Continuous supply system of propylene carbonylation catalyst
By designing a continuous supply system for catalyst preparation tanks and storage tanks, the problem of unstable catalyst supply was solved, the catalyst activity was maintained continuously and the safety of the reaction was improved, thus ensuring the stability and safety of the propylene carbonylation reaction.
Patent Information
- Application Number
- CN202423065987.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-12
- Publication Date
- 2026-02-17
- Estimated Expiration
- 2034-12-12
AI Technical Summary
In the existing technology, the catalyst supply system in the propylene carbonylation reaction cannot achieve continuous and stable supply, resulting in decreased catalyst activity and insufficient reaction safety. In particular, the presence of flammable and explosive gases under high temperature and high pressure conditions increases the danger.
A continuous supply system comprising a catalyst preparation tank and a catalyst storage tank was designed. The interior of the storage tank is divided into an aqueous phase chamber and an oil phase chamber by a partition. Combined with a vacuum pump and nitrogen input, a continuous and homogeneous supply of catalyst is achieved, and the aqueous and oil phases are separated under abnormal operating conditions to ensure catalyst activity and reaction safety.
This ensures the continuous maintenance of catalyst activity, enhances the safety and stability of the reaction, guarantees the continuity and safety of the propylene carbonylation reaction, and avoids the risk of catalyst deactivation and oxygen-induced explosion.
Smart Images
Figure CN223915352U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to the technical field of chemical synthesis, specifically relates to a continuous feeding system of propylene carbonylation catalyst. BACKGROUND
[0002] Butanol and octanol are important organic chemical, fine chemical and chemical auxiliary raw materials, are widely used in the synthesis of lubricant, solvent, defoaming agent, additive, antioxidant and so on and the industry such as photography, printing and dyeing, paper sizing. The wide use of butanol and octanol promotes the butanol and octanol consumption and output to increase year by year.
[0003] At present, the process of producing butyraldehyde by propylene carbonylation reaction is most widely used in butanol and octanol production, which uses n-butyraldehyde as solvent, and propylene and synthesis gas generate n-butyraldehyde and isobutyraldehyde under the action of catalyst, n-butyraldehyde and isobutyraldehyde are separated by isomerization tower, and n-butyraldehyde obtained after separation is condensed and dehydrated to generate octylene aldehyde under the catalysis of sodium hydroxide, and octylene aldehyde is hydrogenated to produce crude octanol, and the product octanol is obtained by rectification.
[0004] The catalyst used in propylene carbonylation reaction is generally rhodium phosphine catalyst, such as acetylacetone triphenyl phosphine rhodium carbonyl, and the rhodium contained in the catalyst is a rare noble metal, which needs to be recycled and reused by separating the catalyst in the product-catalyst separation process after the completion of the carbonylation reaction. With the extension of the use time of the catalyst, the catalyst gradually deactivates, and part of the recycled catalyst needs to be washed and activated, and new catalyst needs to be added to maintain a certain reaction rate. In the actual process, in order to promote the full contact between the catalyst and the reaction material, the catalyst is dispersed in the solvent, and then mixed with the recycled catalyst, and then input into the carbonylation reaction process. In order to continuously input the catalyst into the reaction system, a continuous catalyst feeding system needs to be developed to match the continuous propylene carbonylation reaction process. UTILITY MODEL CONTENT
[0005] In view of the deficiencies in the prior art, the utility model discloses a continuous feeding system of propylene carbonylation catalyst, which can continuously and stably provide catalyst to the propylene carbonylation reaction process and promote the anaerobic control of the reaction process.
[0006] In order to realize the above technical purpose, the utility model provides a continuous feeding system of propylene carbonylation catalyst, which comprises a catalyst preparation tank and a catalyst storage tank, wherein:
[0007] The first feed inlet of the catalyst preparation tank is connected with a solvent input pipe, and the second feed inlet is used for inputting catalyst, and the first discharge port is connected with the first feed inlet of the catalyst storage tank;
[0008] The catalyst storage tank comprises a shell, a partition plate parallel to the central axis of the shell is arranged in the shell, the partition plate is connected with the bottom and the wall of the shell but not connected with the top of the shell, and the shell is divided into a water phase cavity and an oil phase cavity; the second feeding port of the catalyst is connected with a recycled catalyst input pipe, and the recycled catalyst input pipe extends to the water phase cavity or the oil phase cavity; the first discharging port of the catalyst storage tank is connected with a downstream carbonylation reaction process, the second discharging port is connected with a downstream water separation process, and the third discharging port is connected with a vacuum pump.
