CN106861591B - Melt polymerization falling film reactor and method for carrying out melt polymerization - Google Patents
Melt polymerization falling film reactor and method for carrying out melt polymerization Download PDFInfo
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- CN106861591B CN106861591B CN201710213570.2A CN201710213570A CN106861591B CN 106861591 B CN106861591 B CN 106861591B CN 201710213570 A CN201710213570 A CN 201710213570A CN 106861591 B CN106861591 B CN 106861591B
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- 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 invention relates to a melt polymerization falling film reactor and a melt polymerization method, comprising a cylinder body, wherein the top of the cylinder body is provided with a feeding pipe, the upper part of the cylinder body is provided with a vacuum port, the bottom of the cylinder body is provided with a discharge port, the inner cavity of the cylinder body is provided with at least one group of falling film units along the axial direction, the falling film units respectively comprise a liquid receiving distribution device and a falling film assembly positioned below the liquid receiving distribution device, the falling film assembly comprises a plurality of film forming sheets parallel to the axis of the cylinder body, the film forming sheets are mutually parallel and uniformly arranged at intervals, and falling film strip slits extending along the length direction of the film forming sheets are respectively arranged on the film forming sheets. Each film forming sheet can be provided with a plurality of falling film strip gaps, and each falling film strip gap can be divided into a plurality of sections. The melt polymerization process comprises the steps of: the melt enters the liquid receiving pipe from the feeding pipe, flows out from the liquid distribution holes of the distribution plate after being heated, correspondingly falls into the material receiving gap of the film forming sheet, and then correspondingly enters the falling film strip slit to form a film, and the steps are repeated. The invention can enlarge the falling film area and improve the devolatilization efficiency.
Description
Technical Field
The invention relates to a polymerization reactor, in particular to a melt polymerization falling film reactor; the invention also relates to a method for melt polymerization by adopting the melt polymerization falling film reactor, belonging to the technical field of polymer production.
Background
At the initial stage of melt polymerization, namely when the melt viscosity is 50-200 Pa.s, the molecular weight of the polymer is low, the viscosity of the system is not high, and stirring, mixing, heat transfer, mass transfer (discharging of low-molecular by-products) and the like are not difficult; at the later stage of polymerization, namely when the melt viscosity is 200-4000 Pa.s, the melt fluidity is poor, the liquid film is weakened, and the heat transfer and mass transfer are very difficult.
The polymerization of fuse-element divide into intermittent type polymerization and continuous polymerization, the intermittent type polymerization device adopts vertical area stirred reation kettle, carry out the growth of molecular chain under vacuum state, the horizontal reation kettle of area stirring is adopted to the continuous device, the stirring form has two kinds of cage and disc type, two kinds of polymerization modes all need set up stirring, machine seal, bearing etc. along with the increase of fuse-element viscosity, stirring power also needs corresponding increase, energy consumption and equipment maintenance expense corresponding increase, the polymerization later stage, the fuse-element is easily rotatory together with the agitator to produce certain blind spot, fuse-element viscosity is inhomogeneous, cause the degradation serious, the color and luster turns yellow. In addition, the traditional falling film is usually carried out on the outer wall of a pipeline or the inner wall of a cylinder, the specific surface area of the falling film is small, and only single-side devolatilization can be realized.
The polymerization reaction is a reversible reaction, if a condition influencing the balance, such as concentration, temperature, pressure and the like, is changed, the reaction can be carried out towards the direction of increasing the polymerization degree, and in the polymerization process, small molecular products generated by the polymerization reaction are continuously removed from a melt to break the reaction balance and further increase the molecular weight; the unconverted monomers are removed from the high-viscosity system at the end of the polymerization in order to ensure the quality of the melt, both of which involve devolatilization of the high-viscosity melt.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a falling film reactor for melt polymerization, which can enlarge the falling film area of a melt and improve the devolatilization efficiency.
In order to solve the technical problems, the melt polymerization falling film reactor comprises a vertical cylindrical barrel, wherein a barrel heating device covers the periphery of the barrel, a feeding pipe is installed in the center of the top of the barrel, a vacuum port is formed in the upper portion of the barrel, a discharge port is formed in the conical bottom of the barrel, at least one group of falling film units are axially arranged in the inner cavity of the barrel, each falling film unit comprises a liquid receiving distribution device and a falling film assembly located below the liquid receiving distribution device, each falling film assembly comprises a plurality of film forming sheets parallel to the axis of the barrel, the film forming sheets are parallel to each other and are uniformly arranged at intervals, and falling film strip slits extending in the length direction of the film forming sheets are respectively arranged on the film forming sheets.
