw material to be supplied, etc. Examples of the unsaturated aldehyde and unsaturated carboxylic acid to be produced include acrolein and acrylic acid, methacrolein and methacrylic acid, etc., and examples of the conjugated diene include 1,3 - butadiene, isoprene, etc. Each of the plurality of reaction tubes 20 included in the multitubular reactor 10 is filled with a catalyst. Preferably, the information of the one to several reaction tubes is obtained from one to several reaction tubes respectively from sections A, B, and C.
[0012] <Information regarding the catalyst> In this invention, information relating to the catalyst means the catalyst reserve ratio and information relating to trial loading of the catalyst (hereinafter referred to as "prior information"), and other information necessary to calculate the amount of catalyst required for loading and the amount to be loaded into each reaction tube (specifically, the bulk density of each catalyst layer, the particle size and strength of the catalyst, and similar information). Generally, catalysts are packed into a reaction tube 20 of a multitubular reactor in multiple layers of different catalyst species. Figure 2 is a schematic diagram showing the catalyst layers packed into one reaction tube 20. In the example shown in Figure 2, four catalyst layers 22, 24, 26, and 28 packed on a support ring 30 are shown. Each of the multiple layers has a different activity, and for example, the fourth catalyst layer 28 may have low activity at the inlet side where the raw materials are supplied, and the activity may increase towards the outlet side (support ring 30 side) (counting from the inlet side, the activity of the fourth catalyst layer 28 < the activity of the third catalyst layer 26 < the activity of the second catalyst layer 24 < the activity of the first catalyst layer 22). By supplying raw materials to the reaction tube 20 packed with catalysts in multiple layers and controlling operating conditions such as temperature, at least one of the target unsaturated aldehydes, unsaturated carboxylic acids, and conjugated dienes is produced. The aforementioned information regarding the catalyst is, in principle, required for the catalyst in each layer, i.e., for all types of catalysts packed into the layer; however, this does not exclude cases where it is used only for the catalyst in one of the layers.
[0013] <Steps to obtain> Figure 3 is a flowchart showing the method according to this embodiment. The method according to this embodiment includes an acquisition step S1 in which a computer device acquires information about the reaction tube and information about the catalyst. In acquisition step S1, the computer device may acquire reaction tube information through input from the user's terminal of the multi-tube reactor 10 or through input from the computer device administrator via a keyboard or other input device. The user of the multi-tube reactor 10 and the computer device administrator may be the same person. Specific examples of the acquisition step include the following, but are not limited to these, as long as they acquire information about the reaction tube and the catalyst. Specifically, the reaction tube information can be obtained in the following ways: [1] by acquiring the inner diameter, outer diameter, thickness, length, etc., as design values for the reaction tubes and inputting them into a computer device; or [2] by sampling several tubes from an actual multi-tube reactor, measuring the inner diameter, outer diameter, thickness, length, etc., and obtaining the average, maximum, minimum, mode, or median value for each, and inputting them into a computer device. Furthermore, it is more preferable to acquire the number of reaction tubes in a multi-tube reactor, minus the number of reaction tubes that include thermocouples, as described later, from the total number of reaction tubes, and inputting that number into a computer device. Regarding reaction tubes containing thermocouples, in multi-tube reactors for exothermic reactions such as the present invention, it is common practice to install temperature measuring devices in the catalyst of several reaction tubes to visualize the amount of heat generated during the reaction, and to measure the temperature distribution from the inlet side to the outlet side of the reaction tube. Reaction tube information naturally includes information about such temperature measuring devices (e.g., thermocouples), such as the outer diameter and length of the thermocouple, information about the temperature measurement point, information about the dimensions and specifications of the device control for the measuring device, information about the outer diameter, length and specifications of the equipment for enclosing the measuring device (e.g., a temperature sheath for enclosing the thermocouple as a measuring device), and information about the inner diameter, outer diameter, thickness and length of the reaction tube in which the thermocouple is installed. In particular, the inner diameter and length of the reaction tube in which the thermocouple is installed, the outer diameter and length of the thermocouple, and the number of reaction tubes containing thermocouples in the multi-tube reactor are acquired by a computer device. In calculating the required amount of catalyst, the following information from the acquisition step S1 above is particularly important: the inner diameter, length, and number of reaction tubes without thermocouples, the inner diameter, length, and number of reaction tubes with thermocouples, and the outer diameter of the thermocouples. Next, information regarding the catalyst, such as the bulk density of each catalyst layer, the particle size and strength of the catalyst, and similar information, is acquired by a computer device. Of these, the information regarding the bulk density of each catalyst layer is important. Possible methods for measuring or calculating this include, for example, laboratory-scale measurement using a graduated cylinder, referring to past packing data obtained from the same reactor, and referring to packing data from equivalent reaction tubes (including trial packing data using several reaction tubes in the reactor), but all of these are included in the present invention.
