CN101596440B - Macromolecular material polymerization reaction kettle - Google Patents
Macromolecular material polymerization reaction kettle Download PDFInfo
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- CN101596440B CN101596440B CN2009103038599A CN200910303859A CN101596440B CN 101596440 B CN101596440 B CN 101596440B CN 2009103038599 A CN2009103038599 A CN 2009103038599A CN 200910303859 A CN200910303859 A CN 200910303859A CN 101596440 B CN101596440 B CN 101596440B
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Abstract
The invention discloses a macromolecular material polymerization reaction kettle. The kettle comprises a kettle body, an upper closed cover, a drive sealing device, a stirring device, a feed and discharge port, wherein the upper part of the kettle body is an inverted cone-shaped wide mouth; the middle part of the kettle body is of a bucket shape; the lower part of the kettle body is cone; the kettle body is provided with a heating jacket 14 with a spiral flow channel and a heat insulation layer 9; the upper closed cover 6 is provided with a heating jacket 7, a heat insulation layer 9, a vacuum port 8 and a feed port 12; the stirring device consists of a stirring shaft 5, an inner strip-shaped spiral stirring paddle 3, an outer strip-shaped spiral stirring paddle 2, a scraping blade 16 and a supporting oar 18; the drive sealing device consists of a motor, a retarder and a sealing machine; and the upper part of the stirring shaft is connected with the drive sealing device. The macromolecular material polymerization reaction kettle has good stirring effect and high heat and mass transferring efficiency, can solve the difficult problems of pole climbing and devolatilization of high-viscosity fusant and is in particular suitable for the polymerization reaction of a high-viscosity macromolecular material.
Description
Technical field
The present invention relates to still reaction equipment, especially relate to a kind of macromolecular material polymerization reaction kettle.
Background technology
Polymerization reaction kettle adopts slurry formula, anchor formula or the two combination to change the agitator of structure more at present.China's invention " butadiene rubber polymerization reaction kettle " (application number: 200520022805.2) proposed a kind of butadiene rubber polymerization reaction kettle, comprise kettle, the top of kettle is provided with agitating device, agitating device comprises the shaft that pierces into middle part in the kettle downward vertically, the described shaft that is positioned at described kettle is respectively equipped with a plurality of paddles from top to bottom, each paddle lateral surface matches with the madial wall of kettle, the arrangement interlaced with each other of neighbouring paddle, the bottom of described kettle is provided with end agitating device, end agitating device comprises the following shaft of upwards wearing vertically to advance bottom in the kettle, and the top of following shaft is equipped with end paddle.Its purpose is to provide a kind of Temperature Distribution of polymerisation that makes more to become rationally, and good radially mixed effect is arranged, and can improve the average molecular mass of product, reduces the butadiene rubber polymerization reaction kettle of the degree of branching and microgel content.
China's invention " suspension polymerization still " (application number: 95206570.3) proposed a kind of suspension polymerization still that is used to make the organic polymer spheroid, comprised a tall and thin shape kettle and one group of interchangeable frame or oar formula or frame and oar combination type stirrer that is plugged in the kettle.The reactor fluid level is less in the linear velocity difference at each axial difference place in the polymerization whipping process, thereby can obtain the comparatively polymerization single polymerization monomer of homogeneous of granularity.
China's invention " the three-phase spiral agitator of quantity-produced rubber asphalt production equipment " has proposed a kind of three-phase spiral agitator of quantity-produced rubber asphalt production equipment, supporting seat is provided with the motor that links by connector and vertical agitating auger, be provided with bearing between the upper end of vertical agitating auger and the supporting seat, the drive bevel gear that is arranged on vertical agitating auger lower end links with the driven wheel of differential that is arranged on the horizontal agitating auger.The present invention is installed in the agitator tank of quantity-produced rubber asphalt production equipment, the rubber-asphalt mixture of agitator tank internal upper part from the top down the rubber-asphalt mixture of rotational flow, bottom from the middle part both sides and rotate up mobile to the left and right, make rubber-asphalt mixture fully mix in agitator tank, the pitch drawback is leaked in the end that has overcome the existing level spiral agitator.It has reasonable in design, advantage such as efficient is high, rubber powder and pitch mix, and can use on quantity-produced rubber asphalt production equipment, also can use on the bigger mixer in other space.
For macromolecular polymerization reaction, the heat and mass of course of reaction greatly influences reaction process and polymer molecular weight; The high viscosity liquid in polymerization later stage is easy to generate " pole-climbing " effect (material along shaft make progress " climbing ") under stirring action, thereby causes that machinery is malfunctioning and stir fault such as inefficacy; The agitator stirring efficiency that traditional slurry formula, anchor formula or the two combination change structure is low, dispersion and the liquid level renewal that distributes is slow, can not satisfy the mass-and heat-transfer requirement of large-size reactor, to sum up, prior art does not relate to the problems such as " pole-climbings " that solves the molecular material polymerisation as yet.
