Catalytic rectifying tower for thermal decomposition tert-butyl removal reaction

By integrating a distillation column, tubular reactor, and heated vessel into a catalytic distillation column, a continuous thermal decomposition of tert-butyl compounds to detert-butyl reaction was achieved, solving the problems of low reaction efficiency and numerous by-products in existing technologies, and improving production efficiency and equipment utilization.

CN222324274UActive Publication Date: 2025-01-10HUNAN XINLING CHEM CO LTD
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Patent Information

Application Number
CN202421153587.5
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-05-24
Publication Date
2025-01-10
Estimated Expiration
2034-05-24

AI Technical Summary

Technical Problem

In existing technologies, the detert-butylation reaction is generally carried out in batch operation, which results in low reaction efficiency, low production efficiency and large amount of by-products, especially a large amount of isobutylene oligomers.

Method used

A catalytic distillation column is designed, integrating the distillation column body, tubular reactor, and heating vessel into a single upper and lower structure. This enables the continuous production of tert-butyl compounds through thermal decomposition. The thermal decomposition reaction is carried out using concentrated sulfuric acid or solid acid catalysts, and the separation is achieved through the distillation column body.

Benefits of technology

This technology enables efficient and continuous production of tert-butyl compounds, reduces the amount of isobutylene oligomers generated, improves production efficiency, and saves equipment installation space and investment.

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Abstract

The utility model discloses a catalytic rectifying tower for thermal decomposition tert-butyl removal reaction, which comprises a rectifying tower body, a tubular reactor and a heating kettle body, the rectifying tower body, the tubular reactor and the heating kettle body are of a vertical integral structure, the rectifying tower body is positioned above the tubular reactor, and the heating kettle body is positioned below the tubular reactor. The rectification tower body, the tubular reactor and the heating kettle body are integrated together, the thermal decomposition tert-butyl removal reactor has the functions of a thermal decomposition tert-butyl removal reactor and a rectification tower, continuous industrial production of thermal decomposition tert-butyl removal of tert-butyl aromatic hydrocarbon compounds is achieved, the production efficiency is high, the amount of isobutene oligomer is small, and meanwhile the equipment installation land is saved.
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Description

Technical Field

[0001] The utility model relates to the field of catalytic distillation, in particular to a catalytic distillation tower for thermally decomposing and removing tert-butyl groups of tert-butyl compounds. Background Art

[0002] At present, the de-tert-butylation reaction generally adopts a process of first intermittent reaction and then distillation. For example, CN102898281A discloses a method for producing m-cresol and 6-tert-butyl-m-cresol by thermal decomposition reaction of 4,6-di-tert-butyl-m-cresol under the action of a catalyst, 4,6-di-tert-butyl-m-cresol and a catalyst are sent into a reactor according to a certain mass ratio, and the reaction temperature is controlled to be 120-210°C for thermal decomposition reaction. After the reaction, the materials are sent to a distillation tower to obtain m-cresol and 6-tert-butyl-m-cresol respectively. The device used in this method is intermittent operation, and the reaction efficiency and production efficiency are low. In addition, the reaction product isobutylene cannot be discharged quickly, and polymerization reaction is easy to occur, resulting in a large amount of by-products.

[0003] There is also an intermittent process for producing meta-cresol using concentrated sulfuric acid as a catalyst, which is commonly used by domestic peers in the industry. The actual production process is complicated to operate, has low production efficiency, and produces a large amount of by-products such as isobutylene oligomers. Summary of the invention

[0004] In view of the deficiencies in the prior art, the purpose of the utility model is to provide a catalytic distillation tower for thermal decomposition and detert-butylation of tert-butyl compounds, which has the functions of a thermal decomposition and detert-butylation reactor and a distillation tower, and can realize continuous industrial production of thermal decomposition and detert-butylation of tert-butyl compounds.

[0005] The technical solution adopted by the utility model is: a catalytic distillation tower for thermal decomposition and de-tert-butylation reaction, comprising a distillation tower body, a tubular reactor and a heating kettle body, wherein the distillation tower body, the tubular reactor and the heating kettle body are an upper and lower integral structure, the distillation tower body is located above the tubular reactor, and the heating kettle body is located below the tubular reactor.

