Tetrahydrofuran purification device

Abstract

The utility model belongs to the technical field of chemical solvent preparation, and particularly relates to a tetrahydrofuran purification device. The utility model provides a tetrahydrofuran purification device. The tetrahydrofuran purification device comprises a feed port, a catalytic hydrogenation reaction part, a gas phase discharge port, a liquid phase discharge port, a heavy component removal tower and an absorption tower. In the application, through the catalytic hydrogenation part, the impurity dihydrofuran in the tetrahydrofuran is hydrogenated to generate the tetrahydrofuran, the impurities n-butyraldehyde and isobutyraldehyde are hydrogenated to generate alcohols which are easily separated from the tetrahydrofuran, through determination, the content of the impurity dihydrofuran in the purified tetrahydrofuran is reduced to 3 ppm or below, the alcohols are separated in the heavy component removal tower, and the content of the tetrahydrofuran in the tetrahydrofuran is reduced to 3 ppm or below. The purity and the quality of tetrahydrofuran are effectively improved, and the purification device structure and the purification process are simple.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of chemical solvent preparation, and particularly relates to a tetrahydrofuran purification device. BACKGROUND

[0002] Tetrahydrofuran is an organic solvent with excellent performance widely used in industrial production, and has the characteristics of low toxicity, low boiling point, good fluidity and excellent solubility, and has very wide application. The prepared tetrahydrofuran generally contains dihydrofuran and aldehyde alcohol impurities which are difficult to separate, and has the problems of low purity and environmental pollution.

[0003] It is particularly important to remove the above-mentioned impurities for the tetrahydrofuran refining process. In the prior art, tetrahydrofuran containing water is contacted with a strong acid cation exchange resin to convert dihydrofuran in the tetrahydrofuran into hydroxytetrahydrofuran. The process is divided into a dihydrofuran removal process, an aldehyde removal process, a dehydration process and a subsequent deacidification and hydrogenation process, and the process flow is long.

[0004] Therefore, it has become a problem to be solved by those skilled in the art to develop a tetrahydrofuran purification device to solve the technical defect that the tetrahydrofuran refining process procedure is complicated in the prior art. CONTENT OF THE INVENTION

[0005] Therefore, it is necessary to provide a tetrahydrofuran purification device to solve the technical defect that the tetrahydrofuran refining process procedure is complicated in the prior art.

[0006] The application provides a tetrahydrofuran purification device, which comprises a feed inlet, a catalytic hydrogenation reaction part, a gas phase discharge port, a liquid phase discharge port, a heavy component removal tower and an absorption tower, the feed inlet is communicated with the catalytic hydrogenation reaction part, the catalytic hydrogenation reaction part is communicated with the heavy component removal tower through the liquid phase discharge port, and the catalytic hydrogenation reaction part is communicated with the absorption tower through the gas phase discharge port.

[0007] The absorption tower comprises a hollow cavity, an absorption part, a gaseous discharge end and a liquid discharge end, the absorption part is arranged in the interior of the hollow cavity, the liquid discharge end is arranged at the bottom end of the hollow cavity, and the gaseous discharge end is arranged at the top end of the hollow cavity.

[0008] In one of the embodiments, the catalytic hydrogenation reaction part is a bubble bed reactor and / or a trickle bed reactor.

[0009] In one of the embodiments, the purification device further comprises a heat exchanger, and the heat exchanger is arranged between the feed inlet and the catalytic hydrogenation reaction part.

[0010] In one of the embodiments, the purification device further comprises a reducing gas inlet and a micro-nano bubble generator.

[0011] The reducing gas sequentially passes through the micro-nano bubble generator and the reducing gas inlet, and the reducing gas inlet is in communication with the catalytic hydrogenation reaction part.

[0012] In one of the embodiments, the purification device further comprises a catalytic activation part, which is in communication with the bottom end of the catalytic hydrogenation reaction part.

[0013] The catalytic activation part provides an activation gas source for the catalytic hydrogenation reaction part.