Compared with the prior art, the invention has the following beneficial effects: the melt enters the inner cavity of the cylinder body from the feeding pipe, firstly falls into the top layer liquid-containing distribution device, is heated in the liquid-containing distribution device, flows out of the falling film assembly towards the lower side, falls on the top of each film-forming piece in a one-to-one correspondence manner and correspondingly enters each falling film strip slit, a film is formed in each falling film strip slit, the melt is subjected to polymerization reaction under the action of high temperature of the inner cavity of the cylinder body, and small molecular products generated by the polymerization reaction are continuously removed from the two sides of the film and are extracted from a vacuum port at the upper part of the cylinder body; the melt film continuously flows downwards slowly along each falling film strip slit while being polymerized and devolatilized until entering a next layer of liquid receiving and distributing device to be heated, mixed and redistributed again, then the film is formed again in the falling film strip slit of the next component film sheet, the falling film devolatilization is repeated until the melt flows out from the bottom of the lowest component film sheet, and the melt after the viscosity increase is discharged from a discharge hole at the bottom of the cylinder body. The film is formed by the falling film strip seams of the film forming pieces, and the film forming pieces are very thin in wall thickness and very small in occupied space, so that a group of falling film assembly can be provided with a plurality of film forming pieces and a plurality of falling films.
As an improvement of the invention, the falling film strip gaps are respectively provided with a plurality of falling film strip gaps along the width direction of each film forming sheet, and the falling film strip gaps are mutually parallel and are uniformly spaced. Each film forming sheet can form a plurality of films extending along the vertical direction, so that the area of the film on each film forming sheet can be increased by several times, and the devolatilization efficiency is further improved.
As a further improvement of the invention, each falling film strip gap is uniformly divided into more than two sections by a strip gap parting strip along the height direction. Because the falling film strip seam is too long and is easy to deform, the two sides of the strip seam are difficult to ensure to be completely parallel or absolutely kept in the same plane, a plurality of strip seam parting strips connected with the two sides of the falling film strip seam are arranged along the elevation of each falling film strip seam, the slotting height of each section of strip seam can be reduced under the condition of keeping the total falling film height unchanged, the stability of the shape of the falling film strip seam from top to bottom is ensured, the melt is retarded by the strip seam parting strips, a film can be formed in the strip seam below more uniformly, and the uniformity and the stability of the falling film are improved.
As a further improvement of the invention, the front side and the rear side of the upper end of each membrane forming piece are respectively provided with an upper lug, the center of each lug is respectively provided with an upper pin hole, two parallel suspension shafts sequentially penetrate through the corresponding upper pin holes of each membrane forming piece, and the membrane forming pieces are connected in series to form a group and are suspended in the cylinder. Two parallel suspension shafts penetrate into upper lugs at the upper ends of the film forming sheets, the upper ends of the film forming sheets are suspended in the inner cavity of the cylinder, the lower ends of the film forming sheets are suspended by self weight and are in a stable balanced state, falling film strip seams on the film forming sheets can be automatically ensured to be parallel to the axis of the cylinder, and a uniform film can be formed on the falling film strip seams by a melt.
As a further improvement of the invention, the front side and the rear side of the lower end of each film forming sheet are respectively provided with a lower lug, the center of each lower lug is respectively provided with a lower pin hole, and two mutually parallel connecting shafts sequentially penetrate through the corresponding lower pin holes of each film forming sheet to fixedly connect the lower ends of the film forming sheets with each other. The lower ends of the membrane forming pieces are fixed into a whole through the connecting shaft, so that the integrity of the falling film assembly can be improved, the integral suspension dead weight is increased, the rigidity of each membrane forming piece is improved, and the lower ends of the individual membrane forming pieces are prevented from being deviated.
As a further improvement of the invention, the membrane forming plates are mutually spaced by upper spacer bushes and lower spacer bushes which are equal in length, the upper spacer bushes are respectively sleeved on the suspension shaft, the lower spacer bushes are respectively sleeved on the connecting shaft, snap springs are respectively arranged on the outer sides of an upper pin hole and a lower pin hole of the membrane forming plate positioned on the outermost side, and the snap springs are respectively embedded in a snap spring groove of the suspension shaft or the connecting shaft. The upper spacer bush and the lower spacer bush uniformly separate the film forming sheets, so that the equal distance between the adjacent film forming sheets can be ensured, the accurate positioning of the film forming sheets on the suspension shaft or the connecting shaft can be ensured through the positioning of the snap spring, the film forming sheets are ensured to be kept in a vertical state after being suspended, and the quality of the falling film is improved.
As a further improvement of the invention, two ends of the suspension shaft are symmetrically provided with reduced hanging grooves, the hanging grooves are respectively clamped in J-shaped hooks, the J-shaped hooks are distributed with semicircular bottoms matched with the hanging grooves, the front side of each semicircular bottom extends upwards to be higher than the top of the suspension shaft, and the rear side of each semicircular bottom is higher than the front side and is connected below the liquid receiving and distributing device. Hang the groove card and make the suspension shaft obtain axial positioning in J-shaped couple in the semicircular bottom of J-shaped couple, suspension shaft can freely rotate in J-shaped couple simultaneously for the falling film sub-assembly can keep at vertical state under the dead weight effect, and belongs to stable balance, even the lower extreme of falling film sub-assembly takes place the swing, can reply the plumb line rapidly, ensures that each film forming piece is in vertical state. The front side of the J-shaped hook is higher than the top of the suspension shaft, so that the suspension reliability is ensured, the suspension shaft can be conveniently clamped into the J-shaped hook, or the suspension shaft can be taken out from the J-shaped hook, the falling film assembly can be conveniently replaced, or the falling film assembly can be conveniently taken out and cleaned.
