CN105854734A - Row-up pipe film falling melt phase polycondensation method for preparing high-viscosity melt and reactor thereof - Google Patents
Row-up pipe film falling melt phase polycondensation method for preparing high-viscosity melt and reactor thereof Download PDFInfo
- Publication number
- CN105854734A CN105854734A CN201610302101.3A CN201610302101A CN105854734A CN 105854734 A CN105854734 A CN 105854734A CN 201610302101 A CN201610302101 A CN 201610302101A CN 105854734 A CN105854734 A CN 105854734A
- Authority
- CN
- China
- Prior art keywords
- liquid film
- falling liquid
- pipe
- tube
- melt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1887—Stationary reactors having moving elements inside forming a thin film
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/32—Packing elements in the form of grids or built-up elements for forming a unit or module inside the apparatus for mass or heat transfer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
- B01J2219/00085—Plates; Jackets; Cylinders
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses relates to a row-up pipe film falling melt phase polycondensation method for preparing high-viscosity melt and a reactor thereof. The row-up pipe film falling melt phase polycondensation method is characterized in that melt monomer blend or pre-polymer forms waterfall-type film falling flow among row-up inter-pipe film falling support pipes to realize melt polycondensation, melt falls off the pipes and gathers to the bottom of the reactor for further stirring and uniformizing, and materials are discharged after reaction. The reactor used in this method is of integral vertical structure and comprises a shell, a heating medium tank at the upper end, inter-pipe film falling support pipes connected with the heating medium tank, a material tank, a bottom shell at the lower end, and a blender and so on. The film falling support pipes with inner pipes inside are vertically hung and rowed up, and orifices are communicated with the heating medium tank for flowing of the heating medium. The reactor has the advantages of low flowing resistance, no dead corners, large filming area, and fast surface upgrading, and plug flow is realized. Moreover, the reactor is applicable to melt polycondensation of high-viscosity melt such as PET.
Description
Technical field
The present invention relates to a kind of falling film type melt polycondensation reaction method in high glutinous polymer production and melt polycondensation reaction equipment.
Background technology
Polycondensation reaction is a reversible balanced reaction, carrying out along with polycondensation reaction, little molecule compounds needs to get rid of timely and effectively reaction system, so that polymer molecular weight improves constantly, including polyethylene terephthalate (PET), PTT (PTT), polybutylene terephthalate (PBT) (PBT), PEN (PEN), polyamide (PA) and Merlon (PC) etc. including polymer all by polycondensation reaction prepare.The implementation of polycondensation reaction mainly has melt polycondensation, solid phase polycondensation, a solution polycondensation etc., wherein melt polycondensation because its reaction efficiency is high, flow process is short, energy-conserving and environment-protective and meet the advantages such as flexibility large-scale production and be widely adopted.During melt-polycondensation produces the glutinous material of height, carrying out along with reaction, reaction system viscosity sharply increases, the little molecule generated is got rid of more and more difficult, mass transfer becomes the governing factor of process, and therefore using the high-quality polycondensation reaction equipment being provided that big mass transfer specific surface area is the key implementing efficient melt polycondensation.
According to melt polycondensation reaction feature, in polycondensation reactor, melt need to have and good flows into film properties so that forming the melt films that thickness is suitable, and maintain bigger film forming area, the thickest meeting of melt films causes little molecule removing difficulty, and melt films is the thinnest, and melt can be made long and degrade at inner member superficial residence time；The design of reactor inner member is constantly mixed to strengthen as far as possible the interface of melt films and is updated while need to ensureing melt flows；Additionally, the time of staying that material is in reactor requires the homogeneous controlled heavy polymer obtaining required narrow ditribution with this.Therefore, preferably melt polycondensation reaction device should meet Flow of Goods and Materials is laminar flow, without dead band, the mass transfer area obtained in unit interval maximizes with the ratio (film forming efficiency) of volume of material, Surface Renewal is fast, and the diffusion path of little molecule is short matches to adapt to the requirement in differential responses stage with transitivity change with polymerization process.
Presently disclosed vertical falling-film melt polycondensation reaction device has the tower polycondensation reactor of screen, extratubal falling film polycondensation reactor etc..Tube sheet tower reactor relies primarily on the design of inner member and makes fused materials film forming on pipe or plate surface texture, its film forming area and Surface Renewal frequency have raised relative to the polycondensation reactor of tradition Horizontal stirring, but its embedding structure is complicated, it is easily generated stagnant area, cause melt to be degraded, the application producing the glutinous material of height has difficulties.Extratubal falling film reactor can make material trickle downwards along tube outer surface film-like, owing to material is natural to dirty by gravity, the problem not havinging blocking, this kind of reactor has that structure is relatively easy, mass transfer interface is big and the reaction temperature advantage such as uniformly, but owing to the liquid film of wall-attachment free falling-film flowing presents the VELOCITY DISTRIBUTION of semi-parabolic type from inside to outside, the top layer speed of melt films is much larger than near wall region, and the outer membrane time of staying is too short and the inner layer film time of staying is long.
