CN212548360U - Multi-kettle reaction rectifying device - Google Patents
Multi-kettle reaction rectifying device Download PDFInfo
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- CN212548360U CN212548360U CN202021861551.4U CN202021861551U CN212548360U CN 212548360 U CN212548360 U CN 212548360U CN 202021861551 U CN202021861551 U CN 202021861551U CN 212548360 U CN212548360 U CN 212548360U
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Abstract
The utility model discloses a multi-kettle reactive distillation device, which comprises a reaction kettle and a distillation column which are connected in series in a multi-stage manner; the side wall of the first-stage reaction kettle is connected with a material adding unit; along the main material flow direction, a liquid phase discharge port arranged at the upper part of the upper stage reaction kettle is sequentially connected to a feed port of the lower stage reaction kettle; the top of any stage of reaction kettle is provided with a gas phase discharge port, the gas phase discharge port at the top of the first stage of reaction kettle is connected to the bottom gas inlet of the second stage of reaction kettle, and the gas phase discharge ports from the second stage of reaction kettle to the last stage of reaction kettle are respectively connected to the rectifying tower so as to carry out rectification separation on light components. The utility model discloses the structure of well heat exchanger tube bank makes the mass transfer heat transfer efficiency in reation kettle at different levels high, and the multistage reation kettle of built-in special construction heat exchanger tube bank combines gradient viscosity, the control of gradient temperature that can the industrialization was implemented, can realize the reaction rectification of high viscosity, easy polymer system, can reduce steam consumption and waste water discharge again.
Description
Technical Field
The utility model belongs to the technical field of chemical production, a many kettles reaction rectification device is related to.
Background
The reactive distillation is to complete the reaction and the distillation separation simultaneously in the same system. Because the reaction process and the rectification process are carried out in the same equipment, compared with the traditional reaction unit series connection separation unit, the process is simplified, and the equipment cost is saved; and the reaction heat can be used for the liquid phase in the vaporization tower, thereby reducing the load of vaporization heat; and finally, the product is continuously removed by rectification separation, so that the occurrence of side reaction is avoided, the selectivity of the product is greatly improved, the product quality is improved, and the subsequent rectification operation cost is reduced.
Although the reactive distillation has many advantages, when the reactive distillation is applied to materials which have high viscosity and are easy to polymerize, a heat exchange tube bundle is difficult to arrange in the reaction kettle for heat transfer, the heat transfer can only be realized by adopting a jacket of the reaction kettle, the heat transfer area of the jacket is small, the vaporization heat of the reaction materials cannot be provided, and the reactive distillation is difficult to realize. Part of the process adopts the steps that firstly, steam is injected into a reactor to directly heat materials, and simultaneously, the steam carries light components to rise and enter a rectifying tower, so that the light components are removed from a high-viscosity material system. Because steam is a heating medium and a stripping medium, the consumption is high, the waste water is generated more, secondary pollution is caused, and the environmental protection cost is improved.
Therefore, there is a great need for providing a multi-kettle reactive distillation apparatus and process with high mass and heat transfer efficiency and capable of being industrially implemented for high-viscosity and easy-to-polymerize systems, which can achieve reactive distillation of high-viscosity and easy-to-polymerize systems and reduce steam consumption and wastewater discharge.
Disclosure of Invention
To the problem among the above-mentioned prior art, the utility model aims at providing a but the many kettles reaction rectifier unit of gradient viscosity control of mass transfer heat transfer efficiency height, industrialization implementation, can realize the reaction rectification of high viscosity, easy polymer system, can reduce steam consumption and waste water discharge again.
One of the purposes of the utility model provides a many kettles reaction rectification device, the technical scheme who adopts as follows:
a multi-kettle reactive distillation device comprises a reaction kettle and a distillation column which are connected in series in a multistage way;
the side wall of the first-stage reaction kettle is connected with a material adding unit; along the main material flow direction, a liquid phase discharge port arranged at the upper part of the upper stage reaction kettle is sequentially connected to a feed port of the lower stage reaction kettle; the top of any stage of reaction kettle is provided with a gas phase discharge port, the gas phase discharge port at the top of the first stage of reaction kettle is connected to the bottom gas inlet of the second stage of reaction kettle, and the gas phase discharge ports from the second stage of reaction kettle to the last stage of reaction kettle are respectively connected to the rectifying tower so as to carry out rectification separation on light components.
Preferably, the outer wall of the first-stage reaction kettle is provided with a jacket, and a heat exchange tube bundle is arranged in any one stage of reaction kettle and used for heating and vaporizing materials in each stage of reaction kettle.
Further, the heat exchange tube bundle I in the first-stage reaction kettle is arranged along the central axis of the first-stage reaction kettle;
the heat exchange tube bundle I is wholly positioned below the liquid level in the kettle, and the distance L between the top end of the heat exchange tube bundle I and the liquid level1And the bottom end of the reaction kettle penetrates through the bottom of the first-stage reaction kettle and extends downwards.
Furthermore, except the first-stage reaction kettle, a heat exchange tube bundle II in any stage of reaction kettle is horizontally placed at the lower part of each stage of reaction kettle along the side wall of the kettle.
Furthermore, the bottom end of the heat exchange tube bundle II along the length direction of the heat exchange tube bundle II penetrates through the side wall of the stage of reaction kettle and extends outwards.
Furthermore, 1 layer or 2 layers of heat exchange tube bundles II are distributed in each stage of kettle, and the heat exchange tube bundles II positioned on the same layer are uniformly distributed on the cross section in the horizontal direction along the circumference.
Furthermore, the heat exchange tubes of the heat exchange tube bundle I and the heat exchange tube bundle II are double-layer sleeves and comprise outer tubes and inner tubes arranged in the outer tubes, annular gaps between the outer tubes and the inner tubes are used for circulating steam, and the tops of the inner tubes along the length direction of the tubes are communicated with the interiors of the outer tubes and are used for enabling the inner tubes to circulate condensate;
a steam inlet is formed in the bottom of the outer pipe along the length direction of the pipe and is used for introducing steam; the bottom of the double-layer sleeve along the length direction of the pipe is provided with a condensate outlet for discharging condensate after steam heat exchange condensation in a backflow mode.
Preferably, the reaction kettle is in 3-4 stages connected in series.
Preferably, the bottom of the at least 1 stage reaction kettle is also connected with a low boiling point reaction monomer feeding pipeline.
Preferably, besides the first-stage reaction kettle, the bottom of any stage reaction kettle is also connected with a steam feeding pipeline for heating and steam stripping the materials in the kettle.