As a further improvement of the invention, a plurality of semicircular or V-shaped material receiving notches are uniformly distributed on the top of each membrane forming piece, and each material receiving notch corresponds to the falling film strip seam below one by one and is coaxial. The semicircular or V-shaped material receiving notch is convenient for receiving melt falling from the upper part, and the melt flows to the lowest part of the semicircular or V-shaped notch under the action of gravity and automatically falls by aiming at the axis of the falling film strip slit at the lower part, so that the melt accurately enters the falling film strip slit and forms an even film.
As a further improvement of the invention, each liquid receiving and distributing device comprises a liquid receiving pipe coaxial with the cylinder body, the upper end of the liquid receiving pipe is opened, the bottom of the liquid receiving pipe is provided with a detachable distributing plate, and liquid distributing holes corresponding to the material receiving notches one by one are distributed on the distributing plate. The liquid receiving pipe at the uppermost end receives the melt falling from the feeding pipe, and the liquid receiving pipe at the lower end receives the melt falling from the falling film assembly at the upper part; after the melt enters the liquid receiving pipe, a plurality of beams synchronously flow out from the liquid distribution holes on the distribution plate, and the melt beams flowing out from the liquid distribution holes respectively form a film in the falling film strip seam of the film forming sheet because the liquid distribution holes are aligned with the receiving notch below. The smaller the melt viscosity is, the smaller the diameter of the liquid distribution hole is, and the distribution plate can be detached, so that the distribution plate can be conveniently replaced according to the needs of products.
As a further improvement of the invention, each liquid receiving and distributing device further comprises a liquid receiving and distributing device shell covering the outer side of the liquid receiving tube, a closed liquid receiving tube heating cavity is formed between the inner wall of the liquid receiving and distributing device shell and the outer side wall of the liquid receiving tube, the outer end of the liquid receiving and distributing device shell is provided with a flange cover plate connected to the cylinder body, and the axis of the flange cover plate is perpendicularly intersected with the axis of the liquid receiving tube; the flange cover plate is connected with a temperature measuring port, an electric heating rod port and a heating medium expansion port. Connect liquid distributor horizontal insertion barrel inner chamber, when the blind flange is fixed on the barrel outer wall, connect the liquid pipe just in time and barrel coaxial line, connect convenient dismantlement through the blind flange, be convenient for change or clear up the distribution plate. The heating cavity of the liquid receiving pipe is filled with heat conducting oil, and the temperature measuring port is a sleeve with a closed inner end head, so that the temperature of the heating cavity of the liquid receiving pipe can be detected, and temperature measuring components can be replaced on line; the electric heating rod is inserted into the liquid receiving pipe heating cavity from the electric heating rod port to heat the heat conducting oil, and one or more electric heating rod ports can be arranged as required; the heating medium expansion port is connected with the heating medium expansion groove to adjust the change of the volume of the heating medium in the heating cavity of the liquid receiving pipe.
As a further improvement of the invention, the inner cavity of the liquid receiving pipe is provided with a heating coil. The heating intensity can be improved, and the temperature of the melt is more uniform.
As a further improvement of the present invention, a vacuum sampler is respectively installed below each falling film assembly, the outer end of each vacuum sampler is respectively fixed on a sampling port seat, and each sampling port seat is respectively connected to the cylinder wall of the cylinder. The melt flowing out of the falling film assembly can be tested and analyzed through the vacuum sampler, and the temperature, the pressure and other parameters in the cylinder body can be adjusted according to test data.
As a further improvement of the invention, the aperture of the liquid distribution holes positioned at the lower layer is sequentially larger than that of the liquid distribution holes positioned at the upper layer. The lower the layer, the higher the viscosity of the melt, and the aperture of the liquid distribution hole is increased in sequence, which is beneficial to the smooth outflow of the melt.
As a further improvement of the invention, the cylinder heating device is a heating jacket or a half-pipe heater.
Another object of the present invention is to overcome the problems of the prior art and to provide a method for melt polymerization using a melt polymerization falling film reactor, which can form a very large film-reducing area for the melt, improve devolatilization efficiency, and reduce energy consumption.
