Tert-butyl alcohol purification device

Through the purification device composed of a distillation tower and an adsorption tower, the problem of difficult removal of impurities in co-oxidation of propylene oxide co-oxidation method is solved, and the production of high-purity tert-butanol is achieved, reducing production costs and improving production efficiency.

CN223299585UActive Publication Date: 2025-09-05NOVASHIN CO LTD
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Patent Information

Application Number
CN202422561091.8
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-10-22
Publication Date
2025-09-05
Estimated Expiration
2034-10-22

AI Technical Summary

Technical Problem

In the existing co-oxidation process of propylene oxide co-producing tert-butanol, impurities are difficult to separate, resulting in difficulty in reaching 99.9% of purity and high production costs.

Method used

The purification device consisting of a distillation tower, a reboiler, a tower kettle liquid condenser and an adsorption tower is used to remove low boiling matter, and the adsorption tower is adsorbed impurities. The purification process is monitored by online detection equipment, and the adsorption tower is switched and regenerated to achieve the production of high-purity tert-butanol.

Benefits of technology

The purity of tert-butanol is achieved to reach 99.9%, reducing production costs, improving production efficiency and operating stability of the device.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model belongs to the technical field of organic matter purification devices, and particularly relates to a tertiary butanol purification device. The purification device comprises a rectifying tower, a reboiler, a tower kettle liquid condenser and an adsorption tower; the bottom of the rectifying tower is connected with a reboiler; the reboiler is used for supplying heat to the rectifying tower; a raw material inlet is formed in the rectifying tower, and the rectifying tower is connected with an external tert-butyl alcohol raw material pipeline through the raw material inlet and used for guiding a tert-butyl alcohol crude product into the rectifying tower; a gas phase outlet is formed in the top of the rectifying tower and is used for guiding out rectified low-boiling-point substances; the top of the rectifying tower is provided with a liquid phase outlet, the liquid phase outlet is connected with a tower kettle liquid condenser through a rectifying tower bottom liquid phase pipeline, the tower kettle liquid condenser is connected with the adsorption tower through a tower kettle cooling liquid pipeline, the top of the adsorption tower is provided with a product outlet, and the product outlet leads out pure tert-butyl alcohol through a pure tert-butyl alcohol pipeline. The TBA purification device can purify TBA to obtain high-purity TBA of which the purity is greater than or equal to 99.9%, so that the market requirement is met.
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Description

Technical Field

[0001] The utility model belongs to the technical field of organic matter purification devices, in particular to a tert-butyl alcohol purification device. Background Art

[0002] Tert-butyl alcohol (TBA), as a precursor for the production of important chemical raw materials such as methyl tert-butyl ether, high-purity isobutylene, and methyl methacrylate, is widely used in many fields such as coatings, medicine, and agriculture.

[0003] The main industrial production methods for tert-butyl alcohol include propylene oxide co-oxidation to produce TBA, sulfuric acid hydration, and resin hydration. Among them, the propylene oxide co-oxidation method produces TBA with fewer impurities and higher purity, making it the most economical TBA production method.

[0004] However, the process of co-producing TBA by propylene oxide co-oxidation is complex. The co-produced TBA carries impurities such as water, methanol, acetone, methyl acetate, sec-butanol, isopropanol, and methyl ethyl ketone, which are difficult to separate. After industrial refining, the factory can produce TBA with a purity of 99.5%. However, it is difficult to completely remove impurities such as isopropanol, sec-butanol, and water in TBA, and the purification is relatively difficult. As a result, the production of high-purity TBA is difficult and the price is relatively high. Utility Model Content

[0005] In order to improve the deficiencies of the existing technology, the utility model provides a tert-butanol purification device, which can purify TBA, especially TBA co-produced by propylene oxide co-oxidation, to obtain high-purity TBA with a purity of ≥99.9%, meeting market needs.

