Regeneration device for olefin epoxidation deactivated titanium silicalite molecular sieve catalyst
By constructing a regeneration device composed of methanol distillation towers, the activity of titanium silicon molecular sieve is restored by using methanol washing and acidification treatment, the problem of activity reduction caused by small pore size is solved, and efficient regeneration and economic benefits are achieved.
Patent Information
- Application Number
- CN202422384801.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-29
- Publication Date
- 2025-08-01
- Estimated Expiration
- 2034-09-29
AI Technical Summary
The existing titanium silicon molecular sieve catalysts have a decrease in activity due to small pore size in olefin epoxidation reaction, and high-temperature calcination and regeneration will reduce the specific surface area and destroy the lattice structure, affecting the reaction efficiency.
A regeneration device consisting of a methanol distillation tower, a methanol reboiler, a catalyst acidifying kettle, a methanol reflux pump, etc. is used to restore the catalyst activity through methanol washing and acidification treatment, and an anchor stirrer and membrane tube are used to prevent catalyst loss.
It realizes efficient regeneration of the catalyst, restores catalytic activity, is simple to operate and has high economic benefits.
Smart Images
Figure CN223170934U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the field of chemical industry, in particular to a regeneration device for a titanium silicon molecular sieve catalyst deactivated by olefin epoxidation. Background Art
[0002] In recent years, titanium silicate molecular sieves have received widespread attention as catalysts for olefin epoxidation. In a series of catalytic epoxidation reactions such as ketoamine oximation and olefin epoxidation, titanium silicate molecular sieves have shown good activity. However, due to the small pore size of titanium silicate molecular sieves, it is not conducive to the diffusion of reactants and products, resulting in a rapid decrease in catalyst activity after a period of reaction. The catalyst must be regenerated before it can be used.
[0003] Currently, the common method for regenerating molecular sieve catalysts is high-temperature calcination. After calcination and regeneration, the specific surface area of the catalyst will decrease. At the same time, high temperature may cause the destruction of the catalyst lattice structure, thereby affecting the reaction efficiency. Utility Model Content
[0004] In view of the above-mentioned defects or deficiencies in the prior art, it is desired to provide a regeneration device for a deactivated titanium silicalite catalyst for olefin epoxidation.
[0005] According to the technical solution provided in the embodiment of the present application, a regeneration device for a deactivated titanium silicon molecular sieve catalyst for olefin epoxidation includes a methanol distillation tower, a methanol reboiler, a methanol cooler, a catalyst acidification kettle, a methanol reflux pump, a methanol feed pump, a fresh methanol storage tank, a bag filter, and an acid storage tank. The discharge port of the methanol distillation tower is connected to the methanol cooler through a pipeline, and the bottom discharge port and the side return port of the methanol distillation tower are connected to the methanol reboiler through a return pipe. The methanol cooler is connected to the catalyst acidification kettle feed port a through a pipeline. The catalyst acidification kettle discharge port a is connected to the methanol reflux pump through a pipeline, the methanol reflux pump is connected to the side of the methanol distillation tower feed port a through a pipeline, the fresh methanol storage tank discharge port is connected to the methanol feed pump through a pipeline, the outlet pipe of the methanol feed pump is connected in parallel to the pipeline between the catalyst acidification kettle and the methanol distillation tower, the catalyst acidification kettle discharge port b is connected to the bag filter through a pipeline, the bag filter is connected to the fresh methanol storage tank feed port through a pipeline, and the methanol distillation tower kettle is connected to the acid liquid storage tank through a pipeline.
[0006] In the present invention, further, the number of plates in the methanol distillation tower is 10-20.
[0007] In the present invention, further, the solvent that the methanol distillation tower should be initially provided with is fresh methanol.
[0008] In the present invention, further, the bottom of the methanol distillation tower intermittently discharges a small amount of acid liquid to the acid liquid storage tank.
[0009] In the present utility model, further, the catalyst acidification kettle is provided with a jacket.
[0010] In the present utility model, further, the catalyst acidification kettle is provided with an electric stirrer, and the electric stirrer is an anchor stirrer, and a feeding port is arranged at the top of the catalyst acidification kettle.
[0011] In the present utility model, further, 1 - 2 membrane tubes should be arranged at the end of the pipeline where the methanol reflux pump enters the catalyst acidification kettle.
