Heavy component efficient recovery and reutilization device for tertiary butanol dehydration process

The combined distillation and extraction process efficiently recovers methyl tert-butyl ether and tert-butanol from the dehydration process of tert-butanol, solving the problem of ineffective separation and recovery of valuable components in heavy materials, achieving economical and efficient reuse, and reducing the production cost of isobutylene.

CN224236105UActive Publication Date: 2026-05-15ZHEJIANG CENWAY MATERIALS CO LTD
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Patent Information

Application Number
CN202521443544.5
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-07-10
Publication Date
2026-05-15
Estimated Expiration
2035-07-10

AI Technical Summary

Technical Problem

In the chemical production process of dehydrating tert-butanol to prepare isobutylene, a large amount of unreacted tert-butanol and methyl tert-butyl ether contained in the heavy component material could not be effectively separated and recovered, resulting in economic losses and waste of raw materials, and increasing production costs.

Method used

A two-stage series distillation and extraction system is used. The device, consisting of a distillation column, condenser, reflux tank, reflux pump, and extraction column, utilizes the differences in boiling points and water solubility of the components to recover methyl tert-butyl ether and tert-butanol, achieving efficient separation and reuse.

Benefits of technology

The recovery rate of tert-butanol reached 99% and methyl tert-butyl ether reached 95%, which reduced the raw material consumption and significantly reduced the production cost of isobutylene.

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Abstract

The utility model provides a device for efficiently recovering and reusing heavy components in a tertiary butanol dehydration process. The device comprises a rectifying tower; a condenser; a reflux tank; a reflux pump; an extraction column; a feed line; one end of the tower top steam pipeline is connected with a tower top steam outlet of the rectifying tower, and the other end is connected with a condensation inlet of the condenser; a condensate line; one end of the reflux suction pipeline is connected with the liquid outlet of the reflux tank, and the other end is connected with the fluid inlet of the reflux pump; one end of the reflux supply pipeline is connected with a fluid outlet of the reflux pump, a first branch at the other end of the reflux supply pipeline is connected with the upper part of the rectifying tower, and a second branch at the other end of the reflux supply pipeline is connected with an external methyl tert-butyl ether product storage tank; one end of the intermediate material pipeline is connected with the tower kettle material outlet of the rectifying tower, and the other end is connected with the material inlet of the extraction tower; and a water washing agent supply line. According to the utility model, methyl tert-butyl ether and tert-butyl alcohol in heavy components in the tert-butyl alcohol dehydration process can be efficiently recovered and reutilized.
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Description

Technical Field

[0001] This utility model relates to a heavy component recovery and reuse device, specifically a high-efficiency recovery and reuse device for heavy components in a tert-butanol dehydration process, belonging to the field of chemical equipment technology. Background Technology

[0002] In the chemical production process of dehydrating tert-butanol (TBA) to prepare isobutylene, the reaction products need to be purified by distillation to obtain the target product, isobutylene. During the separation process, a liquid stream consisting of multiple components, known as the "heavy component," is usually separated from the bottom of the heavy component removal column. This stream is typically sold cheaply as low-concentration tert-butanol, resulting in very low added value.

[0003] Analysis revealed that the heavy component contained a large amount of valuable chemicals, including approximately 35% unreacted tert-butanol (TBA) and a staggering 40% methyl tert-butyl ether (MTBE), a byproduct. Tert-butanol is a core raw material for isobutylene production, while MTBE is itself a major chemical raw material and a high-octane gasoline additive. In the existing process, these high-value components have not been effectively separated and recovered, resulting not only in significant economic losses but also in a serious waste of raw materials, directly increasing the production cost of isobutylene.

[0004] Therefore, there is an urgent need in the field to develop a device that can economically and efficiently recover valuable components from this particular heavy component material. Utility Model Content

[0005] Based on the above background, the purpose of this utility model is to provide a device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process, which can efficiently recover and reuse methyl tert-butyl ether and tert-butanol in the heavy components in the tert-butanol dehydration process.

[0006] To achieve the above-mentioned objectives, this utility model provides the following technical solution:

[0007] A device for efficient recovery and reuse of heavy components in a tert-butanol dehydration process includes:

[0008] A distillation column, wherein the distillation column is provided with a raw material inlet, a top steam outlet, and a bottom material outlet;

[0009] A condenser, wherein the condenser is provided with a condensation inlet and a condensation outlet;

[0010] A reflux tank, wherein the reflux tank is provided with a liquid inlet and a liquid outlet;

[0011] A reflux pump, wherein the reflux pump is provided with a fluid inlet and a fluid outlet;

[0012] The extraction tower is equipped with a material inlet, a washing agent inlet, a raffinate outlet at the top of the tower, and an extract phase outlet at the bottom of the tower.