Summary of the invention
First purpose of the present invention is for the deficiencies in the prior art, a kind of falling liquid film melt polycondensation reaction method between one-tenth comb preparing melt with high viscosity is provided, reaction temperature uniform, controllable can be made, effectively it is expanded into membrane area, improve melt film forming efficiency and the Surface Renewal of melt, strengthening melt flows becomes the homogeneity of film uniformity and the time of staying, raising polycondensation reaction efficiency and height to stick the product quality of material.To this end, propose techniques below scheme；
. a kind of falling liquid film melt polycondensation reaction method between one-tenth comb, it is characterized in that: described method uses falling liquid film between the heat-exchange tube being configured with arranged in rows to prop up the reactor of stay tube, during between the pipe of arranged in rows, falling liquid film props up stay tube, between pipe, falling liquid film props up stay tube is proximity association, and tube pitch is 0.1 with the ratio of caliber
~ 20, make melt material when flowing downward, between the pipe of arranged in rows, falling liquid film props up and is connected to curtain between stay tube, between pipe, falling liquid film props up formation waterfall shape film evaporation device between stay tube, and carry out melt polycondensation reaction, volatilize small-molecule substance from the two sides of described waterfall shape falling liquid film, improves material molecular melt amount.
Further, described material is when flowing downward, and the most also between described pipe, falling liquid film props up stay tube outer wall and forms extratubal falling film, and the melt material of waterfall shape film evaporation device that between described pipe, falling liquid film props up between stay tube is connected with the melt material of extratubal falling film.
It is a further object to provide falling liquid film melt polycondensation reaction device between a kind of one-tenth comb, reaction temperature uniform, controllable can be made, effectively it is expanded into membrane area, improve melt film forming efficiency and the Surface Renewal of melt, strengthening melt flows becomes the homogeneity of film uniformity and the time of staying, raising polycondensation reaction efficiency and height to stick the product quality of material.To this end, the present invention is by the following technical solutions:
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb, described reactor includes upright shell, it is characterized in that described reactor also includes that between the heat-exchange tube of arranged in rows, falling liquid film props up stay tube, it is arranged on the material material feeding box of upright shell upper end, the base plate of material material feeding box is cloth lamina membranacea, the falling liquid film of arranged in rows props up stay tube through cloth lamina membranacea, cloth lamina membranacea has film distribution structure, film distribution structure includes that between respective tube, falling liquid film props up the cloth film slit in region between stay tube, between pipe, falling liquid film props up stay tube is proximity association, make melt material when flowing downward, between the pipe of arranged in rows, falling liquid film props up and is connected to curtain between stay tube, between pipe, falling liquid film props up formation waterfall shape film evaporation device between stay tube, and carry out melt polycondensation reaction, volatilize small-molecule substance from the two sides of described waterfall shape falling liquid film, improve material molecular melt amount.
On the basis of using technique scheme, the present invention also can use technical scheme further below simultaneously, or uses these solution pool:
Prop up with falling liquid film between comb and between stay tube, be provided with or without connecting filament between the pipe of lateral connection adjacent two pipes, between two pipe pipes connecting filament radical be 0 ~
1000, a diameter of 0.1 mm ~ 20 mm, between pipe connecting filament radical be the tube pitch of 0 be 0.1 ~ 10 from the ratio with caliber, between pipe connecting filament radical be the tube pitch of 1 ~ 1000 be 0.1 ~ 20 from the ratio with caliber.
Falling liquid film between comb is become to prop up stay tube through cloth lamina membranacea right angle setting, cloth lamina membranacea is provided with multiple rows of film distribution structure, film distribution structure include for and pipe between falling liquid film support pipe and form the cloth film slit at position between the cloth fenestra in falling liquid film gap and respective tube, and slit connects with hole, the outer cloth film of stay tube is propped up for material melt falling liquid film between pipe in the space that falling liquid film props up between stay tube between cloth fenestra hole wall and pipe.
Upright shell is arranged over heating agent at material material feeding box and flows out casing and heating agent inflow casing, heating agent flows into casing and is provided with reactor Heating medium, heating agent flows out and responds the outlet of device heating agent on casing, and between the pipe of described arranged in rows, falling liquid film props up stay tube and flows into casing with heating agent and heating agent outflow casing communicates；Melt material inlet pipe flows out casing from heating agent and heating agent flows into casing and passes, and passes to material material feeding box；Upright shell top is provided with vacuum pumping opening, is provided with agitator in drain pan, and its power is incoming by bottom, is provided with material outlet bottom drain pan.