[0014] In one of the embodiments, the top of the catalytic hydrogenation reaction part is provided with a gas-liquid separation groove, and the fluid after reaction of the catalytic hydrogenation reaction part is separated into gas phase and liquid phase through the gas-liquid separation groove and then enters the gas phase outlet and the liquid phase outlet respectively.

[0015] In one of the embodiments, the gas-liquid separation groove is of a double-layer structure, and a porous partition plate is arranged in the middle, the upper outlet is a gas phase outlet, the lower outlet is a liquid phase outlet, and a condensing jacket layer is optionally arranged outside the gas-liquid separation groove, and condensing water is introduced into the condensing jacket layer.

[0016] In one of the embodiments, a filtering part is arranged in the gas-liquid separation groove.

[0017] In one of the embodiments, the purification device further comprises a combustion part, which is in communication with the gas phase outlet, and the gas flowing out of the gas phase outlet enters the combustion part.

[0018] In one of the embodiments, the purification device further comprises a pressure stabilizing part, which is arranged between the gaseous outlet end and the ignition module.

[0019] In one of the embodiments, the absorption tower is a packed tower and / or a plate tower.

[0020] In one of the embodiments, the absorption tower is a packed tower, the packing height of the packed tower is 4-8 meters, and the packing type of the packed tower includes a silk screen type structured packing and / or a corrugated plate structured packing, for example, a CY silk screen type structured packing and / or a BX type plate corrugated structured packing of Sulzer Company.

[0021] In summary, the application provides a tetrahydrofuran purification device, comprising: a feed inlet, a catalytic hydrogenation reaction part, a gas phase discharge port, a liquid phase discharge port, a heavy component removal tower and an absorption tower. In the technical solution provided by the application, the impurity dihydrofuran in the tetrahydrofuran is hydrogenated to generate tetrahydrofuran by the catalytic hydrogenation part, and the impurities n-butyl aldehyde and isobutyl aldehyde are hydrogenated to generate alcohol which is easy to separate from tetrahydrofuran. It is determined that the content of the impurity dihydrofuran in the purified tetrahydrofuran is reduced to below 3 ppm, and the alcohol is separated in the heavy component removal tower, thereby effectively improving the purity and quality of the tetrahydrofuran. The purification device has the advantages of simple structure and purification process, low energy consumption and no additional environmental pollution. The application provides a tetrahydrofuran purification device, which solves the technical defects of the prior art that the tetrahydrofuran refining process is complicated. BRIEF DESCRIPTION OF DRAWINGS

[0022] In order to more clearly illustrate the technical solutions in the embodiments of the application or the prior art, the drawings needed to be used in the embodiments or the prior art description will be briefly introduced. Obviously, the drawings in the following description are only embodiments of the application, and those skilled in the art can obtain other drawings according to the provided drawings without creating any creative labor.

[0023] Figure 1 In the technical solution provided by the embodiments of the application, a structural schematic diagram of a tetrahydrofuran purification device is provided.

[0024] Among them, the catalytic hydrogenation reaction part A, the absorption tower B and the heat exchanger C. DETAILED DESCRIPTION

[0025] The application provides a tetrahydrofuran purification device to solve the technical defects of the prior art that the tetrahydrofuran refining process is complicated.

[0026] In order to make the above-mentioned purposes, features and advantages of the application more obvious and easy to understand, the specific embodiments of the application will be described in detail below. In the following description, a large number of specific details are set forth in order to fully understand the application. However, the application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without departing from the spirit of the application, therefore the application is not limited by the specific embodiments disclosed below.

[0027] In the description of the present application, it should be understood that the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate the orientation or positional relationship shown in the drawings, which are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as a limitation of the present application.

[0028] In addition, the terms "first", "second" are only for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined with "first", "second" can explicitly or implicitly include at least one of the features. In the description of the present application, the meaning of "a plurality of" is at least two, such as two, three, etc., unless otherwise explicitly specified and limited.

