CN106000250B - It is a kind of at falling liquid film melt polycondensation reaction method and its reactor between comb - Google Patents
It is a kind of at falling liquid film melt polycondensation reaction method and its reactor between comb Download PDFInfo
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- CN106000250B CN106000250B CN201610303700.7A CN201610303700A CN106000250B CN 106000250 B CN106000250 B CN 106000250B CN 201610303700 A CN201610303700 A CN 201610303700A CN 106000250 B CN106000250 B CN 106000250B
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- 238000006068 polycondensation reaction Methods 0.000 title claims abstract description 55
- 239000007788 liquid Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 80
- 239000004744 fabric Substances 0.000 claims abstract description 45
- 238000001704 evaporation Methods 0.000 claims abstract description 13
- 230000008020 evaporation Effects 0.000 claims abstract description 13
- 239000010408 film Substances 0.000 claims description 79
- 239000000463 material Substances 0.000 claims description 63
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 11
- 239000000289 melt material Substances 0.000 claims description 11
- 239000011552 falling film Substances 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 8
- 239000000155 melt Substances 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- 150000003384 small molecules Chemical class 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 50
- -1 polyethylene terephthalate Polymers 0.000 abstract description 7
- 229920000642 polymer Polymers 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 abstract description 4
- 239000005020 polyethylene terephthalate Substances 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract 1
- 239000012528 membrane Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 229920001707 polybutylene terephthalate Polymers 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 3
- 239000012071 phase Substances 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
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000002708 enhancing effect Effects 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
- 239000007787 solid Substances 0.000 description 2
- 239000007790 solid phase Substances 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
- 206010023126 Jaundice Diseases 0.000 description 1
- 229920001730 Moisture cure polyurethane Polymers 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 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
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical compound C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 210000003429 pore cell Anatomy 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000006276 transfer reaction Methods 0.000 description 1
- MEYZYGMYMLNUHJ-UHFFFAOYSA-N tunicamycin Natural products CC(C)CCCCCCCCCC=CC(=O)NC1C(O)C(O)C(CC(O)C2OC(C(O)C2O)N3C=CC(=O)NC3=O)OC1OC4OC(CO)C(O)C(O)C4NC(=O)C MEYZYGMYMLNUHJ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polyesters Or Polycarbonates (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)
Abstract
The present invention relates to a kind of into falling liquid film melt polycondensation reaction method between comb, molten prepolymer flows downward from hole between cloth diaphragm plate and pipe, a kind of waterfall type film evaporation device is formed between U-tube in a row and carries out melt polycondensation reaction, melt converges to reactor bottom by being discharged after blender stirring homogenizing after being slid between pipe.Implement this method reactor be integral vertical type structure, including shell, the heating agent babinet and its connected body feed tank of upper end, U-tube and lower end bottom case, blender etc..U-tube vertical hanging is in a row arranged, and uniformly across cloth diaphragm plate hole, U-tube port is communicated with heating agent babinet to be flowed for heating agent.This reactor have flow resistance it is small, without dead zone, area is big for film forming, Surface Renewal is fast, the residence time is uniform controllable, the advantages that meeting Flexible Production, is suitable for the production of the polymer such as polyethylene terephthalate.
Description
Technical field
The present invention relates to a kind of falling film type melt polycondensation reaction methods and melt polycondensation reaction equipment in polymer production.
Background technology
Polycondensation reaction is a kind of continuous reversible polymerization reaction for generating micromolecular compound, including poly terephthalic acid second two
Alcohol ester（PET）, polypropylene terephthalate（PTT）, polybutylene terephthalate (PBT)（PBT）, poly- naphthalenedicarboxylic acid second two
Alcohol ester（PEN）, polyamide（PA）And makrolon（PC）Polymer Deng including is made by polycondensation reaction.This Type of Collective
The similar feature of object is exactly in polycondensation process, it is necessary to persistently carry out excluding the devolatilization work of the micromolecular compound of generation
Skill is carried out with promoting to react constantly positive, thus material stickiness is high, and especially in the polycondensation later stage, material dynamic viscosity can be sent out
The variation of the raw order of magnitude, this reaction are to be related to the change that chemical reaction is coupled with heat and mass to stick process.Therefore, polycondensation reaction is imitated
Fruit depends on the flow behavior and Mass and heat transfer Interfacial Characteristics of material.