Preferably, the steam feeding pipeline is provided with a steam distributor.
Preferably, the rectifying tower is arranged above the second-stage reaction kettle; the bottom of the rectifying tower is tangentially provided with a gas phase feed inlet along a lateral line and a liquid phase reflux port communicated with the second-stage reaction kettle;
preferably, the height of the bottom of the rectifying tower from the first tray is 1.8-2.5m, and the ascending flow velocity of the gas-phase material is controlled to be less than 2 m/s.
The utility model discloses utilize foretell device can also provide a many kettles reaction rectification technology, include following step:
s1, heating and reacting the materials through a first-stage reaction kettle, feeding the liquid-phase discharged material of the first-stage reaction kettle into a second-stage reaction kettle for continuous heating and reacting, and feeding the gas-phase discharged material of the first-stage reaction kettle into the bottom of the second-stage reaction kettle for stirring and stripping gas of the second-stage reaction kettle;
s2, continuously heating and reacting the liquid-phase material in the second-stage reaction kettle, vaporizing and rising the light component, separating the light component in the second-stage reaction kettle in a rectifying tower, and discharging the liquid phase in the reaction to a third-stage reaction kettle to finish the reaction;
and S3, heating the liquid phase material in a third-stage reaction kettle for deep reaction, separating the gas phase material in the third-stage reaction kettle in a rectifying tower, and directly discharging the liquid phase material out or feeding the liquid phase material into the next-stage reaction kettle for continuous duplication.
Preferably, the temperature of materials in the multistage reaction kettle along the main material flow direction is controlled to be increased by 5-15 ℃ in sequence.
Preferably, the low boiling point reaction monomer is introduced into at least one stage of the multi-stage reaction kettle.
Preferably, the material viscosity of the first-stage reaction kettle is controlled to be below 50cp, and the reaction conversion rate is controlled to be between 70 and 90 percent by selecting and utilizing a low-boiling-point monomer; controlling the material viscosity of the second-stage reaction kettle to be below 100cp, and selectively controlling the reaction conversion rate to be between 90 and 100 percent by using a low-boiling-point monomer; the material viscosity of the third-stage reaction kettle is controlled below 200cp, so that the reaction conversion rate reaches or is basically close to 100%.
Preferably, steam is introduced into each of the reaction vessels except the first reaction vessel.
Preferably, the reaction kettle is set to be 4 stages connected in series; wherein, the adding amount of the steam in the second-stage reaction kettle is controlled to be 0.2-0.5% of the amount of the liquid material in the kettle; the addition amount of steam in the third-stage reaction kettle is 0.4-0.8% of the amount of liquid materials in the kettle; the addition amount of the steam in the fourth-stage reaction kettle is 0.8-1.8% of the amount of the liquid material in the kettle.
The utility model discloses can bring following beneficial effect:
1) in the device, materials firstly enter the first-stage reaction kettle for reaction, and then sequentially enter the subsequent reaction kettles at all stages until the reaction is finished, and light components in the process are gathered to the rectifying kettle and are continuously separated through the rectifying kettle, so that the occurrence of side reactions is reduced, and the reaction efficiency of products is improved; therefore, the utility model discloses a well multistage reation kettle sharing rectifying column realizes going on in step of reaction and separation, improves reaction efficiency.
2) The utility model adopts the heat exchange tube bundles with special structures in each stage of reaction kettle, on one hand, the outer wall of the heat exchange tube is efficiently transferred, the thickness and the viscosity of a heat transfer film are reduced, and the heat transfer efficiency is improved; on the other hand, the self-circulation and the mixing of the materials in the kettle are realized, and the gas and the liquid in the reaction kettle are uniformly mixed by the aid of stripping steam; therefore, when the viscosity of the materials in the kettle is less than 200cp, the gas and the liquid can be completely mixed without a stirrer, and the wall sticking phenomenon of the heat exchange tube is avoided; in addition, the consumption of stripping steam can be reduced, and the environmental protection cost is reduced.
3) The utility model discloses through the multistage reation kettle of establishing ties in the technology, and carry out gradient control to reaction monomer feeding ratio and reaction temperature, realize the control to reaction conversion rate and material viscosity in reation kettle at different levels, improve reaction rectification efficiency.
To sum up, the utility model discloses a heat exchanger tube bank structure makes the mass transfer heat transfer efficiency in reation kettle at different levels high, and the multistage reation kettle of built-in special construction heat exchanger tube bank combines gradient viscosity, the temperature control that can the industrialization was implemented, can realize the reaction rectification of high viscosity, easy polymer system, can reduce steam consumption and waste water discharge again.
Drawings
Fig. 1 is a schematic layout diagram of the reactive distillation device of the present invention.
Fig. 2 is a schematic structural diagram of the heat exchange tube bundle ii in the reaction kettle of the present invention, which is set as 2 layers.
Fig. 3 is a schematic structural diagram of a heat exchange tube bundle ii in the present invention.
Fig. 4 is a schematic diagram of the arrangement of the heat exchange tube bundle ii along the circumferential direction when the heat exchange tube bundle ii is located in the same layer.
Fig. 5 is a schematic structural diagram of a heat exchange tube bundle i in the present invention.
The meanings of the symbols in the drawings are as follows:
1-a first-stage reaction kettle, 10-a material adding unit, 11-a jacket and 12-a heat exchange tube bundle I;
2-a second-stage reaction kettle, 20-a heat exchange tube bundle II, 121/200-an outer tube and 122/201-an inner tube;
3-a third-stage reaction kettle; 4-fourth stage reaction kettle; 5-a rectifying tower; 6-low boiling point reaction monomer feed line;
7-a steam feed conduit, 70-a steam distributor;
a-a liquid phase discharge port, b-a feed port, c-a gas phase discharge port and d-a gas inlet;
e-steam inlet, f-condensate outlet, g-gas phase feed inlet and h-liquid phase reflux inlet.
Detailed Description
In order to more clearly illustrate embodiments of the present invention or technical solutions in the prior art, specific embodiments of the present invention will be described below with reference to the accompanying drawings. It is obvious that the drawings in the following description are only examples of the invention, and that for a person skilled in the art, other drawings and embodiments can be obtained from these drawings without inventive effort.
For the sake of simplicity, only the parts relevant to the present invention are schematically shown in the drawings, and they do not represent the actual structure as a product.