[0014] [Step of outputting the required amount of catalyst to be filled into each reaction tube] The catalyst loading preparation method of the present invention includes a step of calculating the required amount of catalyst to be loaded into each reaction tube. This is the output step S2 in Figure 3, which is performed by the computer device. <Required amount of catalyst to fill each reaction tube> The required amount of catalyst to be packed into each reaction tube is output for each catalyst layer. For example, in Figure 2, the output is provided for the catalyst used in catalyst layer 22, catalyst used in catalyst layer 24, catalyst used in catalyst layer 26, and catalyst used in catalyst layer 28. It is also possible to output the total required amount of catalyst based on the number of reaction tubes, and this step may include outputting this information. This output method calculates the spatial volume from the outer diameter of the reaction tube and the packing length of each catalyst layer, and multiplies this by the bulk density of each catalyst layer to automatically output the required catalyst weight per reaction tube for each catalyst layer using a computer device. As described above, the present invention also includes the ability to automatically output the total required amount for each catalyst layer by multiplying the catalyst weight per reaction tube by the number of reaction tubes (and similarly outputting for reaction tubes including thermocouples, and adding them as needed). In other words, in this specification, the required amount of catalyst refers to the required amount of catalyst per reaction tube or per catalyst layer, while the total required amount of catalyst refers to the total amount of catalyst used in the entire reactor, per catalyst layer.
[0015] [Step of packaging the required amount of catalyst ± a margin of portioning into individual bags.] The catalyst loading preparation method of the present invention optionally further includes a step of packaging catalyst in small bags in amounts equal to the required amount of catalyst ± a repackaging margin (specifically 10% by mass; preferably in order of 5% by mass, 3% by mass, 2% by mass, and 1% by mass) (hereinafter referred to as the repackaging step). This step is the repackaging step S3 in Figure 3. If the actual amount of catalyst to be loaded is small, it may be necessary to load additional catalyst to match the catalyst loading length to the design value, and vice versa (removal of catalyst). However, whether it is easier to load additional catalyst or remove catalyst depends on the number of workers and ancillary equipment at each plant. Taking this into consideration, repackaging to (required amount of catalyst + repackaging margin) or conversely to (required amount of catalyst - repackaging margin) is also included in this application, but for convenience in this invention, it is written as "required amount of catalyst ± repackaging margin". In this step, the required amount of catalyst refers to the required amount of catalyst for each layer to be packed into each reaction tube, and in practice, it is a step of portioning out catalyst in an amount of ±10% by mass of the required amount of catalyst. Furthermore, this step also includes preparing a reserve amount, and it is also possible to add about 0.5% as a reserve amount to the required amount for the total number of reaction tubes. The preferred amounts of this reserve amount are, in order from most preferred, 1.0%, 1.5%, 2.0%, 3.0%, 4.0%, 5.0%, and 10.0%, and the reserve amount may or may not be portioned out. Further portioning also includes portions specially portioned for reaction tubes containing thermocouples. The portioning step S3 may be performed by the person who performed steps S1 and S2, or the output information may be provided to the user via telephone, fax, or network, and the user may perform the step.
[0016] Furthermore, in the portioning step, if the catalyst types differ in multiple catalyst layers and / or if the amount of catalyst to be packed into the reaction tube for the thermocouple differs from the normal catalyst packing length for the reaction tube, it is preferable to portion the materials into visually distinct bags. This helps to avoid mixing up the catalysts at the catalyst packing site and enables planned catalyst packing. The expression "different catalyst species in multiple catalyst layers" is used in the reaction tube to distinguish between multiple catalysts constituting multiple layers. For example, even if catalyst layers 22 and 26 in the catalyst layers 22, 24, 26, and 28 of Figure 2 contain the same catalyst, they are distinguished and divided into visually distinct small bags. Furthermore, "visually different" can mean using small bags of different colors or materials, or it can also mean using different colored tape to distinguish them, changing the size or shape of the bags, or printing on the bags themselves.
[0017] Furthermore, it is more preferable that in the step of packaging the catalyst into individual bags, the amount of air contained in each individual bag is 25% or less of the total volume of the individual bag. The percentage of air relative to the total volume of the individual bags is, in order of increasing preference, 20%, 15%, 10%, 5%, 3%, and 1%. By packaging the catalyst so that no air is contained inside the bag, it is possible to prevent the catalyst from moving inside the bag due to vibration during shipping and transportation, and to prevent uneven distribution of particles inside the bag due to differences in particle size and weight between individual catalyst particles, or, in the case of the catalyst in the dilution layer, due to differences in particle size and weight between the catalyst and the inert balls. From another perspective, by packaging the catalyst so that no air is contained inside the bag, it is possible to prevent the catalyst from being worn down or pulverized due to vibration during shipping and transportation.