[0006] The lower part of the distillation tower body is provided with a material distribution plate, a catalyst inlet and a reaction material inlet, and the mixed material outlet of the heating kettle body is connected with the reaction material inlet of the distillation tower body through a pipeline and a pump.

[0007] A packing layer is arranged on the upper part of the heating kettle body.

[0008] The heating kettle body is connected with a heater, and the heater can be inside the heating kettle body or outside the heating kettle body.

[0009] The tubular reactor, the distillation tower body and the heating kettle body are connected by flanges.

[0010] Compared with the traditional kettle intermittent process, the utility model has the following effects:

[0011] The utility model integrates a distillation tower body, a tubular reactor and a heating kettle body, has the functions of a thermal decomposition and tert-butyl removal reactor and a distillation tower, realizes the continuous industrial production of thermal decomposition and tert-butyl removal of tert-butyl compounds, and has good tert-butyl removal reaction effect of tert-butyl compounds, high production efficiency, and a small amount of by-products such as isobutylene oligomers, while also saving equipment installation land and reducing device investment. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 This is a schematic diagram of the structure of the utility model:

[0013] In the figure: 1. distillation tower body; 2. filler 1; 3. filler 2; 4. tubular reactor; 5. heat exchanger; 6. gas phase outlet; 7. distillation tower reflux liquid phase inlet; 8. feed inlet; 9. heating kettle body; 10. mixed material outlet; 11. catalyst inlet; 12. reaction material inlet; 13. exhaust port 14. drain port; 15. filler 3; 16. upper interface of liquid level gauge; 17. lower interface of liquid level gauge; 18. manhole; 19. flange; 20. heat carrier inlet 1; 21. heat carrier outlet 1; 22. heat carrier inlet 2; 23. heat carrier outlet 2; 24. material distribution plate. DETAILED DESCRIPTION

[0014] The embodiments of the present utility model are further described below in conjunction with the accompanying drawings.

[0015] like Figure 1 As shown, the utility model includes a distillation tower body 1, a tubular reactor 4 and a heating kettle body 9. The distillation tower body 1, the tubular reactor 4 and the heating kettle body 9 are connected by a flange 19 to form an upper and lower integral structure. The distillation tower body 1 is located above the tubular reactor 4, and the heating kettle body 9 is located below the tubular reactor 4.

[0016] The distillation tower body 1 is provided with two layers of packing, which is structured packing or random packing; the top of the distillation tower body 1 is provided with a gas phase outlet 6, which is connected to a cooler through a pipeline; the upper part of the distillation tower body 1 is provided with a distillation tower reflux liquid phase inlet 7, which is connected to the distillation tower body reflux pipeline; the lower part of the distillation tower body 1 is provided with a material distribution plate 24, a catalyst inlet 11 and a reaction material inlet 12, and the material inlet 12 is connected to the material distribution plate 24.

[0017] The tubular reactor 4 is provided with a heat carrier inlet 20 and an exhaust port 13 at the top, and a heat carrier outlet 21 and a liquid discharge port 14 at the bottom. The heat carrier inlet 20 and the heat carrier outlet 21 are respectively connected to the heat carrier pipeline from the outside.

[0018] The upper part of the heating kettle body is provided with a packing layer, the middle part is provided with a feed port 8, and the feed port 8 is connected to the raw material pipeline; the bottom is provided with a mixed material outlet 10, and the mixed material outlet 10 is connected to the reaction material inlet 12 through a pipeline and a pump; the side is provided with an upper interface 16 and a lower interface 17 of the liquid level gauge, which are respectively connected to the liquid level gauge through pipelines. The heating kettle body is also provided with a heat exchanger, and the upper part of the heat exchanger is provided with a heat carrier inlet 22, and the lower part is provided with a heat carrier outlet 23, which are respectively connected to the heat source through pipelines. Example 1