According to an embodiment provided by the present embodiment, as shown in fig. 1, a multi-kettle reactive distillation apparatus is provided, which includes a multi-stage reaction kettle connected in series and a distillation column 5;
the first-stage reaction kettle 1 is connected with a material adding unit 10; along the main material flow direction, a liquid phase discharge port a arranged at the upper part of the upper stage reaction kettle is sequentially connected to a feed port b of the lower stage reaction kettle; the top of any stage of reaction kettle 1 is provided with a gas phase discharge port c, the gas phase discharge port c at the top of the first stage of reaction kettle 1 is connected to the gas inlet d at the bottom of the second stage of reaction kettle 2, and the gas phase discharge ports from the second stage of reaction kettle 2 to the last stage of reaction kettle are respectively connected to the rectifying tower to separate light components. Therefore, the multistage reaction kettle shares one rectifying tower 5, the synchronous reaction and separation are realized, and the reaction efficiency is improved. Especially, the gaseous phase ejection of compact of first order reation kettle 1 directly gets into second order reation kettle, and not direct connection carries out the rectification separation to rectifier 5, can play stirring and steam stripping in second order reation kettle 2 on the one hand, promotes the effect of reaction, and on the other hand can not make a large amount of unreacted low boiling point monomers in the first order reation kettle 1 again take out to the rectifying column, reduces reaction efficiency. Wherein, the main flow direction refers to the flow direction of the main reaction product.
In practical application, the reaction kettle is preferably set to 3-4 stages:
the side wall of the first-stage reaction kettle 1 is connected with a material adding unit 10, specifically, a plurality of reaction monomers (such as a monomer I and a monomer II) are respectively added into the first-stage reaction kettle 1 through pipelines, and more than 70% of reaction is completed in the first-stage reaction kettle 1; a liquid phase discharge port a arranged at the upper part of the first-stage reaction kettle 1 is connected to a feed port b at the bottom of the second-stage reaction kettle 2, so that liquid phase discharge of the first-stage reaction kettle 1 enters the second-stage reaction kettle 2 for continuous reaction, a gas phase discharge port c arranged at the top part of the first-stage reaction kettle 1 is connected to a bottom gas inlet d of the second-stage reaction kettle, and gas phase discharge enters the bottom of the second-stage reaction kettle 2 to be used as stirring and stripping gas of the second-stage reaction kettle 2;
a liquid phase discharge port a arranged at the upper part of the second-stage reaction kettle 2 is connected to a feed port at the bottom of the third-stage reaction kettle 3, so that liquid phase discharge can enter the third-stage reaction kettle 3 for continuous deep reaction, a gas phase discharge port c arranged at the top of the second-stage reaction kettle 2 is connected to the rectifying tower 5 for separation, light components with low boiling points in the rectifying tower 5 are separated from the top of the tower, and heavy components flow back to the second-stage reaction kettle 2 from the tower kettle; the second-stage reaction kettle 2 also has the function of a reboiler of a reactive distillation column 5 except for continuously finishing the reaction, wherein light components are vaporized and rise to enter the distillation column 5, and the liquid phase discharged from the reaction enters a third-stage reaction kettle 3 to ensure that the materials are reacted completely;
a gas-phase discharge hole c of the third-stage reaction kettle 3 is connected to the rectifying tower 5 for purifying light components, and when the reaction kettle is set to be 3-stage, liquid-phase discharge of the third-stage reaction kettle 3 is directly discharged; when the reaction kettle is set to be 4-stage, the liquid phase discharged from the third-stage reaction kettle 3 enters the fourth-stage reaction kettle 4 to be continuously stripped, and the fourth-stage reaction kettle 4 mainly has the function of completely stripping the light components, so that the content of the light components in the heavy components is reduced.
In addition, the rectifying tower 5 is arranged above the second-stage reaction kettle 2, so that a large amount of light components (especially small molecular reaction byproducts) in the second-stage reaction kettle 2 are fully separated from a reaction system, and the reaction and product purification efficiency is improved. Because most of the reaction is completed in the second-stage reaction kettle 2, the viscosity of the material is not too high yet, and the material can be repeatedly vaporized and separated as a reboiler.
As a preferred embodiment, the bottom of at least one stage of the reaction vessel is further connected to a low boiling point reaction monomer feed line 6. Specifically, the selective setting according to the actual working conditions is needed, and the low boiling point reaction monomer feed pipeline 6 is not needed to be arranged for the subsequent reaction kettle which basically finishes the reaction. For example, when the reactors are set to 4 stages in series, the material viscosity of the first stage reactor 1 is controlled to be 50cp or less, and the conversion rate is controlled to be 70 to 90% by controlling the feed rate and the feed ratio of the reactive monomer according to the viscosity change, and the conversion rate is generally controlled by selecting the low boiling point reactive monomer (monomer three). The material viscosity of the second-stage reaction kettle 2 is controlled below 100cp, and the conversion rate is controlled between 90 and 100 percent by controlling the addition amount of a low-boiling-point reaction monomer (monomer III) according to the change condition of the viscosity. The third-stage reaction kettle 3 is used for carrying out deep reaction, and the low-boiling point reaction monomer (monomer III) is controlled according to the feeding ratio of 100 percent of conversion rate, wherein the material viscosity is controlled below 200 cp. The fourth-stage reaction kettle does not need to be filled with low-boiling reaction monomers.
As a preferred another embodiment, in addition to the first-stage reaction vessel 1, the bottom of any stage reaction vessel is connected with a steam feed pipe 7 for heating and stripping the reactants. Preferably, a steam distributor 70 is further disposed on the steam feeding pipe 7. More specifically, as shown in fig. 2, the steam distributor 70 is a straight pipe with a pipe diameter of 50-200mm, a plurality of holes are formed in the side wall of the straight pipe in an inclined manner, the angle α between the side wall of the straight pipe and the vertical direction is 30-45 °, the hole diameter of each hole is 5-20mm, the hole distance between adjacent holes is 10-50mm, and the hole distance between adjacent holes is not less than 2 times of the hole diameter. The inclination angle range of the opening enables the steam to have initial velocity which is upward along the axial direction and initial velocity which is diffused to the periphery along the radial direction, and the opening angle avoids short circuit of the steam in the kettle, improves the distribution of the steam on the whole section of the kettle and improves the steam stripping efficiency; the aperture size and the aperture distance give consideration to the effective dispersion of steam, and the probability of blockage of liquid materials due to too small aperture is reduced. Thereby improving the dispersive steam stripping effect of the steam.
On the basis of the embodiment, the outer wall of the first-stage reaction kettle 1 is provided with a jacket 11, and a heat exchange tube bundle is arranged inside any one stage reaction kettle and used for heating and vaporizing substances in the kettle.