[0006] As mentioned above, the utility model provides a tert-butyl alcohol purification device, which includes a distillation tower, a reboiler, a bottom liquid condenser and an adsorption tower;

[0007] The bottom of the distillation tower is connected to the reboiler, and the reboiler is used to provide heat for the distillation tower;

[0008] The distillation tower is provided with a raw material inlet, and the distillation tower is connected to an external tert-butanol raw material pipeline through the raw material inlet, so as to introduce the crude tert-butanol product into the distillation tower;

[0009] The top of the distillation tower is provided with a gas phase outlet for discharging the low-boiling substances obtained by distillation;

[0010] A liquid phase outlet is provided at the bottom of the distillation tower, and the liquid phase outlet is connected to the bottom liquid condenser through the bottom liquid phase pipeline of the distillation tower. The bottom liquid condenser is connected to the adsorption tower through the bottom coolant pipeline. A product outlet is provided at the top of the adsorption tower, and the product outlet guides the pure tert-butanol after distillation through the pure tert-butanol pipeline.

[0011] According to an embodiment of the present invention, the crude tert-butanol product, that is, the crude TBA product, is TBA co-produced by a propylene oxide co-oxidation process.

[0012] According to an embodiment of the present invention, the crude TBA product is TBA with a purity of ≥95%.

[0013] According to the embodiment of the present utility model, the purification device further includes a tower top condenser and a reflux tank, the gas phase outlet is connected to the tower top condenser through the distillation tower gas phase pipeline, and the tower top condenser is connected to the reflux tank through the tower top condensate pipeline.

[0014] According to the implementation scheme of the present utility model, the reflux tank is provided with a reflux liquid outlet and a condensate outlet. The reflux liquid outlet returns the reflux liquid to the distillation tower through the reflux liquid pipeline, and the condensate outlet transfers the condensate to the outside through the tower top condensate production pipeline.

[0015] According to the embodiment of the present invention, the number of the adsorption towers is greater than or equal to 2; one of them is used for online adsorption, and the others are used as backup for adsorbent regeneration or replacement, for example, including a first adsorption tower and a second adsorption tower.

[0016] According to the embodiment of the present invention, the adsorption tower is filled with a solid adsorbent. Preferably, the solid adsorbent is selected from at least one of activated alumina, zeolite, molecular sieve, activated carbon, modified carbon fiber, macroporous adsorption resin, etc.

[0017] According to the embodiment of the present invention, the adsorption tower is equipped with a heat preservation and heating device to maintain the adsorption temperature at 28°C-40°C.

[0018] According to the embodiment of the present invention, an online detection device is provided on the pure TBA pipeline for monitoring the purification of tert-butanol (for example, monitoring the concentration of tert-butanol, impurity concentration, etc.) and determining whether it is necessary to switch the adsorption tower.

[0019] Beneficial effects

[0020] 1) The tert-butyl alcohol purification device of the present invention comprises a distillation tower, a reboiler, a bottom liquid condenser, and an adsorption tower. The reboiler is used to heat the crude TBA in the distillation tower to remove low-boiling substances such as water, methanol, and acetone from the crude TBA. The remaining portion is condensed by the bottom liquid condenser and then enters the adsorption tower. The filler in the adsorption tower adsorbs the remaining impurities such as methyl acetate, sec-butyl alcohol, and methyl ethyl ketone, thereby obtaining high-purity TBA with a purity of ≥99.9%.

[0021] 2) The tert-butyl alcohol purification device of the utility model includes at least two adsorption towers. When in use, the purification status of the tert-butyl alcohol is monitored in real time by an online detection device on the TBA pipeline to determine whether the impurity adsorption capacity of the current adsorption tower is qualified. If the capacity is unqualified, the standby adsorption tower is switched to. At the same time, the adsorption tower with a high impurity content after use is regenerated, and the adsorption tower can be recycled, thereby improving production efficiency and reducing production costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a schematic structural diagram of the tert-butyl alcohol purification device in the utility model.

