CN212076906U - Side-line reaction type dioxolane production process device - Google Patents
Side-line reaction type dioxolane production process device Download PDFInfo
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- CN212076906U CN212076906U CN202020501045.8U CN202020501045U CN212076906U CN 212076906 U CN212076906 U CN 212076906U CN 202020501045 U CN202020501045 U CN 202020501045U CN 212076906 U CN212076906 U CN 212076906U
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Abstract
The utility model discloses a side reaction formula dioxolane production process units, including reaction rectifying column, extraction rectifying column, heavy-duty tower and lightness-removing column, reaction rectifying column includes reaction rectifying column main part and a plurality of side line reactor, reaction rectifying column main part along vertical direction pass through the tubing pump respectively with a plurality of side line reactor circulation connection, the side line reactor is filled with solid acid catalyst, the middle part of reaction rectifying column main part is equipped with the raw materials feed inlet, and the bottom is equipped with rare formaldehyde and retrieves mouthful, and the top is equipped with the export of thick product; the crude product outlet of the reaction rectifying tower is sequentially connected with the extraction rectifying tower, the heavy component removal tower and the light component removal tower through pipelines, the tower bottom of the extraction rectifying tower is also provided with an extractant recovery port, and the upper part of the extraction rectifying tower is also provided with an extractant feed port. The utility model discloses a continuous production simplifies the tower body structure, reduces manufacturing cost, and the airspeed can be adjusted as required, effectively improves catalyst utilization ratio.
Description
Technical Field
The utility model belongs to the technical field of chemical production, especially, relate to dioxolane's production process units and method.
Background
1, 3-dioxolane (dioxolane, DOX for short) is an important comonomer for producing polyoxymethylene and can be used as an extractant, an organic solvent, a lithium battery electrolytic solvent, an organic intermediate and the like.
At present, the dioxolane is mostly produced by using ethylene glycol and formaldehyde under the action of an acid catalyst. Patent CN10128258A adopts a catalytic rectification tower to react to generate dioxolane, a catalyst is placed on a filler to be coated on the filler, a dioxolane crude product is obtained at the top of the reactive rectification tower, and materials at the bottom of the tower are rectified to recover glycol for recycling. The reaction is carried out in a liquid phase, the reaction is carried out in the tower, the reaction is insufficient, and the structure of the reactive distillation tower is complex, so that the equipment cost of the reactive distillation tower is high. Since dioxolane and water form an azeotrope, it contains 6.7% water. The commonly used treatment method is to extract the dioxolane azeotrope with an alkali metal oxide to remove most of the water and impurities, and then to rectify to obtain the dioxolane product, which is determined to consume a large amount of alkali liquor and produce a large amount of sewage.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the existing problems and deficiencies, the utility model aims to provide a side-line reactive dioxolane production process device, which realizes the continuous production of dioxolane through a reaction rectifying tower of a side-line reactor, the reaction is mainly carried out in the side-line reactor, the structure of the reaction rectifying tower is greatly simplified, and the equipment manufacturing cost is reduced; solid strong acid catalyst is used and is filled in the side line reactor, so that the filling and maintenance difficulty of the catalyst is reduced; the space velocity of the side reactor can be adjusted according to the requirement, so that the utilization rate of the catalyst is further improved; the dioxolane is separated by adopting an extractive distillation mode, and the generation of sewage is reduced.
The technical scheme is as follows: in order to solve the technical problem, the utility model discloses a following technical scheme: a side-line reaction type dioxolane production process device comprises a reaction rectifying tower, an extraction rectifying tower, a heavy component removal tower and a light component removal tower, wherein the reaction rectifying tower comprises a reaction rectifying tower main body and a plurality of side-line reactors, the reaction rectifying tower main body adopts a tower plate structure, the reaction rectifying tower main body is respectively and circularly connected with the plurality of side-line reactors through a pipeline pump along the vertical direction, a solid acid catalyst is filled in the side-line reactors, a raw material feeding port is arranged in the middle of the reaction rectifying tower main body, a dilute formaldehyde recovery port is arranged at the bottom of the reaction rectifying tower main body, and a crude product outlet is arranged at the top of the reaction rectifying tower main body; the crude product outlet of the reaction rectifying tower is sequentially connected with the extraction rectifying tower, the heavy component removal tower and the light component removal tower through pipelines, the tower bottom of the extraction rectifying tower is also provided with an extractant recovery port, and the upper part of the extraction rectifying tower is also provided with an extractant feed port.