In order to solve the technical problems, the method for carrying out melt polymerization by using the melt polymerization falling film reactor sequentially comprises the following steps: the melt enters the inner cavity of the cylinder body from the feeding pipe, firstly falls into the top layer liquid receiving pipe, is heated by a heat medium at the periphery of the liquid receiving pipe, synchronously and uniformly flows out of all liquid distribution holes of a distribution plate at the bottom of the top layer liquid receiving pipe, correspondingly falls into the liquid receiving notches of the membrane forming plates positioned right below the liquid distribution holes one by one, respectively flows out of the bottoms of the liquid receiving notches and correspondingly enters falling film strip seams positioned right below the liquid receiving notches, a thin film is formed in each falling film strip seam, the melt generates polymerization reaction under the action of high temperature of the inner cavity of the cylinder body, and small molecular products generated by the polymerization reaction are continuously removed from two sides of the thin film and are extracted from a vacuum port at the upper part of the cylinder body; the melt film continuously flows downwards slowly along each falling film strip slit while being polymerized and devolatilized until entering a liquid receiving pipe of the next layer to be heated, mixed and redistributed again, then the film is formed again in the falling film strip slit of the next component membrane, the falling film devolatilization is repeated in this way until the melt flows out from the bottom of the lowest component membrane, and the melt after the viscosity increase is discharged from a discharge hole at the bottom of the cylinder body.
Compared with the prior art, the invention has the following beneficial effects: the film is formed by the falling film strip seams of the film forming pieces, and the film forming pieces are very thin in wall thickness and very small in occupied space, so that a group of falling film assembly can be provided with a plurality of film forming pieces and a plurality of falling films.
Drawings
The invention will be described in further detail with reference to the following drawings and detailed description, which are provided for reference and illustration purposes only and are not intended to limit the invention.
FIG. 1 is a schematic structural diagram of a falling film reactor for melt polymerization according to the present invention.
Figure 2 is a schematic diagram of the falling film assembly of figure 1.
Fig. 3 is an enlarged view of a portion a in fig. 2.
Fig. 4 is a schematic structural diagram of a membrane forming sheet in a falling film assembly.
Fig. 5 is an enlarged view of a portion B in fig. 4.
Fig. 6 is a schematic view of the material receiving notch of the film forming sheet in a V shape.
FIG. 7 is a schematic view of a second embodiment of a film forming sheet.
Fig. 8 is a schematic structural view of the liquid receiving and distributing device in fig. 1.
Fig. 9 is a top view of fig. 8.
Fig. 10 is a schematic view of a second embodiment of the receiving and dispensing device.
Fig. 11 is a view taken along line C in fig. 8.
In the figure: 1. a barrel; 1a, a vacuum port; 1b, a discharge hole; 1c, a sampling port seat; 2. a heating jacket; 3. a feeding pipe; 4. a liquid receiving and distributing device; 4a, a liquid receiving pipe; 4b, a distribution plate; 4b1. liquid distribution holes; 4c, a liquid receiving and distributing device shell; 4d, heating the liquid receiving pipe; 4e, a flange cover plate; 4f, a temperature measuring port; 4g, electrically heating a rod mouth; 4h, heating medium expansion ports; 5. a falling film assembly; 5a, forming a membrane; 5a1. falling film strip seam; 5a2. slit parting strips; 5a3. upper lug; 5a4. pin holes; 5a5. lower lug; 5a6. lower pin holes; 5a7. material receiving notch; 5b, hanging the shaft; 5b1, hanging a groove; 5c, arranging a spacer bush; 5d, clamping springs; 5e, connecting the shaft; 5f, lower spacer bush; 6, J-shaped hooks; 7. and (4) a vacuum sampler.
Detailed Description
As shown in fig. 1 to 4, the melt polymerization falling film reactor of the present invention comprises a vertical cylindrical barrel 1, wherein a barrel heating device is covered on the periphery of the barrel 1, and the barrel heating device is a heating jacket 2 or a half-pipe heater. The top of the cylinder body 1 is a flat cover or an end socket, a feeding pipe 3 is installed in the center of the top of the cylinder body 1, a vacuum port 1a is formed in the upper portion of the cylinder body 1, a discharging port 1b is formed in the conical bottom of the cylinder body 1, a falling film unit is axially arranged in the inner cavity of the cylinder body 1, and the falling film unit can be one group, two groups or more than three groups. The falling film unit comprises a liquid receiving and distributing device 4 and a falling film assembly 5 positioned below the liquid receiving and distributing device 4 respectively, the falling film assembly 5 comprises a plurality of film forming sheets 5a parallel to the axis of the cylinder body, the film forming sheets 5a are arranged in parallel and at uniform intervals, and falling film strip slits 5a1 extending along the length direction of the film forming sheets are arranged on the film forming sheets 5a respectively. The cylinder body 1 can be divided into a plurality of sections according to needs, each section is connected through a flange, the falling film assembly 5 can be assembled conveniently, if the diameter of the cylinder body is large, the cylinder body can be made into a whole, a manhole is arranged between the sections, and the falling film assembly 5 can be assembled conveniently.