[0013] The feed line has one end connected to an external low-concentration tert-butanol source and the other end connected to the feed inlet of the distillation column.

[0014] The top vapor pipeline is connected at one end to the top vapor outlet of the distillation column and at the other end to the condensation inlet of the condenser.

[0015] The condensate line is connected at one end to the condensate outlet of the condenser and at the other end to the liquid inlet of the reflux tank.

[0016] The reflux suction line is connected at one end to the liquid outlet of the reflux tank and at the other end to the fluid inlet of the reflux pump.

[0017] The reflux supply pipeline has one end connected to the fluid outlet of the reflux pump, the first branch of the other end connected to the upper part of the distillation column, and the second branch of the other end connected to an external methyl tert-butyl ether product storage tank.

[0018] The intermediate material pipeline is connected at one end to the bottom material outlet of the distillation column and at the other end to the material inlet of the extraction column.

[0019] The washing agent supply pipeline has one end connected to an external process water source and the other end connected to the washing agent inlet of the extraction tower.

[0020] Preferably, the tert-butanol dehydration process heavy component high-efficiency recovery and reuse device also includes a reboiler. The inlet of the reboiler is connected to the bottom of the distillation column, and the outlet of the reboiler is connected to the lower part of the distillation column. The reboiler is used to heat the liquid in the bottom of the distillation column.

[0021] Preferably, the device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process also includes a cooler, which is located on the intermediate material pipeline and is used to cool the material collected from the bottom of the distillation column.

[0022] Preferably, the device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process also includes a bottom pump, which is installed on the intermediate material pipeline and located between the bottom material outlet of the distillation column and the cooler.

[0023] Preferably, the tert-butanol dehydration process high-efficiency recovery and reuse device for heavy components also includes a tert-butanol buffer tank and an extraction phase conveying pipeline. One end of the extraction phase conveying pipeline is connected to the extraction phase outlet of the bottom of the extraction tower, and the other end is connected to the inlet of the tert-butanol buffer tank.

[0024] Preferably, the device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process also includes an extraction phase transfer pump, which is connected to the outlet of the tert-butanol buffer tank.

[0025] Preferably, the device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process also includes a raffinate pipeline, one end of which is connected to the raffinate outlet at the top of the extraction tower for drawing out the raffinate.

[0026] Compared with the prior art, the present invention has the following advantages:

[0027] This invention relates to a device for efficient recovery and reuse of recombinant components in a tert-butanol dehydration process. Through a combination of distillation and water washing extraction, it can efficiently recover valuable components from by-products, with a tert-butanol recovery rate of over 99% and a methyl tert-butyl ether recovery rate of over 95%. This transforms low-value-added by-products into high-value products and reusable raw materials. The recovered tert-butanol can be directly returned to the dehydration reaction system as a raw material, significantly reducing the unit consumption of tert-butanol and thus directly reducing the production cost of isobutylene. Attached Figure Description

[0028] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on the provided drawings without creative effort.

[0029] Figure 1 This is a schematic diagram of a device for efficient recovery and reuse of heavy components in a tert-butanol dehydration process according to this utility model;

[0030] In the diagram: 1. Distillation column; 2. Condenser; 3. Reflux tank; 4. Reflux pump; 5. Extraction column; 6. Reboiler; 7. Cooler; 8. Bottom pump; 9. Tert-butanol buffer tank; 10. Extraction phase transfer pump; 11. Feed line; 12. Top vapor line; 13. Condensate line; 14. Reflux suction line; 15. Reflux supply line; 16. Intermediate material line; 17. Washing agent supply line; 18. Extraction phase transfer line; 19. Raffinate line. Detailed Implementation

[0031] The technical solution of this utility model will be further described in detail below through specific embodiments and in conjunction with the accompanying drawings. It should be understood that the implementation of this utility model is not limited to the following embodiments, and any modifications and / or alterations made to this utility model will fall within the protection scope of this utility model.

[0032] In this invention, unless otherwise specified, all parts and percentages are by weight, and the equipment and raw materials used are commercially available or commonly used in the field. Unless otherwise specified, the methods in the following embodiments are conventional methods in the field. Unless otherwise specified, the components or equipment in the following embodiments are general standard parts or components known to those skilled in the art, and their structures and principles can be learned by those skilled in the art through technical manuals or conventional experimental methods.

[0033] The embodiments of the present invention will be described in detail below with reference to the accompanying drawings. In the following detailed description, many specific details are set forth to facilitate explanation and provide a comprehensive understanding of the embodiments of the present invention. However, one or more embodiments may be practiced by those skilled in the art without these specific details.