[0029] In the present application, unless otherwise explicitly specified and limited, the terms "mounting", "connecting", "connecting", "fixing" and the like should be understood broadly, for example, it can be fixed connection, or detachable connection, or integral; it can be mechanical connection, or electrical connection; it can be directly connected, or indirectly connected through intermediate medium, it can be the internal communication of two elements or the interaction relationship between two elements, unless otherwise explicitly limited. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0030] In the present application, unless otherwise explicitly specified and limited, the first feature is "on" or "under" the second feature, which can be direct contact between the first and second features, or indirect contact between the first and second features through intermediate medium. Moreover, the first feature "above", "above" and "above" the second feature can be directly above or obliquely above the first feature, or only indicate that the horizontal height of the first feature is higher than that of the second feature. The first feature "below", "below" and "below" the second feature can be directly below or obliquely below the first feature, or only indicate that the horizontal height of the first feature is less than that of the second feature.

[0031] It is to be understood that when an element such as a layer, region or substrate is referred to as being "on" or "connected to" another element, it can be directly on or connected to the other element or intervening elements can be present. In contrast, when an element is referred to as being "directly on" or "directly connected to" another element, there are no intervening elements present. It will be understood that, when a member is referred to as being "coupled" or "connected" to another member, it can be directly coupled or connected to the other member or intervening members can be present. As used herein, the term "and / or" includes any and all combinations of one or more of the associated listed items. Expressions such as "at least one of," when preceding the syllables of a list of elements, modify the entire list of elements and do not modify the elements individually.

[0032] Referring now to the drawings Figure 1 The embodiment of the present application provides a kind of tetrahydrofuran purification device, including: feed inlet, catalytic hydrogenation reaction part A, gas phase discharge port, liquid phase discharge port, heavy tower and absorption tower, feed inlet is communicated with catalytic hydrogenation reaction part A, catalytic hydrogenation reaction part A is communicated with heavy tower by liquid phase discharge port, catalytic hydrogenation reaction part is communicated with absorption tower by gas phase discharge port;Absorption tower includes: hollow cavity, absorption part, gaseous discharge end and liquid discharge end, absorption part is arranged in the inside of hollow cavity, liquid discharge end is arranged at the bottom end of hollow cavity, gaseous discharge end is arranged at the top end of hollow cavity.The embodiment of the present application provides a kind of tetrahydrofuran purification device, solves the technical defects of the tedious technical process of tetrahydrofuran refining process in the prior art.

[0033] In the technical scheme provided by the embodiment of the present application, the tetrahydrofuran gas 1 containing impurities enters from the lower end of the catalytic hydrogenation reaction part A, at this time, the tetrahydrofuran does not react in the catalytic hydrogenation reaction part A, the impurity dihydrofuran occurs in the catalytic hydrogenation reaction part to generate tetrahydrofuran by reduction hydrogenation reaction, and the aldehyde impurities, such as n-butyl aldehyde and isobutyl aldehyde, which are difficult to separate from tetrahydrofuran, occur in the catalytic hydrogenation reaction part A to generate alcohol by reduction hydrogenation reaction.

[0034]

[0035] After hydrogenation is completed in the catalytic hydrogenation reaction part A, the liquid phase product 4 enters the heavy tower through the liquid phase discharge port, and the heavy components alcohol are removed in the heavy tower to obtain the purified tetrahydrofuran. The gas phase product 5 enters the absorption tower B through the gas phase discharge port.

[0036] The gas phase product 5 absorbs the residual tetrahydrofuran in the gas phase product 5 in the absorption part of the absorption tower B, and flows out through the liquid discharge end of the absorption tower B, and collects the tetrahydrofuran liquid 8 obtained by absorption. The remaining gas 7 passes through the gaseous discharge end of the absorption tower B and escapes.

[0037] In the technical scheme provided by the present application, in order to effectively ensure the catalytic speed of the catalytic hydrogenation reaction part A, ensure that the impurities dihydrofuran and aldehyde in the tetrahydrofuran can be fully reduced, and ensure good purification effect of the tetrahydrofuran, in the technical scheme provided by the present application, the catalytic hydrogenation reaction part is a bubble bed reactor and / or a trickle bed reactor. The bubble bed reactor and / or the trickle bed reactor can make the impurities in the tetrahydrofuran fully contact with the catalyst, so as to achieve the optimal reduction effect.

