CN105854734B - It is a kind of prepare melt with high viscosity into falling liquid film melt polycondensation reaction method and its reactor between comb - Google Patents
It is a kind of prepare melt with high viscosity into falling liquid film melt polycondensation reaction method and its reactor between comb Download PDFInfo
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- CN105854734B CN105854734B CN201610302101.3A CN201610302101A CN105854734B CN 105854734 B CN105854734 B CN 105854734B CN 201610302101 A CN201610302101 A CN 201610302101A CN 105854734 B CN105854734 B CN 105854734B
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- 239000007788 liquid Substances 0.000 title claims abstract description 113
- 238000006068 polycondensation reaction Methods 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 87
- 239000000463 material Substances 0.000 claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 230000008020 evaporation Effects 0.000 claims abstract description 12
- 238000001704 evaporation Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 167
- 239000004744 fabric Substances 0.000 claims description 44
- 239000000289 melt material Substances 0.000 claims description 15
- 238000012546 transfer Methods 0.000 claims description 15
- 238000009826 distribution Methods 0.000 claims description 11
- 239000011552 falling film Substances 0.000 claims description 10
- 150000003384 small molecules Chemical class 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 54
- 229920000642 polymer Polymers 0.000 abstract description 6
- -1 polyethylene terephthalate Polymers 0.000 abstract description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 abstract description 5
- 239000005020 polyethylene terephthalate Substances 0.000 abstract description 5
- 239000000155 melt Substances 0.000 abstract description 4
- 239000000178 monomer Substances 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 7
- 239000012528 membrane Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 229920001707 polybutylene terephthalate Polymers 0.000 description 4
- 230000002708 enhancing effect Effects 0.000 description 3
- 239000004425 Makrolon Substances 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 239000004417 polycarbonate Substances 0.000 description 2
- 229920000515 polycarbonate Polymers 0.000 description 2
- 239000011112 polyethylene naphthalate Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 210000003429 pore cell Anatomy 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
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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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
-
- 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
- B01J19/1887—Stationary reactors having moving elements inside forming a thin film
-
- 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
- B01J19/32—Packing elements in the form of grids or built-up elements for forming a unit or module inside the apparatus for mass or heat transfer
-
- 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
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
-
- 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
- B01J2219/00085—Plates; Jackets; Cylinders
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
It is a kind of prepare melt with high viscosity into falling liquid film melt polycondensation reaction method and its reactor between comb.The present invention relates to a kind of into falling liquid film melt polycondensation reaction method between comb, molten monomer blend or prepolymer form waterfall shape film evaporation device between falling liquid film support tube pipe between rows of pipe and carry out melt polycondensation reaction, melt between pipe after sliding, it converges to reactor bottom and futher stirs and homogenize, material is discharged after completion of the reaction.Implement the reactor of this method as integral vertical type structure, including falling liquid film support tube between housing, the heating agent babinet of upper end and its connected pipe, body feed tank and the bottom case of lower end, blender etc..The falling liquid film support tube vertical hanging of inner tube is cased with, is in a row arranged, nozzle is communicated with heating agent babinet to be flowed for heating agent.This reactor have many advantages, such as flow resistance it is small, without dead zone, area is big for film forming, Surface Renewal is fast, meet process laminar flow, suitable for the melt polycondensation reaction of the contour glutinous polymer of polyethylene terephthalate.
Description
Technical field
The present invention relates to a kind of falling film type melt polycondensation reaction methods and melt polycondensation reaction in high glutinous polymer production
Equipment.
Background technology
Polycondensation reaction is a reversible balanced reaction, and with the progress of polycondensation reaction, small molecule class compound needs timely
It is effective to exclude reaction system, so as to which polymer molecular weight is continuously improved, including polyethylene terephthalate（PET）、
Polypropylene terephthalate（PTT）, polybutylene terephthalate (PBT)（PBT）, polyethylene naphthalate（PEN）、
Polyamide（PA）And makrolon（PC）Polymer Deng including is made by polycondensation reaction.The implementation master of polycondensation reaction
Have melt polycondensation, solid phase polycondensation, solution polycondensation etc., wherein melt polycondensation because its reaction efficiency is high, flow is short, energy conservation and environmental protection with
And meet the advantages such as flexibility large-scale production and be widely adopted.During the high glutinous material of melt-polycondensation production, with anti-
The progress answered, reaction system viscosity sharply increase, the small molecule of generation exclude it is more and more difficult, mass transfer become the control of process because
Element, therefore be the key that implement efficient melt polycondensation using the high-quality polycondensation reaction equipment that can provide big mass transfer specific surface area.
