CN106861591A - A kind of melt polymerization falling film reactor and the method for carrying out melt polymerization - Google Patents
A kind of melt polymerization falling film reactor and the method for carrying out melt polymerization Download PDFInfo
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- CN106861591A CN106861591A CN201710213570.2A CN201710213570A CN106861591A CN 106861591 A CN106861591 A CN 106861591A CN 201710213570 A CN201710213570 A CN 201710213570A CN 106861591 A CN106861591 A CN 106861591A
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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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/247—Suited for forming thin films
Abstract
The present invention relates to a kind of melt polymerization falling film reactor and the method for carrying out melt polymerization, including cylinder, cylinder top is provided with feed pipe, cylinder top is provided with vacuum port, the bottom of cylinder is provided with discharging opening, the inner chamber of cylinder is provided with least one set of falling liquid film unit vertically, falling liquid film unit includes connecing liquid distributor and positioned at the falling liquid film sub-assembly connect below liquid distributor respectively, falling liquid film sub-assembly includes multi-disc parallel to tubular axis into diaphragm, it is each to be parallel to each other into diaphragm and uniform intervals setting, it is each into being respectively equipped with along the falling liquid film bar seam extended into diaphragm length direction on diaphragm.Each to set multiple tracks falling liquid film bar seam into diaphragm, each falling liquid film bar seam can be divided into multistage.Melt polymerization method comprises the following steps：Melt, into falling into adapter, flows out after heating from feed pipe from the liquid distributing hole of distribution plate, and correspondence falls in the splicing breach into diaphragm, then corresponds in being stitched into falling liquid film bar and forms film, so repeats.The present invention can increase falling liquid film area, improve devolatilization efficiency.
Description
Technical field
The present invention relates to a kind of polymer reactor, more particularly to a kind of melt polymerization falling film reactor；The invention further relates to
A kind of method that use melt polymerization falling film reactor carries out melt polymerization, belongs to polymer production technical field.
Background technology
The melt polymerization initial stage be melt viscosity be 50-200Pa s when, polymer molecular weight is relatively low, and system viscosity is not high, stirs
Mix, mix, conducting heat, mass transfer（Low molecule accessory substance is discharged）Deng not difficult；The polymerization later stage is that melt viscosity is 200-4000Pa
During s, it is very poor that fluidity of molten becomes, and liquid film updates and weakens, and heat transfer and mass transfer are extremely difficult.
The polymerization of melt is divided into batchwise polymerization and continuous polymerization, and batchwise polymerization device uses the reactor of vertical band stirring,
Carry out the growth of strand under vacuum conditions, continuous apparatus using band stirring horizontal reacting kettle, whipped form have cage with
Two kinds of disc type, two kinds of polymerization methodses are both needed to set stirring, machine envelope, bearing etc., with the increase of melt viscosity, power of agitator
Need to accordingly increase, energy consumption and equipment maintenance cost accordingly increase, be polymerized the later stage, melt easily rotates together with agitator, and produces
The certain dead band of life, melt viscosity heterogeneity causes degraded serious, and color and luster turns yellow.Additionally, traditional falling liquid film is generally outside pipeline
Wall or cylinder inboard wall are carried out, and the specific surface area of falling liquid film is small and can only realize one side devolatilization.
Polymerisation is a reversible reaction, if the change affects that a condition such as concentration, temperature, pressure etc. of balance,
Reaction can just be carried out to the direction for increasing the degree of polymerization, in the course of the polymerization process, polymerisation generation constantly be removed from melt
Small molecule product, to break reaction balance, further increases molecular weight；The polymerization later stage need to remove unconverted from the viscous thing system of height
To ensure the quality of melt, both of which is related to the devolatilization of viscous melt high to monomer.
Utility model content
Primary and foremost purpose of the invention is to overcome problems of the prior art, there is provided a kind of melt polymerization falling liquid film is anti-
Device is answered, the falling liquid film area of melt can be increased, improve devolatilization efficiency.
To solve the cylinder of above technical problem, a kind of melt polymerization falling film reactor of the invention, including vertical cylinder
Body, the cylinder is covered over cylinder heater, and the top center of the cylinder is provided with feed pipe, the cylinder
Top is provided with vacuum port, and the conical lower portion of the cylinder is provided with discharging opening, and the inner chamber of the cylinder is provided with least one set vertically
Falling liquid film unit, the falling liquid film unit includes connecing liquid distributor and positioned at the falling liquid film sub-assembly connect below liquid distributor respectively,
The falling liquid film sub-assembly includes multi-disc parallel to tubular axis into diaphragm, each described to be parallel to each other into diaphragm and uniform intervals set
Put, it is each described into being respectively equipped with diaphragm along the falling liquid film bar seam extended into diaphragm length direction.