Between described pipe, falling liquid film props up stay tube employing outer tube sleeve inner tube structure, and inner tube flows out box cover plate with heating agent and communicates, and outer tube flows out casing lower shoe with heating agent and communicates.
Between described pipe falling liquid film prop up stay tube inner tube keep caliber constant, outer tube is straight-run of pipe or the coaxial straight tube of reducing, and the reducing trend of the coaxial straight tube of described reducing is that caliber diminishes from top to bottom.
Between described pipe, falling liquid film props up stay tube outer tube caliber is 2 ~ 30 mm, inner tube diameter is 1 ~
20 mm, outer tube caliber differs 1 ~ 10 mm with inner tube diameter.
Reactor sets heat transfer system and heat-insulation system, and heat transfer system includes that heating agent flows into casing, heating agent flows out casing and falling liquid film props up the circulation path that stay tube forms, and heating agent flows into casing and heating agent flows out and is respectively equipped with reactor Heating medium and the outlet of reactor heating agent on casing；Heat-insulation system includes housing chuck and the drain pan chuck that upright shell and drain pan and periphery thereof be respectively provided with, the upper and lower of housing chuck is respectively equipped with housing chuck Heating medium and the outlet of housing chuck heating agent, the upper and lower of drain pan chuck is respectively equipped with drain pan chuck Heating medium and the outlet of drain pan chuck heating agent, and the thermal medium of heat transfer system and heat-insulation system is passed to outside through Posterior circle operation is heated or cooled.
The present invention can be suitably used for the melt polycondensation reaction of the polymer such as polyethylene terephthalate (PET), PTT (PTT), polybutylene terephthalate (PBT) (PBT), PEN (PEN), polyamide (PA) and Merlon (PC).
The present invention is to stick the mass transfer feature of polycondensation reaction and height on the basis of fluid mechanics dynamics fully realizes, film evaporation device speed and VELOCITY DISTRIBUTION thereof and the strengthening melt interface mass transfer mentality of designing as technical solution is controlled according to melt with high viscosity film forming flow behavior, film forming area is improved with this, strengthen Surface Renewal and the time of staying homogeneity of melt, finally improve product quality.
The present invention uses the vertical pipes of in a row arrangement as falling liquid film support member between pipe, utilize material melt to have high viscosity and viscosity constantly increases the features such as the arrangement with falling liquid film support member, bigger film forming area can be maintained all the time, melt uniform film thickness, flow velocity reaches unanimity, and face keeps laminar flow to move under gravity forces, thus ensure that polymer molecular weight narrowly distributing, the product that continuous production can be excellent and stable can be realized, and the production efficiency of unit volume reactor is greatly increased.Further, arranging supporting wire between the pipe of adjacent two pipes, it for falling liquid film between the pipe of " waterfall " shape, can be strengthened the dispersion of melt and mix, and improves the Surface Renewal frequency of melt films, simultaneously the stability of waterfall shape can be played holding effect again.Reaction method of the present invention is simple and feasible, has and flows into that membrane area is big, Surface Renewal speed is fast, the time of staying is homogeneous controlled, and the series of advantages such as energy consumption is low, easy cleaning, can realize the high-effect melt polycondensation that Mass and heat transfer couples with chemical reaction.
Accompanying drawing explanation
Fig. 1 is the structural representation of embodiment 1 provided by the present invention.
Fig. 2 is the structural representation of embodiment 2 provided by the present invention.
Fig. 3 is the structural representation of embodiment 3 provided by the present invention.
Fig. 4 is cloth lamina membranacea pore cell schematic diagram.
Fig. 5 a is one of straight tube geometric layout schematic diagram passing cloth lamina membranacea of multiple rows of U-tube.
Fig. 5 b be multiple rows of U-tube straight tube through cloth lamina membranacea geometric layout schematic diagram two.
Fig. 5 c be multiple rows of U-tube straight tube through cloth lamina membranacea geometric layout schematic diagram three.
nullParts in figure、Position and numbering: reactor Heating medium 1，Feed pipe 2，Heating agent flows to casing 3，Heating agent flows out casing 4，Heating agent flows out box cover plate 41，Heating agent flows out casing lower shoe 42，Material material feeding box 5，Cloth lamina membranacea 51，Cloth fenestra 511，Cloth film slit 512，Housing chuck Heating medium 6，Upright shell 7，Housing chuck 8，Drain pan flange 9，Drain pan bolt 10，Drain pan chuck Heating medium 11，Drain pan 12，Drain pan chuck 13，Material outlet 14，Drain pan chuck heating agent outlet 15，Agitator 16，Housing chuck heating agent outlet 17，Falling liquid film props up stay tube 18，Outer tube 181，Inner tube 182，Connecting filament 183 between pipe，Vacuum pumping opening 19，Shell flange 20，Casing bolts 21，Reactor heating agent outlet 22，Melt material inlet pipe 23.