According to melt polycondensation reaction feature, melt need to have good flowing filming performance in order to be formed in polycondensation reactor
The appropriate melt films of thickness, and larger film forming area is maintained, melt films are too thick to cause small molecule removing difficult, and melt films
It is too thin, it can so that melt is long in the interior component surface residence time and degrades；The design of reactor component need to ensure to melt
Body obtains constantly mixing while flowing to be updated with the interface for enhancing melt films as far as possible；In addition, material stops in reactor
Stay time requirement is uniform controllably to obtain the heavy polymer of required narrow ditribution with this.Therefore, ideal melt polycondensation reaction
Device should meet Flow of Goods and Materials for laminar flow, no dead zone, the ratio between the mass transfer area obtained in the unit interval and volume of material（Film forming
Efficiency）It maximizes, Surface Renewal is fast, and the diffusion path of small molecule is short to match to adapt to not with transitivity variation with polymerization process
With the requirement of the stage of reaction.
Presently disclosed vertical falling-film melt polycondensation reaction device has the tower polycondensation reactor of screen, extratubal falling film polycondensation reaction
Device etc..Tube sheet tower reactor relies primarily on the design of inner member so that fused materials form a film on pipe or plate surface structure,
Film forming area and Surface Renewal frequency are increased, but its embedding structure is answered relative to the polycondensation reactor of traditional Horizontal stirring
It is miscellaneous, stagnant area is also easy to produce, melt is caused to be degraded, is above had difficulties in the application of the high glutinous material of production.Extratubal falling film reactor can
Material is made to trickle downwards along tube outer surface film-like, due to material by gravity naturally to flowing down, the problem of being not in blocking,
This kind of reactor has many advantages, such as that structure is relatively easy, mass transfer interface is big and reaction temperature is uniform, but since wall-attachment freely drops
The VELOCITY DISTRIBUTION of semi-parabolic type is presented in the liquid film of membrane flow from inside to outside, and the surface layer speed of melt films is much larger than near wall area
Domain, the outer membrane residence time is too short and the inner layer film residence time is long.
Invention content
First purpose of the invention is in view of the deficiencies of the prior art, to provide and a kind of prepare being dropped between comb for melt with high viscosity
Film melt polycondensation reaction method, can make reaction temperature uniform, controllable, effectively be expanded into membrane area, improve melt film forming efficiency and
The Surface Renewal of melt, enhancing melt flows improve polycondensation reaction efficiency and height into film uniformity and the homogeneity of residence time
The product quality of glutinous material.For this purpose, propose following technical scheme；
It is a kind of into falling liquid film melt polycondensation reaction method between comb, it is characterised in that：The method uses and is configured with row in a row
The reactor of falling liquid film support tube between the heat-exchange tube of row, between the pipe of arranged in rows in falling liquid film support tube, falling liquid film support tube between pipe
It is proximity association, the ratio between tube spacing and caliber are 0.1 ~ 20, make melt material when flowing downward, in the pipe of arranged in rows
Between be connected to curtain between falling liquid film support tube, waterfall shape film evaporation device is formed between falling liquid film support tube between pipe, and it is anti-to carry out melt polycondensation
Should, from the two sides of waterfall shape falling liquid film volatilization small-molecule substance, improve material molecular melt amount.
Further, the material is when flowing downward, while also falling liquid film support pipe outer wall is formed outside pipe between the pipe
Falling liquid film, the melt material of the waterfall shape film evaporation device between the pipe between falling liquid film support tube are connected with the melt material of extratubal falling film.
