Catalyst Strength Destruction Device and Its Usage Method

By designing a catalyst strength damage device and using stirring and heating treatment to simulate industrial conditions, the problem of deviation between the catalyst strength detection results and actual application in the prior art is solved, and a fast and accurate catalyst strength comparison is achieved.

CN115128212BActive Publication Date: 2025-07-08SHANGHAI XUNKAI NEW MATERIAL TECH
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Patent Information

Application Number
CN202210667783.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-06-14
Publication Date
2025-07-08
Estimated Expiration
2042-06-14

AI Technical Summary

Technical Problem

The prior art methods for detecting catalyst strength under laboratory conditions are biased from those in actual industrial applications, and it is impossible to effectively simulate the mechanical strength reduction process of the catalyst under industrial conditions, resulting in inaccurate detection results.

Method used

A catalyst strength damage device is designed, including carrier, stirring, heat conductor, heating and cover assembly. By simulating temperature and solvent erosion under industrial application conditions, the catalyst is rapidly reduced by simulating the temperature and solvent erosion under industrial application conditions, and the catalyst is treated with stirring and heat.

Benefits of technology

It can quickly compare the strength of different catalysts, shorten the time for the reduction of catalyst strength, and improve the accuracy and efficiency of detection.

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Abstract

The present invention provides a catalyst strength destruction device, comprising a carrier, a stirring member, a heat conducting member, a heating member and a covering member; the stirring member is arranged at the center position of the carrier; the heat conducting member surrounds one side of the carrier, and an accommodating cavity for containing a solvent is formed between the heat conducting member and the carrier, and a filtering member for containing a catalyst is fixedly arranged in the accommodating cavity; the heating member is used for providing heat for the heat conducting member; the covering member is arranged at the opening end of the filtering member to seal the opening end of the filtering member. The present invention can rapidly reduce the catalyst strength by simulating the conditions in industrial applications, thereby greatly shortening the time for reducing the catalyst strength in actual applications and enabling rapid comparison of the strengths of different catalysts. The present invention also provides a method for using the catalyst strength destruction device.
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Description

Technical Field

[0001] The present invention relates to the field of catalyst strength detection, and particularly to a catalyst strength destruction device and a method for using the same. Background Art

[0002] Supported catalysts are prepared by techniques such as impregnation and precipitation to highly disperse active components and promoters on carriers such as diatomite, alumina, silica, and titanium oxide, forming highly efficient supported catalyst products with catalytic functions. Through different shaping techniques, supported catalysts in different shapes such as powder, cylinder, strip, and clover strip can be prepared. Preparing supported catalysts in different shapes is to meet different application scenarios. Supported catalysts are widely used in olefin hydrogenation units and acetylene hydrogenation units.

[0003] The mechanical strength of supported catalysts is very important in industrial applications. For supported catalysts with excellent performance, in addition to having sufficient activity, selectivity, and lifespan, they must also have sufficient mechanical strength. The mechanical strength of supported catalysts can reflect the anti-crushing performance of the particles of the negative catalyst when subjected to pressure or impact force. Supported catalysts with good mechanical strength can resist various stresses during use, thus maintaining the shape of the supported catalyst. If the mechanical strength of the supported catalyst fails, the supported catalyst will turn into fine powder under the action of external forces, and the fine powder will clog the pipeline, resulting in uneven fluid flow distribution and a sharp increase in pressure drop, thereby reducing the use efficiency of the supported catalyst. In severe cases, it may even lead to unexpected shutdown.

[0004] Currently, there are few strength detection methods under laboratory conditions. The patent with the publication number CN106861734A discloses a wear device for microsphere catalysts, a determination system and method for wear strength, and a method for obtaining the straight pipe wear index. This invention directly places the catalyst and a wear-resistant small ball in the same container for machine wear. However, in actual industrial applications, the fixed-bed supported catalyst is only affected by temperature and solvent scouring. This invention only detects the influence of external forces on the catalyst, and the final measurement results will deviate from the results in actual applications.