Detailed description of the invention
Embodiment 1, referring to the drawings 1,4,5a, 5b, 5c.
In the present embodiment, falling liquid film props up the outer tube 181 of stay tube 18 and uses the straight tube that caliber is constant.
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb preparing melt with high viscosity that the present embodiment is provided, as shown in Figure 1, it includes upright shell 7, it is connected to the material material feeding box of upright shell 7 upper end and the drain pan 12 of lower end, material material feeding box 5 is arranged over heating agent and flows out casing 4, flow out at heating agent and on casing 4, be provided with again heating agent inflow casing 3, heating agent flows into casing 3 and is provided with reactor Heating medium 1, heating agent flows out and responds device heating agent outlet 22 on casing 4, the falling liquid film of arranged in rows props up stay tube 18 and is connected to heating agent outflow casing 4 and heating agent inflow casing 3 to form heating agent circulation path, melt material inlet pipe 23 flows out casing 4 from heating agent and heating agent flows into casing 3 and passes, pass to material material feeding box 5；The base plate of material material feeding box 5 is cloth lamina membranacea 51, cloth lamina membranacea 51 has film distribution structure, upright shell 7 top are provided with vacuum pumping opening 19, and between pipe, falling liquid film props up and is provided with agitator 16 below stay tube 18, and its power is incoming by bottom, is provided with material outlet 14 bottom drain pan 12.
Described reactor includes that between the pipe of arranged in rows, falling liquid film props up stay tube 18, between pipe, falling liquid film props up stay tube is proximity association, make melt material when flowing downward, between the pipe of arranged in rows, falling liquid film props up and is connected to curtain between stay tube, between pipe, falling liquid film props up formation waterfall shape film evaporation device between stay tube, and carry out melt polycondensation reaction, volatilize small-molecule substance from the two sides of described waterfall shape falling liquid film, improves material molecular melt amount.
Between pipe, falling liquid film props up stay tube 18 right angle setting, and lower end is unsettled, often arranges falling liquid film between the pipe having more than and props up stay tube 18 proper alignment, and the axis propping up stay tube 18 with falling liquid film between row's all pipes is in same plane, is separated by between row and row with equidistant keeping parallelism.
Between described pipe, falling liquid film props up stay tube 18 is internal and external casing structure, and outer tube 181 flows out box cover plate 41 with heating agent and communicates, and inner tube 182 flows out casing lower shoe 42 with heating agent and communicates.
As preferably, between pipe, falling liquid film props up stay tube outer tube 181 external diameter is 2 ~ 30 mm, and inner tube external diameter is 1 ~ 20 mm, and it is 1 ~ 10 mm that outer tube caliber differs with inner tube diameter.
Between vertically arranged adjacent two pipes, falling liquid film props up and is provided with connecting filament 183 between horizontal pipe between stay tube 18 pipe, and between pipe, connecting filament 183 length props up the vertical range of stay tube 18 equal to falling liquid film between adjacent two pipes, as preferably, between pipe the radical of connecting filament 183 be 1 ~
1000, a diameter of 0.1 mm ~ 10 mm,
As preferably, between adjacent two pipes, falling liquid film props up the tube pitch of stay tube 18 is 0.1 ~ 20 from the ratio with the caliber of its outer tube 181.
In a row between the pipe of arrangement, falling liquid film props up stay tube 18 through cloth lamina membranacea 51 right angle setting, cloth lamina membranacea 51 is provided with multiple rows of film distribution structure, film distribution structure include for and pipe between falling liquid film prop up stay tube 18 formed falling liquid film gap cloth fenestra 511 and respective tube between the slit 512 at position, and slit 512 connects with hole 511, slit 512 is for making melt flow down with relatively thin thickness between pipe, as shown in Figure 4.Stay tube 18 outer cloth film is propped up for material melt falling liquid film between pipe in the space that falling liquid film props up between stay tube 18 between cloth fenestra hole wall and pipe, formation extratubal falling film flows, the melt material of waterfall shape film evaporation device that between described pipe, falling liquid film props up between stay tube 18 is connected with the melt material of extratubal falling film, increase film forming area the most further, and contribute to the one-tenth curtain stability of waterfall shape film evaporation device, and the viscosity that the material curtain between pipe can utilize material in turn is formed with facilitation to extratubal falling film laminar flow.