Specifically, reaction monomers one to three (2 reaction monomers or more reaction monomers according to different reaction conditions) enter the first-stage reaction kettle 1 from the bottom according to a required stoichiometric proportion, the reaction is carried out under proper process conditions, a heat source required by the reaction is indirectly provided by a heat medium through a jacket 11, and the part with insufficient heat supply of the jacket 11 is provided by a built-in heat exchange tube bundle I12 placed into the first-stage reaction kettle 1 from the lower part.
Preferably, the heat exchange tube bundle I12 in the first-stage reaction kettle 1 is arranged along the central axis of the first-stage reaction kettle 1, the heat exchange tube bundle I12 is wholly below the liquid level, and the distance L between the top end of the heat exchange tube bundle I12 and the liquid level is1，L1Preferably (100-. Specifically, the two ends of the first-stage reaction kettle 1 are of elliptical structures, the middle of the first-stage reaction kettle is of a cylindrical structure, and the bottom end of the heat exchange tube bundle I12 penetrates through the bottom tangent line of the first-stage reaction kettle and extends downwards.
Specifically, the built-in heat exchange tube bundle i 12 in the first-stage reaction kettle 1 can form a high-temperature region around the heat exchange tube bundle to accelerate the reaction and simultaneously expand the volume and reduce the density of surrounding materials, so that a special density distribution field and a directional plug flow are formed in the reactor, and in the vertical direction, a density distribution field with a low bottom density, a high upper density, a low center density and a high kettle wall density is formed in the reaction kettle, and in the radial direction, internal circulation flow from bottom to top is formed in the density distribution field (as shown by an arrow flow in the first-stage reaction kettle in fig. 1). The stirring effect of the evaporated gas phase on the materials is added, so that the reaction materials can be quickly mixed, and the mass transfer and the heat transfer of the reaction kettle can be met without stirring.
The heat exchange tube bundle II 20 in any stage of reaction kettle except the first stage of reaction kettle 1 is horizontally placed at the lower part of the kettle along the side wall of the kettle. The bottom end of the heat exchange tube bundle II 20 along the length direction of the heat exchange tube bundle II penetrates through the side wall of the reaction kettle and extends outwards, and a corresponding steam inlet e and a corresponding condensate outlet f are conveniently arranged on the part, extending outwards, of the heat exchange tube bundle II 20 from the side wall of the reaction kettle. The horizontally arranged heat exchange tube bundle II 20 has cutting and mixing effects on ascending gas-liquid phase mixtures, so that gas and liquid can be mixed more uniformly. Ascending gas-liquid logistics flow through the outer surface of the heat exchange tube due to the fact that the flow channel is narrowed and the speed is increased between the heat exchange tubes of the heat exchange tube bundle II 20, heat exchange efficiency is improved, meanwhile, the cleaning effect is achieved on the heat exchange tube, and the adhesion layer on the outer surface of the heat exchange tube is thinned. Specifically, the heat exchange tube bundle ii 20 forms a special density distribution field inside the reaction kettle, that is, in the vertical direction, the density and viscosity of the material gradually increase from bottom to top, in the radial cross section, the density and viscosity of the material gradually increase from outside to inside, and the volume expansion of the low-density material causes the material to form an inner circulation in which the outer ring is from bottom to top and the inner ring is from top to bottom in the reaction kettle (as shown by the arrow flow direction in fig. 2). Therefore, the arrangement of the heat exchange tube bundle II 20 maximizes the heating and mass transfer efficiency of steam, has high vaporization efficiency of materials, and is not easy to form a heat transfer surface adhesion layer.
Preferably, 1 layer or 2 layers of the heat exchange tube bundles II 20 are distributed in the kettle along the horizontal direction of the side wall, the heat exchange tube bundles II 20 on the same layer are circumferentially and uniformly distributed on the cross section, and no more than 5 heat exchange tube bundles II 20 on any layer are distributed along the circumferential direction.
Specifically, the diameter D of the heat exchange tube bundle I12 and the heat exchange tube bundle II 20 is controlled within the range of (500) and 1500) mm, and the total number of the heat exchange tube bundles II 20 can be between 2 and 10 according to the heat load. Referring to FIG. 5, the spacing L between the opposing heat exchange tube bundles II 20 on the same layer of circumference2Is (300-3Is (100) mm, and the distance between two layers of heat exchange tube bundles II 20 is (600) mm and 1500 mm. In practical application, the total number of the heat exchange tube bundles II 20 in the third-stage reaction kettle 3 and the fourth-stage reaction kettle 4 is 2-6, and the number of single layers arranged along the horizontal direction of the side wall of the kettle is not more than 3.
As shown in fig. 3 and 4, the heat exchange tubes of the heat exchange tube bundle i 12 and the heat exchange tube bundle ii 20 are double-layer sleeves, and include an outer tube 121/200 and an inner tube 122/201 disposed in the outer tube 121/200, an annular space between the outer tube 121/200 and the inner tube 122/201 is used for flowing steam, and the top of the inner tube 122/201 along the length direction of the tubes is communicated with the inside of the outer tube 121/200 to flow condensate through the inner tube 122/201;
the bottom of the outer pipe 121/200 along the length direction of the pipe is provided with a steam inlet e for introducing steam; and a condensate outlet f is formed in the bottom end of the double-layer sleeve along the length direction of the sleeve and is used for discharging condensate after steam heat exchange and cooling.
Specifically, the outer pipe 121, the inner pipe 122, the outer pipe 200 and the inner pipe 201 are matched to form a double-layer sleeve, steam enters the outer pipe 121/200 from a steam inlet e at the bottom of the double-layer sleeve, latent heat is released in the upward movement process to heat materials outside the pipe, condensate is pushed by the steam to flow and rise to the top end to fall into the inner pipe 122/201, flows out of the inner pipe, and is collected together at the bottom end of the heat exchange pipe bundle to be discharged out of the system. That is, the outer tube 121/200 communicates steam with the annulus of the inner tube 122/201, which communicates condensate. The heat exchange tube bundle has the advantages that the contact side of the heat exchange tube bundle and the dividing wall of the material is kept to be high-temperature steam, the heat transfer coefficient is high, the heat transfer efficiency is high, the vaporization rate of the material outside the tube is kept high, and the wall sticking phenomenon is avoided. More specifically, the heat exchange tubes have an outer tube diameter of 40mm-80mm, an inner tube diameter of 20mm-25mm, and a distance between two adjacent heat exchange tubes of 20mm-50mm, and the length L of the heat exchange tubes is shown in FIG. 54Is 1000mm-4000 mm.