[0005] Therefore, it is necessary to develop a catalyst strength destruction device and a method for using the same to solve the above problems existing in the prior art. Summary of the Invention

[0006] The purpose of the present invention is to provide a catalyst strength destruction device. During the use of this device, the catalyst strength can be rapidly reduced by simulating the conditions in industrial applications, thereby greatly shortening the time for reducing the catalyst strength in actual applications and enabling rapid comparison of the strengths of different catalysts.

[0007] To achieve the above purpose, the catalyst strength destruction device of the present invention includes:

[0008] Carrier

[0009] Stirring member, disposed at the central position of the carrier

[0010] Heat conducting member, surrounding one side of the carrier, a receiving cavity for containing a solvent is formed between the heat conducting member and the carrier, and a filtering member for containing a catalyst is fixedly provided in the receiving cavity

[0011] Heating member, configured to provide heat to the heat conducting member

[0012] Covering member, disposed at the open end of the filtering member to seal the open end of the filtering member

[0013] The beneficial effect of the catalyst strength destruction device of the present invention is that: the carrier is used to carry the stirring member and the heat conducting member. The stirring member is disposed at the central position of the carrier, so that the stirring member can stir the solvent contained in the receiving cavity evenly. The heating member is configured to provide heat to the heat conducting member. The heat conducting member surrounds one side of the carrier, a receiving cavity for containing a solvent is formed between the heat conducting member and the carrier, and a filtering member for containing a catalyst is fixedly provided in the receiving cavity. In addition to forming the receiving cavity between the heat conducting member and the carrier, the heat conducting member can also uniformly transfer heat to the solvent, so that the heat is transferred to the catalyst. The covering member is disposed at the open end of the filtering member to seal the open end of the filtering member, preventing the catalyst in the filtering member from flowing under the agitation of the stirring member. During the use of this device, the strength of the catalyst can be quickly reduced by simulating the conditions in industrial applications, thus greatly shortening the time for reducing the strength of the catalyst in actual applications and enabling the quick comparison of the strengths of different catalysts.

[0014] Optionally, the catalyst strength destruction device further includes a fixing member, the fixing member surrounds the outside of the heat conducting member, the horizontal distance from the fixing member to the stirring member is a first distance, the horizontal distance from the heat conducting member to the stirring member is a second distance, the first distance is greater than the second distance, and a partition cavity for containing a heat conducting medium is formed among the heat conducting member, the fixing member and the carrier. The beneficial effect is that: the partition cavity can contain the heat conducting medium, so that the heat can be uniformly transferred to the heat conducting member through the heat conducting medium, and thus the heat can be better transferred to the catalyst.

[0015] Optionally, the difference between the first distance and the second distance is 5 - 10 cm. The beneficial effect is that the content of the heat-conducting medium contained in the separation cavity is just right. If the difference is too large, there will be too much heat-conducting medium, resulting in excessive heat loss during the conduction process. If the difference is too small, there will be too little heat-conducting medium, and the heat-conducting medium is easily evaporated by heat.

[0016] Optionally, the heating element is disposed on at least one of the outer wall of the fixing member, the inner wall of the fixing member, and the bottom of the separation cavity. The beneficial effect is that the heat is more evenly conducted during the conduction process.

[0017] Optionally, the covering member includes a covering portion and a buckling portion. The buckling portion is disposed on the covering portion. The opening end of the filtering member is provided with a engaging portion adapted to the buckling portion. The covering portion and the opening end of the filtering member are hermetically connected through the buckling portion and the engaging portion.

[0018] Optionally, the filtering member includes a plurality of filtering portions. The plurality of filtering portions are fixedly arranged on the bearing member at equal intervals around the center of the stirring member. The beneficial effect is that the catalyst is destroyed under the same conditions as much as possible.