Summary of the invention
The purpose of this invention is to provide the macromolecular material polymerization reaction kettle that a kind of mixing effect is good, heat and mass efficient is high, it can solve a high-viscosity melt pole-climbing difficult problem and devolatilization problem.
In order to achieve the above object, the present invention adopts following technical scheme: a kind of macromolecular material polymerization reaction kettle, comprise kettle, and banded inside spin stirrer paddle and banded external spiral stirrer paddle are installed on the shaft in kettle.
Described banded inside spin stirrer paddle is opposite with described banded external spiral stirrer paddle direction of rotation.
Described banded inside spin stirrer paddle directly is connected on the shaft, and described banded external spiral stirrer paddle is by supporting the oar support and connection on shaft.
The end portion of described banded external spiral stirrer paddle has scraping blade, and the scraping blade two ends are connected with shaft with banded external spiral stirrer paddle respectively.
The gap of described banded external spiral stirrer paddle and inner wall of kettle is 10-20mm.
The gap of described scraping blade and inner wall of kettle is 10-15mm.
Described banded external spiral stirrer paddle is one or more.
Described kettle top is wealthy mouthful of inverted cone-shaped, and the middle part is a round barrel shape, and the bottom is coniform.
The ratio of height to diameter of described kettle is 1.5～3: 1; Kettle lower cone part base angle is 60～90 °, and kettle inverted upper tapered segment angle is 60～90 °.
The ratio of described kettle cylindric section diameter in middle part and banded inside spin stirrer paddle, banded external spiral stirrer paddle, scraping blade width is 5-10.
Be provided with helical flow path in the heating jacket of described kettle.
The upper cover of described kettle is provided with heating jacket and heat-insulation layer.
Described heating jacket gap is 10-20mm.
The feed pipe of described kettle charging aperture stretches into reactor inside, and the feed pipe downstream end vertically is in outward in the round barrel shape part of reactor middle part.
Compared with prior art, beneficial effect of the present invention is mainly reflected in following aspect:
1, kettle top is the wealthy mouth of inverted cone-shaped, and the middle part is a round barrel shape, and the bottom is coniform.The wealthy mouthful of design in kettle top effectively increases liquid level, increases mass transfer activity efficiencies such as devolatilization; The design of kettle lower cone shape effectively increases high-viscosity material discharging ability, reduces material stock in the high viscosity macromolecule material still.
2, the heating of upper cover and INSULATION DESIGN avoid coercibility liquid to condense in capping place, effectively improve mass transfer activity efficiencies such as devolatilization.
3, the chuck gap design is between 10～20mm, helps conduction oil and upgrades, and effectively increases heat transfer efficiency.
4, kettle chuck design helical flow path helps conduction oil and upgrades, and effectively increases heat transfer efficiency.
5, external spiral and inner wall of kettle gap design are 5～30 millimeters, and preferred 10～20 millimeters, the gap design of scraping blade and inner wall of kettle is 5～15 millimeters, preferred 8～12 millimeters; During the shaft rotation, external spiral and scraping blade play the effect of scraping wall, are beneficial to the inner wall of kettle liquid level and upgrade, and improve heat transfer efficiency, avoid the thermal degradation of inwall material.
6, the double helix design on the agitating device, inside spin is opposite with the external spiral direction, when shaft rotates, to pressing down, external spiral upwards pushes away material inside spin with material, and internal and external screw does not directly link to each other, produce leakage current, thereby play the three-dimensional hybrid effect, support the effect that oar also can play dasher, promoted stirring efficiency.
Description of drawings
The present invention will illustrate by example and with reference to the mode of accompanying drawing, wherein:
Fig. 1 is a structural representation of the present invention.
In the Reference numeral, 1 is kettle, and 2 is banded external spiral stirrer paddle, and 3 is banded inside spin stirrer paddle, 4 is wealthy mouthful, and 5 is shaft, and 6 is upper cover, 7 is chuck, and 8 is vacuum port, and 9 is heat-insulation layer, 10 for driving the transmission seal device, and 11 are the conduction oil outlet, and 12 is feeding mouth, 13 are the conduction oil inlet, and 14 is chuck, and 15 is helical flow path, 16 is scraping blade, and 17 is discharging opening, and 18 for supporting oar.
The specific embodiment
Disclosed all features in this specification, or the step in disclosed all methods or the process except mutually exclusive feature and/or step, all can make up by any way.
