CN210543405U - Diethyl toluenediamine combined type continuous reduced pressure distillation purification device - Google Patents

Diethyl toluenediamine combined type continuous reduced pressure distillation purification device Download PDF

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CN210543405U
CN210543405U CN201921325075.1U CN201921325075U CN210543405U CN 210543405 U CN210543405 U CN 210543405U CN 201921325075 U CN201921325075 U CN 201921325075U CN 210543405 U CN210543405 U CN 210543405U
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condenser
distillation
tube
pipeline
outlet
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李强
王晓刚
朱忠杰
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Dongying Hairuibao New Material Co ltd
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Dongying Hairuibao New Material Co ltd
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Abstract

The utility model relates to a combined continuous decompression distillation purification device for diethyl toluenediamine, which comprises a distillation still and a scraper type decompression film evaporator, wherein an outlet on the distillation still is sequentially connected with a condenser and a fine product tank through pipelines, and the condenser or the fine product tank is connected with a vacuum pump; the lower outlet of the distillation kettle is connected with the feed inlet of the wiped film type pressure-reducing film evaporator through a pipeline, the upper outlet of the wiped film type pressure-reducing film evaporator is connected with the upper part of the distillation kettle through a pipeline, and the lower outlet of the wiped film type pressure-reducing film evaporator is connected with the slag charge tank through a pipeline; the condenser is two-stage, and is respectively a first condenser and a second condenser, wherein a cold medium inlet of the first condenser is connected with the crude product tank through a pipeline, and a cold medium outlet is connected with a feed inlet of the distillation kettle; the cold medium inlet of the second condenser is connected with the outlet of the cooling tower through a pipeline, and the cold medium outlet is connected with the inlet of the cooling tower. The utility model discloses a distillation still and wiped film evaporator's combination formula distillation plant can improve distillation efficiency and product purity.