In addition, both ends of any stage of reaction kettle 1 are of an elliptical structure, and the middle part of the reaction kettle is of a cylindrical structure; the length-diameter ratio of any stage of reaction kettle is within the range of 1.2-2. If the aspect ratio is too low, it is detrimental to liquid settling, and if it is too high, it is detrimental to gas phase removal and mixing. Except the first-stage reaction kettle, the distance between the liquid level in each stage of reaction kettle and the top of the reaction kettle is more than 1.5m, and the buffer space can avoid carrying high-viscosity liquid into the rectifying tower.
On the basis of any one of the embodiments, a gas phase feed inlet g is arranged at the bottom of the rectifying tower 5 along the tangential direction of a lateral line; and tangential feeding is carried out by adopting a side line at the bottom so as to reduce entrainment of heavy components to a tray when light components enter the tower. And the bottom of the rectifying tower 5 is provided with a liquid phase reflux port h communicated with the second-stage reaction kettle 2. Preferably, the height from the bottom of the rectifying tower 5 to the first tray is 1.8-2.5m, and the gas phase rising flow velocity is less than 2 m/s; to ensure complete settling of entrained heavies. More preferably, the separation tray at 50% of the lower part of the rectifying tower 5 adopts any one of a plate tower tray or a guide plate tower tray (including a tongue-shaped tower tray) or a float valve tower tray, and the upper tray can be selected to be consistent with the lower tray in form or be selected to be a high-efficiency filler tray.
Except the first-stage reaction kettle, substances such as solvent, byproducts, stripping steam and the like in each-stage reaction kettle enter a rectifying tower and are separated in the rectifying tower, wherein the tower top produces a fraction with the lowest boiling point, the tower produces a light fraction with a slightly higher boiling point, and heavy components flow back to the second-stage reaction kettle.
On the basis of the above embodiment, according to the utility model discloses a reaction rectification device can also implement a many cauldron reaction rectification technology, includes following step:
s1, heating and reacting the materials through a first-stage reaction kettle, feeding the liquid-phase discharged material of the first-stage reaction kettle into a second-stage reaction kettle for continuous heating and reacting, and feeding the gas-phase discharged material into the bottom of the second-stage reaction kettle to be used as stirring and stripping gas of the second-stage reaction kettle;
s2, continuously heating and reacting the liquid-phase material in the second-stage reaction kettle, vaporizing and rising the light component in the liquid-phase material to enter a rectifying tower, and discharging the liquid-phase material in the reaction to enter a third-stage reaction kettle for reaction;
s3, heating the liquid phase material in a third-stage reaction kettle for deep reaction, separating the gas phase material in the third-stage reaction kettle in a rectifying tower, and directly discharging the liquid phase material out or feeding the liquid phase material into the next-stage reaction kettle for continuous duplication.
In the embodiment, after the reaction in the first-stage reaction kettle 1, the liquid-phase heavy component material generated in the reaction sequentially passes through the subsequent several stages of reaction kettles until the reaction is completed by 100%; the gas phase discharged material firstly enters the second-stage reaction kettle 2 to promote the stirring and steam stripping of the materials in the kettle, the gas phase discharged material enters the rectifying tower 5 to purify the light components after the reaction efficiency is improved, and the liquid phase material continuously reacts in the subsequent reaction kettles at all stages and the generated gas phase discharged material also enters the rectifying tower under the steam stripping action so as to further reduce the content of the light components in the heavy components and completely steam strip and separate the light components.
As a preferred embodiment, the temperature in the multi-stage reaction kettle is controlled to be increased by 5-15 ℃ in sequence; so as to slow down the viscosity rising trend caused by the rise of the average molecular weight of the materials and improve the reaction efficiency. Specifically, with the above embodiments, through special settings (not repeated here) of the heat exchange tube bundle i 12 and the heat exchange tube bundle ii 20 in each stage of the reaction kettle, gas-liquid uniform mixing in a non-stirring state and efficient vaporization of light components are realized, and then high yield of reaction products and separation of products and byproducts are realized through reactive distillation.
As another preferred embodiment, a low-boiling monomer is fed into at least one of the multi-stage reaction vessels to increase the conversion of the reaction product. Specifically, the selective setting is required according to the actual working conditions, and for the subsequent reaction kettle which has already reached 100% reaction, the low boiling point monomer is not required to be introduced to promote the reaction.
In practical application, the reaction kettle is set to be 3-4 stages in series, the material viscosity of the first stage reaction kettle 1 is controlled below 50cp, the reaction conversion rate is controlled between 70-90% by controlling the feeding ratio of each reaction monomer and selecting a low boiling point monomer (monomer III) according to the viscosity change condition. The material viscosity of the second-stage reaction kettle 2 is controlled below 100cp, and the conversion rate is controlled between 90 and 100 percent by controlling the addition amount of a low-boiling-point monomer (monomer III) according to the change condition of the viscosity. The third stage reaction vessel 3 is used for deep reaction, and the low boiling point monomer (monomer three) is controlled according to the feeding ratio of 100 percent of conversion rate, wherein the material viscosity is controlled below 200 cp. When reation kettle establishes to 4 grades, 3 liquid phase ejection of compact entering fourth order reation kettle 4 of third order reation kettle continue the steam stripping, and fourth order reation kettle 4 main function carries out thorough steam stripping to the light component, reduces the light component content in the heavy component, because of accomplishing the reaction in the preceding third order reation kettle, need not additionally let in low boiling monomer again.
More preferably, the addition amount of the stripping steam in the second-stage reaction kettle 2 is 0.2-0.5% of the amount of the liquid material in the kettle. Adding stripping steam (or other gas), crushing the liquid phase material which circularly flows in the first-stage reaction kettle 1 together with the gas phase material from the first-stage reaction kettle 1 and the vaporized gas phase in the kettle, mixing the gas phase and the liquid phase on a smaller scale, desorbing the light components wrapped by the liquid, and reducing viscosity of the reaction material. And additionally controlling: the addition amount of the stripping steam in the third-stage reaction kettle 3 is 0.4-0.8% of the amount of the liquid material in the kettle; the addition of the stripping steam in the fourth-stage reaction kettle 4 is 0.7-1.8% of the amount of the liquid material in the kettle, and the byproduct light component is further separated and purified from the heavy component. Wherein "%" represents a mass ratio.
In the above embodiment, the control of the reaction conversion rate and the material viscosity is realized by connecting the multistage reaction kettles in series and controlling the feed ratio and the temperature gradient of each reaction monomer.
Comparative example 1 Synthesis reaction of methyl methacrylate
The reaction system contains a readily polymerizable monomer of methacrylic acid although the viscosity is not high;
reaction monomers: methanol, water, methacrylamide sulfate.
