CN106000250A - Row inter-tube falling film melt phase polycondensation reaction method and reactor thereof - Google Patents
Row inter-tube falling film melt phase polycondensation reaction method and reactor thereof Download PDFInfo
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- CN106000250A CN106000250A CN201610303700.7A CN201610303700A CN106000250A CN 106000250 A CN106000250 A CN 106000250A CN 201610303700 A CN201610303700 A CN 201610303700A CN 106000250 A CN106000250 A CN 106000250A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
- B01J2219/00081—Tubes
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Abstract
The invention relates to a row inter-tube falling film melt phase polycondensation reaction method. A melt prepolymer flows downwards from a film distribution plate and holes between tubes, a waterfall falling film flowing is formed between the U-shaped tubes in rows so that a melt phase polycondensation can be performed, and a melt slides down from the tubes, then condensed at the bottom of a reactor and discharged after stirring is performed to be homogenized through a stirrer. The reactor implementing the method is of an overall vertical structure and comprises a shell, a heating medium box at the upper end, a material box connected with the heating medium box, the U-shaped tubes, a bottom shell at the lower end, a stirrer and the like. The U-shaped tubes are perpendicularly suspended and arranged in rows, uniformly penetrate through holes in the film distribution plate, and the ends of the U-shaped tubes and the heating medium box are communicated to allow a heating medium to flow. The reactor has the advantages that the flowing resistance is small, no dead zone is generated, the film forming area is large, the surface updating speed is high, the standing time is uniform and controllable, and flexible production is met. The method is applicable to production of polyethylene glycol terephthalate and other polymers.
Description
Technical field
The present invention relates to a kind of falling film type melt polycondensation reaction method in polymer production and melt polycondensation reaction equipment.
Background technology
Polycondensation reaction is the reversible polymerization reaction of a kind of continuous generation micromolecular compound, including polyethylene terephthalate (PET), PTT (PTT), polybutylene terephthalate (PBT) (PBT), PEN (PEN), polyamide (PA) and Merlon (PC) etc. including polymer all prepared by polycondensation reaction.As this kind of polymer phase, feature is exactly in polycondensation process, have to last for the process for devolatilization carrying out getting rid of the micromolecular compound produced, carry out to promote to react continuous forward, thus material stickiness is high, particularly in the polycondensation later stage, material dynamic viscosity can occur the change of the order of magnitude, this reaction to relate to, and change that chemical reaction couples with heat and mass sticks process.Therefore, polycondensation reaction effect depends on flow behavior and the Mass and heat transfer Interfacial Characteristics of material.
The polycondensation method preparing heavy polymer generally has melt polycondensation, liquation polycondensation, solid phase polycondensation etc..Current industrial application is most common is process for solid state polycondensation, mainly have benefited from its relatively low polycondensation reaction temperature, so that the probability of polymer generation high temperature degradation is substantially reduced, will not produce coloring or catabolite, and beneficially volatile impurity effusion polymer in.But the subject matter that the method exists is that operation is many, long flow path, before and after reaction, material needs heating cooling the most repeatedly to consume big energy, and solid phase polycondensation process can produce more particulate dust and affect the operations such as follow-up spinning.Melt-polycondensation can prepare high glutinous material in the short period of time, saves multiple working procedure, and melt-polycondensation is applicable to all types of consersion unit, thus compare process for solid state polycondensation and have clear superiority in terms of economy, environmental protection and industrial implementation.
Presently disclosed falling liquid film polycondensation reactor mainly has the melt polycondensation reaction devices such as bar formula, grated plate type, tube wall type to be all dependent on melt to become membrane flow on inner member, compared to tradition horizontal reactor, in the case of greatly reducing energy consumption, improve melt film forming efficiency and the Surface Renewal of equipment.Particularly when the glutinous material viscosity of preparation height, extratubal falling film reactor can make material only become membrane flow by gravity outside pipe, the suitable time of staying is provided to enable material fully to react, but wall-attachment film evaporation device can make melt films cause outer layer liquid film flow velocity fast because of the speed difference of inside and outside tunic completely, and inner layer film is slower, cause partial material to invest for a long time to degrade on reactor inner member, jaundice, affect final products quality, the flow velocity of melt films free fall then can be made too fast for the bar formula free falling-film that falls and the time of staying is too short, and melt face during falling liquid film shrinks substantially, film forming efficiency is the lowest.Hence it is imperative that develop a kind of melt polycondensation reaction device, in can making reactor, material filming performance is good, and Surface Renewal is fast, the time of staying is homogeneous, without dead band, easily cleans, energy consumption is low, and course of reaction meets flowing, mixing and Mass and heat transfer demand, it is achieved high-effect polycondensation.