Description

Diethyl toluenediamine combined type continuous reduced pressure distillation purification device
Technical Field
The invention relates to a combined continuous reduced pressure distillation and purification device for diethyl toluenediamine, belonging to the technical field of fine chemical engineering.
Background
Diethyltoluenediamine (english name, Diethyltoluenediamine) refers to two isomeric mixtures of Diethyltoluenediamine, i.e., two isomeric mixtures that are commercially available: 76% of 3, 5-Diethyl-2, 4-diaminotoluene (3, 5-Diethyl-toluene-2, 4-diamine) and 24% of 3, 5-Diethyl-2, 6-diaminotoluene (3, 5-Diethyl-toluene-2, 6-diamine), DETDA for short. The diethyl toluene diamine is used as a chain extender for reaction injection molding of polyurethane, polyurethane coating, epoxy resin and alkyd resin curing agent. Pesticide, dye intermediate, plastic, rubber and oil antioxidant. The diethyl toluene diamine is an aromatic diamine curing agent of polyurethane elastomers and epoxy resins, is used for casting, coating and adhesives, and is also a chain extender of polyurethane and polyurea elastomers. The polyurethane prepolymer has high reaction speed with the polyurethane prepolymer, is mainly used for a reaction casting type polyurethane system and a spraying polyurethane (urea) elastic coating system, and has the advantages of high reaction speed, short demoulding time, high initial strength, hydrolysis resistance of a product, heat resistance and the like. In addition, the product can be used as antioxidant for elastomer, lubricant and industrial oil, and chemical synthesis intermediate.
Conventional synthesis of diethyltoluenediamine (DETDA): toluene Diamine (TDA) and ethylene are used as raw materials, and are subjected to alkylation reaction at high temperature and high pressure in the presence of a catalyst, and the catalyst is refined. The purification is currently achieved by distillation, which usually requires several distillations in a still to obtain diethyltoluenediamine with higher purity and lighter color, and has the following disadvantages: 1. multiple distillation operations, complicated steps and low efficiency, 2, the color of the product is deepened due to multiple times of distillation in the distillation kettle, and 2, because the synthesis reaction of the diethyltoluenediamine is a polymerization reaction, more residues are left after distillation, and the residues are accumulated at the bottom of the distillation kettle and are difficult to clean.
The existing condenser is usually a conventional shell-and-tube heat exchanger, which usually comprises a shell and a plurality of heat exchange tubes arranged at intervals in the shell, wherein inner cavities of the heat exchange tubes are used as tube passes, and the heat exchange tubes and the shell are used as shell passes, cold and hot fluids respectively flow in the tube passes and the shell passes to realize heat exchange, and a heat medium is condensed; however, in actual use, a short circuit condition of heat exchange media exists, namely, some heat exchange media directly flow out of the heat exchanger without heat exchange, for example, when the heat exchanger is transversely arranged, hot steam is mainly distributed in the upper space of the heat exchanger when flowing away from a shell pass, and the heat exchange area of the lower part is not fully utilized, so that the heat exchange is insufficient, and the condensing effect is poor; when the cold medium such as cooling water flows through the shell pass, when the flow rate is insufficient, the cooling water is only deposited in the lower space of the heat exchanger, and the heat exchange area of the upper part is not fully utilized, so that the heat exchange is insufficient, and the condensation effect is also poor. The reason for the above-mentioned defect is mainly that there is a part of heat exchange area that is not fully utilized, namely the effective heat exchange area is low, or the heat exchange area utilization rate is low.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the combined continuous reduced pressure distillation and purification device for the diethyl toluenediamine, which has good distillation and purification effects.
The technical scheme of the invention is as follows:
the utility model provides a diethyl toluene diamine combination formula is distillation purification device in succession reduces pressure, includes stills, the stills top is equipped with the feed inlet and exports with last, the stills below is equipped with down the export, go up the export and connect gradually condenser and diethyl toluene diamine fine work jar through the pipeline, be connected with the vacuum pump on condenser or the diethyl toluene diamine fine work jar:
the distillation kettle is characterized by also comprising a wiped film type pressure-reducing evaporator, wherein the lower outlet of the distillation kettle is connected with the feed inlet of the wiped film type pressure-reducing evaporator through a pipeline, the upper outlet of the wiped film type pressure-reducing evaporator is connected with the upper part of the distillation kettle through a pipeline, and the lower outlet of the wiped film type pressure-reducing evaporator is connected with a slag tank through a pipeline;
and a branch pipeline is arranged on a connecting pipeline between the lower outlet of the distillation kettle and the feed inlet of the wiped film pressure-reducing evaporator and is connected with the upper part of the distillation kettle.
Furthermore, the condensers are two stages which are connected in sequence and respectively comprise a first condenser connected with the distillation still and a second condenser connected with the refined diethyl toluenediamine tank, wherein a cold medium inlet of the first condenser is connected with the crude diethyl toluenediamine tank through a pipeline, and a cold medium outlet is connected with a feed inlet of the distillation still; and a cold medium inlet of the second condenser is connected with an outlet of the cooling tower through a pipeline, and a cold medium outlet is connected with an inlet of the cooling tower.
Further, the condenser is a shell-and-tube condenser.