Reaction rectifying device
The reactor comprises four stages of reaction kettles and a rectifying tower which are connected in series, and the materials enter a feed inlet of a next-stage reaction kettle after entering a first-stage reaction kettle 1 for reaction; the top of any stage of reaction kettle is provided with a gas phase discharge port, the gas phase discharge port at the top of the first stage of reaction kettle is connected to the bottom gas inlet of the second stage of reaction kettle, and the gas phase discharge ports from the second stage of reaction kettle to the last stage of reaction kettle are respectively connected to a rectifying tower so as to carry out rectification separation on light components; and the former three-stage reaction kettle introduces low boiling point reaction monomer through a low boiling point monomer pipeline 6 to promote reaction conversion rate, and the latter three-stage reaction kettle adds steam through a steam pipeline 7 for steam stripping.
However, different from fig. 1, the four-stage reaction kettle in this embodiment is provided with a jacket on the outer wall of the kettle for jacket type heat exchange without a built-in heat exchange tube bundle.
Methacrylic acid, water and methanol are produced at the top of the rectifying tower, and the final liquid phase discharged from the reaction kettle is ammonium bisulfate, sulfuric acid and H2A mixture of O.
Reactive distillation process
The materials are heated and reacted through a first-stage reaction kettle, a third monomer is introduced, the feeding proportion and the temperature of each reaction monomer are adjusted, and the reaction conversion rate of the first-stage reaction kettle is controlled to be 90%; gas-phase materials in the first-stage reaction kettle enter a second-stage reaction kettle to be stirred and heated for steam stripping, liquid-phase materials continue to finish reaction in the second-stage reaction kettle, the temperature of the second-stage reaction kettle is monitored and controlled to be higher than 10 ℃ of the first-stage reaction kettle through a thermometer, 1% of steam is injected into the second-stage reaction kettle (the ratio of the steam to the amount of the liquid materials in the second-stage reaction kettle), the reaction conversion rate of the second-stage reaction kettle is controlled to be 95%, light components in the steam are vaporized and rise to enter a rectifying tower for separation, and liquid-phase materials in the reaction enter a third-stage reaction kettle to finish; the liquid phase material is deeply reacted in a third-stage reaction kettle, the heating temperature is controlled to be higher than 15 ℃ of the second-stage reaction kettle, 1% of steam is injected into the third-stage reaction kettle (the ratio of the heating temperature to the amount of the liquid material in the third-stage reaction kettle), the reaction is completed, the light component in the liquid phase material is vaporized and ascended to enter a rectifying tower for separation, the reacted liquid phase material is discharged to enter a fourth-stage reaction kettle, the temperature of the fourth-stage reaction kettle is controlled to be higher than 15 ℃ of the second-stage reaction kettle, 1% of steam is injected into the fourth-stage reaction kettle (the ratio of the heating temperature to the amount of the liquid material in.
Results of the reaction
Reaction conversion rate: 99.5% and the steam consumption was 3.5% of the feed. The water content in the reaction effluent liquid phase mixture was 26%. The residence time of the materials in each reaction kettle is 1 hour.
Example 1 Synthesis of methyl methacrylate
The reaction system and the reaction monomers were the same as in comparative example 1;
reaction rectifying device
The reactor comprises four stages of reaction kettles and a rectifying tower which are connected in series, and the materials enter a feed inlet of a next-stage reaction kettle after entering a first-stage reaction kettle 1 for reaction; the top of any stage of reaction kettle is provided with a gas phase discharge port, the gas phase discharge port at the top of the first stage of reaction kettle is connected to the bottom gas inlet of the second stage of reaction kettle, and the gas phase discharge ports from the second stage of reaction kettle to the fourth stage of reaction kettle are respectively connected to a rectifying tower so as to carry out rectification separation on light components; and the former three-stage reaction kettle introduces low boiling point reaction monomer through a low boiling point monomer pipeline 6 to promote reaction conversion rate, and the latter three-stage reaction kettle adds steam through a steam pipeline 7 for steam stripping.
However, different from fig. 1, in this example, the first-stage reaction vessel is not provided with the heat exchange tube bundle i 12, and only jacket heating is adopted, and the second-stage reaction vessel, the third-stage reaction vessel and the fourth-stage reaction vessel are all provided with 4 heat exchange tube bundles ii 20 in total, as shown in fig. 2. The interval L between the opposite heat exchange tube bundles II 20 in the same layer along the circumferential direction2Is 600 mm; the diameter D of the heat exchange tube bundle II 20 is 800 mm; the distance between the two layers is 800 mm; the diameter of the outer pipe 200 of the heat exchange pipe is 60mm, and the diameter of the inner pipe 201 is 25 mm.
Methacrylic acid, water and methanol are produced at the top of the rectifying tower, and the final liquid phase discharged from the reaction kettle is ammonium bisulfate, sulfuric acid and H2A mixture of O.
Reactive distillation process
The same as example 1 except that: the reaction conversion rate of the first-stage reaction kettle is controlled to be 85 percent; the reaction conversion rate of the second-stage reaction kettle is controlled at 95%, and 0.3% of steam (the ratio of the steam to the liquid material in the second-stage reaction kettle) is injected into the second-stage reaction kettle; the third-stage reaction kettle has complete reaction, and 0.6 percent of steam (the ratio of the steam to the liquid material in the third-stage reaction kettle) is injected into the third-stage reaction kettle; the fourth stage reactor was fed with 0.7% steam (ratio to the amount of liquid material in the stage).
Results of the reaction
Reaction conversion rate: 99.9% and steam consumption was 1.6% of the feed. The water content in the liquid phase mixture discharged from the reaction is 17%. The residence time of the material in each reactor was 0.7 hours. The water content in the effluent liquid phase was better than that in comparative example 1 regardless of residence time, stripping steam consumption, and effluent liquid phase.
Example 2
This example is substantially the same as the reaction system, reactive distillation apparatus and corresponding process of example 1. The difference is only that:
reaction rectifying device
1. The fourth-stage reaction kettle is not arranged, and the stripping step of the fourth-stage reaction kettle is correspondingly eliminated.
2. A heat exchange tube bundle I12 with the diameter D of 600mm is arranged in the first-stage reaction kettle. The distance between the top of the heat exchange tube bundle I12 and the liquid level is 500 mm.
Reactive distillation process
The reaction conversion rate of the first-stage reaction kettle is controlled at 95 percent; the reaction of the second-stage reaction kettle is completed, and 0.6 percent of steam (the ratio of the steam to the liquid material in the second-stage reaction kettle) is injected into the second-stage reaction kettle; the third stage reactor was fed with 0.8% steam (ratio to the amount of liquid material in the stage).