The polycondensation method for preparing heavy polymer usually has melt polycondensation, melt polycondensation, solid phase polycondensation etc..Work at present
It is process for solid state polycondensation to be applied most common in industry, mainly has benefited from its lower polycondensation reaction temperature, so that polymer is sent out
The possibility of raw high temperature degradation substantially reduces, and not will produce coloring or decomposition product, and is conducive to volatile impurity effusion polymerization
In object.But main problem existing for this method is that process is more, long flow path, react front and back material need repeatedly heating repeatedly cooling and
Big energy is consumed, and solid phase polycondensation process will produce more particulate dust and influence the operations such as follow-up spinning.Melt polycondensation
Method can prepare high glutinous material in a relatively short period of time, save multiple working procedure, and melt-polycondensation is suitable for all types of consersion units,
Thus process for solid state polycondensation is compared to have a clear superiority in terms of economy, environmental protection and industrial implementation.
It is equal that presently disclosed falling liquid film polycondensation reactor mainly falls the melt polycondensation reactions device such as a formula, grated plate type, tube wall type
It is to be improved compared to traditional horizontal reactor in the case where greatly reducing energy consumption at membrane flow on inner member by melt
The melt film forming efficiency and Surface Renewal of equipment.Especially when preparing high glutinous material viscosity, extratubal falling film reactor can make
Material only leans on gravity at membrane flow outside pipe, provides the suitable residence time and material is enable fully to react, but complete attached wall
Formula film evaporation device can make melt films because the speed difference of inside and outside tunic causes outer layer liquid film flow velocity fast, and inner layer film is slower, causes portion
Divide material to invest for a long time in reactor component and degradation, jaundice occurs, influence final products quality, and falls a formula and freely drop
The flow velocity that film then can make melt films freely land is too fast and the residence time is too short, and melt film surface during falling liquid film shrink it is bright
Aobvious, film forming efficiency is very low.Hence it is imperative that developing a kind of melt polycondensation reaction device, material filming performance in reactor can be made
Good, Surface Renewal is fast, and the residence time is uniform, no dead zone, easy to clean, and low energy consumption, and reaction process meets flowing, mixing and caloic
Transmission demand realizes high-effect polycondensation.
Invention content
First purpose of the invention is in view of the deficiencies of the prior art, to provide a kind of at falling liquid film melt polycondensation reaction between comb
Method can make reaction temperature uniform, controllable, effectively be expanded into membrane area, improve the surface of melt film forming efficiency and melt more
Newly, enhancing melt flows are at the homogeneity of film uniformity and melt residence time, the glutinous object of final raising polycondensation reaction efficiency and height
The product quality of material, proposes following technical scheme thus；
It is a kind of at falling liquid film melt polycondensation reaction method between comb, it is characterised in that：The method is used configured in a row row
The reactor of the U-shaped heat-exchange tube of row, heating agent is flowed into from U type pipes one end when work, other end outflow；Melt material is downward
When flowing, it is connected to curtain between the straight tube of the U-shaped heat-exchange tube of arranged in rows, forms waterfall shape film evaporation device between straight tube, and
Melt polycondensation reaction is carried out, from the two sides of waterfall shape falling liquid film volatilization small-molecule substance, improves material molecular melt amount, at
The straight tube of the U-shaped heat-exchange tube of arrangement is proximity association, while as the skeletal support pipe of the curtain, tube spacing and caliber
The ratio between be 0.1 ~ 20.