Further, the shell-and-tube condenser comprises a shell and a tube group arranged in the shell, and an annular space is formed between the shell and the tube group; the pipe group is combined and comprises a central pipe and peripheral pipes on the periphery, the cross sections of the central pipe and the peripheral pipes are regular hexagons, and the peripheral pipes are six and are respectively attached to six side surfaces of the central pipe; the annular space and the central tube are used as the shell pass of the condenser, and two ends of the annular space and the central tube are respectively connected with the inlet and the outlet of the first heat exchange medium, and the peripheral tube is used as the tube pass of the condenser, and two ends of the peripheral tube are respectively connected with the inlet and the outlet of the second heat exchange medium.
Furthermore, the six peripheral pipes are attached to each other and located on the same concentric circle, and the adjacent peripheral pipes are communicated through holes in the contact side face.
Further, the tube groups are arranged in the shell in a plurality of groups at intervals.
Furthermore, the shell is a cylindrical cavity, one group of pipe groups is arranged at the center of the cylindrical cavity as a central pipe group, the other group of pipe groups are arranged around the central pipe group as peripheral pipe groups, and the peripheral pipe groups are positioned on the same concentric circle.
Furthermore, the peripheral pipe group is formed by a central pipe group outwards and arranged in a plurality of circles with diameters sequentially increased, and the peripheral pipe group of each circle is located on the same concentric circle.
According to the combined continuous distillation device consisting of the distillation kettle and the wiped film evaporator, the distillation efficiency and the product purity can be improved, the product purity reaches over 99 percent, the product is light yellow, and the requirements of the subsequent procedures on the product quality can be basically met; meanwhile, the distilled fraction, namely the distillation bottom liquid is transferred into the thin film evaporator, even if solid slag is formed, the solid slag can be scraped by a scraper and collected, and accumulation and blockage cannot be caused; and the application of the secondary condenser can recover the distillation waste heat, thereby achieving the effect of saving energy; furthermore the utility model discloses replace single heat exchange tube among the conventional shell and tube type heat exchanger for combination formula nest of tubes, improved cold and hot medium at the inside distribution homogeneity of heat exchanger (the shell side enlarges to each center tube and annular space, prevents the short circuit through forced distribution) and area of contact, improved the condensation effect greatly through improving effective heat transfer area.
Drawings
FIG. 1 is a schematic view showing the construction of a combined continuous distillation purification apparatus for diethyltoluenediamine according to example 1;
FIG. 2 is a schematic view showing the structure of a combined continuous distillation purification apparatus for diethyltoluenediamine according to example 2;
FIG. 3 is a schematic cross-sectional view of a shell-and-tube condenser in example 3;
FIG. 4 is a schematic cross-sectional view of a tube group of the shell-and-tube condenser in example 3;
FIG. 5 is a schematic view showing the arrangement of through-holes in the peripheral tube side of the tube group in the shell-and-tube condenser in example 3;
FIG. 6 is a schematic cross-sectional view of a shell-and-tube condenser in example 4;
FIG. 7 is a schematic diagram of the heat exchange flow of the shell-and-tube condenser in examples 3 and 4;
in the figure: 1. the device comprises a distillation still, 2, a wiped film evaporator, 3, a slag tank, 4, a first condenser, 5, a second condenser, 6, a fine tank, 7, a vacuum pump, 8, a coarse tank, 9, a cooling tower, 10, a shell, 11, a pipe group, 12, a central pipe, 13, a peripheral pipe, 14, a through hole, 15, a condenser, 16, a feeding pipeline, 17, an annular space, 18, a shell side pipeline, 19 and a pipe side pipeline.
Detailed Description
Example 1
Referring to fig. 1, a combined continuous vacuum distillation and purification device for diethyl toluenediamine comprises a distillation still 1 and a wiped film evaporator 2, wherein a feed inlet and an upper outlet are arranged above the distillation still 1, a lower outlet is arranged below the distillation still 1, a feed pipeline 16 is connected to the feed inlet, the upper outlet is sequentially connected with a condenser 15 and a fine product tank 6 through pipelines, and a vacuum pump 7 is connected to the fine product tank 6.
The lower outlet of the distillation still 1 is connected with the feed inlet of the wiped film evaporator 2 through a pipeline, and a branch pipeline is arranged on the pipeline and is connected with the upper part of the distillation still 1. The upper outlet of the wiped film evaporator 2 is connected with the upper part of the distillation kettle 1 through a pipeline, and the lower outlet is connected with the slag tank 3 through a pipeline; the wiped film evaporator 2 is provided with a pressure reducing device.
The working process is as follows: the diethyl toluenediamine crude product enters a distillation kettle 1 through a feeding pipeline 16 (the synthesized diethyl toluenediamine crude product directly enters the distillation kettle from the synthesis kettle), the temperature of the distillation kettle 1 and the temperature of a scraper-type pressure-reducing film evaporator 2 are both increased, a vacuum pump is started for reduced pressure distillation, the diethyl toluenediamine crude product in the distillation kettle 1 synchronously enters the scraper-type pressure-reducing film evaporator 2 through pipelines, a gas-liquid mixed phase at the upper part of the diethyl toluenediamine crude product subjected to reduced pressure distillation in the scraper-type pressure-reducing film evaporator 2 enters the distillation kettle 1, and a distillation bottom liquid and residues are scraped by a scraper and then enter a residue tank 3; the gas phase in the distillation still 1 enters the condenser 15 through the upper outlet, the condensed refined diethyl toluene diamine product enters the refined product tank 6, and if the product purity is unqualified, the condensed refined diethyl toluene diamine product can be fed into the distillation still 1 through the feed pipeline 16 again for re-rectification.