Disclosed arbitrary feature in this specification (comprising any accessory claim, summary and accompanying drawing) is unless special narration all can be replaced by other equivalences or the alternative features with similar purpose.That is, unless special narration, each feature is an example in a series of equivalences or the similar characteristics.
As shown in Figure 1, macromolecular material reactor provided by the present invention mainly comprises with lower member: kettle 1, banded external spiral stirrer paddle 2, banded inside spin stirrer paddle 3, wealthy mouthful 4, shaft 5, upper cover 6, chuck 7, vacuum port 8, heat-insulation layer 9, drive transmission seal device 10, conduction oil outlet 11, feeding mouth 12, conduction oil inlet 13, chuck 14, helical flow path 15, scraping blade 16, discharging opening 17 supports oar 18.
The kettle 1 of macromolecular material reactor provided by the present invention mainly is made up of wealthy mouthful of the inverted cone-shaped on top, round barrel shape middle part and coniform bottom three parts, and this three part welds together.The ratio of height to diameter of this reactor (kettle height and diameter ratio, the kettle diameter of this moment is the diameter of drum position, middle part) is 1～5: 1, preferred 1.5～3: 1.This kettle lower cone part base angle is 45～120 °, preferred 60～90 °.This kettle inverted upper tapered segment angle is 45～120 °, preferred 60～90 °.
Be provided with heating jacket 7 and heat-insulation layer 9, vacuum port 8, charging aperture 12 at the upper cover 6 of reactor, charging aperture can have one or more according to purposes, the downstream of charging aperture can be provided with feed pipe, the feed pipe end vertically is in outward in the round barrel shape part of reactor middle part, and material spilling is at wealthy mouthful of place of kettle when avoiding charging.Vacuum port 8 is connected with vavuum pump by behind adapter and condenser, pans, the surge tank, makes to be in vacuum state in the still, and discharges the fugitive constituent that reaction produces.
The reactor top is provided with and drives sealing device 10, drive sealing device and comprise drive motors, reduction box, mechanical seal, drive sealing device in order to drive the agitating device in the reactor, drive motors is preferably continuously adjustable, can regulate mixing speed as required.Agitating device is made up of shaft 5, banded inside spin stirrer paddle 3, banded external spiral stirrer paddle 2, scraping blade 16, support oar 18, and shaft vertically is provided with and is positioned on the central axis of reactor.Banded inside spin stirrer paddle 3 welds or is riveted on the shaft 5.Banded external spiral stirrer paddle 2 is connected with shaft 5 by supporting oar 18, banded external spiral stirrer paddle 2 can be one or more, the direction of rotation of banded inside spin stirrer paddle 3 and banded external spiral stirrer paddle 2 is opposite, scraping blade 16 is positioned at banded external spiral stirrer paddle 2 lower end positions, scraping blade 16 two ends are connected with banded external spiral stirrer paddle 2 with shaft 5 respectively, connected mode can adopt welding or riveted joint, the outward flange of banded external spiral stirrer paddle 2 and the gap of inner wall of kettle are 5-30mm, preferred 10-20mm, the outward flange of scraping blade 16 and the gap of inner wall of kettle are 5-15mm, preferred 8-12mm.Banded inside spin stirrer paddle width, banded external spiral stirrer paddle width, scraping blade width are respectively 0.05～0.20 times of kettle middle part drum diameter, preferred 0.08～0.15 times.
The upper cover of reactor adopts flange to be connected with kettle, available asbestos pad or metal gasket sealing between flange.
Kettle at reactor is provided with heating jacket 14 and the heat-insulation layer 9 that has helical flow path 15.But admittance deep fat in the helical flow path of heating jacket 14, conduction oil transmits the reactor heating by heat, and conduction oil enters helical flow path from conduction oil inlet 13, flows out from conduction oil outlet 11, by pipe flow will backheat oil oven.Conduction oil inlet 13 is arranged on the bottom of kettle, and conduction oil outlet 11 is arranged on the top of kettle, is beneficial to heat transmission.The be laid in outer surface of heating jacket 14 of heat-insulation layer 9 is to reduce heat loss.The gap of heating jacket 14 is 10～20 millimeters, and preferred 14～18 millimeters, the more common design gaps of chuck gap design is little by about 50%, is beneficial to conduction oil and upgrades, and cuts down the consumption of energy, and improves heat transfer efficiency.The gap of heating jacket 7 also is 10～20 millimeters, preferably also is 14～18 millimeters, also is the purpose that reaches same.
Autoclave body bottom at reactor is provided with discharging opening 17, and the discharging opening diameter is 0.05～0.20 times of kettle middle part drum diameter, preferred 0.08～0.15 times.Discharging opening is provided with bleeder valve, and bleeder valve can be manual, pneumatic or electronic.During the material in reactor reaction, bleeder valve cuts out sealing, and bleeder valve is opened discharging during discharging.