[0034] This invention discloses an efficient recovery and reuse device for heavy components in a tert-butanol dehydration process, comprising a two-stage distillation system and an extraction system connected in series. The first-stage distillation system utilizes the difference in boiling points of the components to preferentially separate low-boiling-point methyl tert-butyl ether. The second-stage extraction system utilizes the high water solubility of tert-butanol to separate it from other components that are poorly soluble in water.

[0035] The distillation system specifically includes a distillation column 1, a condenser 2, a reflux tank 3, a reflux pump 4, and a reboiler 6, as well as a feed line 11, a top vapor line 12, a condensate line 13, a reflux suction line 14, and a reflux supply line 15. The distillation column 1 has a feed inlet, a top vapor outlet, and a bottom product outlet. The condenser 2 has a condensation inlet and a condensation outlet. The reflux tank 3 has a liquid inlet and a liquid outlet. The reflux pump 4 has a fluid inlet and a fluid outlet. One end of the feed line 11 is connected to an external low-concentration tert-butanol source, and the other end is connected to the feed inlet of the distillation column 1. One end of the top vapor line 12 is connected to the top vapor outlet of the distillation column 1, and the other end is connected to the condensation inlet of the condenser 2. One end of the condensate line 13 is connected to the condensation outlet of the condenser 2, and the other end is connected to the liquid inlet of the reflux tank 3. One end of the reflux suction line 14 is connected to the liquid outlet of the reflux tank 3, and the other end is connected to the fluid inlet of the reflux pump 4. One end of the reflux supply line 15 is connected to the fluid outlet of the reflux pump 4, and the first branch of the other end is connected to the upper part of the distillation column 1 to send most of the liquid back to the upper part of the distillation column 1 as reflux. The second branch of the other end is used to connect to an external methyl tert-butyl ether product storage tank to draw out the methyl tert-butyl ether product. The inlet of the reboiler 6 is connected to the bottom of the distillation column 1, and the outlet of the reboiler 6 is connected to the lower part of the distillation column 1. The reboiler 6 is used to heat the liquid in the bottom of the distillation column 1.

[0036] The extraction system includes an extraction column 5, a tert-butanol buffer tank 9, an extractant phase transfer pump 10, a washing agent supply line 17, an extractant phase transfer line 18, and a raffinate phase line 19. The extraction column 5 has a material inlet, a washing agent inlet, a raffinate phase outlet at the top of the column, and an extractant phase outlet at the bottom of the column. One end of the washing agent supply line 17 is connected to an external process water source, and the other end is connected to the washing agent inlet of the extraction column 5. One end of the extractant phase transfer line 18 is connected to the extractant phase outlet at the bottom of the extraction column 5, and the other end is connected to the inlet of the tert-butanol buffer tank 9. The extractant phase transfer pump 10 is connected to the outlet of the tert-butanol buffer tank 9. One end of the raffinate phase line 19 is connected to the raffinate phase outlet at the top of the extraction column 5 for discharging the raffinate phase. The raffinate phase outlet at the top of the column is connected to the outside via the raffinate phase line 19, providing a discharge channel for the remaining, water-insoluble, and low-value organic phase after extraction and separation, allowing it to be collected as a byproduct.

[0037] The distillation system and the extraction system are connected via an intermediate processing unit. The intermediate processing unit includes an intermediate feed line 16, a bottom pump 8, and a cooler 7. One end of the intermediate feed line 16 is connected to the bottom outlet of the distillation column 1, and the other end is connected to the inlet of the extraction column 5. The cooler 7 is located on the intermediate feed line 16 and is used to cool the bottom product from the distillation column 1. The extraction separation effect is highly sensitive to temperature. Cooling the high-temperature bottom product discharged from the distillation column 1 can significantly improve the solubility of tert-butanol in water while reducing the solubility of other impurities, thereby improving the separation efficiency and product purity of the subsequent extraction column 5. The bottom pump 8 is located on the intermediate feed line 16, between the bottom outlet of the distillation column 1 and the cooler 7.

[0038] The workflow of the device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process is described below.

[0039] The heavy component material containing methyl tert-butyl ether (MTBE) and tert-butanol, from the bottom of the external de-heavy column, is fed into the distillation column 1 via feed line 11. The bottom liquid in the lower part of the distillation column 1 is heated to 85-95°C by the reboiler 6 to provide a heat source for the distillation process. The MTBE with the lower boiling point preferentially vaporizes and accumulates at the top of the column. The vapor at the top of the column is condensed by the condenser 2 and enters the reflux tank 3. After being pressurized by the reflux pump 4, part of it is returned to the top of the column as reflux, and the other part is collected as high-purity MTBE product.