[0012] In summary, the beneficial effects of the present application are as follows: This device has the advantages of simple operation, good regeneration activity, and high economic benefits. Description of the Drawings
[0013] By reading the detailed description of the non - restrictive embodiments with reference to the following drawings, other features, purposes, and advantages of the present application will become more obvious:
[0014] Figure 1 It is a structural schematic diagram of the catalyst regeneration device.
[0015] Reference numerals in the figure:
[0016] 1 - Methanol rectification tower; 2 - Methanol reboiler; 3 - Methanol cooler; 4 - Catalyst acidification kettle; 5 - Methanol reflux pump; 6 - Methanol feed pump; 7 - Fresh methanol storage tank; 8 - Bag filter; 9 - Acid liquid storage tank. Detailed Embodiments
[0017] The following further elaborates on the present application in conjunction with the drawings and embodiments. It can be understood that the specific embodiments described herein are only used to explain the relevant utility model and do not limit the utility model. Additionally, it should be noted that for the sake of description, only the parts related to the utility model are shown in the drawings.
[0018] It should be noted that, without conflict, the embodiments in the present application and the features in the embodiments can be combined with each other. The following will detail the present application with reference to the drawings and embodiments.
[0019] As Figure 1 shown, the regeneration device for the deactivated titanium - silicon molecular sieve catalyst used in the present application is composed of a methanol rectification tower 1, a methanol reboiler 2, a methanol cooler 3, a catalyst acidification kettle 4, a methanol reflux pump 5, a methanol feed pump 6, a fresh methanol storage tank 7, a bag filter 8, an acid liquid storage tank 9, etc.;
[0020] As Figure 1As shown in the figure, the outlet of the methanol distillation column 1 is connected to the methanol cooler 3. The methanol cooler 3 can cool the distilled methanol. The methanol reboiler 2 is arranged on the side of the methanol distillation column 1 through a pipeline, and the methanol reboiler 2 heats the methanol distillation column 1. The number of trays of the methanol distillation column 1 is 10 - 20. The solvent initially set in the methanol distillation column 1 should be fresh methanol, and the top temperature of the methanol distillation column 1 is set at 64.7 °C, and the temperature of the methanol cooler 3 is set at 5 - 15 °C. A small amount of acid liquid is intermittently discharged from the bottom of the methanol distillation column 1 to the acid liquid storage tank 9.
[0021] As Figure 1 shown in the figure, the methanol cooler 3 is connected to the feed inlet of the catalyst acidification kettle 4 through a pipeline. The outlet at the top of the catalyst acidification kettle 4 is connected to the methanol reflux pump 5 through a pipeline. The catalyst acidification kettle 4 is equipped with a jacket, and the heating medium is steam or hot water with a temperature of 55 - 60 °C. The catalyst acidification kettle 4 is equipped with an electric stirrer, and the electric stirrer is an anchor-type stirrer. There is a feeding port at the top of the catalyst acidification kettle 4 for adding catalyst and acid. 1 - 2 membrane tubes should be arranged at the end of the pipeline where the methanol reflux pump 5 enters the catalyst acidification kettle 4 to prevent the catalyst from being drawn into the methanol distillation column. There is acid in the catalyst acidification kettle 4, and the acid is one of hydrochloric acid, sulfuric acid, and nitric acid.
[0022] As Figure 1 shown in the figure, the methanol reflux pump 5 is connected to the side of the feed inlet a of the methanol distillation column 1 through a pipeline. The fresh methanol storage tank 7 is connected to the methanol feed pump 6 through a pipeline. The outlet pipe of the methanol feed pump 6 is in parallel with the pipelines of the methanol distillation column 1 and the catalyst acidification kettle 4. The methanol flow rate extracted by the methanol reflux pump 6 is equal to the methanol evaporation amount of the methanol distillation column 1 to keep the liquid level in the acidification kettle stable. The outlet b of the catalyst acidification kettle 4 is connected to the bag filter 8 through a pipeline. The bag filter 8 is connected to the feed inlet of the fresh methanol storage tank 7 through a pipeline. The bottom of the methanol distillation column 1 is connected to the feed inlet of the acid liquid storage tank 9 through a pipeline.