[0019] The material containing 4,6-di-tert-butyl-meta-cresol enters the heating kettle body 9 from the feed inlet 8, and is mixed with the material at the bottom of the tubular reactor 4 in the heating kettle body 9. After the mixed material is heated to 160°C by the heat exchanger 5, it comes out through the mixed material outlet 10, and continuously enters the reaction material inlet 12 through the pipeline and pump, and then enters the tubular reactor 4 after passing through the material distribution plate. Concentrated sulfuric acid is added through the catalyst inlet 11, and 4,6-di-tert-butyl-meta-cresol undergoes thermal decomposition and de-tert-butylation reaction under the action of concentrated sulfuric acid catalyst. The reaction gas phase product rises and enters the distillation tower body 1 for distillation separation, and the gas phase material containing isobutylene and meta-cresol is extracted from the top of the distillation tower body 1.

[0020] The results show that: 4,6-di-tert-butyl-meta-cresol material with a purity of 96.56% is continuously fed, concentrated sulfuric acid is used as a catalyst, the conversion rate of 4,6-di-tert-butyl-meta-cresol is greater than 99%, the yield of isobutylene oligomers is less than 8%, and the content of intermediate cresols in the reflux liquid phase inlet material of the distillation tower is greater than 90%. Example 2

[0021] The material containing 4,6-di-tert-butyl-meta-cresol enters the heating kettle body 9 from the feed inlet 8, and is mixed with the material at the bottom of the tubular reactor 4 in the heating kettle body 9. After the mixed material is heated to 180°C by the heat exchanger 5, it comes out through the mixed material outlet 10, and continuously enters the reaction material inlet 12 through the pipeline and pump, and then enters the tubular reactor 4 after passing through the material distribution plate 24. 4,6-di-tert-butyl-meta-cresol undergoes thermal decomposition and de-tert-butylation reaction under the action of the solid acid catalyst. The reaction gas phase product rises and enters the distillation tower body 1 for distillation separation, and the gas phase material containing isobutylene and meta-cresol is extracted from the top of the distillation tower body 1.

[0022] The results show that: 4,6-di-tert-butyl-meta-cresol material with a purity of 96.26% is continuously fed, sulfuric acid is used as a catalyst, the conversion rate of 4,6-di-tert-butyl-meta-cresol is greater than 99%, the yield of isobutylene oligomers is less than 8%, and the content of intermediate cresols in the reflux liquid phase inlet material of the distillation tower is greater than 90%.

[0023] The embodiments described in the present invention are merely descriptions of the implementation methods, and are not intended to limit the concept and scope of the present invention. Without departing from the design concept of the present invention, various modifications and improvements made to the technical solutions of the present invention by engineers and technicians in this field should all fall within the protection scope of the present invention.

Claims

1. A catalytic distillation tower for thermal decomposition and removal of tert-butyl groups, characterized in that: The invention comprises a distillation tower body, a tubular reactor and a heating kettle body, wherein the distillation tower body, the tubular reactor and the heating kettle body are an upper and lower integral structure, the distillation tower body is located above the tubular reactor, and the heating kettle body is located below the tubular reactor.

2. A catalytic distillation tower for thermal decomposition and tert-butyl removal according to claim 1, characterized in that: The distillation tower body is provided with two layers of fillers, the lower part of the distillation tower body is provided with a material distribution plate, a catalyst inlet and a reaction material inlet, and the mixed material outlet of the heating kettle body is connected to the reaction material inlet of the distillation tower body through a pipeline and a pump.

3. A catalytic distillation tower for thermal decomposition and tert-butyl removal according to claim 1, characterized in that: A packing layer is arranged on the upper part of the heating kettle body.

4. A catalytic distillation tower for thermal decomposition and tert-butyl removal according to claim 1, characterized in that: The heating kettle body is connected with a heater, and the heater is inside the heating kettle body, or outside the heating kettle body and connected through a pipeline.

5. A catalytic distillation tower for thermal decomposition and tert-butyl removal according to claim 1, characterized in that: The tubular reactor, the distillation tower body and the heating kettle body are connected by flanges.

Citation Information

Patent Citations

  • Method for co-producing 2, 6-butylated hydroxytoluene and m-cresol as well 6-tertiry butyl m-cresol by utilizing cresol mixture

    CN102898281A