[0019] Optionally, the plurality of filtering portions are all filter meshes with fixed shapes. The filter meshes are fixedly arranged on the bearing member. The beneficial effect is to prevent the filter meshes from shaking under the agitation of the stirring member, thus affecting the catalyst destruction process.

[0020] Optionally, the aperture of the filter mesh is 0.1 - 2 mm. The beneficial effect is to prevent the catalyst from dispersing out of the filter mesh.

[0021] Another object of the present invention is to provide a method for using the catalyst strength destruction device, including the following steps:

[0022] S1: Measure the strength of the fresh catalyst;

[0023] S2: Fill the inside of the filtering member with the fresh catalyst, and use the covering member to seal the opening end of the filtering member so that the fresh catalyst is fixed inside the filtering member;

[0024] S3: Pour the solvent into the accommodating cavity and submerge the opening end of the filtering member with the solvent;

[0025] S4: Simultaneously start the stirring member and the heating element to perform stirring treatment and heating treatment on the fresh catalyst to obtain the destroyed catalyst;

[0026] S5: Measure the strength of the destroyed catalyst.

[0027] The beneficial effects of the method for using the catalyst strength destruction device of the present invention are as follows: Measure the strength of the fresh catalyst; Fill the interior of the filter element with the fresh catalyst, and use the closing member to seal the open end of the filter element so that the fresh catalyst is fixed inside the filter element to prevent the fresh catalyst from flowing inside the filter element; Pour the solvent into the accommodating cavity and submerge the open end of the filter element with the solvent to ensure that the fresh catalyst inside the filter element is submerged by the solvent; At the same time, turn on the stirring member and the heating member to perform stirring treatment and heating treatment on the fresh catalyst to obtain the destroyed catalyst; Measure the strength of the destroyed catalyst. During the use of this device, the catalyst strength can be rapidly reduced by simulating the conditions in industrial applications, thereby greatly shortening the time for reducing the catalyst strength in actual applications and enabling rapid comparison of the strengths of different catalysts.

[0028] Optionally, the stirring speed of the stirring treatment is 100 - 1500 revolutions per minute, and the stirring time of the stirring treatment is 4 - 24 hours.

[0029] Optionally, the heating temperature of the heating treatment is 30 - 100 degrees Celsius, and the heating time of the heating treatment is 4 - 24 hours.

[0030] Optionally, the shape of the catalyst is any one or more of cylindrical, strip-shaped, three-leaf strip-shaped, spherical, and irregular granular.

[0031] Optionally, the solvent is one or both of water and organic solvents.

[0032] Optionally, the solvent is a mixed solvent of water and organic solvents, and the mass ratio of water to the organic solvent is 10 - 90%. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 It is a schematic structural diagram of the catalyst strength destruction device in some embodiments of the present invention;

[0034] Figure 2 It is a schematic structural diagram of the catalyst strength destruction device in some other embodiments of the present invention;

[0035] Figure 3 It is a schematic structural diagram of the closing member in an embodiment of the present invention;

[0036] Figure 4 It is a schematic structural diagram of the filter element in an embodiment of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0037] To make the objectives, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be described clearly and completely below. Apparently, the described embodiments are some but not all of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention. Unless otherwise defined, the technical terms or scientific terms used herein shall have the ordinary meanings as understood by those of ordinary skill in the art to which the present invention pertains. The words such as "including" used herein are intended to mean that the elements or items appearing before this word cover the elements or items listed after this word and their equivalents, without excluding other elements or items.

[0038] Figure 1 It is a schematic structural diagram of a catalyst strength destruction device in some embodiments of the present invention; Figure 2 It is a schematic structural diagram of a catalyst strength destruction device in some other embodiments of the present invention; Figure 3 It is a schematic structural diagram of a covering member in an embodiment of the present invention; Figure 4 It is a schematic structural diagram of a filtering member in an embodiment of the present invention.