Summary of the invention
First purpose of the present invention is for the deficiencies in the prior art, one is provided to become falling liquid film melt polycondensation reaction method between comb, reaction temperature uniform, controllable can be made, effectively it is expanded into membrane area, improve melt film forming efficiency and the Surface Renewal of melt, strengthening melt flows becomes the homogeneity of film uniformity and melt residence time, final raising polycondensation reaction efficiency and height to stick the product quality of material, proposes techniques below scheme for this；
A kind of falling liquid film melt polycondensation reaction method between one-tenth comb, it is characterised in that: described method uses the reactor of the U-shaped heat-exchange tube being configured with arranged in rows, and during work, heating agent flows into from U type pipe one end, and the other end flows out；Melt material is when flowing downward, it is connected to curtain between the straight tube of the U-shaped heat-exchange tube of arranged in rows, waterfall shape film evaporation device is formed between straight tube, and carry out melt polycondensation reaction, volatilize small-molecule substance from the two sides of described waterfall shape falling liquid film, improves material molecular melt amount, and the straight tube of the U-shaped heat-exchange tube of arranged in rows is proximity association, simultaneously as the skeletal support pipe of described curtain, tube pitch is 0.1 ~ 20 with the ratio of caliber.
Further, described material, when flowing downward, the most also forms extratubal falling film at described straight tube outer wall, and the melt material of waterfall shape film evaporation device between described straight tube is connected with the melt material of extratubal falling film.
It is a further object to provide falling liquid film melt polycondensation reaction device between a kind of one-tenth comb, reaction temperature uniform, controllable can be made, effectively it is expanded into membrane area, improve melt film forming efficiency and the Surface Renewal of melt, strengthening melt flows becomes the homogeneity of film uniformity and the time of staying, raising polycondensation reaction efficiency and height to stick the product quality of material.To this end, the present invention is by the following technical solutions:
Become falling liquid film melt polycondensation reaction device between comb, described reactor includes upright shell, it is characterized in that described reactor also includes the U-shaped heat-exchange tube of arranged in rows, it is arranged on the material material feeding box on upright shell top, the base plate of material material feeding box is cloth lamina membranacea, the straight tube of the U-shaped heat-exchange tube of arranged in rows passes cloth lamina membranacea, cloth lamina membranacea has film distribution structure, film distribution structure includes the cloth film slit in region between corresponding straight tube, the straight tube proximity association of the U-shaped heat-exchange tube of arranged in rows, tube pitch is 0.1 ~ 20 with the ratio of caliber, make material melt when flowing downward, it is connected to curtain between the straight tube of the U-shaped heat-exchange tube of arranged in rows, waterfall shape film evaporation device is formed between straight tube, and carry out melt polycondensation reaction.
On the basis of using technique scheme, the present invention also can use technical scheme further below simultaneously, or uses these solution pool:
Connecting filament between horizontal pipe can be provided with or without between the adjacent straight tube pipe between two straight tube pipes of U-shaped heat-exchange tube and with row's U-shaped heat-exchange tube of two adjacent groups, between the pipe of two straight tubes, connecting filament radical is 0 ~ 1000, a diameter of 0.1 mm ~ 10 mm, between pipe connecting filament radical be the tube pitch of 0 be 0.1 ~ 10 with the ratio of caliber, between pipe connecting filament radical be 1 ~
The tube pitch of 1000 is 0.1 ~ 20 with the ratio of caliber.
The U-shaped heat-exchange tube of arranged in rows passes cloth lamina membranacea right angle setting, cloth lamina membranacea is provided with multiple rows of film distribution structure, film distribution structure include for and U-shaped heat-exchange tube straight tube form the cloth film slit in region between the cloth fenestra in falling liquid film gap and corresponding straight tube, and slit connects with hole, the space between cloth fenestra hole wall and straight tube is for material melt cloth film outside straight tube.
Upright shell is arranged over heating agent at material material feeding box and flows out casing and heating agent inflow casing, heating agent flows into casing and is provided with reactor Heating medium, heating agent flows out and responds the outlet of device heating agent on casing, U-shaped heat-exchange tube one end of described arranged in rows flows into casing with heating agent and communicates, and the other end flows out casing with heating agent and communicates；Melt material inlet pipe passes to material material feeding box；Upright shell top is provided with vacuum pumping opening, is provided with agitator in drain pan, and its power is incoming by bottom, is provided with material outlet bottom drain pan.