[0040] The high-temperature mixture remaining after separation in the bottom of distillation column 1, mainly containing tert-butanol, is pressurized by the bottom pump 8, cooled to approximately 40°C by the cooler 7, and then enters extraction column 5. Simultaneously, process water enters extraction column 5 through the washing agent supply line 17. Inside the column, the water and material come into full contact, utilizing the high water solubility of tert-butanol to extract it from other water-poor organic phases into the aqueous phase, forming the extract phase.

[0041] Inside extraction tower 5, the denser extract phase (tert-butanol aqueous solution) settles to the bottom of the tower and enters the tert-butanol buffer tank 9 via extract phase delivery pipeline 18. Finally, the extract phase delivery pump 10 returns the solution to the dehydration reaction tower of the main process, realizing the reuse of raw materials. The less dense raffinate phase is drawn off from the top of the tower as a by-product.

[0042] With the above-mentioned device, the by-product streams that were previously processed at low cost are now thoroughly and efficiently separated and utilized, significantly improving the economic efficiency of the entire process.

[0043] This article uses specific examples to illustrate the principles and implementation methods of this utility model. The descriptions of the above embodiments are only for the purpose of helping to understand the method and core ideas of this utility model. It should be noted that for those skilled in the art, several improvements and modifications can be made to this utility model without departing from the principles of this utility model, and these improvements and modifications also fall within the protection scope of the claims of this utility model.

Claims

1. A device for efficient recovery and reuse of heavy components in a tert-butanol dehydration process, characterized in that: The tert-butanol dehydration process includes a high-efficiency recovery and reuse device for heavy components, comprising: A distillation column (1) is provided with a raw material inlet, a top steam outlet, and a bottom material outlet; Condenser (2), wherein the condenser (2) is provided with a condensation inlet and a condensation outlet; The reflux tank (3) is provided with a liquid inlet and a liquid outlet; A reflux pump (4) is provided with a fluid inlet and a fluid outlet; Extraction tower (5), wherein the extraction tower (5) is provided with a material inlet, a washing agent inlet, a raffinate outlet at the top of the tower and an extract phase outlet at the bottom of the tower; The feed line (11) is connected at one end to an external low-concentration tert-butanol source and at the other end to the feed inlet of the distillation column (1). The top steam pipeline (12) is connected at one end to the top steam outlet of the distillation column (1) and at the other end to the condensation inlet of the condenser (2); The condensate line (13) is connected at one end to the condensate outlet of the condenser (2) and at the other end to the liquid inlet of the return tank (3); The reflux suction line (14) is connected at one end to the liquid outlet of the reflux tank (3) and at the other end to the fluid inlet of the reflux pump (4); The reflux supply line (15) is connected at one end to the fluid outlet of the reflux pump (4), and the first branch at the other end is connected to the upper part of the distillation column (1), and the second branch at the other end is used to connect to the external methyl tert-butyl ether product storage tank. The intermediate material pipeline (16) is connected at one end to the bottom material outlet of the distillation column (1) and at the other end to the material inlet of the extraction column (5); The washing agent supply pipeline (17) is connected at one end to an external process water source and at the other end to the washing agent inlet of the extraction tower (5).

2. The device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process according to claim 1, characterized in that: The tert-butanol dehydration process heavy component high-efficiency recovery and reuse device also includes a reboiler (6). The inlet of the reboiler (6) is connected to the bottom of the distillation column (1), and the outlet of the reboiler (6) is connected to the lower part of the distillation column (1). The reboiler (6) is used to heat the liquid in the bottom of the distillation column (1).

3. The device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process according to claim 1, characterized in that: The device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process also includes a cooler (7), which is located on the intermediate material pipeline (16) and is used to cool the material collected from the bottom of the distillation column (1).

4. The device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process according to claim 3, characterized in that: The device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process also includes a bottom pump (8), which is located on the intermediate material pipeline (16) and between the bottom material outlet of the distillation column (1) and the cooler (7).

5. The device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process according to claim 1, characterized in that: The tert-butanol dehydration process high-efficiency recovery and reuse device for heavy components also includes a tert-butanol buffer tank (9) and an extraction phase delivery pipeline (18). One end of the extraction phase delivery pipeline (18) is connected to the extraction phase outlet of the bottom of the extraction tower (5), and the other end is connected to the inlet of the tert-butanol buffer tank (9).

6. The device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process according to claim 5, characterized in that: The device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process also includes an extraction phase transfer pump (10), which is connected to the outlet of the tert-butanol buffer tank (9).

7. The device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process according to claim 1, characterized in that: The device for efficient recovery and reuse of heavy components in the tert-butanol dehydration process also includes a raffinate pipeline (19), one end of which is connected to the raffinate outlet at the top of the extraction tower (5) for drawing out the raffinate.