Often arrangement membrane structure has more than one cloth membrane pores unit, and each unit includes a hole 511 and a seam 512, and as preferably, hole wall is dentation, as shown in Figure 4, so that the space that between the hole wall in hole 51 and pipe, falling liquid film props up between stay tube is essentially slot.As preferably, the pipe end radius that the inner ring radius (R1) of slot props up stay tube straight tube with falling liquid film is identical, slot outer shroud radius (R2) is 0.1 ~ 10 mm with the difference of inner ring radius (R1), and the width (L1) of slit 512 is 0.1 ~ 10 mm, and length (L2) is 1 ~ 200 mm.
Fig. 5 a, 5b, 5c are respectively falling liquid film between multi coil and prop up the stay tube 18 several examples through cloth lamina membranacea geometric layout.Between neighbouring two groups of pipes of adjacent two rows, falling liquid film props up falling liquid film between four pipes of stay tube 18 and props up the summit, axis of stay tube and be connected to parallelogram.
As preferably, between the pipe of arranged in rows falling liquid film prop up the vertical range between row and row of stay tube 18 be 10 ~
200 mm, between pipe, falling liquid film props up the most overall right angle setting of stay tube 18.
Reactor has heat transfer system, flows into falling liquid film between casing 3, heating agent outflow casing 4 and pipe including heating agent and props up stay tube 18 and the circulation path of composition thereof, and heating agent flows into casing 3 and heating agent flows out and is respectively equipped with reactor Heating medium 1 and reactor heating agent outlet 22 on casing 4.
Reactor is provided with heat-insulation system, the housing chuck 8 being respectively provided with including upright shell 7 and drain pan 12 and periphery thereof and drain pan chuck 13, the upper and lower of housing chuck 8 is respectively equipped with housing chuck Heating medium 6 and housing chuck heating agent outlet 17, and the upper and lower of drain pan chuck 13 is respectively equipped with drain pan chuck Heating medium 11 and drain pan chuck heating agent outlet 15.
The thermal medium of heat transfer system and heat-insulation system is passed to outside through Posterior circle operation is heated or cooled.
The reactor top being made up of heating agent inflow casing 3, heating agent outflow casing 4 and material material feeding box 5 is connected by shell flange 20 and casing bolts 21 with upright shell 7, upright shell 7 is connected by drain pan flange 9 and drain pan bolt 10 with drain pan 12, it is simple to dismounting maintenance and installation.
The melt polycondensation process using above-mentioned polycondensation reactor is:
During reactor work, heating agent falling liquid film between pipe props up the inner tube port of stay tube and flows to, then flows out from outer tube port, is then circulated to polycondensation reactor outside through Posterior circle operation is heated or cooled.
Material inlet is positioned at heating agent and flows into directly over casing crown center, and molten monomer blend or prepolymer constantly inject from material inlet, and the heating agent that wore long flows into the feed pipe of casing and heating agent outflow casing and flows in material material feeding box.
Melt enters falling liquid film between the pipe of arranged in rows after the hole on cloth lamina membranacea distributes and supports area under control, falling liquid film is formed at the outer uniformly cloth film of pipe, " waterfall " shape film evaporation device is formed between pipe, carry out melt polycondensation reaction, between pipe, melt maintains certain thickness to flow through equally spaced connecting filament, and the little molecule that reaction generates is extracted out from vacuum pumping opening.
Melt falling liquid film between pipe props up between stay tube pipe after landing, finally converges to bottom polycondensation reactor, stirs reaction further through agitator and homogenizes material, completes reacted melt and discharges from the material outlet of reactor bottom.
Embodiment 2, referring to the drawings 2,4,5a, 5b, 5c.
In the present embodiment, between pipe, falling liquid film props up the outer tube 181 of stay tube 18 and uses the coaxial straight tube of reducing.
Between pipe, falling liquid film props up the outer tube 181 of stay tube 18 below cloth lamina membranacea 51 with equidistant interior reducing, becomes multistage diameter not once the logical straight tube of continuous phase, and the most each section coaxial, props up bottom stay tube 18 to falling liquid film between pipe below cloth lamina membranacea 51, and straight tube external diameter reduces the most piecemeal.
As preferably, outer tube 181 reducing hop count 2 ~ 100, below cloth lamina membranacea 51, first paragraph straight tube external diameter is 20 ~ 30 mm, near a diameter of 1 ~ 10mm of final stage straight tube of one end at the bottom of pipe.
On the outer tube 181 of reducing, between the pipe of each section of reducing outer tube, connecting filament 183 length tube pitch corresponding thereto keeps equal.
Other parts and the implementation of the present embodiment are same as in Example 1, in fig. 2, and the implication that representative that drawing reference numeral is identical with Fig. 1 is identical.