Further, the material is when flowing downward, while also forming extratubal falling film in the straight tube outer wall, described straight
The melt material of waterfall shape film evaporation device between pipe is 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, and reaction temperature can be made equal
It is even controllable, it is effectively expanded into membrane area, improves the Surface Renewal of melt film forming efficiency and melt, enhancing melt flows film forming is equal
The homogeneity of even property and residence time improves the product quality of polycondensation reaction efficiency and high glutinous material.For this purpose, the present invention use with
Lower technical solution：
At falling liquid film melt polycondensation reaction device between comb, the reactor includes upright shell, it is characterised in that the reaction
Device further includes the U-shaped heat-exchange tube of arranged in rows, the material material feeding box on upright shell top, the bottom plate of material material feeding box is arranged
Straight tube for cloth diaphragm plate, the U-shaped heat-exchange tube of arranged in rows passes through cloth diaphragm plate, cloth diaphragm plate to have film distribution structure, film distribution structure packet
Include 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 spacing and caliber it
Than being 0.1 ~ 20, makes material melt when flowing downward, curtain is connected 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 carries out melt polycondensation reaction.
On the basis of using above-mentioned technical proposal, the present invention can also use technical solution further below simultaneously, or
These solution pools are used：
It can be equipped between 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
Or it is not provided with connecting filament between lateral pipe, connecting filament radical is 0 ~ 1000 between the pipe of two straight tubes, a diameter of 0.1 mm ~ 10
The ratio between mm, connecting filament radical is 0 between pipe tube spacing and caliber are 0.1 ~ 10, the pipe that connecting filament radical is 1 ~ 1000 between pipe
The ratio between spacing and caliber are 0.1 ~ 20.
The U-shaped heat-exchange tube of arranged in rows passes through cloth diaphragm plate right angle setting, cloth diaphragm plate to be equipped with multiple rows of film distribution structure, cloth film
Structure includes that the cloth film in region between cloth fenestra and corresponding straight tube for forming falling liquid film gap U-shaped heat-exchange tube straight tube is narrow
Seam, and slit is connected to hole, the gap between cloth fenestra hole wall and straight tube is used for material melt cloth film outside straight tube.
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, has the outlet of reactor heating agent, U-shaped heat-exchange tube one end of the arranged in rows on heating agent outflow babinet
Babinet is flowed into heating agent to communicate, the other end is communicated with heating agent outflow babinet；Melt material inlet pipe passes to material material feeding box；Vertical shell
Body top is equipped with vacuum pumping opening, and blender is equipped in bottom case, and power is passed to by bottom, and bottom case bottom is equipped with material outlet.
The U-shaped heat-exchange tube right angle setting of arranged in rows, lower end is hanging, is in same with the axis for arranging U-shaped heat-exchange tube
The central axes vertex of plane, four straight tubes of adjacent two rows of neighbouring two groups of U-tubes is connected to parallelogram.
The straight tube of U-shaped heat-exchange tube can be the coaxial straight tube of reducing, the reducing trend of the coaxial straight tube of reducing be from up to
Under, caliber becomes smaller, and U-shaped heat-exchange tube outer diameter is 1 ~ 50 mm.
It includes that heating agent flows into babinet, heating agent flows out babinet and U-shaped that reactor, which has heat transfer system and heat-insulation system, heat transfer system,
The circulation path of heat-exchange tube and its composition, heating agent flow on babinet and heating agent outflow babinet and are respectively equipped with reactor Heating medium
It is exported with reactor heating agent；Heat-insulation system includes upright shell and bottom case and its peripheral shell chuck being respectively set and bottom case folder
The upper and lower part of set, shell chuck is respectively equipped with shell chuck Heating medium and the outlet of shell chuck heating agent, bottom case chuck
Upper and lower part is respectively equipped with bottom case chuck Heating medium and the outlet of bottom case chuck heating agent, the heating agent of heat transfer system and heat-insulation system
Flow of media is to the external circular flow after being heated or cooled.
The present invention is suitable for polyethylene terephthalate（PET）, polypropylene terephthalate（PTT）, poly- pair
Benzene dicarboxylic acid butanediol ester（PBT）, polyethylene naphthalate（PEN）, polyamide（PA）And makrolon（PC）Deng polymerization
The melt polycondensation reaction of object.