[0039] In view of the problems existing in the prior art, with reference to Figure 1 and Figure 2 , an embodiment of the present invention provides a catalyst strength destruction device 100, including:

[0040] A carrier 1;

[0041] A stirring member 2, arranged at the central position of the carrier 1;

[0042] A heat conducting member 3, surrounding one side of the carrier 1, and a containing cavity 4 for containing a solvent is formed between the heat conducting member 3 and the carrier 1. A filtering member 5 for containing a catalyst is fixedly arranged in the containing cavity 4;

[0043] A heating member 6, used to provide heat for the heat conducting member 3;

[0044] The covering member 7 is arranged at the open end of the filter member 5 to seal the open end of the filter member 5. The carrier member 1 is used to carry the stirring member 2 and the heat conducting member 3. The stirring member 2 is arranged at the central position of the carrier member 1 so that the stirring member 1 can stir the solvent contained in the accommodating cavity 4 evenly. The heating member 6 is used to provide heat for the heat conducting member 3. The heat conducting member 3 surrounds one side of the carrier member 1, and an accommodating cavity 4 for containing the solvent is formed between the heat conducting member 3 and the carrier member 1. A filter member 5 for containing the catalyst is fixedly arranged in the accommodating cavity 4. Besides forming the accommodating cavity 4 between the heat conducting member 3 and the carrier member 1, the heat conducting member 3 can also transfer heat evenly to the solvent, so that the heat is transferred to the catalyst. The covering member 7 is arranged at the open end of the filter member 5 to seal the open end of the filter member 5, preventing the catalyst in the filter member 5 from flowing under the agitation of the stirring member 2. During the use of this device, by simulating the conditions in industrial applications, the strength of the catalyst can be rapidly reduced, thus greatly shortening the time for the reduction of the catalyst strength in actual applications and enabling the rapid comparison of the strengths of different catalysts.

[0045] In some embodiments of the present invention, the catalyst strength destruction device 100 further includes a fixing member 8. The fixing member 8 surrounds the outside of the heat conducting member 3. The horizontal distance from the fixing member 8 to the stirring member 2 is a first distance, and the horizontal distance from the heat conducting member 3 to the stirring member 2 is a second distance. The first distance is greater than the second distance. A partition cavity 9 for containing a heat conducting medium is formed among the heat conducting member 3, the fixing member 8 and the carrier member 1. The partition cavity 9 can contain the heat conducting medium, so that heat can be evenly transferred to the heat conducting member 3 through the heat conducting medium, and thus the heat can be better transferred to the catalyst.

[0046] In some embodiments of the present invention, referring to Figure 2 , the difference between the first distance and the second distance is L, and the difference value L is 5 - 10 cm. This makes the content of the heat conducting medium contained in the partition cavity 9 just right. If the difference is too large, too much heat conducting medium will be contained, resulting in excessive heat loss during the conduction process; if the difference is too small, too little heat conducting medium will be contained, and the heat conducting medium is easily evaporated by the heat.

[0047] In some possible embodiments of the present invention, the difference value L between the first distance and the second distance is any one of 5 cm, 6 cm, 7 cm, 8 cm, 9 cm and 10 cm. In some specific embodiments, the difference value L between the first distance and the second distance is 7 cm.

[0048] In some possible embodiments of the present invention, both the fixing member and the heat conducting member are cylindrical, and the difference L between the first distance and the second distance is the horizontal distance between the inner wall of the fixing member and the outer wall of the heat conducting member.

[0049] In some embodiments of the present invention, the stirring member 2 includes a base and a stirring rod. The stirring rod is movably connected to the base, and the base is fixedly arranged at the central position of the bearing member.

[0050] In some embodiments of the present invention, the catalyst strength destruction device further includes a driving member. The driving member is connected to the stirring rod to drive the stirring rod to agitate the solvent, and at the same time, the driving member can control the stirring speed of the stirring rod. The structure of the driving member is a common device and will not be described in detail here.