[0009] In one aspect of the utility model, the above technical solution can realize supplement of newly prepared catalyst solution into the recycled and washed catalyst, so that the catalyst solution maintains high catalyst activity. Specifically, with the reaction, the recycled catalyst gradually deactivates, and the propylene carbonylation is a strong exothermic reaction, which causes the occurrence of side reactions and further affects the catalytic activity, so it is necessary to supplement the newly prepared catalyst into the recycled catalyst. In the utility model, the new catalyst solution is prepared in the catalyst preparation tank, the pipeline connected between the catalyst preparation tank and the catalyst storage tank is used for supplementing the newly prepared catalyst into the recycled and washed catalyst, and after the two are mixed and homogenized in the catalyst storage tank, the first discharging port continuously and stably outputs the catalyst solution to the downstream carbonylation reaction process.
[0010] In another aspect of the utility model, the anaerobic control of the subsequent carbonylation reaction process can be promoted. In the propylene carbonylation reaction, propylene and synthesis gas comprising carbon monoxide (CO) and hydrogen (H2) generate butyraldehyde under the action of the catalyst. In this process, carbon monoxide and hydrogen are both flammable and explosive gases, and the presence of oxygen may increase the risk of the reaction system, such as causing explosion. In addition, the rhodium phosphine catalyst used in the reaction process has high sensitivity to oxygen, and the presence of oxygen may cause the catalyst to deactivate or performance to decrease, thereby affecting the reaction and the selectivity of the product. The third discharging port of the catalyst storage tank used for mixing the newly prepared catalyst solution and the recycled and washed catalyst solution is connected with the vacuum pump, so that the catalyst storage tank is in negative pressure or micro-negative pressure, which is beneficial to the precipitation of dissolved oxygen in the liquid phase in the shell, thereby improving the safety of the subsequent carbonylation reaction and maintaining the catalytic activity of the catalyst.
[0011] The utility model discloses another aspect, above technical scheme can be in the catalyst washing recovery process, the water content of the catalyst circulatingly washed and recovered is too high when the working condition of failure, effectively separate the water contained in catalyst solution. Specifically, the casing of catalyst storage tank is provided with the baffle, and the casing is divided into water phase cavity and oil phase cavity, and the circulating recovery catalyst input pipe extends to the water phase cavity, makes the oil phase in the circulating recovery catalyst overflow to the oil phase cavity through the baffle, mixes with the catalyst solution input from the catalyst preparation tank, and then is input to the downstream carbonylation reaction process from the first discharge port in the lower part of the oil phase cavity, and the water phase accumulates in the lower part of the water phase cavity and is finally input to the downstream washing water separation process through the second discharge port for further treatment, thereby improving the stability of the propylene carbonylation production process.
[0012] Compared with the prior art, the utility model has the advantages that: the utility model discloses a catalyst preparation tank and a catalyst storage tank, which are combined to supplement new catalyst into the circulating recovery catalyst, so as to maintain the catalytic activity of the catalyst solution; the catalyst storage tank is connected with a vacuum pump, which is beneficial to the precipitation of dissolved oxygen in the catalyst solution, improves the safety of the downstream carbonylation reaction, and improves the catalytic activity; by arranging a baffle in the catalyst storage tank, the water phase and the oil phase in the circulating recovery catalyst can be separated when the water washing tower or the gas tower fails, so that the catalyst solution can be continuously and stably provided to the propylene carbonylation reaction process. BRIEF DESCRIPTION OF DRAWINGS
[0013] The drawings accompanying the specification of this application form a part hereof, serve to provide further understanding of the application, and together with the description of the exemplary embodiments of the application given herein, serve to explain the application. In the drawings:
[0014] Figure 1 Fig. 1 shows a structure diagram of a continuous supply system of the propylene carbonylation catalyst according to the utility model;
[0015] Figure 2 Fig. 2 shows another structure diagram of the continuous supply system of the propylene carbonylation catalyst according to the utility model.