The U-shaped heat-exchange tube right angle setting of arranged in rows, lower end is unsettled, is in same plane with the axis arranging U-shaped heat-exchange tube, and the summit, axis of four straight tubes of neighbouring two groups of U-tube of adjacent two rows is connected to parallelogram.
The straight tube of U-shaped heat-exchange tube can be the coaxial straight tube of reducing, and the reducing trend of the coaxial straight tube of described reducing is that caliber diminishes from top to bottom, and U-shaped heat-exchange tube external diameter is 1 ~ 50 mm.
Reactor has heat transfer system and heat-insulation system, heat transfer system includes that heating agent flows into casing, heating agent flows out casing and U-shaped heat-exchange tube and the circulation path of composition thereof, and heating agent flows into casing and heating agent flows out and is respectively equipped with reactor Heating medium and the outlet of reactor heating agent on casing；Heat-insulation system includes housing chuck and the drain pan chuck that upright shell and drain pan and periphery thereof be respectively provided with, the upper and lower of housing chuck is respectively equipped with housing chuck Heating medium and the outlet of housing chuck heating agent, the upper and lower of drain pan chuck is respectively equipped with drain pan chuck Heating medium and the outlet of drain pan chuck heating agent, and the thermal medium of heat transfer system and heat-insulation system is passed to outside through Posterior circle operation is heated or cooled.
The present invention is applicable to the melt polycondensation reaction of the polymer such as polyethylene terephthalate (PET), PTT (PTT), polybutylene terephthalate (PBT) (PBT), PEN (PEN), polyamide (PA) and Merlon (PC).
The present invention utilizes polycondensation reaction material melt to have the advantages that in viscosity height and course of reaction, viscosity constantly increases, find to realize film evaporation device between the pipe of " waterfall " shape the most in the reactor, bigger film forming area can be maintained all the time, melt uniform film thickness, flow velocity reaches unanimity, face keeps laminar flow to move under gravity forces, thus ensure that polymer molecular weight narrowly distributing, the product that continuous production can be excellent and stable can be realized, and the production efficiency of unit volume reactor is greatly increased.Present invention discover that the U-shaped heat-exchange tube of in a row arrangement as the melt polycondensation reaction device of falling liquid film support member be suitable for very much this reaction method reactor, further, supporting wire between the pipe of adjacent two pipes is set, it can be for falling liquid film between the pipe of " waterfall " shape, strengthen melt dispersion with mix, improve the Surface Renewal frequency of melt films, the stability of waterfall shape can be played holding effect again simultaneously.Reaction method of the present invention is simple and feasible, has and flows into that membrane area is big, Surface Renewal speed is fast, the time of staying is homogeneous controlled, and the series of advantages such as energy consumption is low, easy cleaning, can realize the high-effect melt polycondensation that Mass and heat transfer couples with chemical reaction.
Accompanying drawing explanation
Fig. 1 is the structural representation of embodiment 1 provided by the present invention.
Fig. 2 is the structural representation of embodiment 2 provided by the present invention.
Fig. 3 is the structural representation of embodiment 3 provided by the present invention.
Fig. 4 is cloth lamina membranacea pore cell schematic diagram.
Fig. 5 a is one of straight tube geometric layout schematic diagram passing cloth lamina membranacea of multiple rows of U-tube.
Fig. 5 b be multiple rows of U-tube straight tube through cloth lamina membranacea geometric layout schematic diagram two.
Fig. 5 c be multiple rows of U-tube straight tube through cloth lamina membranacea geometric layout schematic diagram three.
Parts in figure, position and numbering: reactor Heating medium 1, feed pipe 2, heating agent flows to casing 3, heating agent flows out casing 4, heating agent flows out box cover plate 41, heating agent flows out casing lower shoe 42, material material feeding box 5, cloth lamina membranacea 51, cloth fenestra 511, cloth film slit 512, housing chuck Heating medium 6, upright shell 7, housing chuck 8, drain pan flange 9, drain pan bolt 10, drain pan chuck Heating medium 11, drain pan 12, drain pan chuck 13, material outlet 14, drain pan chuck heating agent outlet 15, agitator 16, housing chuck heating agent outlet 17, U-tube 18, connecting filament 181 between pipe, vacuum pumping opening 19, shell flange 20, casing bolts 21, reactor heating agent outlet 22, melt material inlet pipe 23.