The melt enters the inner cavity of the cylinder body from the feeding pipe 3, firstly falls into the top layer liquid-receiving distribution device 4, is heated in the liquid-receiving distribution device 4, flows out of the falling film assembly 5 downwards, falls on the top of each film-forming sheet 5a in a one-to-one correspondence manner and enters each falling film strip slit 5a1 in correspondence manner, a film is formed in each falling film strip slit 5a1, the melt is subjected to polymerization reaction under the action of high temperature of the inner cavity of the cylinder body, and small molecular products generated by the polymerization reaction are continuously removed from two sides of the film and are extracted from a vacuum port 1a at the upper part of the cylinder body; the melt film continues to flow downwards slowly along each falling film strip slit 5a1 while being polymerized and devolatilized until entering the next layer of liquid receiving and distributing device 4 to be heated, mixed and redistributed again, then the film is formed again in the falling film strip slit 5a1 of the next film forming piece 5a, the falling film devolatilization is repeated in this way until the melt flows out from the bottom of the film forming piece 5a in the lowest group, and the melt after the thickening is discharged from a discharge port 1b at the bottom of the cylinder.
The plurality of falling film strip slits 5a1 are provided along the width direction of each film forming sheet 5a, and the falling film strip slits 5a1 are parallel to each other and are uniformly spaced. A plurality of films extending along the vertical direction can be formed on each film forming piece 5a, so that the area of the film on each film forming piece 5a can be increased by several times, and the devolatilization efficiency is further improved.
The front side and the rear side of the upper end of each film forming piece 5a are respectively provided with an upper lug 5a3, the center of each upper lug 5a3 is respectively provided with an upper pin hole 5a4, two parallel suspension shafts 5b sequentially penetrate through the corresponding upper pin holes 5a4 of each film forming piece 5a, and the film forming pieces 5a are connected in series into a group and suspended in the cylinder 1. Two parallel suspension shafts 5b penetrate into upper lugs 5a3 at the upper end of each film forming sheet 5a, the upper end of each film forming sheet 5a is suspended in the inner cavity of the cylinder, the lower end of each film forming sheet 5a hangs down by self weight and is in a stable balanced state, falling film strip slits 5a1 on each film forming sheet 5a can be automatically ensured to be parallel to the axis of the cylinder 1, and the melt can form a uniform film on the falling film strip slits 5a1.
The front and back sides of the lower end of each film forming piece 5a are respectively provided with a lower lug 5a5, the center of each lower lug 5a5 is respectively provided with a lower pin hole 5a6, and two mutually parallel connecting shafts 5e sequentially penetrate through the corresponding lower pin holes 5a6 of each film forming piece 5a to fixedly connect the lower ends of the film forming pieces 5a with each other. The lower ends of the film forming sheets 5a are fixed into a whole through a connecting shaft 5e, so that the integrity of the falling film assembly 5 can be improved, the integral suspension dead weight is increased, the rigidity of each film forming sheet 5a is improved, and the lower ends of the individual film forming sheets 5a are prevented from being deviated.
The membrane forming pieces 5a are mutually spaced through upper spacer bushes 5c and lower spacer bushes 5f which are equal in length, the upper spacer bushes 5c are respectively sleeved on the suspension shafts 5b, the lower spacer bushes 5f are respectively sleeved on the connecting shaft 5e, snap springs 5d are respectively arranged on the outer sides of the upper pin holes 5a4 and the lower pin holes 5a6 of the membrane forming pieces 5a which are positioned on the outermost sides, and the snap springs 5d are respectively embedded in snap spring grooves of the suspension shafts 5b or the connecting shaft 5e. The upper spacer 5c and the lower spacer 5f uniformly separate the film forming sheets 5a, so that the equal spacing between the adjacent film forming sheets 5a can be ensured, the accurate positioning of the film forming sheets 5a on the suspension shaft 5b or the connecting shaft 5e can be ensured through the positioning of the snap spring 5d, the suspended film forming sheets 5a are ensured to be kept in a vertical state, and the quality of the falling film is improved.
The two ends of the hanging shaft 5b are symmetrically provided with reducing hanging grooves 5b1, the hanging grooves 5b1 are clamped in the J-shaped hooks 6 respectively, the J-shaped hooks 6 are provided with semicircular bottoms matched with the hanging grooves 5b1, the front side of each semicircular bottom extends upwards to be higher than the top of the hanging shaft 5b, and the rear side of each semicircular bottom is higher than the front side and is connected below the liquid receiving and distributing device shell 4c. The hanging groove 5b1 is clamped at the semicircular bottom of the J-shaped hook 6, so that the hanging shaft 5b obtains axial positioning in the J-shaped hook 6, meanwhile, the hanging shaft 5b can freely rotate in the J-shaped hook 6, the falling film assembly 5 can be kept in a vertical state under the action of self weight, the stable balance is achieved, even if the lower end of the falling film assembly 5 swings, the hanging line can be quickly restored, and the film forming sheets 5a are ensured to be in a vertical state. The front side of the J-shaped hook 6 is higher than the top of the hanging shaft 5b, so that the hanging reliability is ensured, the hanging shaft 5b is conveniently clamped into the J-shaped hook 6, or the hanging shaft 5b is taken out from the J-shaped hook 6, the falling film assembly 5 is conveniently replaced, or the falling film assembly 5 is taken out for cleaning.