[0023] Among them, 1. TBA raw material pipeline, 2. distillation tower gas phase pipeline, 3. distillation tower bottom liquid phase pipeline, 4. tower top condensate pipeline, 5. reflux liquid pipeline, 6. tower top condensate production pipeline, 7. tower bottom cooling liquid pipeline, 8. pure TBA pipeline. DETAILED DESCRIPTION

[0024] The following will further explain the structure of the present invention in detail with reference to specific embodiments. It should be understood that the following embodiments are merely exemplary illustrations and explanations of the present invention and should not be construed as limiting the scope of protection of the present invention. All technologies implemented based on the above-mentioned content of the present invention are included within the scope of protection intended by the present invention.

[0025] In the description of the present invention, it should be noted that the terms "center", "up", "down", "left", "right", "vertical", "horizontal", "inside", "outside", etc., indicating directions or positional relationships, are based on the directions or positional relationships shown in the accompanying drawings. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction. Therefore, they cannot be understood as limitations on the present invention.

[0026] In the description of this utility model, it should be noted that, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "connected" should be understood in a broad sense. For example, they can refer to fixed connections, detachable connections, or integral connections; mechanical connections, electrical connections; direct connections, indirect connections through an intermediate medium, and internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in this utility model based on the specific circumstances.

[0027] Example 1

[0028] See also Figure 1As shown, a tert-butanol purification device includes a distillation tower A, a reboiler B, a bottom liquid condenser C, a top condenser D, a reflux tank E, and several adsorption towers. The number of adsorption towers is set according to actual needs. During use, one adsorption tower is used for adsorption, and the other adsorption towers are kept in standby. In this embodiment, there are two adsorption towers: a first adsorption tower F1 and a second adsorption tower F2.

[0029] A raw material inlet is provided on the distillation tower A, which is connected to the external TBA raw material pipeline 1 through the raw material inlet for introducing the crude TBA product produced by the propylene oxide co-oxidation process (especially suitable for TBA with a content of ≥95% as a by-product of the co-oxidation process) into the distillation tower A.

[0030] A gas phase outlet is provided at the top of the distillation tower A, which is connected to the top condenser D through the distillation tower gas phase pipeline 2. The top condenser D is connected to the reflux tank E through the top condensate pipeline 4. The reflux tank E is provided with a reflux liquid outlet and a condensate outlet. The reflux liquid outlet returns the reflux liquid to the distillation tower A through the reflux liquid pipeline 5, and the condensate outlet transfers the condensate to the outside through the top condensate production pipeline 6.

[0031] A liquid phase outlet is provided at the bottom of the distillation tower A, which is connected to the bottom liquid condenser C through the distillation tower bottom liquid phase pipeline 3. The bottom liquid condenser C is connected to the first adsorption tower F1 and / or the second adsorption tower F2 through the bottom coolant pipeline 7. Specifically, the connection point is located at the bottom of the first adsorption tower F1 and the second adsorption tower F2. The top of the first adsorption tower F1 and the second adsorption tower F2 is provided with a product outlet, and the product outlet discharges pure TBA through the pure TBA pipeline 8.

[0032] The bottom of distillation tower A is connected to reboiler B, which provides heat for distillation tower A. Low-boiling substances in the crude TBA product in distillation tower A are evaporated by the heat and then flow through distillation tower A's vapor outlet and distillation tower vapor pipeline 2 to the overhead condenser D for cooling and condensation. The condensate flows back to the top of distillation tower A through the reflux outlet and reflux pipeline 5, while the remainder is withdrawn as low-boiling substances. The bottom liquid of distillation tower A is cooled in condenser C and then flows into the first adsorption tower F1 and the second adsorption tower F2. Two adsorption towers are installed: one for online adsorption and the other as a standby for adsorbent regeneration or replacement.

[0033] The adsorption tower is equipped with a heat preservation and heating device to maintain the adsorption temperature at 28℃-40℃.

[0034] The first adsorption tower F1 and the second adsorption tower F2 are filled with a solid adsorbent, which is selected from at least one of activated alumina, zeolite, molecular sieve, activated carbon, modified carbon fiber, macroporous adsorption resin, etc. The adsorbent is used to adsorb methanol and acetone, and partially adsorb esters, isobutanol, sec-butanol, ketones, etc.