The present invention has the characteristics that viscosity constantly increases in viscosity height and reaction process using polycondensation reaction material melt,
It was found that can realize film evaporation device between the pipe of " waterfall " shape in the reactor under certain condition, larger film forming face can be maintained always
Product, melt uniform film thickness, flow velocity reach unanimity, and film surface keeps laminar flow to move under gravity forces, to ensure that polymerization
Molecular weight of product narrowly distributing, it can be achieved that continuous production performance it is excellent and stablize product, and unit volume reactor production effect
Rate greatly increases.Present invention discover that melt polycondensation reaction device right and wrong of the U-shaped heat-exchange tube in a row arranged as falling liquid film support element
It is often applicable in the reactor of this reaction method, further, supporting wire between the pipe of adjacent two pipe is set, " waterfall " can be directed to
Falling liquid film between the pipe of shape, reinforces the dispersion of melt and mixes, and improves the Surface Renewal frequency of melt films, while again can be to waterfall shape
Stability play the role of holding.Reaction method of the present invention is simple and feasible, and with flowing into, membrane area is big, Surface Renewal is fast
Rate is fast, the residence time is uniform controllable, and the series of advantages such as low energy consumption, easy cleaning are, it can be achieved that Mass and heat transfer and chemical reaction
The high-effect melt polycondensation of coupling.
Description of the drawings
Fig. 1 is the structural schematic diagram of embodiment 1 provided by the present invention.
Fig. 2 is the structural schematic diagram of embodiment 2 provided by the present invention.
Fig. 3 is the structural schematic 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 the 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 flows out box cover plate 41, and heating agent flows out babinet lower plate 42, material material feeding box 5, cloth diaphragm plate 51, cloth fenestra
511, cloth film slit 512, shell chuck Heating medium 6, upright shell 7, shell 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, U-tube 18, connecting filament 181 between pipe, vacuum pumping opening 19, shell flange 20, casing bolts 21, instead
Device heating agent is answered to export 22, melt material inlet pipe 23.
Specific implementation mode
Embodiment 1, with reference to attached drawing 1,4,5a, 5b, 5c.
In the present embodiment, U heat exchange 18（Hereinafter referred to as U-tube comprising the straight tube of both sides and bottom end connect
Connect the bend pipe of both sides straight tube）Straight tube using the constant straight tube of caliber.
The present embodiment is provided a kind of at falling liquid film melt polycondensation reaction device between comb, as shown in Figure 1, it includes vertical shell
Body 7, is connected to the material material feeding box of 7 upper end of upright shell and the bottom case 12 of lower end, and 5 top of material material feeding box is equipped with heating agent and flows out
Babinet 4, heating agent outflow babinet 4 on again equipped with heating agent flow into babinet 3, heating agent flow into babinet 3 be equipped with reactor heating agent into
Mouth 1, heating agent, which flows out, has reactor heating agent to export 22 on babinet 4,18 one end of U-tube of arranged in rows and heating agent flow into 3 phase of babinet
Logical, the other end is communicated with heating agent outflow babinet 4, and melt material inlet pipe 23 flows out babinet 4 from heating agent and heating agent flows into babinet 3 and wears
It crosses, passes to material material feeding box 5；The bottom plate of material material feeding box 5 is cloth diaphragm plate 51, has film distribution structure, upright shell 7 on cloth diaphragm plate 51
Top is equipped with vacuum pumping opening 19, and 18 lower section of U-tube is equipped with blender 16, and power is passed to by bottom, and 12 bottom of bottom case is set
There is material outlet 14.
It is proximity association with the straight tube of U-shaped heat-exchange tube 18 is arranged in the U-shaped heat-exchange tube 18 of arranged in rows, it is U-shaped
The straight tube of heat-exchange tube 18 plays the role of falling liquid film support element between pipe, and it is downward that tube spacing makes material melt pass through film distribution structure
When flowing, 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 pipe, goes forward side by side
Row melt polycondensation reaction.Small molecule by-product passes through vacuum pumping opening 19 from the two sides devolatilization of the waterfall shape falling liquid film
Discharge.