Kettle can be provided with temperature-measuring port, can one or more temperature-measuring ports be set at kettle as required.Kettle can be provided with the viscosity test mouth, at the viscosity test mouth viscosity tester can be set, on-line testing viscosity.
Kettle of the present invention, upper cover, chuck, helical flow path, discharging opening, agitating device, driving
The sealing device material is to be common use material or equipment.Kettle of the present invention, pipeline, valve, upper cover all need according to the requirement of reactor vacuum, reaction mass viscosity, discharging pressure design bearing capacity.
The following examples will give further instruction to the present invention, but therefore the present invention is not subjected to any restriction.
Embodiment 1
According to macromolecular material reactor of description of the invention.The drum part of reactor highly is 1200mm, and internal diameter is 1100mm, and the height of wealthy notch portion is 390m, and wealthy mouthful of base angle is 60 °, and the tapered segment base angle is 90 °, and discharging opening diameter in center is 100mm at the bottom of the still, and bleeder valve is set.The chuck gap is 16mm, insulation layer thickness 50mm.The shaft diameter is 160mm, inside spin blade width 100mm, and external spiral blade and scraping blade width are 100mm.Feed tube diameter is 200mm, stretches into 150mm in the still.Be equipped with the water ring Roots vacuum unit of maximum exhaust capacity 300L/s.
When carrying out hard segment content in the reactor and be 58% thermoplastic polyester elastomer polycondensation process, absolute pressure is 100Pa, does not have " pole-climbing " phenomenon, and in 3.5 hours reaction time, product performance viscosity is between 1.55～1.58, and molecular weight product is big, quality is even.When theoretical load is 800kg, actual discharging 795kg.
Comparative Examples 1
An existing reactor, drum type, drum diameter 1100mm, height 1200mm, anchor agitator, chuck gap 40mm, insulation layer thickness 50mm.The shaft diameter is 160mm, anchor diameter 100mm.Be equipped with the water ring Roots vacuum unit of maximum exhaust capacity 300L/s.
When carrying out hard segment content in the reactor and be 58% thermoplastic polyester elastomer polycondensation process, absolute pressure is 200Pa, and " pole-climbing " phenomenon is arranged, and in 4.5 hours reaction time, product performance viscosity is between 1.33～1.42, and molecular weight product is little, quality is inhomogeneous.When theoretical load is 800kg, actual discharging 770kg.
The present invention is not limited to the aforesaid specific embodiment.The present invention expands to any new feature or any new combination that discloses in this manual, and the arbitrary new method that discloses or step or any new combination of process.
Claims (6)
1. a macromolecular material polymerization reaction kettle, comprise kettle (1), it is characterized in that: described kettle (1) top is wealthy mouthful of inverted cone-shaped, the middle part is a round barrel shape, the bottom is coniform, and banded inside spin stirrer paddle (3) and banded external spiral stirrer paddle (2) are installed on the shaft (5) in kettle (1); Described banded inside spin stirrer paddle (3) is opposite with described banded external spiral stirrer paddle (2) direction of rotation; Described banded inside spin stirrer paddle (3) directly is connected on the shaft (5), and described banded external spiral stirrer paddle (2) is by supporting oar (18) support and connection on shaft (5); The end portion of described banded external spiral stirrer paddle (2) has scraping blade (16), and scraping blade (16) two ends are connected with shaft (5) with banded external spiral stirrer paddle (2) respectively, and the upper cover of described reactor (6) is provided with vacuum port (8).
2. macromolecular material polymerization reaction kettle according to claim 1 is characterized in that: described banded external spiral stirrer paddle (2) is 10-20mm with the gap of inner wall of kettle.
3. macromolecular material polymerization reaction kettle according to claim 1 is characterized in that: described scraping blade (16) is 10-15mm with the gap of inner wall of kettle.
4. macromolecular material polymerization reaction kettle according to claim 1 is characterized in that: be provided with helical flow path (15) in the heating jacket of described kettle (14).
5. macromolecular material polymerization reaction kettle according to claim 1 is characterized in that: the upper cover of described kettle (6) is provided with heating jacket (7) and heat-insulation layer (9).
6. according to claim 4 or 5 described macromolecular material polymerization reaction kettles, it is characterized in that: described heating jacket gap is 10-20mm.
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Effective date of registration: 20220628 Address after: 618400 Mazu Town, Shifang City, Deyang City, Sichuan Province Patentee after: SICHUAN KEXIN MECHANICAL AND ELECTRICAL EQUIPMENT Co.,Ltd. Address before: 618407 Mazu Town, Shifang, Sichuan Patentee before: SICHUAN SUNSHINE PLASTICS Co.,Ltd. |