[0051] In some embodiments of the present invention, the heating member 6 is arranged on at least one of the outer wall of the fixing member 8, the inner wall of the fixing member 8, and the bottom of the partition cavity 9, so that the heat is more uniform during the conduction process.

[0052] In some embodiments of the present invention, the heating member 6 is a heating coil, and the heating coil is fixed to the outer wall of the fixing member 8 by any one of an adhesive, a snap connection, and a threaded connection. In some other embodiments, the heating coil is fixed to the inner wall of the fixing member 8 by any one of an adhesive, a snap connection, and a threaded connection. In still some other embodiments, the heating coil is fixed to the bottom of the partition cavity 9 by any one of an adhesive, a snap connection, and a threaded connection.

[0053] In some embodiments of the present invention, heating coils are fixedly arranged on both the outer wall of the fixing member 8 and the bottom of the partition cavity 9. In some other embodiments, heating coils are arranged on both the inner wall of the fixing member 8 and the bottom of the partition cavity 9.

[0054] In some embodiments of the present invention, heating coils are arranged on the outer wall of the fixing member 8, the inner wall of the fixing member 8, and the bottom of the partition cavity 9.

[0055] In some specific embodiments of the present invention, the adhesive is a glue adhesion structure, and the adhesive is a glue adhesion structure with a high temperature resistance greater than 100 °C. The adhesive is a high-temperature resistant glue adhesion structure, which avoids the melting of the adhesive due to the high temperature of the heating coil itself, and ensures the firmness between the heating coil and the outer wall of the fixing member 8 and between the heating coil and the inner wall of the fixing member 8.

[0056] In some embodiments of the present invention, the covering member includes a covering portion and a buckling portion. The buckling portion is provided on the covering portion. An engaging portion adapted to the buckling portion is provided at the open end of the filter element. The covering portion and the open end of the filter element are hermetically connected through the buckling portion and the engaging portion.

[0057] In some specific embodiments of the present invention, referring to Figure 3 and Figure 4 , the covering member 7 includes a covering portion 71 and two buckling portions 72. The two buckling portions 72 are symmetrically provided on the covering portion 71. Two engaging portions 51 adapted to the two buckling portions 72 are provided at the open end of the filter element 5. The covering portion 71 and the open end of the filter element 5 are hermetically connected through the buckling portion 72 and the engaging portion 51.

[0058] In some embodiments of the present invention, referring to Figure 1 and Figure 4 , the filter element 5 includes a plurality of filtering portions 52. The plurality of filtering portions 52 are fixedly arranged on the carrier 1 at equal intervals around the center of the stirring member 2. So that the catalyst is destroyed under the same conditions as much as possible.

[0059] In some embodiments of the present invention, the plurality is greater than or equal to 3. In some specific embodiments, the plurality is any one of 4, 6, 8, 10, and 12. In some more specific embodiments, referring to Figure 1 , the plurality is 4. In some other more specific embodiments, referring to Figure 2 , the plurality is 8.

[0060] In some embodiments of the present invention, the plurality of filtering portions 52 are all filter meshes with fixed shapes. The filter meshes are fixedly arranged on the carrier. To prevent the filter meshes from shaking under the agitation of the stirring member, thereby affecting the destruction process of the catalyst.

[0061] In some possible embodiments of the present invention, the shape of the filter mesh is any one of cylindrical, spherical, and cubic.

[0062] In some other possible embodiments of the present invention, the filter mesh is fixedly arranged at the bottom of the carrier 1 by any one of an adhesive, a snap connector, and a threaded connector.

[0063] In some embodiments of the present invention, the aperture of the filter mesh is 0.1 - 2 mm. To prevent the catalyst from dispersing out of the filter mesh.