As shown in fig. 5, a plurality of semicircular material receiving notches 5a7 are uniformly distributed on the top of each film forming sheet 5a, and each material receiving notch 5a7 is in one-to-one correspondence with the falling film strip slits 5a1 below and coaxial with the falling film strip slits.
As shown in fig. 6, the material receiving notch 5a7 may be a V-shaped notch, and the tip of the V-shaped notch is respectively corresponding to the falling film strip slits 5a1 below one by one and coaxial.
The semicircular or V-shaped material receiving notch 5a7 is convenient for receiving melt falling from above, the melt flows to the lowest part of the semicircular or V-shaped notch under the action of gravity and automatically falls towards the axis of the falling film strip slit 5a1 below, so that the melt accurately enters the falling film strip slit 5a1 and forms a uniform film.
As shown in fig. 7, each falling film strip slit 5a1 can be divided into two or more sections uniformly in the height direction by a strip slit divider 5a2. Because the falling film strip slits 5a1 are easy to deform due to overlong length, the two sides of the strip slits are difficult to ensure to be completely parallel or absolutely kept in the same plane, a plurality of strip slit parting strips 5a2 connected with the two sides of the falling film strip slits 5a1 are arranged along the elevation of each falling film strip slit 5a1, the slotting height of each section of strip slit can be reduced under the condition of keeping the total falling film height unchanged, the stability of the shape of the falling film strip slit 5a1 from top to bottom is ensured, the melt is retarded by the strip slit parting strips 5a2, a thin film can be formed in the strip slits below more uniformly, and the uniformity and the stability of the falling film are improved.
As shown in fig. 8 to 10, each liquid receiving and distributing device 4 includes a liquid receiving tube 4a coaxial with the cylinder, an upper end of the liquid receiving tube 4a is open, a detachable distributing plate 4b is disposed at the bottom of the liquid receiving tube 4a, and liquid distributing holes 4b1 corresponding to the material receiving notches 5a7 are distributed on the distributing plate 4b. The cross section of the liquid receiving tube 4a may be square or circular. The uppermost liquid receiving pipe 4a receives the melt falling from the feeding pipe 3, and the lower liquid receiving pipe 4a receives the melt falling from the upper falling film assembly 5; after the melt enters the liquid receiving pipe 4a, a plurality of beams synchronously flow out from the liquid distribution holes 4b1 on the distribution plate 4b, and because the liquid distribution holes 4b1 are aligned with the receiving notches 5a7 below, the melt beams flowing out from the liquid distribution holes 4b1 respectively form a film in the falling film strip slits 5a1 of the film forming sheet 5a. The smaller the melt viscosity is, the smaller the diameter of the liquid distribution hole 4b1 is, and the distribution plate 4b can be detached, so that the distribution plate 4b can be replaced according to the needs of products.
Each liquid receiving and distributing device 4 further comprises a liquid receiving and distributing device shell 4c covering the outer side of the liquid receiving pipe 4a, a closed liquid receiving pipe heating cavity 4d is formed between the inner wall of the liquid receiving and distributing device shell 4c and the outer side wall of the liquid receiving pipe 4a, a flange cover plate 4e connected to the barrel body 1 is arranged at the outer end of the liquid receiving and distributing device shell 4c, and the axis of the flange cover plate 4e is perpendicularly intersected with the axis of the liquid receiving pipe 4 a; the flange cover plate 4e is connected with a temperature measuring port 4f, an electric heating rod port 4g and a heating medium expansion port 4h.
Connect liquid distributor 4 level to insert the barrel inner chamber, when flange apron 4e was fixed on the barrel outer wall, connect liquid pipe 4a just in time and barrel coaxial line, connect convenient the dismantlement through flange apron 4e, be convenient for change or clear up distribution plate 4b. The liquid receiving pipe heating cavity 4d is filled with heat conducting oil, the temperature measuring port 4f is a sleeve with a closed inner end, the temperature of the liquid receiving pipe heating cavity 4d can be detected, and a temperature measuring component can be replaced on line; the electric heating rod is inserted into the liquid receiving pipe heating cavity 4d from the electric heating rod port 4g to heat the heat conducting oil, and one or more electric heating rod ports 4g can be arranged as required. The heating medium expansion port 4h is connected to a heating medium expansion tank to adjust the change in volume of the heating medium in the liquid receiving pipe heating chamber 4d.