It is a further object to provide a kind of into falling liquid film melt polycondensation reaction device between comb, reaction temperature can be made equal
It is even controllable, membrane area is effectively expanded into, improves the Surface Renewal of melt film forming efficiency and melt, enhancing melt flows film forming is equal
Even property and the homogeneity of residence time improve polycondensation reaction efficiency and the product quality of high glutinous material.For this purpose, the present invention use with
Lower technical solution：
It is a kind of into falling liquid film melt polycondensation reaction device between comb, the reactor includes upright shell, it is characterised in that described
Reactor further includes falling liquid film support tube between the heat-exchange tube of arranged in rows, the material material feeding box for being arranged on upright shell upper end, object
The bottom plate for expecting material feeding box is cloth diaphragm plate, and the falling liquid film support tube of arranged in rows passes through cloth diaphragm plate, and cloth diaphragm plate has film distribution structure, cloth film
Structure includes the cloth film slit in region between falling liquid film support tube between respective tube, and falling liquid film support tube is proximity association between pipe, makes melt
Material is connected to curtain between the pipe of arranged in rows when flowing downward between falling liquid film support tube, is formed between falling liquid film support tube between pipe
Waterfall shape film evaporation device, and melt polycondensation reaction is carried out, from the two sides of waterfall shape falling liquid film volatilization small-molecule substance, improve
Material molecular melt amount.
Using on the basis of above-mentioned technical proposal, the present invention can also simultaneously using technical solution further below or
These solution pools are used：
With being provided with or without connecting filament between the pipe of adjacent two pipe of lateral connection between falling liquid film support tube between comb, between two pipe pipes
Connecting filament radical is 0 ~ 1000, the mm of a diameter of 0.1 mm ~ 20, the tube spacing that connecting filament radical is 0 between pipe from caliber it
Than being 0.1 ~ 10, connecting filament radical is 1 ~ 1000 between pipe tube spacing is from being 0.1 ~ 20 with the ratio between caliber.
Cloth diaphragm plate right angle setting is passed through into falling liquid film support tube between comb, cloth diaphragm plate is equipped with multiple rows of film distribution structure, cloth film knot
Structure includes being used for the cloth film slit at the position between the cloth fenestra in falling liquid film support tube formation falling liquid film gap and respective tube between pipe, and narrow
Seam is connected with hole, and the gap between cloth fenestra hole wall and pipe between falling liquid film support tube is used for material melt falling liquid film support tube between pipe
Outer cloth film.
Upright shell is equipped with heating agent outflow babinet above material material feeding box and heating agent flows into babinet, and heating agent flows into babinet and sets
There is reactor Heating medium, there is reactor heating agent to export on heating agent outflow babinet, falling liquid film support tube between the pipe of the arranged in rows
Babinet is flowed into heating agent and heating agent outflow babinet communicates；Melt material inlet pipe flows out babinet from heating agent and heating agent flows into babinet and wears
It crosses, passes to material material feeding box；Upright shell top is equipped with vacuum pumping opening, is equipped with blender in bottom case, power is passed by bottom
Enter, bottom case bottom is equipped with material outlet.
Falling liquid film support tube uses outer tube sleeve inner tube structure between the pipe, and inner tube is communicated with heating agent outflow box cover plate, outside
Pipe is communicated with heating agent outflow babinet lower plate.
Between the pipe falling liquid film support tube inner tube keep caliber it is constant, outer tube be straight-run of pipe or the coaxial straight tube of reducing, institute
The reducing trend of the coaxial straight tube of reducing is stated as from top to bottom, caliber becomes smaller.
Between the pipe falling liquid film support tube outer tube caliber be 2 ~ 30 mm, inner tube diameter be 1 ~ 20 mm, outer tube caliber with
Inner tube diameter differs 1 ~ 10 mm.
Reactor sets heat transfer system and heat-insulation system, and heat transfer system includes heating agent and flows into babinet, heating agent outflow babinet and drop
The circulation path of film support tube composition, heating agent, which is flowed on babinet and heating agent outflow babinet, is respectively equipped with reactor Heating medium and anti-
Device heating agent is answered to export；Heat-insulation system includes upright shell and bottom case and its peripheral housing chuck set respectively and bottom case chuck,
The upper and lower part of housing chuck is respectively equipped with housing chuck Heating medium and the outlet of housing chuck heating agent, the top of bottom case chuck
The thermal medium of bottom case chuck Heating medium and the outlet of bottom case chuck heating agent, heat transfer system and heat-insulation system is respectively equipped with lower part
It is passed to external by Posterior circle operation is heated or cooled.