Embodiment 3, referring to the drawings 3,4,5a, 5b, 5c.
In the present embodiment, between pipe, falling liquid film props up the outer tube 181 of stay tube 18 is the straight tube that caliber is constant, and between adjacent two pipes, falling liquid film props up between stay tube without connecting filament between horizontal pipe.
As preferably, between adjacent tubes, falling liquid film props up the tube pitch of stay tube is 0.1 ~ 10 from the ratio with its caliber.
Other parts and the implementation of the present embodiment are same as in Example 1, in figure 3, and the implication that representative that drawing reference numeral is identical with Fig. 1 is identical.
The foregoing is only the specific embodiment of the present invention, but the architectural feature of the present invention is not limited thereto, any those skilled in the art is in the field of the invention, and change or the modification made all are contained among protection scope of the present invention.
Claims (10)
1. one kind becomes falling liquid film melt polycondensation reaction method between comb, it is characterized in that: described method uses falling liquid film between the heat-exchange tube being configured with arranged in rows to prop up the reactor of stay tube, during between the pipe of arranged in rows, falling liquid film props up stay tube, between pipe, falling liquid film props up stay tube is proximity association, tube pitch is 0.1 ~ 20 with the ratio of caliber, make melt material when flowing downward, between the pipe of arranged in rows, falling liquid film props up and is connected to curtain between stay tube, between pipe, falling liquid film props up formation waterfall shape film evaporation device between stay tube, and carry out melt polycondensation reaction, volatilize small-molecule substance from the two sides of described waterfall shape falling liquid film, improve material molecular melt amount.
2. falling liquid film melt polycondensation reaction method between a kind of one-tenth comb as claimed in claim 1, it is characterized in that: described material is when flowing downward, the most also between described pipe, falling liquid film props up stay tube outer wall and forms extratubal falling film, and the melt material of waterfall shape film evaporation device that between described pipe, falling liquid film props up between stay tube is connected with the melt material of extratubal falling film.
null3. one kind becomes falling liquid film melt polycondensation reaction device between comb，Described reactor includes upright shell (7)，It is characterized in that described reactor also includes that between the heat-exchange tube of arranged in rows, falling liquid film props up stay tube (18)、It is arranged on the material material feeding box (5) of upright shell (7) upper end，The base plate of material material feeding box (5) is cloth lamina membranacea (51)，The falling liquid film of arranged in rows props up stay tube (18) through cloth lamina membranacea (51)，Cloth lamina membranacea (5) has film distribution structure，Film distribution structure includes that between respective tube, falling liquid film props up cloth film slit (512) in region between stay tube，Between pipe, falling liquid film props up stay tube is proximity association，Make melt material when flowing downward，Between the pipe of arranged in rows, falling liquid film props up and is connected to curtain between stay tube，Between pipe, falling liquid film props up formation waterfall shape film evaporation device between stay tube，And carry out melt polycondensation reaction，Volatilize small-molecule substance from the two sides of described waterfall shape falling liquid film，Improve material molecular melt amount.
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb the most according to claim 3, it is characterized in that: prop up connecting filament (183) between the pipe being provided with or without adjacent two pipes of lateral connection between stay tube (18) with falling liquid film between comb, between two pipe pipes, connecting filament (183) radical is 0 ~ 1000, a diameter of 0.1 mm ~ 20 mm, between pipe connecting filament (183) radical be the tube pitch of 0 be 0.1 ~ 10 from the ratio with caliber, between pipe connecting filament (183) radical be the tube pitch of 1 ~ 1000 be 0.1 ~ 20 from the ratio with caliber.
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb the most according to claim 3, it is characterized in that: become falling liquid film between comb to prop up stay tube (18) through cloth lamina membranacea (51) right angle setting, cloth lamina membranacea (51) is provided with multiple rows of film distribution structure, film distribution structure include for and pipe between falling liquid film prop up stay tube (18) and form cloth film slit (512) at position between the cloth fenestra (511) in falling liquid film gap and respective tube, and slit connects with hole, the outer cloth film of stay tube is propped up for material melt falling liquid film between pipe in the space that falling liquid film props up between stay tube between cloth fenestra hole wall and pipe.
6. falling liquid film melt polycondensation reaction device between a kind of one-tenth comb as claimed in claim 2, it is characterized in that upright shell (7) is arranged over heating agent at material material feeding box (5) and flows out casing (4) and heating agent inflow casing (3), heating agent flows into casing (3) and is provided with reactor Heating medium (1), heating agent flows out and responds device heating agent outlet (22) on casing (4), and between the pipe of described arranged in rows, falling liquid film props up stay tube (18) and flows into casing (3) with heating agent and heating agent outflow casing (4) communicates；Melt material inlet pipe flows out casing (4) from heating agent and heating agent flows into casing (3) and passes, and passes to material material feeding box (5)；Upright shell (7) top is provided with vacuum pumping opening (19), and drain pan (12) bottom is provided with material outlet (14).