Preferably, the reaction rectifying tower main body is further provided with a filler filled with a catalyst.
Preferably, the extractive distillation column, the heavy component removal column and the light component removal column adopt a plate column or a packed column.
Preferably, the number of the side line reactors is 1-5.
Preferably, the reactive distillation tower is also provided with a liquid acidic catalyst feeding hole.
Preferably, the extractant recovery port of the extractive distillation column is connected with the raw material feed port of the reactive distillation column through a pipeline.
Has the advantages that: compared with the prior art, the utility model realizes the continuous production of dioxolane through the reactive distillation column of the side line reactor, the reaction is mainly carried out in the side line reactor, the height of the reactive distillation column is greatly reduced, the structure of the tower body is simplified, and the manufacturing cost of equipment is reduced; solid strong acid catalyst is used and is filled in the side line reactor, so that the filling and maintenance difficulty of the catalyst is reduced; more importantly, the space velocity of the side reactor can be adjusted according to the requirement, so that the utilization rate of the catalyst is further improved; the dioxolane is separated by adopting an extractive distillation mode, and the generation of sewage is reduced.
Drawings
FIG. 1 is a schematic structural diagram of the side-line reactive dioxolane production process device of the present invention.
Wherein, the reaction rectifying tower 1, the side line reactor 2, the extraction rectifying tower 3, the heavy component removing tower 4 and the light component removing tower 5.
Detailed Description
The present invention will be further clarified by the following description with reference to the attached drawings and specific examples, which should be understood as being merely illustrative of the present invention and not limiting the scope of the present invention, and modifications of various equivalent forms of the present invention by those skilled in the art after reading the present invention, all fall within the scope defined by the appended claims of the present application.
Based on the utility model discloses a technological method of side line reaction formula device production dioxolane mainly includes following step:
(1) and (3) reaction rectification: formaldehyde and ethylene glycol are used as raw materials, and generation and separation of dioxolane are realized in a reaction rectifying tower. The outside of the reactive distillation tower is connected with a side line reactor filled with a catalyst, formaldehyde and ethylene glycol are fed into the middle part of the reactive distillation tower, and liquid on a tower plate in the reactive distillation tower is led out of the tower and enters the side line reactor, so that the reaction is mainly carried out in the side line reactor. Adding a trace amount of acid liquid catalyst into the tower kettle, so that a small amount of glycol in the tower kettle can also be completely reacted. The azeotrope of dioxolane and water obtained at the tower top is rectified and separated, and the waste water at the tower bottom is sent to a formaldehyde recovery device.
In the process, the molar ratio of the fed formaldehyde to the ethylene glycol is 1:1, the operating pressure of the reaction rectification is 0.01MPa-0.5MPa, and the theoretical plate number of the reaction rectification tower is 20-50 theoretical plates. The number of the side line reactors is 1-5. The catalyst adopts resin and Al2O3、SiO2And the like solid acid catalysts. The space velocity of the side reactor is controlled to be 1-10h-1. The temperature of the side line reactor is controlled at 60-100 ℃.
The acidic liquid catalyst is selected from inorganic acid or organic acid, such as sulfuric acid, sulfonic acid, phosphonic acid, and carboxylic acid, which volatilizes under the reaction conditions. Sulfonic acid-based catalysts such as methylbenzenesulfonic acid, xylenesulfonic acid, and the like are preferable because of their low corrosiveness.
As a preferable scheme, a plurality of filling materials filled with the catalyst can be arranged inside the reactive distillation column to replace the acidic liquid catalyst so as to avoid the corrosion of liquid to the metal of the column body.
(2) And (3) refining a product: and (3) carrying out reactive distillation to obtain a dioxolane crude product, and then sending the dioxolane crude product into an extraction and distillation tower, wherein an extracting agent and the crude product interact to destroy azeotropic composition. Firstly, a crude product of dioxolane enters from the middle part of an extraction and rectification tower, an extractant enters from the upper part of the tower, and dioxolane with the concentration of about 95 percent is obtained at the top of the tower. Then, the dioxolane is separated from impurities such as water, methanol and the like in a heavy component removal tower and a light component removal tower to obtain dioxolane products with the concentration of more than 99 percent.
In the product refining process, the addition amount of the extracting agent in the extraction and rectification tower is 5-50 wt% of the feeding amount of the dioxolane crude product. The operating pressure of the extraction rectifying tower is 0.01MPa-0.5 MPa. The extractant is ethylene glycol, 1,3 propylene glycol, MIBK, isopropyl ether, cyclohexane, benzene, n-hexane, n-butyl acetate and other solvents. The preferential use of ethylene glycol can reduce the entering of other organic media into the system and reduce the subsequent separation cost.
As shown in figure 1, concentrated formaldehyde with the concentration of 60 percent and ethylene glycol with the concentration of 99.8 percent enter a reactive distillation tower from the middle part. The formaldehyde, the water and the ethylene glycol flow downwards, the materials are pumped out by a circulating pump and sent into an external side reactor, and the side reactor is internally provided with acidic cation exchange resin. The material after reaction returns to the reaction rectifying tower. The boiling point of the produced dioxolane is less than that of ethylene glycol, formaldehyde and water, so that the dioxolane is continuously vaporized from the liquid phase and enters the upper tower plate to break the liquid phase balance, and the reaction is continuously carried out towards the production direction of the dioxolane. A crude product containing 91.5% of dioxolane is obtained at the top of the column. 5% dilute formaldehyde solution is obtained at the tower bottom and is sent to formaldehyde recovery.
The ethylene glycol enters the extraction rectifying tower from the upper part, the ethylene glycol breaks an azeotropic system of the dioxolane and water in an extraction section, 95.1 percent of dioxolane is obtained at the tower top, and the ethylene glycol aqueous solution at the tower bottom returns to the reaction rectifying tower for recycling. The concentrated dioxolane solution passes through a de-weighting tower to remove the heavy components such as ethylene glycol, formic acid and the like, and dioxolane with the concentration of 98.2 percent is obtained at the bottom of the tower. Light components such as methanol and the like are removed through a light component removal tower, and high-purity dioxolane with the purity of 99.9 percent is obtained at the bottom of the tower.
Claims (6)
1. A side line reaction type dioxolane production process device is characterized in that: the device comprises a reaction rectifying tower, an extraction rectifying tower, a heavy component removing tower and a light component removing tower, wherein the reaction rectifying tower comprises a reaction rectifying tower main body and a plurality of side line reactors, the reaction rectifying tower main body adopts a tower plate structure, the reaction rectifying tower main body is respectively and circularly connected with the side line reactors through a pipeline pump along the vertical direction, a solid acid catalyst is filled in the side line reactors, the middle part of the reaction rectifying tower main body is provided with a raw material feeding hole, the bottom part of the reaction rectifying tower main body is provided with a dilute formaldehyde recycling hole, and the top part of the reaction rectifying tower main body is provided with a crude product outlet; the crude product outlet of the reaction rectifying tower is sequentially connected with the extraction rectifying tower, the heavy component removal tower and the light component removal tower through pipelines, the tower bottom of the extraction rectifying tower is also provided with an extractant recovery port, and the upper part of the extraction rectifying tower is also provided with an extractant feed port.
2. The side-line dioxolane production process set-up according to claim 1, wherein: the reaction rectifying tower main body is also provided with a filler filled with a catalyst.
3. The side-line dioxolane production process set-up according to claim 1, wherein: the extractive distillation column, the heavy component removal column and the light component removal column adopt plate columns or packed columns.
4. The side-line dioxolane production process set-up according to claim 1, wherein: the number of the side line reactors is 1-5.
5. The side-line dioxolane production process set-up according to claim 1, wherein: the reaction rectifying tower is also provided with a liquid acid catalyst feeding hole.
6. The side-line dioxolane production process set-up according to claim 1, wherein: and an extractant recovery port of the extraction rectifying tower is connected with a raw material feeding port of the reaction rectifying tower through a pipeline.
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| CN202020501045.8U CN212076906U (en) | 2020-04-08 | 2020-04-08 | Side-line reaction type dioxolane production process device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115260147A (en) * | 2022-08-22 | 2022-11-01 | 凯瑞环保科技股份有限公司 | Process device and method for synthesizing dioxolane by using extractive catalytic distillation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115260147A (en) * | 2022-08-22 | 2022-11-01 | 凯瑞环保科技股份有限公司 | Process device and method for synthesizing dioxolane by using extractive catalytic distillation |
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