The inner cavity of the liquid receiving pipe 4a can be also provided with a heating coil to improve the heating intensity and make the temperature of the melt more uniform.
The aperture of the liquid distribution hole positioned on the lower layer is sequentially larger than that of the liquid distribution hole positioned on the upper layer. The lower the layer, the higher the viscosity of the melt, and the sequentially increased aperture of the liquid distribution holes 4b1, which is beneficial to the smooth outflow of the melt.
The feed pipe 3 extends along the axis of the barrel 1, and the lower end of the feed pipe 3 is provided with an umbrella-shaped outlet, a flat outlet or a melt distributor. The distribution plate 4b is convenient for the melt to be quickly distributed and ensures that the melt can uniformly and synchronously flow out from each liquid distribution hole 4b1.
A vacuum sampler 7 is respectively arranged below each falling film assembly 5, the outer end head of each vacuum sampler 7 is respectively fixed on a sampling port seat 1c, and each sampling port seat 1c is respectively connected on the cylinder wall of the cylinder body 1. The melt flowing out of the falling film assembly 5 can be analyzed by a vacuum sampler 7, and the temperature, pressure and other parameters in the cylinder 1 can be adjusted according to the analysis data.
The invention discloses a method for carrying out melt polymerization by using a melt polymerization falling film reactor, which sequentially comprises the following steps: the melt enters the inner cavity of the cylinder body 1 from the feeding pipe 3, firstly falls into the top liquid receiving pipe 4a, is heated by a heat medium at the periphery of the liquid receiving pipe 4a, simultaneously and uniformly flows out of all liquid distribution holes 4b1 of the bottom distribution plate 4b of the top liquid receiving pipe, and correspondingly falls into the material receiving notches 5a7 of the membrane forming piece 5a positioned right below the liquid distribution holes 4b1 one by one, then respectively flows out of the bottom of the material receiving notches 5a7 and correspondingly enters the falling film strip slits 5a1 positioned right below the material receiving notches 5a7, a film is formed in all the falling film strip slits 5a1, the melt is subjected to polymerization reaction under the action of high temperature of the inner cavity of the cylinder body, and small molecular products generated by the polymerization reaction are continuously removed from two sides of the film and are extracted from the vacuum port 1a at the upper part of the cylinder body; the melt film continues to slowly flow downwards along each falling film strip slit 5a1 while undergoing polymerization and devolatilization until entering the next layer of liquid receiving pipe 4a to be heated again, mixed and redistributed, then the film is formed again in the falling film strip slit 5a1 of the next film forming piece 5a, the falling film devolatilization is repeated in such a way until the melt flows out from the bottom of the film forming piece 5a in the lowest group, and the melt after the tackification is discharged from a discharge port 1b at the bottom of the cylinder body.
According to the invention, the film is formed through the falling film strip slits 5a1 of each film forming piece 5a, and the film forming pieces 5a are very thin in wall thickness and small in occupied space, so that a group of falling film assembly 5 can be provided with a plurality of film forming pieces 5a and a plurality of falling films.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention. In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention. Technical features of the present invention which are not described may be implemented by or using the prior art, and will not be described herein.
Claims (13)
1. The utility model provides a fuse-element polymerization falling film reactor, includes vertical cylindric barrel, the periphery of barrel covers there is barrel heating device, the inlet pipe is installed at the top center of barrel, the upper portion of barrel is equipped with the vacuum mouth, the toper bottom of barrel is equipped with discharge gate, its characterized in that: the falling film unit comprises a liquid receiving distribution device and a falling film assembly positioned below the liquid receiving distribution device, the falling film assembly comprises a plurality of film forming sheets parallel to the axis of the cylinder body, the film forming sheets are parallel to each other and are uniformly arranged at intervals, and falling film strip slits extending along the length direction of the film forming sheets are arranged on the film forming sheets;
the falling film strip gaps are respectively provided with a plurality of channels along the width direction of each film forming sheet, and the falling film strip gaps are parallel to each other and are uniformly spaced;
the top of each film forming piece is uniformly distributed with a plurality of semicircular or V-shaped material receiving notches, and each material receiving notch is respectively in one-to-one correspondence with the falling film strip seam below and has a coaxial line.
2. The melt polymerization falling film reactor of claim 1, wherein: each falling film strip slit is evenly divided into more than two sections by strip slit parting strips along the height direction.
3. The melt polymerization falling film reactor of claim 1, wherein: the front side and the rear side of the upper end of each membrane forming piece are respectively provided with an upper lug, the center of each lug is respectively provided with an upper pin hole, two parallel suspension shafts sequentially penetrate through the corresponding upper pin holes of each membrane forming piece, and the membrane forming pieces are connected in series to form a group and are suspended in the cylinder.
4. The melt polymerization falling film reactor of claim 3, wherein: the front side and the rear side of the lower end of each film forming sheet are respectively provided with a lower lug, the center of each lower lug is respectively provided with a lower pin hole, and two mutually parallel connecting shafts sequentially penetrate through the corresponding lower pin holes of each film forming sheet to fixedly connect the lower ends of the film forming sheets with each other.