Detailed description of the invention
Embodiment 1, referring to the drawings 1,4,5a, 5b, 5c.
In the present embodiment, U heat exchange 18(hereinafter referred to as U-tube, it includes the straight tube of both sides and at the bend pipe of connection both sides, bottom straight tube) straight tube use the straight tube that caliber is constant.
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb that the present embodiment is provided, as shown in Figure 1, it includes upright shell 7, it is connected to the material material feeding box of upright shell 7 upper end and the drain pan 12 of lower end, material material feeding box 5 is arranged over heating agent and flows out casing 4, flow out at heating agent and on casing 4, be provided with again heating agent inflow casing 3, heating agent flows into casing 3 and is provided with reactor Heating medium 1, heating agent flows out and responds device heating agent outlet 22 on casing 4, U-tube 18 one end of arranged in rows flows into casing 3 with heating agent and communicates, the other end flows out casing 4 with heating agent and communicates, melt material inlet pipe 23 flows out casing 4 from heating agent and heating agent flows into casing 3 and passes, pass to material material feeding box 5；The base plate of material material feeding box 5 is cloth lamina membranacea 51, cloth lamina membranacea 51 has film distribution structure, upright shell 7 top are provided with vacuum pumping opening 19, are provided with agitator 16 below U-tube 18, and its power is incoming by bottom, is provided with material outlet 14 bottom drain pan 12.
In the U-shaped heat-exchange tube 18 of arranged in rows, straight tube with the U-shaped heat-exchange tube 18 of row is all proximity association, the straight tube of U-shaped heat-exchange tube 18 serves the effect of falling liquid film support member between pipe, when its tube pitch makes material melt be flowed downward by film distribution structure, it is connected to curtain between the straight tube of the U-shaped heat-exchange tube of arranged in rows, between pipe, form waterfall shape film evaporation device, and carry out melt polycondensation reaction.Small molecule by-product is from the two sides devolatilization of described waterfall shape falling liquid film, and then is discharged by vacuum pumping opening 19.
Described U-tube 18 right angle setting, lower end is unsettled, the neat arranged in rows of many single u-shaped pipe 18, is in same plane with the axis of row's U-tube 18, is separated by between row and row with equidistant keeping parallelism.
As preferably, two straight tube tube pitch of U-tube 18 and the adjacent straight tube tube pitch of adjacent two U-tube 18 are equal, tube pitch from the ratio with the pipe external diameter of U-tube be 0.1 ~
20。
As preferably, the straight tube pipe range of U-tube 18 is 0.5 ~ 30 m, external diameter is 1 ~
50 mm。
Connecting filament 181 between transverse pipe can be provided with between 18 liang of straight tubes of vertically arranged U-tube and between the adjacent straight tube of adjacent two U-tube, between pipe, connecting filament length is equal to the vertical dimension of two pipes, as preferably, between the pipe of adjacent two straight tubes, connecting filament radical is 1 ~ 1000, a diameter of 0.1 mm ~ 10 mm.
In a row the U-tube 18 of arrangement is through cloth lamina membranacea 51 right angle setting, cloth lamina membranacea 51 is provided with multiple rows of film distribution structure, film distribution structure include for and U-shaped heat-exchange tube 18 straight tube form the cloth film slit 512 between the cloth fenestra 511 in falling liquid film gap and corresponding straight tube, and slit 512 connects with hole 511, slit 512 is for making material melt films flow down with relatively thin thickness between pipe, as shown in Figure 4；Space between cloth fenestra hole wall and straight tube is for material melt cloth film outside straight tube, formation extratubal falling film flows, the melt material of waterfall shape film evaporation device between described straight tube is connected with the melt material of extratubal falling film, increase film forming area the most further, and contribute to the one-tenth curtain stability of waterfall shape film evaporation device, and the viscosity that the material curtain between pipe can utilize material in turn is formed with facilitation to extratubal falling film laminar flow.
Often arrangement membrane structure has more than one cloth membrane pores unit, and each unit includes a hole 511 and a seam 512, and as preferably, hole wall is dentation, as shown in Figure 4, so that the space between the hole wall in hole 511 and straight tube is essentially slot.As preferably, the internal ring radius (R of slot1) identical with the pipe end radius of U-tube straight tube, slot outer shroud radius (R2) and internal ring radius (R1) difference be 0.1 ~
10 mm, the width (L of slit 5121) it is 0.1 ~ 10 mm, length (L2) it is 1 ~ 200 mm.
The summit, axis of four straight tubes of neighbouring two groups of U-tube 18 of adjacent two rows is connected to parallelogram, and Fig. 5 a, 5b, 5c are respectively the straight tube several examples through cloth lamina membranacea geometric layout of multiple rows of U-tube 18.
As preferably, the U-tube 18 of arranged in rows vertical dimension between row and row is 10 ~ 200 mm, U-tube in a row overall right angle setting.
Reactor is provided with heat transfer system, flows into casing 3, heating agent outflow casing 4 and U-tube 18 and the circulation path of composition thereof including heating agent, and heating agent flows into casing 3 and heating agent flows out and is respectively equipped with reactor Heating medium 1 and reactor heating agent outlet 22 on casing 4.
Reactor is provided with heat-insulation system, the housing chuck 8 being respectively provided with including upright shell 7 and drain pan 12 and periphery thereof and drain pan chuck 13, the upper and lower of housing chuck 8 is respectively equipped with housing chuck Heating medium 6 and housing chuck heating agent outlet 17, and the upper and lower of drain pan chuck 13 is respectively equipped with drain pan chuck Heating medium 11 and drain pan chuck heating agent outlet 15.
The thermal medium of heat transfer system and heat-insulation system is passed to outside through Posterior circle operation is heated or cooled.
The reactor top being made up of heating agent inflow casing 3, heating agent outflow casing 4 and material material feeding box 5 is connected by shell flange 20 and casing bolts 21 with upright shell 7, upright shell 7 is connected by drain pan flange 9 and drain pan bolt 10 with drain pan 12, it is simple to dismounting maintenance and installation.
The melt polycondensation process using above-mentioned polycondensation reactor is:
During reactor work, heating agent flows to from U type pipe Single port, then flows out from another port, then flows out to polycondensation reactor outside through Posterior circle operation is heated or cooled.
Material inlet is positioned at heating agent and flows into directly over casing crown center, and pre-polymer melt is constantly injected from material inlet, and the heating agent that wore long flows into the feed pipe of casing and heating agent outflow casing and flows into material material feeding box.
Melt enters the U-tube district of arranged in rows after the hole on cloth lamina membranacea distributes, outside U-tube straight tube, uniform cloth film forms falling liquid film, " waterfall " shape film evaporation device is formed between straight tube pipe, carry out melt polycondensation reaction, between pipe, melt maintains certain thickness to flow through equally spaced connecting filament, and the little molecule that reaction generates is extracted out from vacuum pumping opening.
Melt after landing, finally converges to bottom polycondensation reactor between U-tube pipe, stirs reaction further through agitator and homogenizes material, completes reacted melt and discharges from the material outlet of reactor bottom.
Embodiment 2, referring to the drawings 2,4,5a, 5b, 5c.
In the present embodiment, the straight tube of U-tube 18 uses the coaxial straight tube of reducing of connection.
The straight tube of U-tube 18 with equidistant interior reducing, becomes diameter not once the logical straight tube of continuous phase below cloth lamina membranacea 51, and the most coaxially, to U-tube 18 bottom below cloth lamina membranacea 51, caliber is gradually reduced.
In the U-tube of reducing, between each section of U-tube straight tube, the tube pitch of the variable diameter straight tube that the length of connecting filament is corresponding with it is from keeping equal.
Other parts and the implementation of the present embodiment are same as in Example 1, in fig. 2, and the implication that representative that drawing reference numeral is identical with Fig. 1 is identical.
Case study on implementation 3, referring to the drawings 3,4,5a, 5b, 5c.
In the present embodiment, U-tube 18 straight part is the straight tube that caliber is constant, between 18 liang of straight tubes of U-tube and arranges together between adjacent two straight tubes of adjacent U-tube 18 all without connecting filament.
As preferably, U-tube 18 tube pitch is 0.1 ~ 10 from the ratio with caliber.
Other parts and the implementation of the present embodiment are same as in Example 1, in figure 3, and the implication that representative that drawing reference numeral is identical with Fig. 1 is identical.
The foregoing is only the specific embodiment of the present invention, but the architectural feature of the present invention is not limited thereto, any those skilled in the art is in the field of the invention, and change or the modification made all are contained among protection scope of the present invention.
Claims (9)
1. one kind becomes falling liquid film melt polycondensation reaction method between comb, it is characterised in that: described method uses the reactor of the U-shaped heat-exchange tube being configured with arranged in rows, and during work, heating agent flows into from U type pipe one end, and the other end flows out；Melt material is when flowing downward, it is connected to curtain between the straight tube of the U-shaped heat-exchange tube of arranged in rows, waterfall shape film evaporation device is formed between straight tube, and carry out melt polycondensation reaction, volatilize small-molecule substance from the two sides of described waterfall shape falling liquid film, improves material molecular melt amount, and the straight tube of the U-shaped heat-exchange tube of arranged in rows is proximity association, simultaneously as the skeletal support pipe of described curtain, tube pitch is 0.1 ~ 20 with the ratio of caliber.
2. falling liquid film melt polycondensation reaction method between a kind of one-tenth comb as claimed in claim 1, it is characterized in that: described material is when flowing downward, the most also forming extratubal falling film at described straight tube outer wall, the melt material of waterfall shape film evaporation device between described straight tube is connected with the melt material of extratubal falling film.
null3. one kind becomes falling liquid film melt polycondensation reaction device between comb，Described reactor includes upright shell (7)，It is characterized in that described reactor also includes the U-shaped heat-exchange tube (18) of arranged in rows、It is arranged on the material material feeding box (5) on upright shell (7) top，The base plate of material material feeding box (5) is cloth lamina membranacea (51)，The straight tube of the U-shaped heat-exchange tube (18) of arranged in rows passes cloth lamina membranacea (51)，Cloth lamina membranacea (51) has film distribution structure，Film distribution structure includes cloth film slit (512) in region between corresponding straight tube，The straight tube proximity association of the U-shaped heat-exchange tube (18) of arranged in rows，Tube pitch is 0.1 ~ 20 with the ratio of caliber，Make material melt when flowing downward，It is connected to curtain between the straight tube of the U-shaped heat-exchange tube of arranged in rows，Waterfall shape film evaporation device is formed between straight tube，And carry out melt polycondensation reaction.
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb the most according to claim 3, it is characterized in that: between the adjacent straight tube pipe between two straight tube pipes of U-shaped heat-exchange tube (18) and with row's U-shaped heat-exchange tube of two adjacent groups (18), connecting filament (181) between horizontal pipe can be provided with or without, between the pipe of two straight tubes, connecting filament radical is 0 ~ 1000, a diameter of 0.1 mm ~ 10 mm, between pipe connecting filament radical be the tube pitch of 0 be 0.1 ~ 10 with the ratio of caliber, between pipe connecting filament radical be the tube pitch of 1 ~ 1000 be 0.1 ~ 20 with the ratio of caliber.
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb the most according to claim 3, it is characterized in that: the U-shaped heat-exchange tube (18) of arranged in rows passes cloth lamina membranacea (51) right angle setting, cloth lamina membranacea (51) is provided with multiple rows of film distribution structure, film distribution structure include for and U-shaped heat-exchange tube (18) straight tube form cloth film slit (512) in region between the cloth fenestra (511) in falling liquid film gap and corresponding straight tube, and slit connects with hole, the space between cloth fenestra hole wall and straight tube is for material melt cloth film outside straight tube.
6. falling liquid film melt polycondensation reaction device between a kind of one-tenth comb as claimed in claim 3, it is characterized in that upright shell (7) is arranged over heating agent at material material feeding box (5) and flows out casing (4) and heating agent inflow casing (3), heating agent flows into casing (3) and is provided with reactor Heating medium (1), heating agent flows out and responds device heating agent outlet (22) on casing (4), U-shaped heat-exchange tube (18) one end of described arranged in rows flows into casing (3) with heating agent and communicates, and the other end flows out casing (4) with heating agent and communicates；Melt material inlet pipe passes to material material feeding box (5)；Upright shell (7) top is provided with vacuum pumping opening (19), and drain pan (12) bottom is provided with material outlet (14).
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb the most according to claim 3, it is characterised in that: U-shaped heat-exchange tube (18) right angle setting of arranged in rows, lower end is unsettled, is in same plane with the axis arranging U-shaped heat-exchange tube (18).
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb the most according to claim 3, it is characterized in that: the straight tube of U-shaped heat-exchange tube (18) can be the coaxial straight tube of reducing, the reducing trend of the coaxial straight tube of described reducing is from top to bottom, caliber diminishes, and U-shaped heat-exchange tube (18) external diameter is 1 ~ 50 mm.
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb the most according to claim 3, it is characterized in that: reactor has heat transfer system and heat-insulation system, heat transfer system includes that heating agent flows into casing (3), heating agent flows out casing (4) and U-shaped heat-exchange tube (18) and the circulation path of composition, and heating agent flows into casing (3) and heating agent flows out and is respectively equipped with reactor Heating medium (1) and reactor heating agent outlet (22) on casing (4)；Heat-insulation system includes housing chuck (8) and the drain pan chuck (13) that upright shell (7) and drain pan (12) and periphery thereof be respectively provided with, the upper and lower of housing chuck (8) is respectively equipped with housing chuck Heating medium (6) and housing chuck heating agent outlet (17), the upper and lower of drain pan chuck (13) is respectively equipped with drain pan chuck Heating medium (11) and drain pan chuck heating agent outlet (15), and the thermal medium of heat transfer system and heat-insulation system is passed to outside through Posterior circle operation is heated or cooled.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107029637A (en) * | 2017-05-11 | 2017-08-11 | 浙江理工大学 | A kind of high viscosity fluid filming device |
| CN110813225A (en) * | 2019-10-10 | 2020-02-21 | 浙江理工大学 | Melt polycondensation reactor and falling film element thereof |
| CN112090388A (en) * | 2020-09-07 | 2020-12-18 | 浙江大学 | Continuous flow reactor and application thereof in chemical reaction and synthesis |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3316064A (en) * | 1964-04-30 | 1967-04-25 | Hitachi Ltd | Apparatus for continuous polycondensation reaction |
| GB1113357A (en) * | 1964-09-17 | 1968-05-15 | Basf Ag | Continuous polycondensation of lactams |
| CN103319705A (en) * | 2013-06-17 | 2013-09-25 | 浙江理工大学 | Melt polycondensation reaction method, and reactor and falling film tube used for same |
| CN203400699U (en) * | 2013-06-17 | 2014-01-22 | 浙江理工大学 | Melt phase polycondensation reactor and external pipe falling film element |
| CN205815656U (en) * | 2016-05-09 | 2016-12-21 | 浙江理工大学 | Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb |
-
2016
- 2016-05-09 CN CN201610303700.7A patent/CN106000250B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3316064A (en) * | 1964-04-30 | 1967-04-25 | Hitachi Ltd | Apparatus for continuous polycondensation reaction |
| GB1113357A (en) * | 1964-09-17 | 1968-05-15 | Basf Ag | Continuous polycondensation of lactams |
| CN103319705A (en) * | 2013-06-17 | 2013-09-25 | 浙江理工大学 | Melt polycondensation reaction method, and reactor and falling film tube used for same |
| CN203400699U (en) * | 2013-06-17 | 2014-01-22 | 浙江理工大学 | Melt phase polycondensation reactor and external pipe falling film element |
| CN205815656U (en) * | 2016-05-09 | 2016-12-21 | 浙江理工大学 | Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107029637A (en) * | 2017-05-11 | 2017-08-11 | 浙江理工大学 | A kind of high viscosity fluid filming device |
| CN107029637B (en) * | 2017-05-11 | 2023-06-06 | 浙江理工大学 | High-viscosity fluid film distributor |
| CN110813225A (en) * | 2019-10-10 | 2020-02-21 | 浙江理工大学 | Melt polycondensation reactor and falling film element thereof |
| CN110813225B (en) * | 2019-10-10 | 2022-06-03 | 浙江理工大学 | Melt polycondensation reactor and falling film element thereof |
| CN112090388A (en) * | 2020-09-07 | 2020-12-18 | 浙江大学 | Continuous flow reactor and application thereof in chemical reaction and synthesis |
| CN112090388B (en) * | 2020-09-07 | 2022-04-12 | 浙江大学 | Continuous flow reactor and application thereof in chemical reaction and synthesis |
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| CN106000250B (en) | 2018-08-21 |
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Application publication date: 20161012 Assignee: ZHEJIANG GUXIANDAO GREEN FIBER Co.,Ltd. Assignor: Zhejiang University of Technology Contract record no.: X2021330000001 Denomination of invention: A method and reactor of falling film fusion polycondensation between rows of tubes Granted publication date: 20180821 License type: Common License Record date: 20210108 |