And (3) reaction results:
reaction conversion rate: 99.95% and the stripping steam consumption was 1.4% of the feed. The water content in the liquid phase mixture discharged from the reaction was 17.3%. The residence time of the material in each reactor was 0.8 hours.
Example 3
This example is substantially the same as the reaction system, reactive distillation apparatus and corresponding process of example 1. The difference is only that:
reactive distillation process
The reaction conversion rate of the first-stage reaction kettle is controlled at 90 percent; the reaction conversion rate of the second-stage reaction kettle is controlled at 95%, and the steam injected into the second-stage reaction kettle is 0.25% (the ratio of the steam to the material quantity); the third-stage reaction kettle is completely reacted, and 0.6 percent of steam (the ratio of the steam to the material quantity) is injected into the third-stage reaction kettle; the fourth stage reactor was fed with 0.7% steam (ratio to the amount of feed).
And (3) reaction results:
reaction conversion rate: 99.94% and the steam consumption was 1.55% of the feed. The water content in the liquid phase mixture discharged from the reaction is 17%. The residence time of the material in each reactor was 0.7 hours.
Example 4
This example is substantially the same as the reaction system, reactive distillation apparatus and corresponding process of example 1. The difference is only that:
reaction rectifying device
As shown in fig. 1, a heat exchange tube bundle I12 with the diameter D of 600mm is arranged in the first-stage reaction kettle in addition to being heated by a jacket; the distance between the top of the heat exchange tube bundle I12 and the liquid level is 500 mm.
Reactive distillation process
The reaction conversion rate of the first-stage reaction kettle is controlled at 90 percent; the reaction conversion rate of the second-stage reaction kettle is controlled to be 98 percent, and 0.3 percent of steam (the ratio of the steam to the amount of the liquid material in the second-stage reaction kettle) is injected into the second-stage reaction kettle; the third reaction kettle has complete reaction, and the third reaction kettle injects 0.6 percent of steam (the ratio of the steam to the liquid material in the third reaction kettle); the fourth stage reactor was fed with 0.7% steam (ratio to the amount of liquid material in the stage).
Results of the reaction
Reaction conversion rate: 99.98% and the stripping steam consumption was 1.6% of the feed. The water content in the liquid phase mixture discharged from the reaction is 16.8 percent. The residence time of the material in each reactor was 0.7 hours.
Comparative example 2: synthesis of bis-2, 2,6, 6-tetramethylpiperidinol sebacate (high viscosity system)
Reaction monomers: piperidinol, dimethyl sebacate and n-heptane as solvent
Reaction rectifying device
The device comprises a single reaction kettle (used for esterification) and a rectifying tower, wherein the single reaction kettle is provided with a jacket on the outer wall of a kettle body for jacket type heat exchange, a gas phase outlet of the reaction kettle is directly connected to the rectifying tower, methacrylic acid, water and methanol are produced at the top of the rectifying tower, and the final liquid phase discharge of the reaction kettle is a sebacic acid bis-2, 2,6, 6-tetramethyl piperidinol ester product.
Reactive distillation process
The reaction and the rectification adopt intermittent operation, after a single reaction kettle is stirred and completely reacts for 5 hours, the reaction kettle is decompressed and rectified for 3 hours, the by-product and the solvent are evaporated, and the liquid-phase product is discharged and then enters cooling water to perform flushing crystallization to recover the product.
And (3) reaction results: the product yield is as follows: 90.5 percent. The purity of the product is 98 percent. The reaction conversion rate is low due to poor gas-liquid mass transfer effect. Due to poor separation effect, the purity of the product is not high, and the downstream application of the product is influenced.
EXAMPLE 5 Synthesis of bis-2, 2,6, 6-tetramethylpiperidinol sebacate
The reaction system and the reaction monomers were the same as in comparative example 2:
reaction rectifying device
Comprises three stages of reaction kettles connected in series and a rectifying tower, wherein materials enter a first-stage reaction kettle to react and then sequentially enter a feed inlet of a next-stage reaction kettle; the top of any stage of reaction kettle is provided with a gas phase discharge port, the gas phase discharge port at the top of the first stage of reaction kettle is connected to the bottom gas inlet of the second stage of reaction kettle, and the gas phase discharge ports from the second stage of reaction kettle to the third stage of reaction kettle are respectively connected to a rectifying tower so as to carry out rectification separation on light components; and the three-stage reaction kettle introduces a low-boiling point reaction monomer through a low-boiling point monomer pipeline 6 to promote the reaction conversion rate, and the two-stage reaction kettle is added with steam through a steam pipeline 7 for steam stripping.
Wherein, 1 vertical heat exchange tube bundle I12 is arranged on the central line in the first-stage reaction kettle; two layers of 6 heat exchange tube bundles II 20 shown in figures 3-4 are arranged in the second-stage reaction kettle and the third-stage reaction kettle respectively; the diameter of a heat exchange tube bundle I12 in a first-stage reaction kettle is 800mm, and the distance between the top of the tube bundle and a liquid level L1The diameter of the outer pipe 121 of the heat exchange pipe is 300mm, the diameter of the inner pipe 122 is 25mm, and the distance between adjacent pipes is 30 mm.
The diameter of the heat exchange tube bundle II of the second-stage reaction kettle is 600mm, the distance from the bottom end of the tube bundle along the length direction to the tangent line of the bottom of the reaction kettle is 100mm, the pipe diameter of the outer pipe 200 of the heat exchange tube is 50mm, the pipe diameter of the inner pipe 201 is 20mm, and the distance between adjacent pipes is 30 mm. End spacing L between opposing heat exchange tube bundles on each layer2500mm and a vertical spacing of 600mm between the two layers.
Reactive distillation process
The materials are heated and reacted through a first-stage reaction kettle, a third monomer is introduced, the feeding proportion and the temperature of each reaction monomer are adjusted, the temperature in the first-stage reaction kettle is controlled at 100 ℃, the viscosity in the first-stage reaction kettle is controlled at about 35cp, and the reaction conversion rate is controlled at 80%; introducing the gas phase (methanol and n-heptane) of the first-stage reaction kettle into the bottom of the second-stage reaction kettle, and discharging the liquid phase into the second-stage reaction kettle for continuous reaction; the temperature in the second reaction kettle is controlled to be about 110 ℃, and 0.3 percent of steam (the ratio of the steam to the liquid phase feeding amount) is injected to ensure that the second-stage reaction kettle completely reacts and the viscosity is controlled to be about 150 cp; discharging a liquid phase of the second-stage reaction kettle, allowing the liquid phase to enter a third-stage reaction kettle for deep light component removal, allowing a gas phase (methanol, n-heptane and steam) to enter a rectifying tower for separation, allowing the top of the rectifying tower to produce methanol, allowing heptane and water to be produced in the tower, allowing part of heptane to return to the second-stage reaction kettle after heptane and water are in phase, allowing part of heptane to return to a first-stage reaction kettle (not shown in the figure), and allowing water to enter a downstream recrystallization unit for reuse; the temperature in the third reaction kettle is controlled to be about 125 ℃, and 0.8 percent of steam (the ratio of the steam to the liquid phase feeding amount) is injected to control the viscosity in the third reaction kettle to be less than 200 cp.