The present invention can be suitably used for polyethylene terephthalate（PET）, polypropylene terephthalate（PTT）, it is poly-
Mutual-phenenyl two acid bromide two alcohol ester（PBT）, polyethylene naphthalate（PEN）, polyamide（PA）And makrolon（PC）Deng poly-
Close the melt polycondensation reaction of object.
The present invention is the root on the basis of being fully realized to the mass transfer feature of polycondensation reaction and high glutinous fluid mechanics dynamics
According to melt with high viscosity film forming flow behavior control film evaporation device speed and its VELOCITY DISTRIBUTION and strengthen melt interface mass transfer as technology
The mentality of designing of solution improves film forming area with this, enhances the Surface Renewal of melt and residence time homogeneity, finally carries
High product quality.
The present invention, as falling liquid film support element between pipe, has high viscosity using the vertical pipes in a row arranged using material melt
And viscosity constantly increases the features such as arrangement with falling liquid film support element, can maintain larger film forming area always, melt film thickness is equal
Even, flow velocity reaches unanimity, and film surface keeps laminar flow to move under gravity forces, so as to ensure that polymer molecular weight is distributed
It is narrow, it can be achieved that continuous production performance is excellent and the product stablized, and the production efficiency of unit volume reactor greatly increases.Into one
Ground is walked, supporting wire between the pipe of adjacent two pipe is set, falling liquid film between the pipe of " waterfall " shape can be directed to, strengthen the dispersion of melt with mixing
It closes, improves the Surface Renewal frequency of melt films, while can play the role of holding to the stability of waterfall shape again.It is of the present invention
Reaction method is simple and feasible, and with flowing into, membrane area is big, Surface Renewal rate is fast, residence time uniform controllable and energy consumption
The series of advantages such as low, easy cleaning are, it can be achieved that the high-effect melt polycondensation that Mass and heat transfer is coupled with chemical reaction.
Description of the drawings
Fig. 1 is the structure diagram of embodiment 1 provided by the present invention.
Fig. 2 is the structure diagram of embodiment 2 provided by the present invention.
Fig. 3 is the structure diagram of embodiment 3 provided by the present invention.
Fig. 4 is cloth diaphragm plate pore cell schematic diagram.
Fig. 5 a are that the straight tube of multiple rows of U-tube passes through one of geometric layout schematic diagram of cloth diaphragm plate.
Fig. 5 b are that the straight tube of multiple rows of U-tube passes through the two of the geometric layout schematic diagram of cloth diaphragm plate.
Fig. 5 c are that the straight tube of multiple rows of U-tube passes through the three of the geometric layout schematic diagram of cloth diaphragm plate.
Parts, position and number in figure：Reactor Heating medium 1, feed pipe 2, heating agent flow into babinet 3, heating agent stream
Go out babinet 4, heating agent outflow box cover plate 41, heating agent outflow babinet lower plate 42, material material feeding box 5, cloth diaphragm plate 51, cloth fenestra
511, cloth film slit 512, housing chuck Heating medium 6, upright shell 7, housing chuck 8, bottom case flange 9, bottom case bolt 10, bottom
Shell chuck Heating medium 11, bottom case 12, bottom case chuck 13, material outlet 14, bottom case chuck heating agent outlet 15, blender 16, shell
Body chuck heating agent outlet 17, falling liquid film support tube 18, outer tube 181, inner tube 182, connecting filament 183 between pipe, vacuum pumping opening 19, housing
Flange 20, casing bolts 21, reactor heating agent outlet 22, melt material inlet pipe 23.
Specific embodiment
Embodiment 1, with reference to attached drawing 1,4,5a, 5b, 5c.
In the present embodiment, the outer tube 181 of falling liquid film support tube 18 is using the constant straight tube of caliber.