[0035] The pure TBA pipeline 8 is provided with an online detection device to monitor the purification status of tert-butanol (for example, the concentration of tert-butanol), determine whether the current adsorption tower's ability to adsorb impurities is qualified, and switch to a spare adsorption tower if it is unqualified. At the same time, the adsorption tower with a high impurity content after use is regenerated, and the adsorption tower can be recycled to improve production efficiency and reduce production costs. At the same time, timely switching of the adsorption tower can also effectively and quickly adsorb impurities, thereby effectively increasing the concentration of tert-butanol.

[0036] In the present invention, the TBA raw material pipeline 1, the distillation tower gas phase pipeline 2, the distillation tower bottom liquid phase pipeline 3, the tower top condensate pipeline 4, the reflux liquid pipeline 5, the tower top condensate production pipeline 6, the tower bottom coolant pipeline 7, and the pure TBA pipeline 8 adopt gas or liquid transportation pipelines known in the art.

[0037] The above examples illustrate the specific implementation methods of the present invention. However, the scope of protection of the present invention is not limited to the above-mentioned exemplary implementation methods. Any modifications, equivalent substitutions, improvements, etc. made by those skilled in the art within the spirit and principles of the present invention shall be included in the scope of protection of the claims of the present invention.

Claims

1. A tert-butyl alcohol purification device, characterized in that, The purification device includes a distillation tower, a reboiler, a bottom liquid condenser and an adsorption tower; The bottom of the distillation tower is connected to the reboiler, and the reboiler is used to provide heat for the distillation tower; The distillation tower is provided with a raw material inlet, and the distillation tower is connected to an external tert-butanol raw material pipeline through the raw material inlet, so as to introduce the crude tert-butanol product into the distillation tower; The top of the distillation tower is provided with a gas phase outlet for discharging the low-boiling substances obtained by distillation; A liquid phase outlet is provided at the bottom of the distillation tower, and the liquid phase outlet is connected to the bottom liquid condenser through the bottom liquid phase pipeline of the distillation tower. The bottom liquid condenser is connected to the adsorption tower through the bottom coolant pipeline. A product outlet is provided at the top of the adsorption tower, and the product outlet leads pure tert-butanol through the pure tert-butanol pipeline.

2. The tert-butyl alcohol purification device according to claim 1, wherein The crude tert-butanol product is tert-butanol with a purity of ≥95%.

3. The tert-butyl alcohol purification device according to claim 2, wherein The crude tert-butanol is tert-butanol co-produced by propylene oxide co-oxidation.

4. The tert-butyl alcohol purification device according to claim 1, characterized in that The purification device further comprises a tower top condenser and a reflux tank, the gas phase outlet is connected to the tower top condenser via a distillation tower gas phase pipeline, and the tower top condenser is connected to the reflux tank via a tower top condensate pipeline.

5. The tert-butyl alcohol purification device according to claim 4, characterized in that The reflux tank is provided with a reflux liquid outlet and a condensate outlet. The reflux liquid outlet returns the reflux liquid to the distillation tower through the reflux liquid pipeline, and the condensate outlet transfers the condensate to the outside through the tower top condensate extraction pipeline.

6. The tert-butyl alcohol purification device according to any one of claims 1 to 5, characterized in that The number of the adsorption towers is greater than or equal to 2; one of them is used for online adsorption, and the others are used as backup for adsorbent regeneration or replacement.

7. The tert-butyl alcohol purification device according to any one of claims 1 to 5, characterized in that: The adsorption tower is filled with solid adsorbent.

8. The tert-butyl alcohol purification device according to any one of claims 1 to 5, characterized in that: The adsorption tower is equipped with a heat preservation and heating device.

9. The tert-butyl alcohol purification device according to any one of claims 1 to 5, characterized in that: The pure tert-butanol pipeline is provided with an online detection device for monitoring the purification of tert-butanol and determining whether it is necessary to switch the adsorption tower.