And (3) reaction results: reaction residence time 4 hours, product yield: 99.5 percent. The purity of the product is 99.8%.
Example 6
This example is substantially the same as the reaction system, reactive distillation apparatus and corresponding process of example 5. The difference is only that:
in the reaction device: the diameter D of a heat exchange tube bundle I12 in a first-stage reaction kettle is 1000mm, and the distance between the top of the tube bundle and the liquid level L1Is 300mm, the pipe diameter of the outer pipe 121 of the heat exchange pipe is 60mm, the pipe diameter of the inner pipe 122 is 25mm, and the distance between the adjacent pipes is 30 mm.
In the reaction rectification process: the reaction conversion rate of the first-stage reaction kettle is controlled at 90%, the temperature in the first-stage reaction kettle is controlled at 105 ℃, the viscosity is controlled at about 45cp, the gas phase (methanol and n-heptane) of the first-stage reaction kettle is introduced into the bottom of the second-stage reaction kettle, and the liquid phase is discharged and enters the second-stage reaction kettle for continuous reaction; the temperature in the second reaction kettle is controlled to be about 120 ℃, the reaction of the second reaction kettle is completely carried out, 0.3% of steam is injected into the second reaction kettle, the viscosity is controlled to be about 150cp, the liquid phase discharged from the second reaction kettle enters the third reaction kettle to deeply remove light components, the gas phase (methanol, n-heptane and steam) enters a rectifying tower to be separated, the top of the rectifying tower produces methanol, heptane and water are produced in the tower, after the heptane and the water are in phase, part of the heptane returns to the second reaction kettle, part of the heptane returns to the first reaction kettle, and the water enters a downstream recrystallization unit to be reused; the temperature in the third reaction kettle is controlled to be about 130 ℃, the viscosity of the third reaction kettle is controlled to be below 200cp, and 0.8 percent of steam is injected.
And (3) reaction results:
reaction residence time 4 hours, product yield: 99.3 percent. The purity of the product is 99.8%.
It should be noted that the above embodiments can be freely combined as necessary. The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The utility model provides a many cauldron reaction rectifier unit which characterized in that:
comprises a multistage reaction kettle and a rectifying tower which are connected in series;
the side wall of the first-stage reaction kettle is connected with a material adding unit; along the main material flow direction, a liquid phase discharge port arranged at the upper part of the upper stage reaction kettle is sequentially connected to a feed port of the lower stage reaction kettle; the top of any stage of reaction kettle is provided with a gas phase discharge port, the gas phase discharge port at the top of the first stage of reaction kettle is connected to the bottom gas inlet of the second stage of reaction kettle, and the gas phase discharge ports from the second stage of reaction kettle to the last stage of reaction kettle are respectively connected to the rectifying tower so as to carry out rectification separation on light components.
2. The multi-tank reactive distillation apparatus of claim 1, wherein:
the outer wall of the first-stage reaction kettle is provided with a jacket, and a heat exchange tube bundle is arranged in any one stage of reaction kettle and used for heating and vaporizing materials in each stage of reaction kettle.
3. The multi-tank reactive distillation apparatus of claim 2, wherein:
the heat exchange tube bundle I in the first-stage reaction kettle is arranged along the central axis of the first-stage reaction kettle;
the heat exchange tube bundle I is wholly positioned below the liquid level in the kettle,and the top end of the heat exchange tube bundle I is separated from the liquid level by L1And the bottom end of the reaction kettle penetrates through the bottom of the first-stage reaction kettle and extends downwards.
4. The multi-tank reactive distillation apparatus of claim 2, wherein:
except the first-stage reaction kettle, a heat exchange tube bundle II in any stage of reaction kettle is horizontally placed at the lower part of each stage of reaction kettle along the side wall of the kettle.
5. The multi-tank reactive distillation apparatus of claim 4, wherein:
and 1 or 2 layers of heat exchange tube bundles II are distributed in each stage of kettle, and the heat exchange tube bundles II on the same layer are uniformly distributed on the cross section in the horizontal direction along the circumference.
6. The multi-tank reactive distillation apparatus of claim 2, wherein:
the heat exchange tubes of the heat exchange tube bundle are double-layer sleeves and comprise outer tubes and inner tubes arranged in the outer tubes, annular gaps between the outer tubes and the inner tubes are used for circulating steam, and the tops of the inner tubes along the length direction of the tubes are communicated with the interiors of the outer tubes and are used for enabling the inner tubes to circulate condensate;
a steam inlet is formed in the bottom of the outer pipe along the length direction of the pipe and is used for introducing steam; the bottom of the double-layer sleeve along the length direction of the pipe is provided with a condensate outlet for discharging condensate after steam heat exchange condensation in a backflow mode.
7. The multi-tank reactive distillation apparatus of claim 1, wherein:
the reaction kettle is arranged into 3-4 stages in series;
and/or;
the bottom of the at least 1 stage reaction kettle is also connected with a low boiling point reaction monomer feeding pipeline.
8. The multi-tank reactive distillation apparatus of claim 1, wherein:
the bottom of any stage of reaction kettle is connected with a steam feeding pipeline besides the first stage of reaction kettle;
and a steam distributor is arranged on the steam feeding pipeline.
9. The multi-tank reactive distillation apparatus of claim 1, wherein:
the rectifying tower is arranged above the second-stage reaction kettle; the bottom of the rectifying tower is tangentially provided with a gas phase feed inlet along a lateral line and a liquid phase reflux port communicated with the second-stage reaction kettle;
and/or;
the height between the bottom of the rectifying tower and the first tray is 1.8-2.5m, and the ascending flow velocity of the gas-phase material is controlled to be less than 2 m/s.
10. The multi-tank reactive distillation apparatus of claim 1, wherein:
in the multistage reaction kettle along the feeding direction, the temperature of materials in the kettle is controlled to be increased by 5-15 ℃.
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