Relative to prior art, the present invention achieves following beneficial effect：Melt enters cylinder lumen from feed pipe, first
Fall into during top layer connects liquid distributor, while being heated in liquid distributor is connect, falling liquid film sub-assembly outflow downwards on one side,
Melt is corresponded and forms film in each falling liquid film bar seam into the top of diaphragm and in the corresponding seam into each falling liquid film bar each,
There is polymerisation in the presence of cylinder lumen high temperature in melt, the small molecule product that polymerisation is produced from the both sides of film not
The disconnected removing and vacuum port from cylinder top is extracted；Melt film is polymerized devolatilization while continuing slow along each falling liquid film bar seam
Flow downwards, until after be heated again in liquid distributor into next layer being connect, mix, being redistributed, at next group
Film is formed again into the falling liquid film bar seam of diaphragm, so repeats falling liquid film devolatilization until melt constitutes the bottom of diaphragm from bottom one
Portion is flowed out, and the melt after thickening is discharged from the discharging opening of cylinder body bottom.The present invention by each falling liquid film bar slit into diaphragm into
Film, because the wall thickness into diaphragm is very thin, take up space very little, therefore one group of falling liquid film sub-assembly can have multiple into diaphragm,
Also just there are multiple falling liquid films, compared with traditional extratubal falling film, the area of falling liquid film is greatly expanded, makes melt that there is greatly ratio
Surface area, and each film two faces in the high-temperature space, the small molecule product that polymerisation is produced can be from thin
The both sides of film constantly remove and the vacuum port from cylinder top is extracted, and substantially increase devolatilization efficiency and the devolatilization uniformity, together
When play energy-saving effect.
Used as improvement of the invention, the falling liquid film bar seam is respectively equipped with multiple tracks, each road drop along each width into diaphragm
Film bar seam is parallel to each other and uniform intervals.Each can make each film forming into that can form a plurality of vertically extending film on diaphragm
Film size increasing on piece is several times greater, further increases devolatilization efficiency.
As a further improvement on the present invention, each falling liquid film bar seam is uniformly divided into two sections along short transverse by bar seam parting bead
More than.Deformation is easily caused because falling liquid film bar seam is long, bar seam both sides is difficult to ensure that and is substantially parallel or is definitely maintained at same
In individual plane, the bar for setting multiple connection falling liquid film bar seam both sides along the elevation that each falling liquid film bar is stitched stitches parting bead, can keep total drop
In the case that film is highly constant, every section of fluting of bar seam is reduced highly, it is ensured that the stabilization of falling liquid film bar seam shape from top to bottom, melt
After blocking through bar seam parting bead, film more uniformly can be formed in the bar seam of lower section, improve the uniformity and stabilization of falling liquid film
Property.
As a further improvement on the present invention, upper lug, each institute are respectively provided on two sides with before and after each upper end into diaphragm
The center for stating upper lug is respectively equipped with pin-and-hole, two suspended axles being parallel to each other sequentially pass through it is each go up pin-and-hole accordingly into diaphragm,
By each into diaphragm series connection is for one group and is suspended in the cylinder.Two suspended axles being parallel to each other penetrate each into the upper of diaphragm upper end
In lug, each upper end into diaphragm is suspended on cylinder lumen, respectively the lower end into diaphragm is hung down by means of deadweight, in stable equilibrium's shape
State, can automatically ensure axis of each falling liquid film bar seam on diaphragm parallel to cylinder, it is ensured that melt can be sewed in falling liquid film bar
Form uniform film.
As a further improvement on the present invention, lower lug, each institute are respectively provided on two sides with before and after each lower end into diaphragm
The center for stating lower lug is respectively equipped with lower pin-and-hole, and two connecting shafts being parallel to each other are sequentially passed through each descends the pin-and-hole will accordingly into diaphragm
Respectively it is mutually permanently connected into the lower end of diaphragm.Respectively it is fixed as one by connecting shaft into the lower end of diaphragm, falling liquid film group can be improved
The globality of component, increases overall pendency deadweight, improves each rigidity into diaphragm, prevents indivedual lower ends into diaphragm from occurring inclined
Move.
As a further improvement on the present invention, each upper spacer and lower spacer phase between diaphragm by equal length
Mutually it is spaced, each upper spacer is set on the suspended axle, and each lower spacer is set in the connecting shaft,
Jump ring is respectively equipped with positioned at the outermost upper pin-and-hole into diaphragm and lower pin-and-hole outside, the jump ring is inlaid in the suspension respectively
In the jump-ring slot of axle or connecting shaft.Upper spacer and lower spacer are by each into evenly spaced between diaphragm, it can be ensured that adjacent into diaphragm
Between spacing it is equal, can ensure each into diaphragm accurate positioning on suspended axle or connecting shaft by the positioning of jump ring, it is ensured that
Each quality for being maintained at vertical state into diaphragm, improving falling liquid film after suspension.
As a further improvement on the present invention, the two ends of the suspended axle are arranged with the suspension groove of undergauge, described outstanding
Hang groove to be stuck in J-hook, the J-hook distribution has the semicircular base being adapted with the suspension groove,
The top higher than the suspended axle is extended upwardly on front side of each semicircular base, the rear side of each semicircular base is high
In front side and it is connected to the lower section for connecing liquid distributor.The semicircular base that suspension groove is stuck in J-hook causes suspension
Axle obtains axially position in J-hook, while suspended axle can freely be rotated in J-hook so that falling liquid film sub-assembly exists
Vertical state is positively retained under Gravitative Loads, and belongs to stable equilibrium, even if the lower end of falling liquid film sub-assembly swings, can be fast
Speed is returned to catenary, it is ensured that each to be in vertical state into diaphragm.The front side of J-hook both ensure that higher than the top of suspended axle
The reliability of suspension, is easy to suspended axle to snap in J-hook again, or takes out suspended axle from J-hook, is conveniently replaceable falling liquid film combination
Part, or falling liquid film sub-assembly is taken out into cleaning.
As a further improvement on the present invention, it is each described into being evenly distributed with multiple semicircle or V-arrangements at the top of diaphragm
Splicing breach, each splicing breach is corresponded and coaxial line with the falling liquid film bar seam of lower section respectively.The splicing of semicircle or V-arrangement
Breach is easy to accept the melt that top falls, and melt under gravity, flows to the lowest part of semicircle or V-notch, from
The axis of dynamic alignment lower section falling liquid film bar seam falls so that melt is accurately into falling liquid film bar seam and forming uniform film.
As a further improvement on the present invention, each liquid distributor that connects respectively includes being connect with the cylinder coaxial line
Liquid pipe, the upper end open of the adapter, the bottom of the adapter is provided with dismountable distribution plate, is distributed on the distribution plate
Have and each one-to-one liquid distributing hole of splicing breach.The adapter of the top accepts the melt fallen from feed pipe, lower section
Adapter accept the melt that is fallen from top falling liquid film sub-assembly；After melt enters adapter, the liquid distributing hole shape from distribution plate
Synchronously flowed out into multi beam, due to the splicing breach below liquid distributing hole alignment, therefore from the melt beam of liquid distributing hole outflow it is each it is comfortable into
Film is formed in the falling liquid film bar seam of diaphragm.Melt viscosity is smaller, and the diameter of liquid distributing hole is also smaller, and distribution plate is detachable, is easy to root
Distribution plate is changed the need for according to product.
As a further improvement on the present invention, each liquid distributor that connects also includes covering on connecing on the outside of the adapter
Liquid distributor housing, forms connecing for closing between the inwall for connecing liquid distributor housing and the lateral wall of the adapter
Liquid pipe heating chamber, the flange plate that the external end head for connecing liquid distributor housing is provided with and is connected on the cylinder is described
The axis of flange plate intersects vertically with the axis of the adapter；Temperature-measuring port, electrically heated rod are connected with the flange plate
Mouth and heating agent expansion hatch.Connect liquid distributor and be horizontally inserted cylinder lumen, when flange plate is fixed on cylinder body outer wall, connect liquid
Pipe just with cylinder coaxial line, by flange plate dismounting easy to connect, be easy to change distribution plate or cleared up.Adapter
Conduction oil is full of in heating chamber, temperature-measuring port is the sleeve pipe of inner termination closing, can detect adapter heating chamber temperature and
Thermometric component can online be changed；Electrically heated rod is added from electrically heated rod mouthful insertion adapter heating chamber to conduction oil
Heat, can be arranged as required to one or more electrically heated rods mouthful；Heating agent expansion hatch is connected with heating medium expansion slot, and liquid is connect to adjust
The change of heating agent volume in pipe heating chamber.
As a further improvement on the present invention, the inner chamber of the adapter is provided with heating coil.Heating intensity can be improved,
Make the temperature of melt more uniform.
As a further improvement on the present invention, vacuum sampler is separately installed with below each falling liquid film sub-assembly, respectively
The external end head of the vacuum sampler is separately fixed on sample tap seat, and each sample tap seat is connected to the cylinder
On barrel.Assay can be carried out to the melt flowed out from falling liquid film sub-assembly by vacuum sampler, and according to analysis data
Temperature, pressure and other parameters in adjusting cylinder body.
As a further improvement on the present invention, positioned at the liquid distributing hole aperture of lower floor successively more than the liquid distributing hole hole of last layer
Footpath.More toward lower floor, the viscosity of melt is bigger, and the aperture of liquid distributing hole increases successively, is conducive to melt smoothly to flow out.
As a further improvement on the present invention, the cylinder heater is heating jacket or half pipe heater.
It is another object of the present invention to overcome problems of the prior art, there is provided use melt polymerization falling liquid film
The method that reactor carries out melt polymerization, can make the great falling liquid film area of melt composition, improve devolatilization efficiency, reducing energy consumption.
Be solve above technical problem, the method that use melt polymerization falling film reactor of the invention carries out melt polymerization,
In turn include the following steps：Melt enters cylinder lumen from feed pipe, falls into first in top layer adapter, while by adapter
The heating of periphery heating agent, while from the synchronous uniform outflow of each liquid distributing hole of top layer adapter bottom distribution plate, corresponding
In the splicing breach into diaphragm immediately below liquid distributing hole, then respectively it is located at since the bottom outflow correspondence of splicing breach enters
In falling liquid film bar seam immediately below splicing breach, film is formed in each falling liquid film bar seam, melt is in the presence of cylinder lumen high temperature
Generation polymerisation, the small molecule product that polymerisation is produced constantly is removed and from the vacuum port on cylinder top from the both sides of film
It is extracted；Melt film is polymerized devolatilization while continue slowly to be flowed downwards along each falling liquid film bar seam, until into next layer
Adapter in be heated again, mix, redistribute after, form film again in the falling liquid film bar seam of next composition diaphragm,
So falling liquid film devolatilization is repeated until melt is from the bottom outflow of the composition diaphragm of bottom one, and melt after thickening is from cylinder body bottom
Discharging opening is discharged.
Relative to prior art, the present invention achieves following beneficial effect：The present invention is by each falling liquid film bar into diaphragm
Into film, because the wall thickness into diaphragm is very thin, take up space slit very little, thus one group of falling liquid film sub-assembly can have it is multiple into
Diaphragm, also just has multiple falling liquid films, compared with traditional extratubal falling film, greatly expands the area of falling liquid film, melt is had pole
Big specific surface area, and each film two faces in the high-temperature space, the small molecule product that polymerisation is produced can
It is extracted with the vacuum port from the continuous removing in the both sides of film and from cylinder top, substantially increases devolatilization efficiency and devolatilization is uniform
Degree, while playing energy-saving effect.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description, accompanying drawing only provide with reference to
Illustrate to use, be not used to the limitation present invention.
Fig. 1 is the structural representation of melt polymerization falling film reactor of the present invention.
Fig. 2 is the structural representation of falling liquid film sub-assembly in Fig. 1.
Fig. 3 is the enlarged drawing at A positions in Fig. 2.
Fig. 4 is the structural representation in falling liquid film sub-assembly into diaphragm.
Fig. 5 is the enlarged drawing at B positions in Fig. 4.
The splicing breach that Fig. 6 is into diaphragm is the schematic diagram of V-arrangement.
Fig. 7 is into the schematic diagram of second embodiment of diaphragm.
Fig. 8 is to connect the structural representation of liquid distributor in Fig. 1.
Fig. 9 is the top view of Fig. 8.
Figure 10 is the schematic diagram for connecing second embodiment of liquid distributor.
Figure 11 is the C direction views in Fig. 8.
In figure：1. cylinder；1a. vacuum ports；1b. discharging openings；1c. sample taps seat；2. heating jacket；3. feed pipe；4. connect
Liquid distributor；4a. adapters；4b. distribution plates；4b1. liquid distributing holes；4c. connects liquid distributor housing；4d. adapters are heated
Chamber；4e. flange plates；4f. temperature-measuring ports；4g. electrically heated rods mouthful；4h. heating agent expansion hatches；5. falling liquid film sub-assembly；5a. is into diaphragm；
5a1. falling liquid films bar is stitched；5a2. bars stitch parting bead；5a3. upper lugs；The upper pin-and-holes of 5a4.；Lug under 5a5.；Pin-and-hole under 5a6.；5a7. connects
Material breach；5b. suspended axles；5b1. hangs groove；The upper spacers of 5c.；5d. jump rings；5e. connecting shafts；Spacer under 5f.；6.J shapes are hung
Hook；7. vacuum sampler.
Specific embodiment
As shown in Figures 1 to 4, melt polymerization falling film reactor of the invention includes the cylinder 1 of vertical cylinder, cylinder 1
Be covered over cylinder heater, cylinder heater is the pipe heater of heating jacket 2 or half.The top of cylinder 1 is flat
Lid or end socket, the top center of cylinder 1 are provided with feed pipe 3, and the top of cylinder 1 is provided with vacuum port 1a, the conical lower portion of cylinder 1
Discharging opening 1b is provided with, the inner chamber of cylinder 1 is provided with falling liquid film unit vertically, and falling liquid film unit can be one group, two groups or more than three groups.
Falling liquid film unit includes connecing liquid distributor 4 and positioned at the falling liquid film sub-assembly 5 for connecing the lower section of liquid distributor 4, falling liquid film sub-assembly 5 respectively
Including multi-disc parallel to tubular axis into diaphragm 5a, respectively it is parallel to each other into diaphragm 5a and uniform intervals is set, respectively into diaphragm 5a
On be respectively equipped with along into diaphragm length direction extend falling liquid film bar stitch 5a1.Cylinder 1 can as needed carry out some segmentations, often
Connected by flange between segmentation, be easy to assembling falling liquid film sub-assembly 5, such as barrel diameter is larger, may be alternatively configured a section entirety, between
Manhole is set, is easy to assembling falling liquid film sub-assembly 5.
Melt enters cylinder lumen from feed pipe 3, falls into first during top layer connects liquid distributor 4, is connecing liquid distributor 4
Middle one side is heated, and falling liquid film sub-assembly 5 downwards flows out on one side, and melt corresponds each into the top of diaphragm 5a and right
Should enter in each falling liquid film bar seam 5a1, film is formed in each falling liquid film bar seam 5a1, melt is sent out in the presence of cylinder lumen high temperature
Raw polymerisation, the small molecule product that polymerisation is produced constantly is removed and from the vacuum port 1a on cylinder top from the both sides of film
It is extracted；Melt film is polymerized devolatilization while continue slowly to be flowed downwards along each falling liquid film bar seam 5a1, until into next
Connecing for layer be heated again in liquid distributor 4, mix, redistribute after, in the falling liquid film bar seam 5a1 of next composition diaphragm 5a
Film is formed again, falling liquid film devolatilization is so repeated up to melt from the bottom outflow of the composition diaphragm of bottom one 5a, after thickening
Melt is discharged from the discharging opening 1b of cylinder body bottom.
Falling liquid film bar stitches 5a1 and is respectively equipped with multiple tracks along each width into diaphragm 5a, and each road falling liquid film bar seam 5a1 is parallel to each other
And uniform intervals.Each can make each into the film on diaphragm 5a into that can form a plurality of vertically extending film on diaphragm 5a
Area increasing is several times greater, further increases devolatilization efficiency.
It is each into upper lug 5a3 is respectively provided on two sides with before and after the upper end of diaphragm 5a, the center of each upper lug 5a3 is respectively equipped with
Pin-and-hole 5a4, the two suspended axle 5b being parallel to each other sequentially pass through it is each go up pin-and-hole 5a4 accordingly into diaphragm 5a, by each into diaphragm 5a strings
Join for one group and be suspended in cylinder 1.The two suspended axle 5b being parallel to each other are penetrated in each upper lug 5a3 into diaphragm 5a upper ends,
Each upper end into diaphragm 5a is suspended on cylinder lumen, respectively the lower end into diaphragm 5a is hung down by means of deadweight, in stability,
Axis of each falling liquid film bar seam 5a1 on diaphragm 5a parallel to cylinder 1 can automatically be ensured, it is ensured that melt can be stitched in falling liquid film bar
Uniform film is formed on 5a1.
It is each into lower lug 5a5 is respectively provided on two sides with before and after the lower end of diaphragm 5a, the center of each lower lug 5a5 is respectively equipped with down
Pin-and-hole 5a6, the two connecting shaft 5e being parallel to each other are sequentially passed through and each are descended pin-and-hole 5a6 accordingly by under each 5a into diaphragm into diaphragm 5a
End is mutually permanently connected.Respectively it is fixed as one by connecting shaft 5e into the lower end of diaphragm 5a, the whole of falling liquid film sub-assembly 5 can be improved
Body, increases overall pendency deadweight, improves each rigidity into diaphragm 5a, prevents from being shifted into the lower end of diaphragm 5a individually.
It is each spaced into the upper spacer 5c and lower spacer 5f between diaphragm 5a by equal length, each upper spacer 5c difference
It is sleeved on suspended axle 5b, each lower spacer 5f is set on connecting shaft 5e, positioned at the outermost upper pin-and-hole into diaphragm 5a
5a4 and lower pin-and-hole 5a6 outsides are respectively equipped with jump ring 5d, and jump ring 5d is inlaid in the jump-ring slot of suspended axle 5b or connecting shaft 5e respectively
In.Upper spacer 5c and lower spacer 5f will be evenly spaced between each 5a into diaphragm, it can be ensured that the spacing between the adjacent 5a into diaphragm
It is equal, can ensure each into diaphragm 5a accurate positionings on suspended axle 5b or connecting shaft 5e by the positioning of jump ring 5d, it is ensured that outstanding
Each quality for being maintained at vertical state into diaphragm 5a, improving falling liquid film after extension.
The two ends of suspended axle 5b are arranged with the suspension groove 5b1 of undergauge, and suspension groove 5b1 is stuck in J-hook 6
In, the distribution of J-hook 6 has the semicircular base being adapted with suspension groove 5b1, is upwardly extended on front side of each semicircular base
To the top higher than suspended axle 5b, the rear side of each semicircular base is connect under liquid distributor housing 4c higher than front side and being connected to
Side.Suspension groove 5b1 is stuck in the semicircular base of J-hook 6 so that suspended axle 5b obtains axially position in J-hook 6, together
When suspended axle 5b can freely be rotated in J-hook 6 so that falling liquid film sub-assembly 5 is positively retained at vertically under Gravitative Loads
State, and belong to stable equilibrium, even if the lower end of falling liquid film sub-assembly 5 swings, quick recoverable to catenary, it is ensured that it is each into
Diaphragm 5a is in vertical state.Top of the front side of J-hook 6 higher than suspended axle 5b both ensure that the reliability of suspension, and just
J-hook 6 is snapped in suspended axle 5b, or takes out suspended axle 5b from J-hook 6, be conveniently replaceable falling liquid film sub-assembly 5, or will
Falling liquid film sub-assembly 5 takes out cleaning.
As shown in figure 5, each into multiple semicircular splicing breach 5a7 are evenly distributed with the top of diaphragm 5a, each splicing lacks
Mouth 5a7 is corresponded and coaxial line with the falling liquid film bar seam 5a1 of lower section respectively.
As shown in fig. 6, splicing breach 5a7 can be V-notch, the tip of V-notch is stitched with the falling liquid film bar of lower section respectively
5a1 is corresponded and coaxial line.
The splicing breach 5a7 of semicircle or V-arrangement is easy to accept the melt that top falls, melt under gravity, to half
The lowest part flowing of circular or V-notch, the axis of automatic alignment lower section falling liquid film bar seam 5a1 falls so that melt accurately enters
In falling liquid film bar seam 5a1 and form uniform film.
As shown in fig. 7, each falling liquid film bar seam 5a1 can be uniformly divided into more than two sections along short transverse by bar seam parting bead 5a2.By
In falling liquid film bar seam, 5a1 is long easily causes deformation, bar is stitched both sides and is difficult to ensure that being substantially parallel or be definitely maintained at same puts down
In face, the bar for setting multiple connection falling liquid film bar seam 5a1 both sides along the elevation of each falling liquid film bar seam 5a1 stitches parting bead 5a2, can keep
In the case that total falling liquid film is highly constant, reduce every section of fluting of bar seam highly, it is ensured that falling liquid film bar seam 5a1 shapes from top to bottom it is steady
It is fixed, after melt blocks through bar seam parting bead 5a2, film more uniformly can be formed in the bar seam of lower section, improve the equal of falling liquid film
Evenness and stability.
As shown in Fig. 8 to Figure 10, liquid distributor 4 is respectively connect respectively including the adapter 4a with cylinder coaxial line, adapter
The upper end open of 4a, the bottom of adapter 4a is provided with dismountable distribution plate 4b, is distributed with distribution plate 4b and each splicing breach
The one-to-one liquid distributing hole 4b1 of 5a7.The section of adapter 4a can be square, or circular.The adapter 4a of the top
The melt that is fallen from feed pipe 3 of undertaking, the adapter 4a of lower section accepts the melt fallen from top falling liquid film sub-assembly 5；Melt enters
After entering adapter 4a, the liquid distributing hole 4b1 from distribution plate 4b forms multi beam and synchronously flows out, below liquid distributing hole 4b1 alignments
Splicing breach 5a7, therefore form film from the falling liquid film bar seam 5a1 of each comfortable film forming piece 5a of melt beam of liquid distributing hole 4b1 outflows.
Melt viscosity is smaller, and the diameter of liquid distributing hole 4b1 is also smaller, and distribution plate 4b is detachable, is easy to change distribution the need for according to product
Plate 4b.
Respectively connecing liquid distributor 4 also includes covering on meet liquid distributor housing 4c on the outside of adapter 4a, connects liquid distribution dress
The adapter heating chamber 4d that closing is formed between the inwall of housing 4c and the lateral wall of adapter 4a is put, liquid distributor housing is connect
The external end head of 4c is provided with and is connected to the flange plate 4e on cylinder 1, and the axis of flange plate 4e hangs down with the axis of adapter 4a
It is straight intersecting；Temperature-measuring port 4f, electrically heated rod mouthful 4g and heating agent expansion hatch 4h are connected with flange plate 4e.
Connect liquid distributor 4 and be horizontally inserted cylinder lumen, when flange plate 4e is fixed on cylinder body outer wall, adapter 4a
Just with cylinder coaxial line, by flange plate 4e dismountings easy to connect, it is easy to that distribution plate 4b is changed or cleared up.Connect liquid
Conduction oil is full of in pipe heating chamber 4d, temperature-measuring port 4f is a sleeve pipe for inner termination closing, can detect adapter heating chamber 4d
Temperature and can online change thermometric component；Electrically heated rod is right from electrically heated rod mouthful 4g insertion adapter heating chambers 4d
Conduction oil is heated, and can be arranged as required to one or more electrically heated rods mouthful 4g.Heating agent expansion hatch 4h expands with heating agent
Groove is connected, to adjust the change of heating agent volume in adapter heating chamber 4d.
The inner chamber of adapter 4a is also provided with heating coil, to improve heating intensity, makes the temperature of melt more uniform.
Positioned at the liquid distributing hole aperture of lower floor successively more than the liquid distributing hole aperture of last layer.More toward lower floor, the viscosity of melt is got over
Greatly, the aperture of liquid distributing hole 4b1 increases successively, is conducive to melt smoothly to flow out.
Feed pipe 3 extends along the axis of cylinder 1, and the lower end of feed pipe 3 is provided with umbrella outlet, flat outlet or melt
Distributor.It is easy to melt to be covered with distribution plate 4b rapidly, it is ensured that melt uniformly can synchronously flow out from each liquid distributing hole 4b1.
The lower section of each falling liquid film sub-assembly 5 is separately installed with vacuum sampler 7, and the external end head of each vacuum sampler 7 is solid respectively
It is scheduled on sample tap seat 1c, each sample tap seat 1c is connected on the barrel of cylinder 1.By vacuum sampler 7 can to from
The melt of the outflow of falling liquid film sub-assembly 5 carries out assay, and adjusts temperature, the pressure and other parameters in cylinder 1 according to analysis data.
The method that the present invention carries out melt polymerization using melt polymerization falling film reactor, in turn includes the following steps：Melt
Enter the inner chamber of cylinder 1 from feed pipe 3, fall into first in top layer adapter 4a, while heated by adapter 4a peripheries heating agent,
While from the synchronous uniform outflows of each liquid distributing hole 4b1 of top layer adapter bottom distribution plate 4b, corresponding positioned at liquid distributing hole
In the splicing breach 5a7 into diaphragm 5a immediately below 4b1, then respectively since the bottom outflow correspondence of splicing breach 5a7 enters position
In falling liquid film bar seam 5a1 immediately below splicing breach 5a7, film is formed in each falling liquid film bar seam 5a1, melt is high in cylinder lumen
There is polymerisation in the presence of temperature, the small molecule product that polymerisation is produced constantly is removed and from cylinder from the both sides of film
The vacuum port 1a in portion is extracted；Melt film be polymerized devolatilization while continue along each falling liquid film bar seam 5a1 slowly flow downwards,
Until after being heated again in the adapter 4a of next layer of entrance, mixed, being redistributed, in the falling liquid film bar of next composition diaphragm 5a
Film is formed again in seam 5a1, so repeats falling liquid film devolatilization until melt increases from the bottom outflow of the composition diaphragm of bottom one 5a
Melt after viscous is discharged from the discharging opening 1b of cylinder body bottom.
The present invention forms film by stitching 5a1 in each falling liquid film bar into diaphragm 5a, because the wall thickness into diaphragm 5a is very thin, accounts for
According to space very little, thus one group of falling liquid film sub-assembly 5 can have it is multiple also just there are multiple falling liquid films into diaphragm 5a, it is and traditional
Extratubal falling film is compared, and greatly expands the area of falling liquid film, melt is had a great specific surface area, and each film two faces
All in high-temperature space, the small molecule product that polymerisation is produced can constantly be removed and from cylinder from the both sides of film
The vacuum port 1a in portion is extracted, and substantially increases devolatilization efficiency and the devolatilization uniformity, while playing energy-saving effect.
The foregoing is only the preferable possible embodiments of the present invention, non-therefore limitation patent protection model of the invention
Enclose.In addition to the implementation, the present invention can also have other embodiment.The skill that all use equivalents or equivalent transformation are formed
Art scheme, all falls within the protection domain of application claims.Technical characteristic of the present invention without description can be by or using now
There is technology to realize, will not be repeated here.
Claims (15)
1. a kind of cylinder of melt polymerization falling film reactor, including vertical cylinder, the cylinder that is covered over of the cylinder adds
Thermal, the top center of the cylinder is provided with feed pipe, and the top of the cylinder is provided with vacuum port, the taper of the cylinder
Bottom is provided with discharging opening, it is characterised in that：The inner chamber of the cylinder is provided with least one set of falling liquid film unit, the falling liquid film list vertically
Unit includes connecing liquid distributor and positioned at the falling liquid film sub-assembly connect below liquid distributor respectively, and the falling liquid film sub-assembly includes many
Piece parallel to tubular axis into diaphragm, it is each it is described be parallel to each other into diaphragm and uniform intervals are set, it is each described on diaphragm points
It is not provided with along the falling liquid film bar seam extended into diaphragm length direction.
2. melt polymerization falling film reactor according to claim 1, it is characterised in that：The falling liquid film bar seam is along each into diaphragm
Width be respectively equipped with multiple tracks, each road falling liquid film bar seam is parallel to each other and uniform intervals.
3. melt polymerization falling film reactor according to claim 2, it is characterised in that：Each falling liquid film bar seam is along height side
More than two sections are uniformly divided into by bar seam parting bead.
4. melt polymerization falling film reactor according to claim 1, it is characterised in that：Before and after each upper end into diaphragm
Upper lug is respectively provided on two sides with, the center of each upper lug is respectively equipped with pin-and-hole, and two suspended axles being parallel to each other are worn successively
Cross and respectively go up pin-and-hole accordingly into diaphragm, by each into diaphragm series connection is for one group and is suspended in the cylinder.
5. melt polymerization falling film reactor according to claim 4, it is characterised in that：Before and after each lower end into diaphragm
Lower lug is respectively provided on two sides with, the center of each lower lug is respectively equipped with lower pin-and-hole, and two connecting shafts being parallel to each other are worn successively
Cross and respectively descend pin-and-hole that each lower end into diaphragm is mutually permanently connected accordingly into diaphragm.
6. melt polymerization falling film reactor according to claim 5, it is characterised in that：It is each it is described between diaphragm by length
The equal upper spacer of degree and lower spacer are spaced, and each upper spacer is set on the suspended axle, it is each it is described under every
Set is set in the connecting shaft, and jump ring is respectively equipped with positioned at the outermost upper pin-and-hole into diaphragm and lower pin-and-hole outside,
The jump ring is inlaid in the jump-ring slot of the suspended axle or connecting shaft respectively.
7. melt polymerization falling film reactor according to claim 4, it is characterised in that：The two ends of the suspended axle symmetrically set
There is the suspension groove of undergauge, the suspension groove is stuck in J-hook, the J-hook distribution has and the suspension
The semicircular base that groove is adapted, extends upwardly to the top higher than the suspended axle on front side of each semicircular base,
The rear side of each semicircular base is higher than front side and is connected to the lower section for connecing liquid distributor.
8. melt polymerization falling film reactor according to claim 2, it is characterised in that：Each top into diaphragm is uniform
Be distributed with the splicing breach of multiple semicircle or V-arrangements, each splicing breach corresponded with the falling liquid film bar seam of lower section respectively and
Coaxial line.
9. melt polymerization falling film reactor according to claim 8, it is characterised in that：Each liquid distributor that connects is distinguished
Including the adapter with the cylinder coaxial line, the upper end open of the adapter, the bottom of the adapter is provided with detachably
Distribution plate, be distributed with the distribution plate and each one-to-one liquid distributing hole of splicing breach.
10. melt polymerization falling film reactor according to claim 9, it is characterised in that：Liquid distributor is connect described in each also
Connect liquid distributor housing on the outside of the adapter including covering on, the inwall for connecing liquid distributor housing connects liquid with described
The adapter heating chamber of closing is formed between the lateral wall of pipe, the external end head for connecing liquid distributor housing is provided with and is connected to
Flange plate on the cylinder, the axis of the flange plate intersects vertically with the axis of the adapter；The blind flange
Temperature-measuring port, electrically heated rod mouth and heating agent expansion hatch are connected with plate.
11. melt polymerization falling film reactors according to claim 9, it is characterised in that：The inner chamber of the adapter is provided with
Heating coil.
12. melt polymerization falling film reactors according to claim 1, it is characterised in that：Under each falling liquid film sub-assembly
Side is separately installed with vacuum sampler, and the external end head of each vacuum sampler is separately fixed on sample tap seat, each described to take
Sample mouthful seat is connected on the barrel of the cylinder.
13. melt polymerization falling film reactors according to claim 9, it is characterised in that：Positioned at the liquid distributing hole aperture of lower floor
Successively more than the liquid distributing hole aperture of last layer.
14. melt polymerization falling film reactors according to claim 1, it is characterised in that：The cylinder heater is to add
Thermal jacket or half pipe heater.
Melt polymerization falling film reactor any one of a kind of 15. use claims 9 to 14 carries out the side of melt polymerization
Method, it is characterised in that in turn include the following steps：Melt enters cylinder lumen from feed pipe, falls into first in top layer adapter,
While heated by adapter periphery heating agent, while from each liquid distributing hole synchronization uniform flow of top layer adapter bottom distribution plate
Go out, correspond in the splicing breach into diaphragm immediately below liquid distributing hole, then respectively since the bottom of splicing breach
In the falling liquid film bar seam that outflow correspondence enters immediately below splicing breach, film is formed in each falling liquid film bar seam, melt is in cylinder
There is polymerisation in the presence of the high temperature of inner chamber, the small molecule product that polymerisation is produced constantly removed from the both sides of film and from
The vacuum port on cylinder top is extracted；Melt film is polymerized devolatilization while continuing slowly to be flowed downwards along each falling liquid film bar seam
It is dynamic, until into after being heated again in next layer of adapter, mix, redistribute, in the falling liquid film bar of next composition diaphragm
Film is formed in seam again, falling liquid film devolatilization is so repeated up to melt from the bottom outflow of the composition diaphragm of bottom one, after thickening
Melt discharged from the discharging opening of cylinder body bottom.
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| CN102527316A (en) * | 2010-12-28 | 2012-07-04 | 上海杰事杰新材料(集团)股份有限公司 | Umbrella falling film polycondensation reactor |
| CN102746499A (en) * | 2012-07-27 | 2012-10-24 | 浙江尤夫高新纤维股份有限公司 | Polycondensation kettle for falling film outside vertical tube |
| 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 |
| CN105536663A (en) * | 2016-01-29 | 2016-05-04 | 扬州惠通化工技术有限公司 | Vertical type stirred-free polymerization reactor |
| CN105561905A (en) * | 2016-02-23 | 2016-05-11 | 扬州惠通化工技术有限公司 | Esterification and polymerization two-kettle system |
| CN206652502U (en) * | 2017-04-01 | 2017-11-21 | 扬州瑞邦化工技术有限公司 | A kind of melt polymerization falling film reactor |
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2017
- 2017-04-01 CN CN201710213570.2A patent/CN106861591B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102527316A (en) * | 2010-12-28 | 2012-07-04 | 上海杰事杰新材料(集团)股份有限公司 | Umbrella falling film polycondensation reactor |
| CN102746499A (en) * | 2012-07-27 | 2012-10-24 | 浙江尤夫高新纤维股份有限公司 | Polycondensation kettle for falling film outside vertical tube |
| 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 |
| CN105536663A (en) * | 2016-01-29 | 2016-05-04 | 扬州惠通化工技术有限公司 | Vertical type stirred-free polymerization reactor |
| CN105561905A (en) * | 2016-02-23 | 2016-05-11 | 扬州惠通化工技术有限公司 | Esterification and polymerization two-kettle system |
| CN206652502U (en) * | 2017-04-01 | 2017-11-21 | 扬州瑞邦化工技术有限公司 | A kind of melt polymerization falling film reactor |
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| CN106861591B (en) | 2022-09-23 |
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