In the device, a crude product of diethyl toluene diamine is fed through a distillation still and then is matched with a wiped film evaporator for combined distillation, finally, a light component of diethyl toluene diamine is evaporated from the upper part of the distillation still and enters a condenser, and a heavy component and residues are scraped by a scraper of the wiped film evaporator and discharged from the bottom, and synchronous feeding and discharging can be realized through the matching of the light component and the heavy component, and the heavy component and the residues are not interfered with each other, so that continuous production can be realized, and the production efficiency is improved.
Example 2
Referring to fig. 2, a combined continuous vacuum distillation purification apparatus for diethyltoluenediamine, based on example 1, further comprises: the condensers are two stages which are connected in sequence and respectively comprise a first condenser 4 connected with the distillation still 1 and a second condenser 5 connected with the fine product tank 6, and a cold medium inlet of the first condenser 4 is connected with the crude product tank 8 through a pipeline, and a cold medium outlet is connected with a feed inlet of the distillation still 1; the cold medium inlet of the second condenser 5 is connected with the outlet of the cooling tower 9 through a pipeline, and the cold medium outlet is connected with the inlet of the cooling tower 9.
The working process is the same as that of the embodiment 1, and the difference is that the diethyl toluene diamine gas distilled from the distillation still is condensed by a secondary condenser, wherein the condensation effect can be improved on the one hand, the distillation waste heat can be fully utilized to preheat the diethyl toluene diamine crude product, and the preheated diethyl toluene diamine crude product enters the distillation still to be distilled, so that the energy-saving effect is achieved.
Example 3
Referring to fig. 3-5, a combined continuous vacuum distillation purification apparatus for diethyltoluenediamine, based on embodiment 1 or 2, further comprises: the first condenser 4 and the second condenser 5 are both shell-and-tube condensers. The shell-and-tube condenser comprises a shell 10 and a tube group 11 arranged in the shell, wherein an annular space 17 is formed between the shell 10 and the tube group 11; the pipe group 11 is combined and comprises a central pipe 12 and peripheral pipes 13 on the periphery, the cross sections of the central pipe 12 and the peripheral pipes 13 are regular hexagons, the peripheral pipes 13 are six and are respectively attached to six side surfaces of the central pipe 12, the six peripheral pipes 13 are attached to each other and are positioned on the same concentric circle, and the adjacent peripheral pipes 13 are communicated through holes 14 on the contact side surfaces; the annular space 17 and the central tube 12 serve as the shell side of the condenser and are connected with the cold medium inlet and outlet at the two ends respectively, and the peripheral tube 13 serves as the tube side of the condenser and is connected with the heat medium inlet and outlet at the two ends respectively.
When the heat exchanger works, high-temperature diethyl toluenediamine gas distilled from a distillation kettle enters a condenser from the upper part through the peripheral pipe 13 (fluids in the peripheral pipe 13 can be communicated with each other through holes to realize sufficient heat exchange), low-temperature cooling liquid or a crude diethyl toluenediamine product enters the condenser through the annular space 17 and the central pipe 12, and cold and hot media perform sufficient heat exchange in the condenser. The utility model discloses in, no matter that kind of shell side of walking of cold and hot medium, also no matter the heat exchanger indulges and puts or transversely puts, because it gets into annular space (the space between nest of tubes and the casing promptly and the space between a plurality of nest of tubes) and center tube simultaneously, consequently can carry out more extensive, even distribution to heat transfer medium to improve effective heat transfer area.
Example 4
Referring to fig. 6, a combined continuous vacuum distillation purification apparatus for diethyltoluenediamine, based on embodiment 1 or 2, further comprises: the shell 10 of the condenser is a cylindrical cavity, and the tube groups 11 are in multiple groups and are arranged in the shell 10 at intervals; one group of tube banks 11 is arranged at the center of the cylindrical cavity as a central tube bank, and the other group of tubes 11 are arranged around the central tube bank as peripheral tube banks, and the peripheral tube banks are located on the same concentric circle.
The heat exchange area of the condenser can be further increased by the aid of the design, and heat exchange effects are improved. In order to further improve the heat exchange effect, the peripheral pipe group can be formed into a plurality of circles with diameters sequentially increased from the central pipe group to the outside, and the peripheral pipe group of each circle is positioned on the same concentric circle.
In the above embodiment, no matter what kind of cold and hot medium walks the shell side, and no matter whether the heat exchanger is vertically arranged or horizontally arranged, because the cold and hot medium simultaneously enters the annular space (i.e. the space between the tube group and the shell and the space between the tube groups) and the central tubes of the tube groups, the fluid capable of controlling the shell side is widely and sufficiently uniformly distributed in the heat exchanger, thereby avoiding the problem of low efficiency caused by heat exchange short circuit.
It is to be understood that the above-described embodiments are only a few, and not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims (8)