[0018] The catalyst is divided into smaller portions according to the required amount of catalyst determined in step S3, within a control range of ± the division margin. The equipment used for division may be an automatic weighing, filling, and packaging machine, or weighing, filling, and packaging may be performed manually. Here, weighing means measuring the prepared catalyst using a balance scale so that it is within the control range of ± the required amount of catalyst; filling means putting the weighed catalyst into small bags; and packaging means removing air from the filled bags as needed (deaeration), sealing the bags, and processing the bags to make them visually different as needed. Furthermore, if necessary, the application also includes weighing the bags again after packaging to confirm that the weight of the filled catalyst is within the control range of ± the required amount of catalyst. The packaged bags are then packed into drums or boxes as needed for transport. As described above, the present invention is a catalyst loading pre-preparation method that outputs the required amount of catalyst through each step using a computer device, and more narrowly, a catalyst loading pre-preparation method that subdivides the catalyst from the outputted required amount. Transporting the catalyst after using such a preparation method can have the following effects. Firstly, it clarifies the required amount of catalyst, and secondly, if further subdivision is performed, it improves the overall efficiency of the work. Regarding the first effect, plants sometimes lack information and know-how regarding catalyst loading pre-preparation, such as past loading information and calculations of required catalyst amounts. In such cases, it is beneficial for the plant to have a catalyst manufacturer with abundant information and know-how calculate the required amount of catalyst in an automatically outputted form, and further clarify the reserve amount, and to share this information, as it can avoid a shortage of catalyst during catalyst loading. Regarding the second effect, even if subdivision is not performed according to the present invention, it will be necessary to subdivide the catalyst by some method when finally loading the catalyst into a multi-tube reactor. Plants often lack the technology, equipment, and know-how for subdividing catalysts, and especially if there is no automatic weighing, filling, and packaging machine, it requires a considerable amount of manpower, which often delays the overall catalyst loading plan. Furthermore, by changing the appearance of the individual packaging bags, it is possible to avoid mixing up the catalysts being filled at the catalyst filling site. Thus, the effects of this invention include enabling efficient and planned catalyst filling operations, and further automating and streamlining the catalyst filling preparation method.
[0019] [Method for filling catalysts] The preferred method of filling according to the present invention is to drop the pre-portioned catalyst from the top of each reaction tube. In this case, since there is a possibility of pulverization or disintegration of the catalyst due to impact, it is more preferable to implement measures such as specifically controlling the humidity and temperature environment, or supplying a dry gas at a constant flow rate from below the reactor. Furthermore, when forming multiple catalyst layers, the layers are packed sequentially from the bottom up. For example, in Figure 2, the catalyst is packed into catalyst layers 22, 24, 26, and 28 in that order.
[0020] <Production of unsaturated aldehyde compounds, unsaturated carboxylic acid compounds, or conjugated diene compounds> The catalyst packing preparation method and the reactor packed with the catalyst by the present invention are used for the production of unsaturated aldehyde compounds, unsaturated carboxylic acid compounds, or conjugated diene compounds. Specifically, examples include the production of acrolein or acrylic acid using propylene as a raw material gas, the production of methacrylic acid using isobutylene as a raw material gas, and the production of 1,3-butadiene using butenes as a raw material gas. The method of supplying the raw material gas may be a conventional single-flow method or a recycling method, and can be carried out under generally used conditions and is not particularly limited. For example, a mixed gas consisting of 1-10% by volume, preferably 4-9% by volume, molecular oxygen 3-20% by volume, preferably 4-18% by volume, water vapor 0-60% by volume, preferably 4-50% by volume, and an inert gas such as carbon dioxide or nitrogen 20-80% by volume, preferably 30-60% by volume, is filled into a reaction tube and then carried out on the catalyst of the present invention at 240-450°C, under atmospheric pressure to 10 atmospheres, with a space velocity of 300-5000 h -1 It is introduced and the reaction is carried out. [Industrial applicability]
[0021] The catalyst preparation method and filling method of the present invention avoid sudden shortages of catalyst volume and cumbersome portioning work at the catalyst filling site, enabling efficient and planned catalyst filling operations. [Explanation of Symbols]
[0022] 10: Multitubular reactor, 20: Reaction tube, 22, 24, 26, 28: Catalyst layer, 30: Support ring, S1: Acquisition step, S2: Output step, S3: Supply step, 40: Air
Claims
1. A catalyst packing preparation method comprising packing a catalyst into a multitubular reactor containing multiple reaction tubes that produce at least one of an unsaturated aldehyde and an unsaturated carboxylic acid by an oxidation reaction using a catalyst, or a conjugated diene by an oxidative dehydrogenation reaction, In a computer device, A step of obtaining information regarding the multitubular reactor and information regarding the catalyst. The step includes outputting the required amount of the catalyst to be filled into each reaction tube, Method for preparing catalysts before filling.
2. Furthermore, the catalyst filling pre-preparation method according to claim 1, further comprising the step of packaging ±10% by mass of the catalyst in small bags according to the required amount of the catalyst.
3. The catalyst loading pre-preparation method according to claim 2, wherein the aforementioned small bags are of different catalyst types and are visually distinct small bags.
4. The catalyst filling pre-preparation method according to claim 2 or 3, wherein in the step of packaging the catalyst into individual bags, the amount of air contained in each individual bag is 25% or less by volume of the total volume of the individual bags.
5. A method for loading a catalyst, comprising loading the catalyst, which has been divided into smaller portions by the catalyst loading preparation method of claim 2 or 3, into the reaction tubes of a multi-tube reactor.