[0064] In some possible embodiments of the present invention, the pore size of the filter screen is any one of 0.1 mm, 0.3 mm, 0.5 mm, 0.8 mm, 1.0 mm, 1.3 mm, 1.5 mm, 1.8 mm, and 2 mm. In some specific embodiments, the pore size of the filter screen is 1.4 mm.

[0065] An embodiment of the present invention provides a method for using the catalyst strength destruction device, including the following steps:

[0066] S1: Measure the strength of the fresh catalyst;

[0067] S2: Fill the interior of the filter element with the fresh catalyst, and use a covering member to seal the open end of the filter element so that the fresh catalyst is fixed inside the filter element;

[0068] S3: Pour the solvent into the accommodating cavity and submerge the open end of the filter element with the solvent;

[0069] S4: Simultaneously turn on the stirring member and the heating member to perform stirring treatment and heating treatment on the fresh catalyst to obtain the destroyed catalyst;

[0070] S5: Measure the strength of the destroyed catalyst. Measure the strength of the fresh catalyst; fill the interior of the filter element with the fresh catalyst, and use a covering member to seal the open end of the filter element so that the fresh catalyst is fixed inside the filter element to prevent the fresh catalyst from flowing inside the filter element; pour the solvent into the accommodating cavity and submerge the open end of the filter element with the solvent to ensure that the fresh catalyst inside the filter element is completely submerged by the solvent; simultaneously turn on the stirring member and the heating member to perform stirring treatment and heating treatment on the fresh catalyst to obtain the destroyed catalyst; measure the strength of the destroyed catalyst. During the use of this device, by simulating the conditions in industrial applications, the strength of the catalyst can be rapidly reduced, thereby greatly shortening the time for reducing the catalyst strength in actual applications and enabling rapid comparison of the strengths of different catalysts.

[0071] In some embodiments of the present invention, the stirring speed of the stirring treatment is 100 - 1500 revolutions per minute, and the stirring time of the stirring treatment is 4 - 24 hours.

[0072] In some embodiments of the present invention, the heating temperature of the heating treatment is 30 - 100 degrees Celsius, and the heating time of the heating treatment is 4 - 24 hours.

[0073] In some embodiments of the present invention, the shape of the catalyst is any one or more than two of cylindrical, strip-shaped, three-leaf strip-shaped, spherical, and irregular granular.

[0074] In some embodiments of the present invention, the solvent is one or both of water and an organic solvent.

[0075] In some embodiments of the present invention, the solvent is a mixed solvent of water and an organic solvent, and the mass ratio of water to the organic solvent is 10 - 90%.

[0076] In Examples 1 - 7 of the present invention, Step S1 is: measuring the strength of the fresh catalyst; Step S2 is: filling the interior of the filter element with the fresh catalyst, and using a covering member to seal the open end of the filter element so that the fresh catalyst is fixed inside the filter element; Step S3 is: pouring the solvent into the accommodating cavity and submerging the open end of the filter element with the solvent; Step S4 is: simultaneously turning on the stirring member and the heating member to perform stirring treatment and heating treatment on the fresh catalyst to obtain a damaged catalyst; Step S5 is: measuring the strength of the damaged catalyst.

[0077] In Examples 1 - 7 of the present invention, the fresh catalyst is a clover - shaped strip - supported nickel catalyst. The length of the clover - shaped strip - supported nickel catalyst is 5 mm, the pore diameter of the filter screen is 2 mm. The destruction conditions of Examples 1 - 7 of the present invention are shown in Table 1, and the specific test results of Examples 1 - 7 of the present invention are shown in Table 2.

[0078] Table 1 Destruction conditions in Examples 1 - 7

[0079] Example Solvent Heating Temperature (°C) Heating Time (h) Stirring Speed (r / min) Stirring Time (h) Example 1 Water 30 24 1500 24 Example 2 Water 100 24 1500 24 Example 3 Water 50 8 100 8 Example 4 Water 30 4 100 4 Example 5 Butynediol 80 8 1000 8 Example 6 Caprolactam 80 8 1000 8 Example 7 Caprolactam 30 24 1000 24

[0080] The present invention also provides Comparative Examples 1 - 4. In Comparative Examples 1 - 4, the fresh catalyst is a clover - shaped strip - supported nickel catalyst, and the length of the clover - shaped strip - supported nickel catalyst is 5 mm.