The present embodiment provided it is a kind of prepare melt with high viscosity into falling liquid film melt polycondensation reaction device between comb, such as Fig. 1 institutes
Show, it includes upright shell 7, is connected to the material material feeding box of 7 upper end of upright shell and the bottom case 12 of lower end, material material feeding box 5
Top is equipped with heating agent and flows out babinet 4, flows into babinet 3 equipped with heating agent again on heating agent outflow babinet 4, heating agent is flowed on babinet 3
Equipped with reactor Heating medium 1, there is reactor heating agent to export 22 on heating agent outflow babinet 4, the falling liquid film support tube 18 of arranged in rows
It is connected to heating agent outflow babinet 4 and heating agent flows into babinet 3 to form heating agent circulation path, melt material inlet pipe 23 is flowed out from heating agent
Babinet 4 and heating agent flow into babinet 3 and pass through, and pass to material material feeding box 5；The bottom plate of material material feeding box 5 be cloth diaphragm plate 51, cloth diaphragm plate 51
On have a film distribution structure, 7 top of upright shell is equipped with vacuum pumping opening 19, and 18 lower section of falling liquid film support tube is equipped with blender between pipe
16, power is passed to by bottom, and 12 bottom of bottom case is equipped with material outlet 14.
Falling liquid film support tube 18 between the pipe of the reactor including arranged in rows, falling liquid film support tube is proximity association between pipe,
Make melt material when flowing downward, curtain is connected between falling liquid film support tube between the pipe of arranged in rows, the falling liquid film support tube between pipe
Between form waterfall shape film evaporation device, and carry out melt polycondensation reaction, volatilize small molecule object from the two sides of the waterfall shape falling liquid film
Matter improves material molecular melt amount.
18 right angle setting of falling liquid film support tube between pipe, lower end is hanging, and falling liquid film support tube 18 is whole between often arranging the pipe for having one or more
Neat arrangement, the axis with falling liquid film support tube 18 between all pipes of row are in same plane, are separated by between row and row with equidistant holding
It is parallel.
Falling liquid film support tube 18 is internal and external casing structure, outer tube 181 and 41 phase of heating agent outflow box cover plate between the pipe
Logical, inner tube 182 is communicated with heating agent outflow babinet lower plate 42.
Preferably, 181 outer diameter of falling liquid film support tube outer tube is 2 ~ 30 mm between pipe, interior pipe outside diameter is 1 ~ 20 mm, outside
Pipe caliber is differed with inner tube diameter as 1 ~ 10 mm.
Connecting filament 183 between lateral pipe is equipped between vertically arranged adjacent two pipes between 18 pipe of falling liquid film support tube, is connected between pipe
Connect vertical range of 183 length of silk equal to falling liquid film support tube 18 between adjacent two pipe, preferably, between pipe connecting filament 183 radical
It is 1 ~ 1000, the mm of a diameter of 0.1 mm ~ 10,
Preferably, between adjacent two pipes falling liquid film support tube 18 tube spacing from the ratio between caliber with its outer tube 181 be 0.1
~ 20。
Falling liquid film support tube 18 passes through 51 right angle setting of cloth diaphragm plate between the pipe in a row arranged, and cloth diaphragm plate 51 is equipped with multiple rows of cloth film
Structure, film distribution structure include being used for the falling liquid film support tube 18 between pipe and are formed between cloth fenestra 511 and the respective tube in falling liquid film gap
The slit 512 at position, and slit 512 is connected with hole 511, slit 512 is for making melt be flowed down between pipe with relatively thin thickness, such as
Shown in Fig. 4.Gap between cloth fenestra hole wall and pipe between falling liquid film support tube 18 is used for material melt falling liquid film support tube between pipe
18 outer cloth films, form extratubal falling film flowing, the melt material of the waterfall shape film evaporation device between the pipe between falling liquid film support tube 18 with
The melt material of extratubal falling film is connected, and not only further increases film forming area, and contributes to the steady into curtain of waterfall shape film evaporation device
It is qualitative, and the material curtain between pipe can utilize the viscosity of material to have facilitation to the formation of extratubal falling film laminar flow in turn.