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb the most according to claim 3, it is characterized in that: between described pipe, falling liquid film props up stay tube (18) and uses outer tube (181) set inner tube (182) structure, inner tube (182) flows out box cover plate (41) with heating agent and communicates, and outer tube (181) flows out casing lower shoe (42) with heating agent and communicates.
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb the most according to claim 7, it is characterized in that: between described pipe falling liquid film prop up stay tube (18) inner tube (182) keep caliber constant, outer tube (181) is straight-run of pipe or the coaxial straight tube of reducing, the reducing trend of the coaxial straight tube of described reducing is that caliber diminishes from top to bottom.
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb the most according to claim 8, it is characterized in that: between described pipe, falling liquid film props up stay tube outer tube (181) caliber is 2 ~ 30 mm, inner tube (182) caliber is 1 ~ 20 mm, and outer tube (181) caliber differs 1 ~ 10 mm with inner tube (182) caliber.
Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb the most according to claim 3, it is characterized in that: reactor sets heat transfer system and heat-insulation system, heat transfer system includes that heating agent flows into casing (3), heating agent flows out casing (4) and falling liquid film props up the circulation path that stay tube (18) forms, and heating agent flows into casing (3) and heating agent flows out and is respectively equipped with reactor Heating medium (1) and reactor heating agent outlet (22) on casing (4)；Heat-insulation system includes housing chuck (8) and the drain pan chuck (13) that upright shell (7) and drain pan (12) and periphery thereof be respectively provided with, the upper and lower of housing chuck (8) is respectively equipped with housing chuck Heating medium (6) and housing chuck heating agent outlet (17), the upper and lower of drain pan chuck (13) is respectively equipped with drain pan chuck Heating medium (11) and drain pan chuck heating agent outlet (15), and the thermal medium of heat transfer system and heat-insulation system is passed to outside through Posterior circle operation is heated or cooled.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610302101.3A CN105854734B (en) | 2016-05-09 | 2016-05-09 | It is a kind of prepare melt with high viscosity into falling liquid film melt polycondensation reaction method and its reactor between comb |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610302101.3A CN105854734B (en) | 2016-05-09 | 2016-05-09 | It is a kind of prepare melt with high viscosity into falling liquid film melt polycondensation reaction method and its reactor between comb |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105854734A true CN105854734A (en) | 2016-08-17 |
| CN105854734B CN105854734B (en) | 2018-06-12 |
Family
ID=56630586
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610302101.3A Active CN105854734B (en) | 2016-05-09 | 2016-05-09 | It is a kind of prepare melt with high viscosity into falling liquid film melt polycondensation reaction method and its reactor between comb |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105854734B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107029637A (en) * | 2017-05-11 | 2017-08-11 | 浙江理工大学 | A kind of high viscosity fluid filming device |
| CN107442059A (en) * | 2017-08-08 | 2017-12-08 | 浙江理工大学 | A kind of falling liquid film melt polycondensation reaction device |
| CN110639461A (en) * | 2018-06-26 | 2020-01-03 | 浙江理工大学 | Falling film devolatilizer and falling film element thereof |
| CN110813225A (en) * | 2019-10-10 | 2020-02-21 | 浙江理工大学 | Melt polycondensation reactor and falling film element thereof |
| CN114790279A (en) * | 2021-01-26 | 2022-07-26 | 惠生工程（中国）有限公司 | Industrial production process method of polyglycolic acid oligomer |
| CN115193383A (en) * | 2022-06-01 | 2022-10-18 | 浙江理工大学 | Horizontal tube falling film melt polycondensation method and reactor and devolatilizer thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4235281A (en) * | 1978-04-07 | 1980-11-25 | The Boeing Company | Condenser/evaporator heat exchange apparatus and method of utilizing the same |
| EP0251839A1 (en) * | 1986-07-04 | 1988-01-07 | FIVES-CAIL BABCOCK, Société Anonyme | Upflow evaporator comprising a liquid-distribution device |
| CN103319728A (en) * | 2013-06-17 | 2013-09-25 | 浙江理工大学 | Melt polycondensation reaction method for preparing high-viscosity molten mass, and special reactor and falling film element used for same |