5. The melt polymerization falling film reactor of claim 4, wherein: the membrane forming plates are mutually spaced through upper spacer bushes and lower spacer bushes which are equal in length, the upper spacer bushes are respectively sleeved on the suspension shaft, the lower spacer bushes are respectively sleeved on the connecting shaft, snap springs are respectively arranged on the outer sides of an upper pin hole and a lower pin hole of the membrane forming plate located on the outermost side, and the snap springs are respectively embedded in snap spring grooves of the suspension shaft or the connecting shaft.
6. The melt polymerization falling film reactor of claim 3, wherein: the hanging device is characterized in that reducing hanging grooves are symmetrically arranged at two ends of the hanging shaft and are respectively clamped in J-shaped hooks, the J-shaped hooks are provided with semicircular bottoms matched with the hanging grooves, the front side of each semicircular bottom extends upwards to be higher than the top of the hanging shaft, and the rear side of each semicircular bottom is higher than the front side and is connected below the liquid receiving and distributing device.
7. The melt polymerization falling film reactor of claim 1, wherein: each liquid receiving and distributing device comprises a liquid receiving pipe coaxial with the barrel, the upper end of the liquid receiving pipe is provided with an opening, the bottom of the liquid receiving pipe is provided with a detachable distributing plate, and liquid distributing holes corresponding to the liquid receiving notches one to one are distributed on the distributing plate.
8. The melt polymerization falling film reactor of claim 7, wherein: each liquid receiving and distributing device further comprises a liquid receiving and distributing device shell covering the outer side of the liquid receiving pipe, a closed liquid receiving pipe heating cavity is formed between the inner wall of the liquid receiving and distributing device shell and the outer side wall of the liquid receiving pipe, a flange cover plate connected to the cylinder body is arranged at the outer end of the liquid receiving and distributing device shell, and the axis of the flange cover plate is vertically intersected with the axis of the liquid receiving pipe; the flange cover plate is connected with a temperature measuring port, an electric heating rod port and a heating medium expansion port.
9. The melt polymerization falling film reactor of claim 7, wherein: and a heating coil is arranged in the inner cavity of the liquid receiving pipe.
10. The melt polymerization falling film reactor of claim 1, wherein: and a vacuum sampler is respectively arranged below each falling film assembly, the outer end of each vacuum sampler is respectively fixed on a sampling port seat, and each sampling port seat is respectively connected on the cylinder wall of the cylinder body.
11. The melt polymerization falling film reactor of claim 7, wherein: the aperture of the liquid distribution hole positioned on the lower layer is sequentially larger than that of the liquid distribution hole positioned on the upper layer.
12. The melt polymerization falling film reactor of claim 1, wherein: the cylinder heating device is a heating jacket or a half-pipe heater.
13. A method of melt polymerization using a melt polymerization falling film reactor according to any of claims 7 to 12, comprising the following steps in sequence: the melt enters the inner cavity of the cylinder body from the feeding pipe, firstly falls into the top liquid receiving pipe, is heated by a heat medium at the periphery of the liquid receiving pipe, synchronously and uniformly flows out from all liquid distribution holes of a distribution plate at the bottom of the top liquid receiving pipe, and correspondingly falls into the liquid receiving notches of the membrane forming plates positioned right below the liquid distribution holes one by one, and then respectively flows out from the bottoms of the liquid receiving notches and correspondingly enters falling film strip seams positioned right below the liquid receiving notches to form a film in all the falling film strip seams, the melt is subjected to polymerization reaction under the action of high temperature of the inner cavity of the cylinder body, and small molecular products generated by the polymerization reaction are continuously removed from two sides of the film and are extracted from a vacuum port at the upper part of the cylinder body; the melt film continuously flows downwards slowly along each falling film strip slit while being polymerized and devolatilized until entering a liquid receiving pipe of the next layer to be heated, mixed and redistributed again, then the film is formed again in the falling film strip slit of the next component membrane, the falling film devolatilization is repeated in this way until the melt flows out from the bottom of the lowest component membrane, and the melt after the viscosity increase is discharged from a discharge hole at the bottom of the cylinder body.
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| 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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| 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 |
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Address after: Building B9, Jinrong Yangzhou Science and Technology Park, No. 158, Ji'an South Road, Yangzhou High-tech Zone, Hanjiang District, Yangzhou City, Jiangsu Province 225127 Patentee after: Yangzhou Ruibang Technology Development Co.,Ltd. Address before: Building B9, Jinrong Yangzhou Science and Technology Park, No. 158, Ji'an South Road, Yangzhou High-tech Zone, Hanjiang District, Yangzhou City, Jiangsu Province 225127 Patentee before: YANGZHOU RUIBANG CHEMICAL INDUSTRY TECHNIQUE |