18 right angle setting of U-tube, lower end is hanging, 18 neat arranged in rows of more single u-shaped pipes, with row's U-tube 18
Axis is in same plane, is separated by between row and row with equidistant keeping parallelism.
Preferably, two straight tube tube spacing of U-tube 18 and the adjacent straight tube tube spacing phase of two neighboring U-tube 18
From the ratio between the pipe outside diameter with U-tube it is 0.1 ~ 20 Deng, tube spacing.
Preferably, the straight tube pipe range of U-tube 18 is 0.5 ~ 30 m, outer diameter is 1 ~ 50 mm.
It can be equipped between transverse pipe between 18 liang of straight tubes of vertically arranged U-tube and between the adjacent straight tube of two neighboring U-tube
Connecting filament 181, connecting filament length is equal to the vertical range of two pipes between pipe, preferably, connecting filament between the pipe of adjacent two straight tubes
Radical is 1 ~ 1000, a diameter of mm of 0.1 mm ~ 10.
The U-tube 18 in a row arranged passes through 51 right angle setting of cloth diaphragm plate, cloth diaphragm plate 51 to be equipped with multiple rows of film distribution structure, cloth film
Structure includes narrow for the cloth film between the cloth fenestra 511 and corresponding straight tube in 18 straight tube of U-shaped heat-exchange tube formation falling liquid film gap
Seam 512, and slit 512 is connected to hole 511, slit 512 is such as schemed for making material melt films be flowed down between pipe with relatively thin thickness
Shown in 4；Gap between cloth fenestra hole wall and straight tube is used for material melt cloth film outside straight tube, forms extratubal falling film flowing,
The melt material of waterfall shape film evaporation device between the straight tube is connected with the melt material of extratubal falling film, not only further increases into
Membrane area, and contribute to waterfall shape film evaporation device at curtain stability, and the material curtain between pipe can utilize the viscous of material in turn
Degree has facilitation to the formation of extratubal falling film laminar flow.
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, to make the gap between the hole wall in hole 511 and straight tube be essentially tooth
Seam.Preferably, the inner ring radius of slot（R1）It is identical as the pipe end radius of U-tube straight tube, slot outer shroud radius（R2）With inner ring
Radius（R1）Difference be 0.1 ~ 10 mm, the width of slit 512（L1）For 0.1 ~ 10 mm, length（L2）For 1 ~ 200 mm.
The central axes vertex of four straight tubes of adjacent two rows of neighbouring two groups of U-tubes 18 is connected to parallelogram, Fig. 5 a,
5b, 5c are respectively that the straight tube of multiple rows of U-tube 18 passes through several examples of cloth diaphragm plate geometric layout.
Preferably, the vertical range of the U-tube 18 of arranged in rows between row and row is 10 ~ 200 mm, U-tube is in a row
Whole right angle setting.
Reactor be equipped with heat transfer system, including heating agent flow into babinet 3, heating agent outflow babinet 4 and U-tube 18 and its composition
It is respectively equipped with reactor Heating medium 1 on circulation path, heating agent inflow babinet 3 and heating agent outflow babinet 4 and reactor heating agent goes out
Mouth 22.
Reactor is equipped with heat-insulation system, including 8 He of shell chuck that upright shell 7 and bottom case 12 and its periphery are respectively set
The upper and lower part of bottom case chuck 13, shell chuck 8 is respectively equipped with shell chuck Heating medium 6 and the outlet of shell 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 the external circular flow after being 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 U type pipe Single ports, then is flowed out from another port, and it is anti-then to flow out to polycondensation
Answer the circular flow after being heated or cooled outside device.
Material inlet is located at heating agent and flows into right among top of the box, and pre-polymer melt is constantly injected from material inlet,
The heating agent that wore long flows into babinet and the feed pipe of heating agent outflow babinet flows into material material feeding box.