[0081] The destruction step of Comparative Example 1 of the present invention is: fixing the clover - shaped strip - supported nickel catalyst in a fixed - bed reactor. The operating temperature of the fixed - bed reactor is 60°C, the feed solvent is water, and the volume space velocity is 1.5 h -1 , and after feeding for 1 month, taking out the clover - shaped strip - supported nickel catalyst to obtain a damaged catalyst, and testing the strength of the damaged catalyst. The specific test results are shown in Table 2.

[0082] The destruction step of Comparative Example 2 of the present invention is: fixing the clover - shaped strip - supported nickel catalyst in a fixed - bed reactor. The operating temperature of the fixed - bed reactor is 60°C, the feed solvent is water, and the volume space velocity is 1.5 h -1 , and after feeding for 4 months, taking out the clover - shaped strip - supported nickel catalyst to obtain a damaged catalyst, and testing the strength of the damaged catalyst. The specific test results are shown in Table 2.

[0083] The destruction procedure of Comparative Example 3 of the present invention is as follows: Fix the clover-shaped nickel-loaded catalyst in a fixed-bed reactor. The operating temperature of the fixed-bed reactor is 60 °C, the feed solvent is water, and the volume space velocity is 1.5 h -1 , and after 10 months of feeding, take out the clover-shaped nickel-loaded catalyst to obtain the destroyed catalyst, and test the strength of the destroyed catalyst. The specific test results are shown in Table 2.

[0084] The destruction procedure of Comparative Example 4 of the present invention is as follows: Fix the clover-shaped nickel-loaded catalyst in a fixed-bed reactor. The operating temperature of the fixed-bed reactor is 60 °C, the feed solvent is an aqueous solution of caprolactam, and the volume space velocity is 1.5 h -1 , and after 10 months of feeding, take out the clover-shaped nickel-loaded catalyst to obtain the destroyed catalyst, and test the strength of the destroyed catalyst. The specific test results are shown in Table 2.

[0085] The volume space velocity refers to the volume flow rate of the feed solvent (at 20 °C, m 3 ·h -1 ) / the volume of the catalyst (m 3 ), which reflects the residence time of the feed solvent in the catalyst bed.

[0086] The catalyst strength test includes the steps of: testing the fresh catalyst and the destroyed catalyst using a catalyst strength tester. The catalyst strength tester is a commercially available product and will not be elaborated here.

[0087] Table 2 Test results of Examples 1-7 and Comparative Examples 1-4

[0088]

[0089]

[0090] Note: The particle strength of the destroyed catalyst in Table 2 = the catalyst strength / the length of the fresh catalyst (i.e., 5 mm = 0.5 cm). The catalyst strength includes the strength of the fresh catalyst and the strength of the destroyed catalyst; the experimental data in Table 2 are the results of averaging the particle strengths of 60-80 destroyed catalysts tested in each example after removing the maximum and minimum values.

[0091] According to the test results of Examples 1-4 in Table 2, it can be seen that the heating temperature, heating time, stirring speed, and stirring time all affect the strength of the catalyst; according to Examples 5 and 6 in Table 2, it can be seen that different solvents also have an impact on the strength of the catalyst.

[0092] According to Example 3 and Comparative Example 3 in Table 2, during the operation of the fixed-bed reactor, the time when the strength degradation rate of the catalyst reaches 21.6% is 10 months, while in the catalyst strength destruction device of the present invention, the time when the strength degradation rate of the catalyst reaches 17.1% is within 8 hours. It can be seen that the catalyst strength destruction device of the present invention can significantly shorten the catalyst strength destruction period.

[0093] Although the embodiments of the present invention have been described in detail above, it is obvious to those skilled in the art that various modifications and changes can be made to these embodiments. However, it should be understood that such modifications and changes are all within the scope and spirit of the present invention described in the claims. Moreover, the present invention described herein can have other embodiments and can be implemented or realized in various ways.

Claims

1. A catalyst strength destruction device for reducing the strength of a supported catalyst, characterized in that, Comprising: A carrier; a stirring member disposed at the central position of the carrier; a heat conducting member surrounding one side of the carrier, the heat conducting member and the carrier forming an accommodation cavity for containing a solvent, and a filter member for containing a catalyst being fixedly disposed in the accommodation cavity; a heating member for providing heat to the heat conducting member; and a covering member disposed at the open end of the filter member to seal the open end of the filter member.

2. The catalyst strength destruction device according to claim 1, characterized in that, It further includes a fixing member surrounding the outside of the heat conducting member. The horizontal distance from the fixing member to the stirring member is a first distance, and the horizontal distance from the heat conducting member to the stirring member is a second distance. The first distance is greater than the second distance, and a separation cavity for containing a heat conducting medium is formed among the heat conducting member, the fixing member and the carrier.

3. The catalyst strength destruction device according to claim 2, wherein The difference between the first distance and the second distance is 5 - 10 cm.

4. The catalyst strength destruction device according to claim 2, wherein, The heating member is disposed on at least one of the outer wall of the fixing member, the inner wall of the fixing member, and the bottom of the separation cavity.

5. The catalyst strength destruction device according to claim 1, characterized in that The covering member includes a covering portion and a buckling portion. The buckling portion is disposed on the covering portion. A buckling portion adapted to the buckling portion is disposed at the open end of the filter member, and the covering portion and the open end of the filter member are hermetically connected through the buckling portion and the buckling portion.

6. The catalyst strength destruction device according to claim 1, characterized in that The filter member includes a plurality of filtering portions, and the plurality of filtering portions are fixedly disposed on the carrier at equal intervals around the center of the stirring member.

7. The catalyst strength destruction device according to claim 6, wherein, The plurality of filtering portions are all filter meshes with fixed shapes, and the filter meshes are fixedly disposed on the carrier.

8. The catalyst strength destruction device according to claim 7, wherein, The aperture of the filter mesh is 0.1 - 2 mm.

9. A method for evaluating the strength of a supported catalyst, characterized in that, Including the following steps: S1: Measuring the strength of a fresh catalyst; S2: Filling the inside of the filter member of the catalyst strength destruction device according to any one of claims 1 - 8 with the fresh catalyst, and using the covering member of the catalyst strength destruction device to seal the open end of the filter member so as to fix the fresh catalyst inside the filter member; S3: Pouring a solvent into the accommodation cavity of the catalyst strength destruction device and submerging the open end of the filter member with the solvent, wherein the solvent is one or both of water and an organic solvent; S4: Simultaneously turning on the stirring member and the heating member of the catalyst strength destruction device to perform stirring treatment and heating treatment on the fresh catalyst to obtain a destroyed catalyst. The stirring speed of the stirring treatment is 100 - 1500 revolutions per minute, the stirring time of the stirring treatment is 4 - 24 hours, the heating temperature of the heating treatment is 30 - 100 °C, and the heating time of the heating treatment is 4 - 24 hours; S5: Measuring the strength of the destroyed catalyst.

10. The method for evaluating the strength of a supported catalyst according to claim 9, wherein, The shape of the catalyst is any one or two or more of cylindrical, strip-shaped, three-leaf strip-shaped, spherical, and irregular granular.

Citation Information

Patent Citations

  • Cyclohexanone preparation catalyst, and preparation method and application thereof

    CN106861734A

  • Catalyst evaluation device

    CN212364205U