Often for arrangement membrane structure there are one above cloth membrane pores unit, each unit includes a hole 511 and a seam
512, preferably, hole wall is dentation, as shown in figure 4, so as to make the gap between the hole wall in hole 51 and pipe between falling liquid film support tube
Essentially slot.Preferably, the inner ring radius of slot（R1）It is identical with the pipe end radius of falling liquid film support tube straight tube, slot outer shroud
Radius（R2）With inner ring radius（R1）Difference for 0.1 ~ 10 mm, the width of slit 512（L1）For 0.1 ~ 10 mm, length
（L2）For 1 ~ 200 mm.
Fig. 5 a, 5b, 5c are respectively several examples that falling liquid film support tube 18 passes through cloth diaphragm plate geometric layout between multi coil.It is adjacent
The central axes vertex of falling liquid film support tube is connected to parallel four side between four pipes of falling liquid film support tube 18 between two rows of neighbouring two groups of pipes
Shape.
Preferably, the vertical range between row and row of falling liquid film support tube 18 is 10 ~ 200 between the pipe of arranged in rows
Mm, the whole right angle setting in a row of falling liquid film support tube 18 between pipe.
Reactor has heat transfer system, including heating agent flow into babinet 3, heating agent outflow babinet 4 and pipe between falling liquid film support tube 18 and
Its circulation path formed, heating agent flow on babinet 3 and heating agent outflow babinet 4 and are respectively equipped with reactor Heating medium 1 and reaction
Device heating agent outlet 22.
Reactor is equipped with heat-insulation system, 8 He of housing chuck set respectively including upright shell 7 and bottom case 12 and its periphery
Bottom case chuck 13, the upper and lower part of housing chuck 8 are respectively equipped with housing chuck Heating medium 6 and the outlet of housing chuck heating agent
17, the upper and lower part of bottom case chuck 13 is respectively equipped with bottom case chuck Heating medium 11 and bottom case chuck heating agent outlet 15.
The thermal medium of heat transfer system and heat-insulation system is passed to external by Posterior circle operation is heated or cooled.
Babinet 3, the reactor top that heating agent outflow babinet 4 and material material feeding box 5 form and upright shell 7 are flowed by heating agent
It being connected by shell flange 20 and casing bolts 21, upright shell 7 is connected with bottom case 12 by bottom case flange 9 and bottom case bolt 10,
Maintenance and installation easy to disassemble.
Use the melt polycondensation process of above-mentioned polycondensation reactor for：
When reactor works, heating agent is flowed into from the inner tube port of falling liquid film support tube between pipe, then is flowed out from outer tube port, then
It is circulated to outside polycondensation reactor by Posterior circle operation is heated or cooled.
Material inlet is located at heating agent and flows into right among top of the box, molten monomer blend or prepolymer from material into
Mouth constantly injection, the heating agent that wore long are flowed into the feed pipe inflow material material feeding box of babinet and heating agent outflow babinet.
Melt is after the hole distribution on cloth diaphragm plate into falling liquid film support area under control, the uniform cloth outside pipe between the pipe of arranged in rows
Film forms falling liquid film, and " waterfall " shape film evaporation device is formed between pipe, carries out melt polycondensation reaction, and melt by connecting at equal intervals between pipe
It connects silk and certain film thickness is maintained to flow, the small molecule for reacting generation is extracted out from vacuum pumping opening.
Melt between falling liquid film support tube pipe between pipe slide after, finally converge to polycondensation reactor bottom, by blender into
One step is stirred to react and homogenizes material, completes the melt after reaction and is discharged from the material outlet of reactor bottom.
Embodiment 2, with reference to attached drawing 2,4,5a, 5b, 5c.
In the present embodiment, the outer tube 181 of falling liquid film support tube 18 uses the coaxial straight tube of reducing between pipe.
The outer tube 181 of falling liquid film support tube 18 becomes multistage diameter not with equidistant interior reducing below cloth diaphragm plate 51 between pipe
Once the straight tube continuously communicated, up and down each section it is coaxial, from 51 lower section of cloth diaphragm plate to 18 bottom of falling liquid film support tube between pipe, straight tube outer diameter
Reduce paragraph by paragraph successively.
Preferably, 181 reducing hop count of outer tube can be 2 ~ 100, it is close to 51 lower section first segment straight tube outer diameter of cloth diaphragm plate
20 ~ 30 mm, a diameter of 1 ~ 10mm of final stage straight tube close to tube bottom one end.