Melt enters the U-tube area of arranged in rows, the uniform cloth film outside U-tube straight tube after the hole distribution on cloth diaphragm plate
Falling liquid film is formed, forms " waterfall " shape film evaporation device between straight tube pipe, carries out melt polycondensation reaction, melt is by equidistant between pipe
Connecting filament and maintain certain film thickness to flow, the small molecule for reacting generation is extracted out from vacuum pumping opening.
Melt finally converges to polycondensation reactor bottom, is futher stirred instead by blender after being slid between U-tube pipe
Material is answered and homogenized, the melt after reaction is completed 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 straight tube of U-tube 18 is using the coaxial straight tube of reducing being connected to.
The straight tube of U-tube 18, with equidistant interior reducing, becomes diameter not once logical straight of continuous phase below cloth diaphragm plate 51
Pipe, up and down coaxially, from 51 lower section of cloth diaphragm plate to 18 bottom end of U-tube, caliber is gradually reduced.
In the U-tube of reducing, between each section of U-tube straight tube the length of connecting filament with its corresponding variable diameter straight tube
Tube spacing is equal from holding.
The other parts and implementation of the present embodiment are same as Example 1, and in fig. 2, drawing reference numeral and Fig. 1 are identical
Represent identical meaning.
Case study on implementation 3, with reference to attached drawing 3,4,5a, 5b, 5c.
In the present embodiment, 18 straight part of U-tube is the constant straight tube of caliber, between 18 liang of straight tubes of U-tube and with row
Connectionless silk between adjacent two straight tube of adjacent U-tube 18.
Preferably, 18 tube spacing of U-tube is from being 0.1 ~ 10 with the ratio between caliber.
The other parts and implementation of the present embodiment are same as Example 1, and in figure 3, drawing reference numeral and Fig. 1 are identical
Represent identical meaning.
Above is only a specific embodiment of the present invention, but the structure feature of the present invention is not limited thereto, Ren Heben
The technical staff in field in the field of the invention, made by changes or modifications all cover among protection scope of the present invention.
Claims (9)
1. a kind of at falling liquid film melt polycondensation reaction method between comb, it is characterised in that：The method, which uses, is configured with arranged in rows
U-shaped heat-exchange tube reactor, heating agent is flowed into from U-tube one end when work, other end outflow；Melt material is flowing downward
When, it is connected to curtain between the straight tube of the U-shaped heat-exchange tube of arranged in rows, forms waterfall shape film evaporation device between straight tube, and carry out
Melt polycondensation reaction improves material molecular melt amount, in a row arranges from the two sides of waterfall shape falling liquid film volatilization small-molecule substance
The straight tube of the U-shaped heat-exchange tube of row is proximity association, while as the skeletal support pipe of the curtain, the ratio between tube spacing and caliber
It is 0.1~20.
2. as described in claim 1 a kind of at falling liquid film melt polycondensation reaction method between comb, it is characterised in that：The material exists
When flowing downward, while also extratubal falling film, the melt of the waterfall shape film evaporation device between the straight tube are formed in the straight tube outer wall
Material is connected with the melt material of extratubal falling film.
3. a kind of at falling liquid film melt polycondensation reaction device between comb, the reactor includes upright shell (7), it is characterised in that described
Reactor further includes the U-shaped heat-exchange tube (18) of arranged in rows, setting in the material material feeding box (5) on upright shell (7) top, object
Expect that the bottom plate of material feeding box (5) is cloth diaphragm plate (51), the straight tube of the U-shaped heat-exchange tube (18) of arranged in rows passes through cloth diaphragm plate (51),
Cloth diaphragm plate (51) has film distribution structure, and film distribution structure includes the cloth film slit (512) in region between corresponding straight tube, the U of arranged in rows
The straight tube proximity association of type heat-exchange tube (18), the ratio between tube spacing and caliber are 0.1~20, and material melt is made to flow downward
When, it is connected to curtain between the straight tube of the U-shaped heat-exchange tube of arranged in rows, forms waterfall shape film evaporation device between straight tube, and carry out
Melt polycondensation reaction.
4. according to claim 3 a kind of at falling liquid film melt polycondensation reaction device between comb, it is characterised in that：U-shaped heat exchange
It can be provided with or without cross between adjacent straight tube pipe between two straight tube pipes of pipe (18) and with row's U-shaped heat-exchange tube of two adjacent groups (18)
To pipe between connecting filament (181), connecting filament radical is 0~1000 between the pipe of two straight tubes, a diameter of 0.1mm~10mm, is connected between pipe
It is 0.1~10 to connect the ratio between tube spacing and caliber that a radical is 0, the tube spacing and caliber that connecting filament radical is 1~1000 between pipe
The ratio between be 0.1~20.
5. according to claim 3 a kind of at falling liquid film melt polycondensation reaction device between comb, it is characterised in that：Arranged in rows
U-shaped heat-exchange tube (18) passes through cloth diaphragm plate (51) right angle setting, cloth diaphragm plate (51) to be equipped with multiple rows of film distribution structure, film distribution structure packet
Include the cloth film for the region between the cloth fenestra (511) and corresponding straight tube in U-shaped heat-exchange tube (18) straight tube formation falling liquid film gap
Slit (512), and slit is connected to hole, the gap between cloth fenestra hole wall and straight tube is used for material melt cloth outside straight tube
Film.
6. as claimed in claim 3 a kind of at falling liquid film melt polycondensation reaction device between comb, it is characterised in that upright shell (7) exists
It is equipped with heating agent outflow babinet (4) above material material feeding box (5) and heating agent flows into babinet (3), heating agent flows into babinet (3) and is equipped with reaction
Device Heating medium (1), heating agent, which flows out, has reactor heating agent to export (22) on babinet (4), the U-shaped heat-exchange tube of the arranged in rows
(18) one end flows into babinet (3) with heating agent and communicates, and the other end is communicated with heating agent outflow babinet (4)；Melt material inlet pipe passes to object
Expect material feeding box (5)；Upright shell (7) top is equipped with vacuum pumping opening (19), and bottom case (12) bottom is equipped with material outlet (14).
7. according to claim 3 a kind of at falling liquid film melt polycondensation reaction device between comb, it is characterised in that：Arranged in rows
U-shaped heat-exchange tube (18) right angle setting, lower end is hanging, and same plane is in the axis for arranging U-shaped heat-exchange tube (18).
8. according to claim 3 a kind of at falling liquid film melt polycondensation reaction device between comb, it is characterised in that：U-shaped heat exchange
The straight tube for managing (18) is the coaxial straight tube of reducing, and the reducing trend of the coaxial straight tube of reducing is from top to bottom that caliber becomes smaller, U-shaped
Heat-exchange tube (18) outer diameter is 1~50mm.
9. according to claim 3 a kind of at falling liquid film melt polycondensation reaction device between comb, it is characterised in that：Reactor has biography
Hot systems and heat-insulation system, heat transfer system include that heating agent flows into babinet (3), heating agent outflow babinet (4) and U-shaped heat-exchange tube (18)
And its 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)；Heat-insulation system includes upright shell (7) and bottom case (12) and its shell that periphery is respectively set
Body chuck (8) and bottom case chuck (13), the upper and lower part of shell chuck (8) be respectively equipped with shell chuck Heating medium (6) and
Shell 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 and is recycled after being heated or cooled
Operation.
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| CN107029637B (en) * | 2017-05-11 | 2023-06-06 | 浙江理工大学 | High-viscosity fluid film distributor |
| CN110813225B (en) * | 2019-10-10 | 2022-06-03 | 浙江理工大学 | Melt polycondensation reactor and falling film element thereof |
| CN112090388B (en) * | 2020-09-07 | 2022-04-12 | 浙江大学 | Continuous flow reactor and application thereof in chemical reaction and synthesis |
Citations (4)
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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2016
- 2016-05-09 CN CN201610303700.7A patent/CN106000250B/en active Active
Patent Citations (4)
| 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 |
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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 |