[0038] In the actual application process, in order to avoid the temperature of the tetrahydrofuran gas 1 containing impurities affecting the catalytic hydrogenation reaction part A, reducing the reaction speed of the catalytic hydrogenation reaction part A and the activity of the catalyst, and at the same time, in the present application, the purification device further comprises a heat exchanger C arranged between the feed inlet and the catalytic hydrogenation reaction part. Before the tetrahydrofuran gas 1 containing impurities enters the catalytic hydrogenation reaction part A, the temperature is reduced to the appropriate interval through the heat exchanger, and the low-temperature tetrahydrofuran liquid 2 containing impurities enters the catalytic hydrogenation reaction part A.

[0039] Further optimization of the technical scheme, in order to ensure that the reduction reaction in the catalytic hydrogenation reaction part A is efficient and fast, the purification device provided by the present application further comprises a reducing gas feed inlet and a micro-nano bubble generator; the reducing gas passes through the micro-nano bubble generator and the reducing gas feed inlet in sequence, and the reducing gas feed inlet is in communication with the catalytic hydrogenation reaction part. Through the reducing gas feed inlet, the reducing gas 3 is introduced into the catalytic hydrogenation reaction part A, in order to make the reducing gas 3 fully contact with the catalyst and the impurities in the catalytic hydrogenation reaction part A, before the reducing gas 3 enters the catalytic hydrogenation reaction part A, it is treated by the micro-nano bubble generator, so that the reducing gas 3 entering the catalytic hydrogenation reaction part A has the characteristics of large specific surface area, slow rising speed, high surface charge and high gas solubility, thereby effectively promoting the rapid and efficient catalytic hydrogenation.

[0040] Further optimization of the technical scheme, in order to effectively improve the activity of the catalyst in the catalytic hydrogenation reaction part A, the purification device provided by the present application further comprises a catalytic activation part in communication with the bottom end of the catalytic hydrogenation reaction part; the catalytic activation part provides an activation gas source for the catalytic hydrogenation reaction part.

[0041] In the improved technical scheme of the present application, the top of the catalytic hydrogenation reaction part is provided with a gas-liquid separation tank, and the fluid after reaction of the catalytic hydrogenation reaction part enters the gas phase discharge port and the liquid phase discharge port respectively through the gas-liquid separation tank. Through the gas-liquid separation tank, the gas phase and liquid phase products can be quickly and effectively separated, and it is ensured that the tetrahydrofuran and the alcohol obtained by reducing the impurity aldehyde can smoothly enter the heavy component removal tower.

[0042] Further optimize the technical scheme, on the basis of ensuring the gas-liquid distribution groove distribution effect, while taking into account the gas-liquid distribution groove structure is simple, easy to clean and maintain, the technical scheme provided by the embodiment of the application, the gas-liquid distribution groove is double-layer structure, the middle is provided with a porous partition, the upper outlet is a gas phase outlet, the lower outlet is a liquid phase outlet, the gas-liquid distribution groove is externally provided with a condensing jacket layer, and the condensing jacket layer is internally passed through condensed water.

[0043] Further optimize the technical scheme, in order to prevent the hole in the gas-liquid distribution groove from being blocked and improve the gas-liquid separation effect, the gas-liquid distribution groove is provided with a filter part, and the filter part is provided with a porous filter material, which can be activated carbon, porous ceramic and other common filter materials.

[0044] The purification device provided by the embodiment of the application further comprises a combustion part, which is in communication with the gas phase discharge port. After the residual gas 7 in the absorption tower B escapes through the gaseous discharge end of the absorption tower B, the residual gas 7 is fully combusted in the combustion part, so that the environment is prevented from being polluted by the residual gas 7 remaining in the air for a long time.

[0045] In order to effectively improve the safety, the purification device provided by the embodiment of the application further comprises a pressure stabilizing part, which is arranged between the gaseous discharge end and the ignition module. The gas 9 is provided through the pressure stabilizing part, and the pressure is kept stable after the gas 9 is mixed with the gas 7, so that the gas pressure is kept constant during the combustion in the combustion part, the combustion process is safer, and dangerous situations such as explosion are avoided during the combustion process.

[0046] In order to effectively optimize the absorption effect of the absorption tower on residual tetrahydrofuran, in the technical scheme provided by the embodiment of the application, the absorption tower B is a packed tower and / or a plate tower.

[0047] Further optimize the technical scheme, in the purification device provided by the embodiment of the application, the absorption tower is a packed tower, the packing height of the packed tower is 4-8 meters, and the packing type of the packed tower includes Suershou CY (silk screen) type regular packing and / or BX type plate corrugated regular packing.

[0048] In order to more clearly show the specific use scene of the purification device provided by the embodiment of the application, the purification method for purifying tetrahydrofuran by using the above purification device is specifically described below.

[0049] The purification method comprises:

[0050] Step one, the tetrahydrofuran gas containing impurities is subjected to catalytic hydrogenation reaction under the action of a catalyst, to obtain a gaseous first product and liquid tetrahydrofuran;

[0051] Step two, the gaseous first product is mixed with an absorbent 6 to obtain a gaseous second product and liquid tetrahydrofuran.

[0052] On the basis of ensuring good catalytic hydrogenation effect of the catalyst, meanwhile, the comprehensive consideration of catalyst cost and catalyst life is taken into account, in the embodiment of the application, in step one, the catalyst is any one or more of nickel-based catalyst, palladium-based catalyst, ruthenium-based catalyst and platinum.

[0053] Further optimize the technical scheme, the catalyst is activated in the activation gas atmosphere, so as to achieve the optimal catalytic effect of the catalyst, in the application, step one further comprises: catalyst activation, the catalyst is activated in the activation gas atmosphere.

[0054] Further optimize the technical scheme, on the basis of ensuring good activation effect of the activation gas on the catalyst, the factors of activation gas cost and safety are taken into account, in the application, the activation gas is: nitrogen and / or hydrogen.

[0055] Similarly, in the application, the activation temperature is 180-220 DEG C, and the activation pressure is 0.07 MPaG.

[0056] In order to ensure good reduction effect of the catalyst hydrogenation, meanwhile, the demand of economic and feasible purification cost is taken into account, in step one of the application, the reducing gas of catalytic hydrogenation reaction is hydrogen, and the hydrogen flow is.

[0057] Similarly, in step one of the application, the temperature of catalytic hydrogenation reaction is 70-140 DEG C, and the pressure of catalytic hydrogenation reaction is 0.4-1.0 MPaG.

[0058] In order to strengthen the absorption effect of the absorption tower B on the residual tetrahydrofuran, the absorption tower B contains the absorbent 6, in the actual application process, in step two, the absorbent 6 includes: desalted water and / or tetrahydrofuran solution.

[0059] It is determined that the above purification device provided by the application can effectively purify the tetrahydrofuran prepared by 1, 4-butanediol cyclization reaction, reduce the content of impurity dihydrofuran in the prepared tetrahydrofuran to less than 3 ppm, and also reduce the aldehyde which is difficult to separate from tetrahydrofuran to alcohol which is easy to separate, which has a significant effect on improving the purity and quality of tetrahydrofuran and effectively improving the quality of tetrahydrofuran product.

[0060] At the same time, there is no loss of tetrahydrofuran in the whole purification process, which ensures the yield of tetrahydrofuran; no by-product is produced in the purification process, which will not pollute the environment, and can be widely applied to the preparation of tetrahydrofuran.

[0061] In summary, the application provides a tetrahydrofuran purification device, comprising: a feed inlet, a catalytic hydrogenation reaction part, a gas phase discharge port, a liquid phase discharge port, a heavy component removal tower and an absorption tower. In the technical solution provided by the application, the impurity dihydrofuran in tetrahydrofuran is hydrogenated to generate tetrahydrofuran by the catalytic hydrogenation part, and the impurities n-butyl aldehyde and isobutyl aldehyde are hydrogenated to generate alcohol which is easy to separate from tetrahydrofuran. It is determined that the content of impurity dihydrofuran in purified tetrahydrofuran is reduced to below 3 ppm, and the alcohol is separated in the heavy component removal tower, effectively improving the purity and quality of tetrahydrofuran, and the purification device has the advantages of simple structure and purification process, low energy consumption and no additional environmental pollution. The application provides a tetrahydrofuran purification device, which solves the technical defects of the prior art that the tetrahydrofuran refining process is complicated.

[0062] The technical features of the above-described embodiments can be combined in any manner. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described, but as long as the combinations of the technical features do not contradict, they should be considered within the scope of the present disclosure. Meanwhile, other embodiments can be derived from the above-described embodiments, so that structure and logic substitutions and changes can be made without departing from the scope of the present disclosure.

[0063] The above-described embodiments only express several embodiments of the application, and the description is more specific and detailed, but it should not be understood as limiting the scope of the patent application. It should be noted that for ordinary skilled persons in the art, without departing from the concept of the application, several modifications and improvements can be made, which are within the scope of the application. Therefore, the protection scope of the patent of the application should be subject to the appended claims.

Claims

1. A tetrahydrofuran purification apparatus, characterized by, The purification device comprises a feed inlet, a catalytic hydrogenation reaction part, a gas phase outlet, a liquid phase outlet, a heavy component removal tower and an absorption tower, the feed inlet is communicated with the catalytic hydrogenation reaction part, the catalytic hydrogenation reaction part is communicated with the heavy component removal tower through the liquid phase outlet, and the catalytic hydrogenation reaction part is communicated with the absorption tower through the gas phase outlet. The absorption tower comprises a hollow cavity, an absorption part, a gaseous outlet end and a liquid outlet end, the absorption part is arranged in the hollow cavity, the liquid outlet end is arranged at the bottom end of the hollow cavity, and the gaseous outlet end is arranged at the top end of the hollow cavity.

2. The purification device of claim 1, wherein, The catalytic hydrogenation reaction part is a bubble bed reactor and / or a trickle bed reactor.

3. Purification device according to claim 1 or 2, characterized in that The purification device further comprises a heat exchanger arranged between the feed inlet and the catalytic hydrogenation reaction part.

4. The purification device of claim 1, wherein, The purification device further comprises a reducing gas inlet and a micro-nano bubble generator. Reducing gas passes through the micro-nano bubble generator and the reducing gas inlet in sequence, and the reducing gas inlet is communicated with the catalytic hydrogenation reaction part.

5. The purification device according to claim 1 or 4, characterized in that The purification device further comprises a catalytic activation part communicated with the bottom end of the catalytic hydrogenation reaction part. The catalytic activation part provides an activation gas source for the catalytic hydrogenation reaction part.

6. The purification device of claim 1, wherein, The top of the catalytic hydrogenation reaction part is provided with a gas-liquid diversion groove. The fluid after reaction of the catalytic hydrogenation reaction part enters the gas phase outlet and the liquid phase outlet respectively through the gas-liquid diversion groove.

7. The purification device of claim 6, wherein, The gas-liquid diversion groove is provided with a filter part.

8. The purification device of claim 6, wherein, The purification device further comprises a combustion part communicated with the gas phase outlet, and the gas outlet from the gas phase outlet enters the combustion part.

9. The purification device of claim 8, wherein, The purification device further comprises a pressure stabilizing part arranged between the gaseous outlet end and an ignition module.

10. The purification device of claim 1, wherein, The absorption tower is a packed tower and / or a plate tower.

11. The purification device of claim 10, wherein, The absorption tower is a packed tower, the packing height of the packed tower is 4-8 meters, and the packing type of the packed tower comprises a wire mesh type structured packing and / or a plate wave type structured packing.

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