| CN103706135A (en) * | 2012-10-08 | 2014-04-09 | 俞天翔 | In-pipe vibration reciprocating spiral reciprocatingly cleaning type falling film evaporator |
-
2016
- 2016-05-09 CN CN201610302101.3A patent/CN105854734B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4235281A (en) * | 1978-04-07 | 1980-11-25 | The Boeing Company | Condenser/evaporator heat exchange apparatus and method of utilizing the same |
| EP0251839A1 (en) * | 1986-07-04 | 1988-01-07 | FIVES-CAIL BABCOCK, Société Anonyme | Upflow evaporator comprising a liquid-distribution device |
| CN103706135A (en) * | 2012-10-08 | 2014-04-09 | 俞天翔 | In-pipe vibration reciprocating spiral reciprocatingly cleaning type falling film evaporator |
| CN103319728A (en) * | 2013-06-17 | 2013-09-25 | 浙江理工大学 | Melt polycondensation reaction method for preparing high-viscosity molten mass, and special reactor and falling film element used for same |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107029637A (en) * | 2017-05-11 | 2017-08-11 | 浙江理工大学 | A kind of high viscosity fluid filming device |
| CN107029637B (en) * | 2017-05-11 | 2023-06-06 | 浙江理工大学 | High-viscosity fluid film distributor |
| CN107442059A (en) * | 2017-08-08 | 2017-12-08 | 浙江理工大学 | A kind of falling liquid film melt polycondensation reaction device |
| CN110639461A (en) * | 2018-06-26 | 2020-01-03 | 浙江理工大学 | Falling film devolatilizer and falling film element thereof |
| CN110639461B (en) * | 2018-06-26 | 2024-04-09 | 浙江理工大学 | Falling film devolatilizer and falling film element thereof |
| CN110813225A (en) * | 2019-10-10 | 2020-02-21 | 浙江理工大学 | Melt polycondensation reactor and falling film element thereof |
| CN110813225B (en) * | 2019-10-10 | 2022-06-03 | 浙江理工大学 | Melt polycondensation reactor and falling film element thereof |
| CN114790279A (en) * | 2021-01-26 | 2022-07-26 | 惠生工程（中国）有限公司 | Industrial production process method of polyglycolic acid oligomer |
| CN115193383A (en) * | 2022-06-01 | 2022-10-18 | 浙江理工大学 | Horizontal tube falling film melt polycondensation method and reactor and devolatilizer thereof |
| CN115193383B (en) * | 2022-06-01 | 2024-01-30 | 浙江理工大学 | Transverse tube falling film melt polycondensation method, reactor and devolatilizer thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105854734B (en) | 2018-06-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105854734A (en) | Row-up pipe film falling melt phase polycondensation method for preparing high-viscosity melt and reactor thereof | |
| CN209205310U (en) | Falling film type devolatilizer and its falling liquid film element | |
| CN103319705B (en) | Melt polycondensation reaction method, and reactor and falling film tube used for same | |
| CN105903424B (en) | A kind of multilayer falls tube type falling-film devolatilization reactor | |
| CN205815656U (en) | Falling liquid film melt polycondensation reaction device between a kind of one-tenth comb | |
| CN106000250B (en) | It is a kind of at falling liquid film melt polycondensation reaction method and its reactor between comb | |
| CN105561905A (en) | Esterification and polymerization two-kettle system | |
| CN105771868A (en) | Esterification and polymerization double-kettle apparatus | |
| CN207221901U (en) | A kind of modified reaction kettle of the esterification | |
| CN206980720U (en) | A kind of chemical industry reactor | |
| CN102527316A (en) | Umbrella falling film polycondensation reactor | |
| CN105734701A (en) | Extinction spinning production process for polylactic acid slice with titanium dioxide | |
| CN110639461B (en) | Falling film devolatilizer and falling film element thereof | |
| CN112871104B (en) | Falling film devolatilizer and falling film element thereof | |
| CN107442059A (en) | A kind of falling liquid film melt polycondensation reaction device | |
| CN205650186U (en) | Two cauldron systems of polymerization esterify | |
| CN105803565B (en) | PLA delustering fibre direct fabrics production technology | |
| CN105944647B (en) | A kind of efficient mass transfer, the gentle liquid-solid reactor device of extensive gas-liquid of heat transfer | |
| CN105536663B (en) | It is a kind of vertical without stirring polymer reactor | |
| CN105714391A (en) | Polylactic acid double-component composite fiber spinning process | |
| CN105734702B (en) | PLA delustering fibre direct fabrics system | |
| CN105080463B (en) | For the polycondensation reactor in the accomplished continuously or intermittently process units of production of polyester | |
| CN112090389B (en) | Reaction assembly and reactor with same | |
| CN205522385U (en) | Two ingredient composite fiber spinning production facilities of polylactic acid | |
| CN205650187U (en) | Esterify and get together two cauldron devices |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |