CN103319705B - Melt polycondensation reaction method, and reactor and falling film tube used for same - Google Patents
Melt polycondensation reaction method, and reactor and falling film tube used for same Download PDFInfo
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- CN103319705B CN103319705B CN201310241529.8A CN201310241529A CN103319705B CN 103319705 B CN103319705 B CN 103319705B CN 201310241529 A CN201310241529 A CN 201310241529A CN 103319705 B CN103319705 B CN 103319705B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
- B01J10/02—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor of the thin-film type
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/247—Suited for forming thin films
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/785—Preparation processes characterised by the apparatus used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
- C08G64/20—General preparatory processes
- C08G64/205—General preparatory processes characterised by the apparatus used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/04—Preparatory processes
-
- 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
- B01J2219/00078—Fingers
Abstract
The invention discloses a melt polycondensation reaction method which comprises steps as follows: a molten monomer blend or prepolymer slides down along the outer wall of a U tube to carry out polycondensation reaction, wherein a heat-transfer medium circularly flows in the U tube; molten masses in all U tubes are mixed at the lower part of a polycondensation reactor to be subjected to stirring reaction and mixing homogeneization; and the product is discharged after the reaction finishes. A polycondensation reactor for implementing the method comprises a vertical shell, an upper end socket, a lower end bottom shell, U tubes, a heat-transfer system, a film distributor, a helical ribbon stirrer and the like. The reactor has the advantages of simple structure, sufficient heat exchange, large film formation area, uniform reaction temperature, high polycondensation efficiency and the like, satisfies the plug flow in the process, and can be used for melt polycondensation reaction for producing polyethylene terephthalate, polytrimethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, polyamide, polycarbonate and the like.
Description
Technical field
The present invention relates to a kind of melt polycondensation reaction method and melt polycondensation reaction equipment and extratubal falling film element.
Background technology
Polycondensation implementation method has melt phase polycondensation, solution polycondensation, solid phase polycondensation and interfacial polycondensation etc., no matter wherein melt phase polycondensation all has obvious advantage from quality, economy, the feature of environmental protection and the industrializing implementation of product, therefore most polyester and polymeric amide etc. all adopt melt-polycondensation to produce, as polyethylene terephthalate (PET), Poly(Trimethylene Terephthalate) (PTT), polybutylene terephthalate (PBT), PEN (PEN), polymeric amide, polycarbonate etc.The Key of Implementation of melt phase polycondensation process is reactor, and desirable polycondensation reactor requirement Flow of Goods and Materials and admixture are good, and heat and mass efficiency is high, and process meets plug flow, to obtain the polymerization product of quality homogeneous, realizes higher polycondensation efficiency simultaneously.
At present, industrial final polycondensation reactor is commonly used Horizontal stirring reactor, mainly contains disc type and cage frame.This class reactor is limited by melt rack bridge, and disk or net sheet must keep larger distance, and the surface-area that causes unit volume melt to have is limited; Limited by structure of reactor, temperature of reaction is even not; Melt residence time in molten bath is grown and affected by statical head, unfavorable to polycondensation process; Inside reactor relies on molten metal pool level poor mobile, and still wall place flow condition is not good, has more dead band; And adhered to by a large amount of melts, stir shaft produces suitable winding degree, further increase glutinous equipment improvement space little.Particularly for the occasion of the high glutinous melt of preparation, its too much dead band, carry secretly, application that severely degrade that limited film forming and Surface Renewal and mistake long residence time cause has limited this class reactor.
Summary of the invention
First object of the present invention is for the deficiencies in the prior art, and a kind of melt polycondensation reaction method is provided, and can guarantee that temperature of reaction is even, improves film forming area, and dispersion and the mixing of strengthening melt, finally improve polycondensation efficiency and product quality.For this reason, the present invention is by the following technical solutions:
Heat-transfer medium is injected in polycondensation reactor from polycondensation reactor outside, then flows into the other end outflow from one end of film supplying tube, then flows out to polycondensation reactor outside by external heat or cooling rear circular flow; Described film supplying tube is U-shaped pipe, at right angle setting;
Molten monomer blend or prepolymer are injected into polycondensation reactor inside continuously from opening for feed, after film applicator distributes, rely on Gravitational sliding from U-shaped film supplying tube upper end along outer wall film forming;
Melt on each film supplying tube converges to polycondensation reactor bottom, further carries out stirring reaction with agitator, and homogenizing material, completes reacted melt and discharges from reactor bottom discharge port.
Another object of the present invention is to provide a kind of melt polycondensation reaction device that uses aforesaid method, by the key structure of appropriate design film applicator and falling liquid film element, agitator is installed, improve film forming efficiency, dispersion and the mixing of strengthening melt, finally improve polycondensation efficiency and product quality.For this reason, the present invention is by the following technical solutions:
A kind of melt polycondensation reaction device, comprise upright shell, be connected in the end socket of upright shell upper end and the drain pan of lower end, end socket top is provided with opening for feed, and upright shell top is provided with vacuum pumping opening, and drain pan bottom is provided with discharge port, it is characterized in that: in described reactor, be provided with film applicator, in described reactor, be also vertically installed with one or more extratubal falling film element, extratubal falling film element is U-shaped film supplying tube, and U-shaped film supplying tube below is provided with agitator;
Described melt polycondensation reaction device is provided with heat-transfer system, heat-transfer system comprises: upper box, U-shaped film supplying tube, lower box are communicated with the circulation path that forms heat-transfer medium successively, heat-transfer medium import and outlet are connected in respectively on upper box and lower box, one end of U-shaped film supplying tube is connected on upper box base plate and communicates with upper box, and the other end of U-shaped film supplying tube is connected to lower box base plate up and down casing and communicates.
Adopting on the basis of technique scheme, the present invention also can adopt following further technical scheme:
Described film applicator is the bin stock dish of Dual-layer structure, and upper strata base plate is drapery panel, and lower floor's base plate is cloth lamina membranacea, and drapery panel and cloth lamina membranacea all have hole, leaves described circular clearance between the hole wall in hole and film supplying tube.
In the present invention, described agitator is helical ribbon agitator, and the power of agitator imports into from drain pan bottom.
U-shaped film supplying tube adopts pipe; Or the straight part of U-shaped film supplying tube adopts bellows tube or corrugated tube; Or the epimere of the straight part of U-shaped film supplying tube is bellows tube or corrugated tube, hypomere is pipe.
Bellows tube is alternately made up of segmental arc and straight length, the difference of crest diameter and straight tube diameter and arc segment length (L
1) ratio be 0.05～1.0; Corrugated tube is selected circular arc type corrugated tube or scaling type corrugated tube or circular arc tangential line type corrugated tube or sinusoidal pattern corrugated tube, and the ratio of the difference of crest diameter and trough diameter and pitch (L) is 0.05～1.0.
The maximum outside diameter of U-shaped film supplying tube is 5～100mm, and the height of U-shaped film supplying tube is 0.5～30m.
The outer chuck that is with of upright shell, the bottom of chuck and top are respectively equipped with the import of jacket heat-preservation medium and jacket heat-preservation media outlet; The outer drain pan chuck that is with of drain pan, the bottom of drain pan chuck and top are respectively equipped with the import of drain pan thermal insulation medium and the outlet of drain pan thermal insulation medium.
End socket is connected by end socket joint flange, joint bolt with upright shell, and upright shell is connected by drain pan joint flange, drain pan joint bolt with drain pan, is convenient to field-strip, installation.
Upright shell inwall is provided with support ring for supporting the casing that film supplying tube, bin stock dish are housed.
The 3rd object of the present invention is to provide a kind of extratubal falling film element, can improve film forming efficiency, accurately controls temperature of reaction, simple in structure.For this reason, the present invention is by the following technical solutions:
Extratubal falling film element is U-shaped film supplying tube, in pipe, is heat-transfer medium path; U-shaped film supplying tube adopts pipe; Or the straight part of U-shaped film supplying tube adopts bellows tube or corrugated tube; Or the epimere of the straight part of U-shaped film supplying tube is bellows tube or corrugated tube, hypomere is pipe;
The difference of crest diameter and straight tube diameter and arc segment length (L
1) ratio be 0.05～1.0; Corrugated tube is selected circular arc type corrugated tube or scaling type corrugated tube or circular arc tangential line type corrugated tube or sinusoidal pattern corrugated tube, and the ratio of the difference of crest diameter and trough diameter and pitch (L) is 0.05～1.0.
The present invention can be for the melt polycondensation reaction of polyethylene terephthalate (PET), Poly(Trimethylene Terephthalate) (PTT), polybutylene terephthalate (PBT), PEN (PEN), polymeric amide, polycarbonate etc.
The present invention adopts the extratubal falling film element of U-shaped pipe as melt polycondensation reaction, and has heat-transfer medium to circulate in U-shaped pipe, and that this reactor has is simple in structure, film forming area is large, heat exchange is abundant, temperature of reaction is even; Simultaneously, below U-shaped film supplying tube, be provided with agitator, make likely to exist the melt of nature difference fully mix and disperse between same film supplying tube and different film supplying tube, and further react under agitation condition, improve quality stability and the homogeneity of melt.
The present invention, on the basis that the rheological characteristics of polycondensation process characteristic and polymer system is fully realized, provides different U-shaped film supplying tubes.Select pipe as film supplying tube, be conducive to flow for the glutinous melt of height, avoid producing and flow in " dead band ", prevent coking and color and luster flavescence; Select bellows tube or corrugated tube as film supplying tube, can increase melt film forming area, control melt flow, the dispersion of strengthening melt with mix, improve film forming efficiency and Surface Renewal frequency, improve polycondensation efficiency; Select bellows tube or corrugated tube and pipe combines as film supplying tube, can adaptive response process in the ever-increasing variation of melt viscosity, epimere adopts bellows tube or corrugated tube to adapt to compared with the melt of low-viscosity, hypomere adopts pipe adaptation height to stick melt.
Further, the present invention is by the double-deck circular clearance design between drapery panel and cloth lamina membranacea and film supplying tube, object is the uniformity of trying one's best of the melt level height in order to make bin stock dish lower floor, can guarantee that like this melt flow on every film supplying tube is identical, reduce the melt quality discrepancy between tube and tube.
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 the structural representation of bellows tube.
Fig. 5 a is the structural representation of circular arc type corrugated tube.
Fig. 5 b is the structural representation of scaling type corrugated tube.
Fig. 5 c is the structural representation of circular arc tangential line type corrugated tube.
Fig. 5 d is the structural representation of sinusoidal pattern corrugated tube.
Component in figure, position and numbering: end socket 1, feed-pipe 2, upper box base plate 3, casing 4, upper box 41, lower box 42, lower box base plate 5, bin stock dish 6, drapery panel 61, hole 611, cloth lamina membranacea 62, hole 621, upright shell 7, chuck 8, jacket heat-preservation medium import 9, drain pan joint flange 10, drain pan chuck 11, drain pan thermal insulation medium import 12, discharge port 13, drain pan 14, drain pan thermal insulation medium outlet 15, drain pan joint bolt 16, U-shaped film supplying tube 17, jacket heat-preservation media outlet 18, vacuum pumping opening 19, support ring 20, heat transfer medium outlet or import 21, heat-transfer medium import or export 22, end socket joint flange 23, end socket joint bolt 24, spacer 25, opening for feed 26, helical ribbon agitator 27.
Embodiment
Embodiment 1, with reference to accompanying drawing 1.
In the present embodiment, U-shaped film supplying tube adopts pipe.
A kind of melt polycondensation reaction device that the present embodiment provides, as shown in Figure 1, it comprises: upright shell 7, be connected in the end socket 1 of upright shell 7 upper ends and the drain pan 14 of lower end, end socket 1 top is provided with opening for feed 26, and upright shell 7 tops are provided with vacuum pumping opening 19, and drain pan 14 bottoms are provided with discharge port 13, in upright shell 7, have many vertically arranged U-shaped film supplying tubes 17, U-shaped film supplying tube 17 belows are provided with agitator 27; Melt polycondensation reaction device has heat-transfer system, comprise: heat-transfer medium import or export 22, upper box 41, U-shaped film supplying tube 17, lower box 42, heat transfer medium outlet or import 21, upper box, U-shaped film supplying tube, lower box are communicated with the circulation path that forms heat-transfer medium successively, be that heat-transfer medium import or export 22 communicates with upper box 41, one end of U-shaped film supplying tube 17 is connected on upper box base plate 3 and communicates with upper box 41, the other end of U-shaped film supplying tube 17 is connected to lower box base plate 5 up and down casings 42 and communicates, and lower box 42 communicates with heat transfer medium outlet or import 21; On U-shaped film supplying tube 17, be provided with film applicator, film applicator is the bin stock dish 6 of Dual-layer structure, bin stock dish 6 upper strata base plates are drapery panel 61, lower floor's base plate is cloth lamina membranacea 62, drapery panel 61 and cloth lamina membranacea 62 have hole 611 and 621, between the hole wall in hole 611,621 and film supplying tube 17, leave circular clearance.The profile of drain pan can be the various housings that are suitable in reactor lower end such as taper.
Opening for feed 26 is in end socket 1 outside, and feed-pipe 2 enters into the top of bin stock dish 6 through the spacer 25 in casing.
The outer chuck 8 that is with of upright shell 7, the bottom of chuck 8 and top are respectively equipped with jacket heat-preservation medium import 9 and jacket heat-preservation media outlet 18.
The outer drain pan chuck 11 that is with of drain pan 14, the bottom of drain pan chuck 11 and top are respectively equipped with drain pan thermal insulation medium import 12 and drain pan thermal insulation medium outlet 15.
End socket 1 is connected by end socket joint flange 23, end socket joint bolt 24 with upright shell 7, and upright shell 7 is connected by drain pan joint flange 10, drain pan joint bolt 16 with drain pan 14, is convenient to field-strip, installation.
As preferably, agitator 27 is helical ribbon agitator, and power imports into from drain pan bottom.
As preferably, the external diameter of U-shaped film supplying tube 17 is 5～100mm, is highly 0.5～30m.
Adopt the melt polycondensation reaction method of above-mentioned polycondensation reactor to be:
Heat-transfer medium enters into the upper box that is in polycondensation reactor inside from polycondensation reactor outside, then flows into and flow out from the other end from one end of U-shaped film supplying tube, flows out to polycondensation reactor outside, by external heat or cooling rear circular flow after lower box converges;
Melt injects continuously from top opening for feed, is transported to bin stock dish by feed-pipe, and bin stock dish adopts Dual-layer structure design, and upper strata base plate is liquid distribution plate, and melt flows down from the circular clearance between liquid distribution plate and film supplying tube and arrives holdup pan lower floor; Lower floor's base plate is cloth lamina membranacea, and melt flows out the circular clearance between cloth lamina membranacea and film supplying tube, relies on Gravitational sliding along film supplying tube outer wall film forming;
Melt on each film supplying tube converges to the bottom of polycondensation reactor, adopts helical ribbon agitator further to carry out stirring reaction in bottom, and homogenizing material, completes reacted melt and discharges from bottom discharge mouth.
In the present embodiment, the straight portion of U-shaped film supplying tube 17 is divided into bellows tube or corrugated tube.
As shown in Figure 4, bellows tube is alternately made up of segmental arc and straight length, crest diameter D
2with straight tube diameter D
1difference and circular arc segment length L
1ratio (D
2-D
1)/L
1=0.05～1.0.
As shown in Figure 5 a, corrugated tube can be selected circular arc type corrugated tube, and the rip cutting skeletal lines that is also corrugated tube is the tangent continuous wave of large small arc-shaped.
As shown in Figure 5 b, corrugated tube can be selected scaling type corrugated tube, is also that corrugated tube is alternately made up of expansion segment and contraction section.
As shown in Figure 5 c, corrugated tube can be selected circular arc tangential line type corrugated tube, and the rip cutting skeletal lines that is also corrugated tube is the continuous wave that circular arc and tangent line replace.
As shown in Fig. 5 d, corrugated tube can be selected sinusoidal pattern corrugated tube, is also that the rip cutting skeletal lines of corrugated tube is for sinusoidal wave.
In corrugated tube, crest diameter D
2with trough diameter D
1the ratio (D of difference and pitch L
2-D
1)/L=0.05～1.0; Described pitch is the peak-to-peak distance of adjacent wave.
As preferably, the crest diameter D of U-shaped film supplying tube 17
2being 5～100mm, is highly 0.5～30m.
The other parts of the present embodiment and implementation method are identical with embodiment 1, in Fig. 2, and the identical implication of representative that drawing reference numeral is identical with Fig. 1.
In the present embodiment, the epimere of the straight part of U-shaped film supplying tube 17 is bellows tube or corrugated tube 172, hypomere is pipe 171, epimere and hypomere are coaxial, and the length of epimere is according to the viscosity height decision of charging melt, and viscosity height length is short, otherwise long, the length of hypomere is according to the viscosity height decision of discharging melt, and viscosity height length is long, otherwise short; The structure of bellows tube, corrugated tube is identical with embodiment's 2.The crest diameter D of U-shaped film supplying tube 17
2being 5～100mm, is highly 0.5～30m.
The other parts of the present embodiment and implementation method are identical with embodiment 1, in Fig. 3, and the identical implication of representative that drawing reference numeral is identical with Fig. 1.
In the present embodiment, according to the viscosity Variation Features of melt in polycondensation process, the corresponding early stage of polycondensation of film supplying tube and the position in later stage have different constructional features, and epimere adopts bellows tube or corrugated tube to adapt to compared with the melt of low-viscosity, and hypomere adopts pipe to adapt to high glutinous melt.
Claims (7)
1. a melt polycondensation reaction method, it is characterized in that described method comprises: heat-transfer medium is injected in polycondensation reactor from polycondensation reactor outside, flow into the other end from one end of extratubal falling film element again and flow out, then flow out to polycondensation reactor outside by external heat or cooling rear circular flow; Described extratubal falling film element is U-shaped pipe, at right angle setting;
Molten monomer blend or prepolymer are injected into polycondensation reactor inside continuously from opening for feed, after film applicator distributes, rely on Gravitational sliding from U-shaped film supplying tube upper end along outer wall film forming;
Melt on each film supplying tube converges to polycondensation reactor bottom, further carries out stirring reaction with agitator, and homogenizing material, completes reacted melt and discharges from reactor bottom discharge port;
Described U-shaped film supplying tube adopts pipe; Or the straight part of U-shaped film supplying tube adopts bellows tube or corrugated tube; Or the epimere of the straight part of U-shaped film supplying tube is bellows tube or corrugated tube, hypomere is pipe;
Bellows tube is alternately made up of segmental arc and straight length, the difference of crest diameter and straight tube diameter and arc segment length (L
1) ratio be 0.05 ~ 1.0; Corrugated tube is selected circular arc type corrugated tube or scaling type corrugated tube or circular arc tangential line type corrugated tube or sinusoidal pattern corrugated tube, and the ratio of the difference of crest diameter and trough diameter and pitch (L) is 0.05 ~ 1.0.
2. application rights requires the melt polycondensation reaction device of method described in 1, comprise upright shell (7), be connected in the end socket (1) of upright shell (7) upper end and the drain pan (14) of lower end, end socket (1) top is provided with opening for feed (26), upright shell (7) top is provided with vacuum pumping opening (19), drain pan (14) bottom is provided with discharge port (13), it is characterized in that: in described reactor, be provided with film applicator, in described reactor, be also vertically installed with one or more extratubal falling film element, extratubal falling film element is U-shaped film supplying tube (17), the top of the straight part of U-shaped film supplying tube (17) also and film applicator forms circular clearance through film applicator, U-shaped film supplying tube (17) below is provided with agitator (27),
Melt polycondensation reaction device is provided with heat-transfer system, heat-transfer system comprises: upper box (41), U-shaped film supplying tube (17), lower box (42) are communicated with the circulation path that forms heat-transfer medium successively, heat-transfer medium import and outlet are connected in respectively on upper box (41) and lower box (42), one end of U-shaped film supplying tube (17) is connected to upper box base plate (3) and above communicates with upper box (41), and the other end of U-shaped film supplying tube (17) is connected to lower box base plate (5) up and down casings (42) and communicates;
Described U-shaped film supplying tube (17) adopts pipe; Or the straight part of U-shaped film supplying tube (17) adopts bellows tube or corrugated tube; Or the epimere of the straight part of U-shaped film supplying tube (17) is bellows tube or corrugated tube (172), and hypomere is pipe (171);
Bellows tube is alternately made up of segmental arc and straight length, the difference of crest diameter and straight tube diameter and arc segment length (L
1) ratio be 0.05 ~ 1.0; Corrugated tube is selected circular arc type corrugated tube or scaling type corrugated tube or circular arc tangential line type corrugated tube or sinusoidal pattern corrugated tube, and the ratio of the difference of crest diameter and trough diameter and pitch (L) is 0.05 ~ 1.0.
3. melt polycondensation reaction device according to claim 2, it is characterized in that: described film applicator is the bin stock dish (6) of Dual-layer structure, upper strata base plate is drapery panel (61), lower floor's base plate is cloth lamina membranacea (62), drapery panel (61) and cloth lamina membranacea (62) all have hole (611,621), between the hole wall of hole (611,621) and film supplying tube (17), leave described circular clearance.
4. melt polycondensation reaction device as claimed in claim 2, is characterized in that: described agitator (27) is helical ribbon agitator, and the power of agitator (27) imports into from drain pan bottom.
5. melt polycondensation reaction device according to claim 2, is characterized in that: the maximum outside diameter of U-shaped film supplying tube (17) is 5 ~ 100mm; The height of U-shaped film supplying tube (17) is 0.5 ~ 30m.
6. melt polycondensation reaction device according to claim 2, is characterized in that: the outer chuck (8) that is with of upright shell (7), and the bottom of chuck and top are respectively equipped with jacket heat-preservation medium import (9) and jacket heat-preservation media outlet (18);
The outer drain pan chuck (11) that is with of drain pan (14), the bottom of drain pan chuck and top are respectively equipped with drain pan thermal insulation medium import (12) and drain pan thermal insulation medium outlet (15).
7. for the extratubal falling film element of method described in claim 1, it is characterized in that: extratubal falling film element is U-shaped film supplying tube (17), is heat-transfer medium path in pipe; U-shaped film supplying tube (17) adopts pipe; Or the straight part of U-shaped film supplying tube (17) adopts bellows tube or corrugated tube; Or the epimere of the straight part of U-shaped film supplying tube (17) is bellows tube or corrugated tube (172), and hypomere is pipe (171);
Bellows tube is alternately made up of segmental arc and straight length, the difference of crest diameter and straight tube diameter and arc segment length (L
1) ratio be 0.05 ~ 1.0; Corrugated tube is selected circular arc type corrugated tube or scaling type corrugated tube or circular arc tangential line type corrugated tube or sinusoidal pattern corrugated tube, and the ratio of the difference of crest diameter and trough diameter and pitch (L) is 0.05 ~ 1.0.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310241529.8A CN103319705B (en) | 2013-06-17 | 2013-06-17 | Melt polycondensation reaction method, and reactor and falling film tube used for same |
| PCT/CN2013/082365 WO2014201767A1 (en) | 2013-06-17 | 2013-08-27 | Melt condensation polymerization reaction method, reactor for same, and falling film tube thereof |
| DE112013007170.3T DE112013007170T5 (en) | 2013-06-17 | 2013-08-27 | Method of melt polycondensation reaction, reactor for same and its falling film tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310241529.8A CN103319705B (en) | 2013-06-17 | 2013-06-17 | Melt polycondensation reaction method, and reactor and falling film tube used for same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103319705A CN103319705A (en) | 2013-09-25 |
| CN103319705B true CN103319705B (en) | 2014-06-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310241529.8A Active CN103319705B (en) | 2013-06-17 | 2013-06-17 | Melt polycondensation reaction method, and reactor and falling film tube used for same |
Country Status (3)
| Country | Link |
|---|---|
| CN (1) | CN103319705B (en) |
| DE (1) | DE112013007170T5 (en) |
| WO (1) | WO2014201767A1 (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203400724U (en) * | 2013-06-17 | 2014-01-22 | 浙江理工大学 | Melt poly-condensation reactor |
| CN104017189B (en) * | 2014-05-28 | 2016-03-23 | 浙江理工大学 | A kind of preparation method without antimony polyester for bottle |
| CN104017191B (en) * | 2014-05-28 | 2016-09-28 | 浙江理工大学 | A kind of preparation method of polyester for bottle |
| CN104815446B (en) * | 2015-05-11 | 2016-06-15 | 沈阳东方钛业股份有限公司 | Single bowl-type supporting No leakage film supplying tube |
| WO2017100493A1 (en) | 2015-12-10 | 2017-06-15 | Uop Llc | Reactor system for use with an ionic liquid catalyst |
| CN106000250B (en) * | 2016-05-09 | 2018-08-21 | 浙江理工大学 | It is a kind of at falling liquid film melt polycondensation reaction method and its reactor between comb |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3214351A (en) * | 1962-02-26 | 1965-10-26 | Saline Water Conversion Corp | Falling film convective distillation unit with direct contact condensation |
| CN202322692U (en) * | 2011-11-22 | 2012-07-11 | 浙江尤夫高新纤维股份有限公司 | Tubular polycondensation reaction kettle |
| CN102492127B (en) * | 2011-11-22 | 2013-06-12 | 浙江尤夫高新纤维股份有限公司 | Tube alignment type condensation polymerization reaction kettle |
| CN102746499B (en) * | 2012-07-27 | 2013-06-05 | 浙江尤夫高新纤维股份有限公司 | Polycondensation kettle for falling film outside vertical tube |
| CN202688243U (en) * | 2012-07-27 | 2013-01-23 | 浙江尤夫高新纤维股份有限公司 | Outside-tube falling film condensation polymerization reaction kettle |
-
2013
- 2013-06-17 CN CN201310241529.8A patent/CN103319705B/en active Active
- 2013-08-27 WO PCT/CN2013/082365 patent/WO2014201767A1/en active Application Filing
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| CN103319705A (en) | 2013-09-25 |
| WO2014201767A1 (en) | 2014-12-24 |
| DE112013007170T5 (en) | 2016-03-10 |
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