[0016] In the above drawings, the following reference signs are used:
[0017] 1-catalyst preparation tank, 2-catalyst storage tank, 21-casing, 22-baffle, 31-solvent input pipe, 32-circulating recovery catalyst input pipe, 33-first nitrogen input pipe, 34-first bubbling device, 35-second nitrogen input pipe, 36-second bubbling device, 37-first branch, 41-liquid level meter, 42-on-off valve. DETAILED DESCRIPTION
[0018] For the convenience of understanding the present application, the present application will be described more fully below with reference to the preferred embodiments thereof. These embodiments, however, are to be regarded as merely illustrative and not restrictive in nature. That is, the present application is not to be limited to the embodiments presented herein.
[0019] Unless otherwise defined, the technical terms used in the following examples have the same meanings as commonly understood by those skilled in the art to which the present application pertains. The test reagents used in the following examples are all conventional biochemical reagents unless otherwise specified. The experimental methods used in the following examples are all conventional methods unless otherwise specified.
[0020] In the present application, unless otherwise explicitly specified and limited, the first feature is "on" or "under" the second feature can include the first and second features directly contact, or can include the first and second features are not directly contact but contact through another feature between them. Moreover, the first feature is "on", "above" and "on the" the second feature includes the first feature above and oblique above the second feature, or just means the first feature is horizontally higher than the second feature. The first feature is "under", "below" and "under" the second feature includes the first feature below and oblique below the second feature, or just means the first feature is horizontally lower than the second feature.
[0021] In addition, the terms "first", "second", "third", "fourth" and the like are used only for descriptive purposes and should not be construed as indicating or implying relative importance or an indicated number of technical features. Therefore, the features defined with "first", "second" and the like can explicitly or implicitly include one or more of the features. In the description of the present application, unless otherwise specified, the meaning of "a plurality of" is two or more.
[0022] Example 1
[0023] A continuous supply system of a propylene carbonylation catalyst, such as Figure 1As shown, the system comprises a catalyst preparation tank 1 and a catalyst storage tank 2, wherein: the first feed port of the catalyst preparation tank 1 is connected to a solvent input pipe 31, the second feed port is used for inputting catalyst, and the first discharge port is connected to the first feed port of the catalyst storage tank 2; the catalyst storage tank 2 comprises a shell 21, a partition plate 22 parallel to the central axis of the shell 21 is arranged in the shell 21, the partition plate 22 is connected to the bottom and the wall of the catalyst storage tank 2 but not connected to the top of the catalyst storage tank 2, thereby dividing the shell 21 into an aqueous phase cavity and an oil phase cavity; the second feed port of the catalyst storage tank 2 is connected to a recycled catalyst input pipe 32, and the recycled catalyst input pipe 32 extends to the aqueous phase cavity or the oil phase cavity; the first discharge port of the catalyst storage tank 2 is connected to a downstream carbonylation reaction process, the second discharge port is connected to a downstream water separation process, and the third discharge port is connected to a vacuum pump.
[0024] In the embodiment, the catalyst preparation tank 1 is used to prepare new catalysts to supplement the recycled catalyst solution, so as to maintain the catalytic activity of the recycled catalyst solution.
[0025] The catalyst storage tank 2 in the embodiment is used for the sufficient mixing of the newly prepared catalysts and the recycled catalysts and continuously inputting the catalyst solution to the subsequent propylene carbonylation reaction process.
[0026] In order to promote the anaerobic control of the subsequent carbonylation reaction process, the third discharge port of the catalyst storage tank 2 is connected to a vacuum pump, so that the shell 21 of the catalyst storage tank 2 maintains a negative pressure or a slight negative pressure, which is beneficial to the precipitation of dissolved oxygen in the catalyst solution, beneficial to the anaerobic operation of the downstream process, and avoids the reduction of the catalytic activity of the catalyst due to the presence of oxygen.
[0027] The catalyst storage tank 2 is provided with a partition plate 22 for dividing the cavity in the shell 21 into an aqueous phase cavity and an oil phase cavity:
[0028] Under normal conditions of catalyst preparation, storage and output, the newly prepared catalyst solution input from the catalyst preparation tank 1 and the catalyst solution recovered after water washing input from the circulating recovery catalyst input pipe 32 are mixed in the water phase cavity and the oil phase cavity in the catalyst storage tank 2; at this time, the embodiment is not limited to the relative positions of the first feed port and the second feed port of the catalyst storage tank 2 on the shell 21 of the catalyst storage tank 2, and can be optionally input into the water phase cavity or the oil phase cavity, or simultaneously input into the water phase cavity or the oil phase cavity; at this time, the relative height of the partition plate 22 in the shell 21 is not limited, and the height beneficial to the mixing of the newly prepared catalyst solution and the circulating recovery catalyst solution can be optionally set by the person skilled in the art; at this time, the relative position of the first discharge port on the shell 21 of the catalyst storage tank 2 is not limited, and the first discharge port can be optionally arranged at the lower part of the shell 21, or at the lower part of the water phase cavity or the oil phase cavity, for leading out the fully mixed catalyst and inputting the catalyst into the subsequent propylene carbonylation reaction process; under normal conditions, the pipeline connected with the second discharge port of the catalyst storage tank 2 will be used as a standby pipeline and will not be put into use.
[0029] When an abnormal condition occurs in the upstream circulating washing and recovery process, the water washing tower for washing the catalyst fails to operate, which will cause a certain amount of water to be contained in the catalyst recovered by the circulating washing and recovery, at this time, the circulating recovery catalyst input pipe 32 will extend to the water phase cavity, the oil phase material in the circulating washing and recovery catalyst will overflow through the partition plate 22 to the oil phase cavity, and will be mixed with the newly prepared catalyst solution input from the catalyst preparation tank 1, and finally will be input into the subsequent carbonylation reaction process through the first discharge port at the lower part of the oil phase cavity; and the water phase accumulated at the lower part of the water phase cavity will be output through the second discharge port of the catalyst storage tank 2 to the downstream washing water separation process for further treatment.
[0030] It should be noted that the position of the water phase cavity or the oil phase cavity relative to the shell 21 is not limited in the utility model, and it can be understood that when an abnormal condition occurs in the upstream circulating recovery catalyst process, the circulating recovery catalyst input pipe 32 extends to the cavity of the catalyst storage tank 2, which is the water phase cavity, and the opposite cavity will be the oil phase cavity.
[0031] Optionally, stirring paddles are arranged in the catalyst preparation tank 1 to promote the dispersion of the solvent and the catalyst.
[0032] It should be noted that in order to promote the process efficiency, the person skilled in the art can arrange a circulating pump, a compressor or other devices or equipment for improving the material flow efficiency on the pipeline for flowing the liquid phase material or the gas phase material based on the utility model, and the protection scope of the utility model is not limited by this.
[0033] Embodiment 2
[0034] Based on the continuous supply system of the propylene carbonylation catalyst shown in embodiment 1, like Figure 2As shown, the third inlet of the catalyst storage tank 2 in this embodiment is connected to the first nitrogen input pipe 33, and the first nitrogen input pipe 33 extends into the catalyst storage tank 2. The third outlet of the catalyst storage tank 2 is connected to a vacuum pump or to a flare. Thus, in the actual process, the first nitrogen input pipe 33 can input nitrogen below the liquid level of the catalyst storage tank 2. By inputting nitrogen into the catalyst storage tank 2, disturbance to the catalyst solution can be formed, which promotes the precipitation of dissolved oxygen therein and promotes the anaerobic control of the subsequent carbonylation reaction process.
[0035] In this embodiment, the third outlet of the catalyst storage tank 2 can be connected to a vacuum pump, so that the first nitrogen input pipe 33 is optimized in cooperation with the vacuum pump to promote the precipitation of dissolved oxygen; alternatively, the third outlet of the catalyst storage tank 2 can not be connected to a vacuum but to a flare, which outputs the nitrogen that is blown into the catalyst solution in the catalyst storage tank 2, so that the system can be operated stably.
[0036] Embodiment 3
[0037] Based on the continuous supply system of the propylene carbonylation catalyst shown in embodiment 2, in this embodiment, the first nitrogen input pipe 33 extends into the aqueous phase cavity and / or the oil phase cavity in the catalyst storage tank 2; the first nitrogen input pipe 33 is used to input nitrogen below the liquid level in the catalyst storage tank 2 to disturb the liquid phase and promote the precipitation of dissolved oxygen, so the first nitrogen input pipe can input the aqueous phase cavity and / or the oil phase cavity in the catalyst storage tank 2 to facilitate its function.
[0038] Embodiment 4
[0039] Based on the continuous supply system of the propylene carbonylation catalyst shown in embodiment 2 or 3, in this embodiment, the first nitrogen input pipe 33 is connected to the first bubbling device 34, which improves the uniformity of nitrogen input below the liquid level in the catalyst storage tank 2 and increases the mass transfer.
[0040] Alternatively, the first bubbling device 34 includes a ring pipe with gas outlet holes that communicates with the first nitrogen input pipe 33. Those skilled in the art can select appropriate bubbling devices as needed to promote the uniform distribution of nitrogen below the liquid level.
[0041] Embodiment 5
[0042] Based on the continuous supply system of the propylene carbonylation catalyst shown in embodiment 1, in this embodiment, the second outlet of the catalyst preparation tank 1 is connected to a vacuum pump, so that the catalyst preparation tank 1 can be kept under negative pressure or micro-negative pressure, which is conducive to the precipitation of dissolved oxygen in the solvent in the catalyst preparation tank 1.
[0043] The present invention does not limit the solvent used to prepare the catalyst. For example, iron-free butyraldehyde or mixed butyraldehyde can be selected. Those skilled in the art can choose according to their needs, and this does not limit the scope of protection of the present invention.
[0044] Example 6
[0045] Based on the continuous supply system of the propylene carbonylation catalyst shown in Example 5, in this example, the third inlet of the catalyst preparation tank 1 is connected to the second nitrogen input pipe 35 and the second nitrogen input pipe 35 extends into the catalyst preparation tank 1, and the second outlet is connected to the vacuum pump. The nitrogen input by the second nitrogen input pipe 35 can cause disturbance below the liquid level in the catalyst preparation tank 1. Combined with the use of the vacuum pump, it can synergistically optimize and promote the release of dissolved oxygen.
[0046] Example 7
[0047] Based on the continuous supply system of the propylene carbonylation catalyst shown in Example 1, in this example, the third inlet of the catalyst preparation tank 1 is connected to the second nitrogen input pipe 35 and the second nitrogen input pipe 35 extends into the catalyst preparation tank 1, and the second outlet is connected to the flare. The nitrogen input by the second nitrogen input pipe 35 can cause disturbance below the liquid surface in the catalyst preparation tank 1 to promote the release of dissolved oxygen in the catalyst solution.
[0048] In the actual process of this embodiment, the input nitrogen gas is output from the second nitrogen gas input pipe 3 and then transported to the flare from the second discharge port of the catalyst preparation tank 1.
[0049] Example 8
[0050] Based on the continuous supply system of the propylene carbonylation catalyst shown in Example 6 or 7, in this example, the second nitrogen input pipe 35 is connected to the second bubbling device 36. Through the dispersing effect of the second bubbling device 36, nitrogen is continuously and uniformly input into the catalyst preparation tank 1, which enhances the disturbance effect and promotes dissolved oxygen evolution.
[0051] Optionally, the second bubbling device 36 includes an annular tube with an outlet hole connected to the second nitrogen inlet pipe 35. Those skilled in the art can select a bubbling device with a suitable structure as needed to promote the uniform distribution of nitrogen under the liquid surface.
[0052] Example 9
[0053] Based on the continuous supply system of propylene carbonylation catalyst shown in Example 1, in this embodiment, a first branch 37 is provided on the pipeline connecting the catalyst preparation tank 1 and the catalyst storage tank 2. The first branch 37 is connected to the downstream carbonylation reaction process, which can realize the direct input of newly prepared catalyst to the downstream carbonylation process. This can meet the catalyst supply requirements of special working conditions or other working conditions when the catalyst is replaced, and improve the stability of the continuous supply system of propylene carbonylation catalyst of this utility model.
[0054] Example 10
[0055] Based on the continuous supply system of propylene carbonylation catalyst shown in Example 1, the catalyst storage tank 2 in this example is equipped with a level gauge 41, and a switch valve 42 connected to the level gauge 41 is installed on the pipeline connected to the first outlet of the catalyst storage tank 2. Through the interlock control of the catalyst storage tank 2 and the catalyst output pipeline, the level of process automation is improved, which is also conducive to improving the safety of the overall propylene carbonylation process.
[0056] Optionally, a second branch is provided on the pipeline connected to the first outlet of the catalyst storage tank 2, and a flow regulating valve connected to the liquid level gauge 41 is provided on the second branch to regulate the flow rate of the catalyst input to the downstream carbonylation reaction process.
[0057] It should be noted that the above description is a further detailed explanation of the present invention in conjunction with specific embodiments, and should not be construed as limiting the specific implementation of the present invention to these descriptions; the dimensional data in this embodiment do not limit the technical solution, but merely illustrate one specific working condition. For those skilled in the art to which this invention pertains, several simple improvements and modifications can be made without departing from the concept of the present invention, and all such improvements and modifications should be considered to fall within the scope of protection of the present invention.
Claims
1. A continuous supply system for a propylene carbonylation catalyst, characterized in that, It includes a catalyst preparation tank (1) and a catalyst storage tank (2), wherein: The first inlet of the catalyst preparation tank (1) is connected to the solvent input pipe (31), the second inlet is used to input the catalyst, and the first outlet is connected to the first inlet of the catalyst storage tank (2). The catalyst storage tank (2) includes a shell (21), and a partition (22) parallel to the central axis of the shell (21) is provided inside the shell (21). The partition (22) is connected to the bottom and tank wall of the catalyst storage tank (2) but not to the top of the catalyst storage tank (2), dividing the interior of the shell (21) into an aqueous phase chamber and an oil phase chamber. The second inlet of the catalyst storage tank (2) is connected to a circulating catalyst input pipe (32), and the circulating catalyst input pipe (32) extends to the aqueous phase chamber or the oil phase chamber. The first outlet of the catalyst storage tank (2) is connected to the downstream carbonylation reaction process, the second outlet is connected to the downstream washing water separation process, and the third outlet is connected to a vacuum pump.
2. The continuous supply system for the propylene carbonylation catalyst according to claim 1, characterized in that, The third inlet of the catalyst storage tank (2) is connected to the first nitrogen input pipe (33), and the first nitrogen input pipe (33) extends into the catalyst storage tank (2). The third outlet of the catalyst storage tank (2) is connected to a vacuum pump or to a flare.
3. The continuous supply system for the propylene carbonylation catalyst according to claim 2, characterized in that, The first nitrogen inlet pipe (33) extends into the water phase chamber and / or oil phase chamber within the catalyst storage tank (2).
4. The continuous supply system for the propylene carbonylation catalyst according to claim 2 or 3, characterized in that, The first nitrogen input pipe (33) is connected to the first bubbling device (34).
5. The continuous supply system for the propylene carbonylation catalyst according to claim 1, characterized in that, The second outlet of the catalyst preparation tank (1) is connected to a vacuum pump.
6. The continuous supply system for the propylene carbonylation catalyst according to claim 5, characterized in that, The third inlet of the catalyst preparation tank (1) is connected to the second nitrogen input pipe (35), and the second nitrogen input pipe (35) extends into the catalyst preparation tank (1), and the second outlet is connected to the vacuum pump.
7. The continuous supply system for the propylene carbonylation catalyst according to claim 1, characterized in that, The third inlet of the catalyst preparation tank (1) is connected to the second nitrogen input pipe (35), and the second nitrogen input pipe (35) extends into the catalyst preparation tank (1), and the second outlet is connected to the flare.
8. The continuous supply system for the propylene carbonylation catalyst according to claim 6 or 7, characterized in that, The second nitrogen inlet pipe (35) is connected to the second bubbling device (36).
9. The continuous supply system for the propylene carbonylation catalyst according to claim 1, characterized in that, A first branch (37) is provided on the pipeline connecting the catalyst preparation tank (1) and the catalyst storage tank (2), and the first branch (37) is connected to the downstream carbonylation reaction process.
10. The continuous supply system for the propylene carbonylation catalyst according to claim 1, characterized in that, The catalyst storage tank (2) is equipped with a level gauge (41), and a switch valve (42) connected to the first outlet of the catalyst storage tank (2) is installed on the pipeline that communicates with the level gauge (41).