1. The utility model provides a diethyl toluene diamine combination formula is distillation purification device in succession reduces pressure, includes stills, the stills top is equipped with the feed inlet and exports with last, the stills below is equipped with down the export, go up the export and connect gradually condenser and diethyl toluene diamine fine work jar through the pipeline, be connected with vacuum pump, its characterized in that on condenser or the diethyl toluene diamine fine work jar:
the distillation kettle is characterized by also comprising a wiped film type pressure-reducing evaporator, wherein the lower outlet of the distillation kettle is connected with the feed inlet of the wiped film type pressure-reducing evaporator through a pipeline, the upper outlet of the wiped film type pressure-reducing evaporator is connected with the upper part of the distillation kettle through a pipeline, and the lower outlet of the wiped film type pressure-reducing evaporator is connected with a slag tank through a pipeline;
and a branch pipeline is arranged on a connecting pipeline between the lower outlet of the distillation kettle and the feed inlet of the wiped film pressure-reducing evaporator and is connected with the upper part of the distillation kettle.
2. The combined continuous reduced pressure distillation and purification device of diethyltoluenediamine according to claim 1, wherein the condensers are two stages connected in sequence, and are respectively a first condenser connected with the distillation still and a second condenser connected with the refined diethyltoluenediamine tank, and a cold medium inlet of the first condenser is connected with the crude diethyltoluenediamine tank through a pipeline, and a cold medium outlet is connected with the feed inlet of the distillation still; and a cold medium inlet of the second condenser is connected with an outlet of the cooling tower through a pipeline, and a cold medium outlet is connected with an inlet of the cooling tower.
3. The combined continuous vacuum distillation purification device of diethyltoluenediamine according to claim 1, wherein said condenser is a shell-and-tube condenser.
4. The combined continuous vacuum distillation purification device of diethyltoluenediamine, according to claim 3, wherein said shell-and-tube condenser comprises a shell and a tube bank mounted therein, said shell and said tube bank forming an annular space therebetween; the pipe group is combined and comprises a central pipe and peripheral pipes on the periphery, the cross sections of the central pipe and the peripheral pipes are regular hexagons, and the peripheral pipes are six and are respectively attached to six side surfaces of the central pipe; the annular space and the central tube are used as the shell pass of the condenser, and two ends of the annular space and the central tube are respectively connected with the inlet and the outlet of the first heat exchange medium, and the peripheral tube is used as the tube pass of the condenser, and two ends of the peripheral tube are respectively connected with the inlet and the outlet of the second heat exchange medium.
5. The combined continuous vacuum distillation purification device for diethyltoluenediamine according to claim 4, wherein said six peripheral tubes are attached to each other and located on the same concentric circle, and adjacent peripheral tubes are connected to each other through a through hole on the side in contact with each other.
6. The combined continuous vacuum distillation purification device of claim 4, wherein the tube banks are arranged in multiple groups and spaced apart in the housing.
7. The combined continuous vacuum distillation purification device of claim 6, wherein the housing is a cylindrical chamber, wherein a group of tubes is disposed as a central tube group at the center of the cylindrical chamber, and the peripheral tube groups are disposed around the central tube group and on the same concentric circle.
8. The combined continuous vacuum distillation purification device of claim 6, wherein the outer tube groups are arranged in a plurality of circles with increasing diameters from the central tube group to the outside, and the outer tube groups of each circle are located on the same concentric circle.
CN201921325075.1U 2019-08-15 2019-08-15 Diethyl toluenediamine combined type continuous reduced pressure distillation purification device Active CN210543405U (en)

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CN201921325075.1U CN210543405U (en) 2019-08-15 2019-08-15 Diethyl toluenediamine combined type continuous reduced pressure distillation purification device

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110368707A (en) * 2019-08-15 2019-10-25 东营海瑞宝新材料有限公司 A kind of diethyl toluene diamine combined type is continuously evaporated under reduced pressure purifying plant

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110368707A (en) * 2019-08-15 2019-10-25 东营海瑞宝新材料有限公司 A kind of diethyl toluene diamine combined type is continuously evaporated under reduced pressure purifying plant
CN110368707B (en) * 2019-08-15 2024-04-26 东营海瑞宝新材料有限公司 Diethyl toluenediamine combined type continuous reduced pressure distillation purification device

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