On the outer tube 181 of reducing, the tube spacing of 183 length of connecting filament corresponding thereto between the pipe of each section of reducing outer tube
Keep equal.
The other parts and implementation of the present embodiment are same as Example 1, and in fig. 2, drawing reference numeral is identical with Fig. 1
Represent identical meaning.
Embodiment 3, with reference to attached drawing 3,4,5a, 5b, 5c.
In the present embodiment, the outer tube 181 of falling liquid film support tube 18 is the constant straight tube of caliber between pipe, falling liquid film between adjacent two pipe
Without connecting filament between lateral pipe between support tube.
Preferably, the tube spacing of falling liquid film support tube is from being 0.1 ~ 10 with the ratio between its caliber between adjacent tubes.
The other parts and implementation of the present embodiment are same as Example 1, and in figure 3, drawing reference numeral is identical with Fig. 1
Represent identical meaning.
Structure feature the foregoing is merely specific embodiments of the present invention, but the present invention is not limited thereto, Ren Heben
The technical staff in field in the field of the invention, all cover among protection scope of the present invention by the variation or modification made.
Claims (10)
- It is 1. a kind of into falling liquid film melt polycondensation reaction method between comb, it is characterised in that：The method uses and is configured with arranged in rows Heat-exchange tube between falling liquid film support tube reactor, between the pipe of arranged in rows in falling liquid film support tube, falling liquid film support tube is between pipe Proximity association, the ratio between tube spacing and caliber are 0.1~20, make melt material when flowing downward, between the pipe of arranged in rows Curtain is connected between falling liquid film support tube, forms waterfall shape film evaporation device between falling liquid film support tube between pipe, and carry out melt polycondensation reaction, From the two sides of waterfall shape falling liquid film volatilization small-molecule substance, material molecular melt amount is improved.
- It is 2. as described in claim 1 a kind of into falling liquid film melt polycondensation reaction method between comb, it is characterised in that：The material exists When flowing downward, while also falling liquid film support pipe outer wall forms extratubal falling film between the pipe, between the pipe between falling liquid film support tube The melt material of waterfall shape film evaporation device is connected with the melt material of extratubal falling film.
- 3. a kind of into falling liquid film melt polycondensation reaction device between comb, the reactor includes upright shell (7), it is characterised in that described Reactor further include falling liquid film support tube (18) between the heat-exchange tube of arranged in rows, be arranged on the material of upright shell (7) upper end into Hopper (5), the bottom plate of material material feeding box (5) are cloth diaphragm plate (51), and the falling liquid film support tube (18) of arranged in rows is across cloth diaphragm plate (51), cloth diaphragm plate (5) has film distribution structure, and film distribution structure includes the cloth film slit in region between falling liquid film support tube between respective tube (512), falling liquid film support tube is proximity association between pipe, makes melt material when flowing downward, the falling liquid film between the pipe of arranged in rows Curtain is connected between support tube, waterfall shape film evaporation device is formed between falling liquid film support tube between pipe, and carry out melt polycondensation reaction, from institute The two sides volatilization small-molecule substance of waterfall shape falling liquid film is stated, improves material molecular melt amount；Upright shell (7) top is equipped with vacuum pumping opening (19), and bottom case (12) bottom is equipped with material outlet (14).
- It is 4. according to claim 3 a kind of into falling liquid film melt polycondensation reaction device between comb, it is characterised in that：It is dropped between comb It is provided with or without connecting filament (183) between the pipe of adjacent two pipe of lateral connection between film support tube (18), connecting filament between two pipe pipes (183) radical is 0~1000, a diameter of 0.1mm~20mm, the tube spacing that connecting filament (183) radical is 0 between pipe from caliber it Than being 0.1~10, connecting filament (183) radical is 1~1000 between pipe tube spacing is from being 0.1~20 with the ratio between caliber.
- It is 5. according to claim 3 a kind of into falling liquid film melt polycondensation reaction device between comb, it is characterised in that：It is dropped between comb Film support tube (18) is equipped with multiple rows of film distribution structure across cloth diaphragm plate (51) right angle setting, cloth diaphragm plate (51), and film distribution structure includes For between pipe falling liquid film support tube (18) form the cloth fenestra (511) in falling liquid film gap and the cloth film slit at position between respective tube (512), and slit is connected with hole, and the gap between cloth fenestra hole wall and pipe between falling liquid film support tube is for material melt between pipe The outer cloth film of falling liquid film support tube.
- It is 6. as claimed in claim 3 a kind of into falling liquid film melt polycondensation reaction device between comb, it is characterised in that upright shell (7) exists Heating agent outflow babinet (4) is equipped with above material material feeding box (5) and heating agent flows into babinet (3), heating agent flows into babinet (3) equipped with reaction Device Heating medium (1), heating agent, which flows out, has reactor heating agent to export (22) on babinet (4), falling liquid film branch between the pipe of the arranged in rows Stay tube (18) flows into babinet (3) with heating agent and heating agent outflow babinet (4) communicates；Melt material inlet pipe flows out babinet (4) from heating agent Babinet (3) is flowed into heating agent to pass through, and passes to material material feeding box (5).
- It is 7. according to claim 3 a kind of into falling liquid film melt polycondensation reaction device between comb, it is characterised in that：It is dropped between the pipe Film support tube (18) covers inner tube (182) structure using outer tube (181), and inner tube (182) flows out box cover plate (41) phase with heating agent Logical, outer tube (181) is communicated with heating agent outflow babinet lower plate (42).
- It is 8. according to claim 7 a kind of into falling liquid film melt polycondensation reaction device between comb, it is characterised in that：It is dropped between the pipe The inner tube (182) of film support tube (18) keeps caliber constant, and outer tube (181) is straight-run of pipe or the coaxial straight tube of reducing, the change The reducing trend of the coaxial straight tube of diameter is from top to bottom, caliber becomes smaller.
- It is 9. according to claim 8 a kind of into falling liquid film melt polycondensation reaction device between comb, it is characterised in that：It is dropped between the pipe Film support tube outer tube (181) caliber is 2~30mm, and inner tube (182) caliber is 1~20mm, outer tube (181) caliber and inner tube (182) caliber differs 1~10mm.
- It is 10. according to claim 3 a kind of into falling liquid film melt polycondensation reaction device between comb, it is characterised in that：Reactor is set Heat transfer system and heat-insulation system, heat transfer system include heating agent and flow into babinet (3), heating agent outflow babinet (4) and falling liquid film support tube (18) circulation path of composition, heating agent flow on babinet (3) and heating agent outflow babinet (4) and are respectively equipped with reactor Heating medium (1) and reactor heating agent exports (22)；The shell that heat-insulation system includes upright shell (7) and bottom case (12) and its periphery is set respectively Body chuck (8) and bottom case chuck (13), the upper and lower part of housing chuck (8) be respectively equipped with housing chuck Heating medium (6) and Housing chuck heating agent exports (17), and the upper and lower part of bottom case chuck (13) is respectively equipped with bottom case chuck Heating medium (11) and bottom Shell chuck heating agent exports (15), and the thermal medium of heat transfer system and heat-insulation system is passed to outside by Posterior circle is heated or cooled Operation.
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| CN201610302101.3A CN105854734B (en) | 2016-05-09 | 2016-05-09 | It is a kind of prepare melt with high viscosity into falling liquid film melt polycondensation reaction method and its reactor between comb |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107029637B (en) * | 2017-05-11 | 2023-06-06 | 浙江理工大学 | High-viscosity fluid film distributor |
| CN107442059B (en) * | 2017-08-08 | 2023-03-28 | 浙江理工大学 | Falling film melt polycondensation reactor |
| CN110639461B (en) * | 2018-06-26 | 2024-04-09 | 浙江理工大学 | Falling film devolatilizer 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 |
| CN114790279B (en) * | 2021-01-26 | 2024-09-27 | 惠生工程（中国）有限公司 | Industrial production process method of polyglycolic acid oligomer |
| CN115193383B (en) * | 2022-06-01 | 2024-01-30 | 浙江理工大学 | Transverse tube falling film melt polycondensation method, reactor and devolatilizer thereof |
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