[0023] As Figure 1 shown in the figure, methanol is pumped into the catalyst acidification kettle 4 through the methanol feed pump 6 to wash the deactivated catalyst therein until the epoxide content therein is less than 1%. Then, a certain amount of methanol is pumped into the catalyst acidification kettle 4 through the methanol feed pump 6, and a small amount of hydrochloric acid is added through the feeding port. Steam or hot water at 55 - 60 °C is introduced into the jacket of the catalyst acidification kettle 4, and the electric stirrer is started. The methanol reboiler 2 and the methanol cooler 3 are turned on. When methanol is extracted, the methanol reflux pump 5 is turned on, and the methanol in the catalyst acidification kettle 4 is pumped into the methanol distillation column 1 through the methanol reflux pump 5, and the methanol enters a circulating state to keep the liquid level in the catalyst acidification kettle 4 stable. After the methanol circulates for a period of time, the methanol in the catalyst acidification kettle 4 is replaced with fresh methanol. Each system is turned off, and the methanol in the catalyst acidification kettle 4 enters the fresh methanol storage tank 7 through the bag filter 8. Thus, the catalyst regeneration is completed.
[0024] In summary, after the regeneration is completed, the catalyst enters the bag filter 8 to filter out the catalyst therein. At this time, the filtrate is high-purity methanol, which can directly enter the fresh methanol storage tank, and the catalyst is taken out from the bag filter 8 and directly used for the reaction. The deactivated catalyst is washed with fresh methanol in a circulating manner under acidic stirring conditions to remove the organic matter in the catalyst, and the organic matter in the catalyst pores is taken out.
[0025] The above description is only for the preferred embodiments of the present application and the description of the technical principle and other solutions used. At the same time, the scope of the utility model involved in the present application is not limited to the technical solutions formed by the specific combination of the above technical features, and should also cover other technical solutions formed by any combination of the above technical features or their equivalent features without departing from the inventive concept of the utility model. For example, the technical solutions formed by the mutual replacement of the above features with the technical features (but not limited to) having similar functions disclosed in the present application.
Claims
1. A regeneration device for a deactivated titanium-silicate molecular sieve catalyst for olefin epoxidation, comprising a methanol rectification column (1), a methanol reboiler (2), a methanol cooler (3), a catalyst acidification kettle (4), a methanol reflux pump (5), a methanol feed pump (6), a fresh methanol storage tank (7), a bag filter (8) and an acid solution storage tank (9), characterized in that: The outlet of the methanol rectification column (1) is connected to the methanol cooler (3) through a pipeline. The bottom outlet and the side return port of the methanol rectification column (1) are connected to the methanol reboiler (2) through a return pipeline. The methanol cooler (3) is connected to the inlet a at the top of the catalyst acidification kettle (4) through a pipeline. The outlet a of the catalyst acidification kettle (4) is connected to the methanol reflux pump (5) through a pipeline. The methanol reflux pump (5) is connected to the inlet a on the side of the methanol rectification column (1) through a pipeline. The outlet of the fresh methanol storage tank (7) is connected to the methanol feed pump (6) through a pipeline. The outlet pipe of the methanol feed pump (6) is connected in parallel to the pipeline between the catalyst acidification kettle (4) and the methanol rectification column (1). The outlet b of the catalyst acidification kettle (4) is connected to the bag filter (8) through a pipeline. The bottom of the methanol rectification column (1) is connected to the acid solution storage tank (9) through a pipeline.
2. The regeneration device for deactivating a titanium silicalite molecular sieve catalyst for olefin epoxidation according to claim 1, characterized in that: The number of trays in the methanol rectification column (1) is 10 - 20.
3. The regeneration device for deactivated titanium silicalite molecular sieve catalyst for olefin epoxidation according to claim 1, characterized in that: The solvent initially provided in the methanol rectification column (1) should be fresh methanol.
4. The regeneration device for deactivating a titanium silicalite molecular sieve catalyst for olefin epoxidation according to claim 1, characterized in that: The bottom of the methanol rectification column (1) intermittently discharges a small amount of acid solution to the acid solution storage tank (9).
5. The regeneration device for deactivating titanium silicalite molecular sieve catalyst for olefin epoxidation according to claim 1, characterized in that: The catalyst acidification kettle (4) is provided with a jacket.
6. The regeneration device for deactivating a titanium-silicate molecular sieve catalyst for olefin epoxidation according to claim 1, characterized in that: The catalyst acidification kettle (4) is provided with an electric stirrer, and the electric stirrer is an anchor-type stirrer. The top of the catalyst acidification kettle (4) is provided with a feeding port.
7. The regeneration device for deactivating a titanium silicalite molecular sieve catalyst for olefin epoxidation according to claim 1, characterized in that: 1 - 2 membrane tubes should be provided at the end of the pipeline where the methanol reflux pump (5) enters the catalyst acidification kettle (4).