CN1241969C - Miniature condensation polymerization synthesis reaction device - Google Patents
Miniature condensation polymerization synthesis reaction device Download PDFInfo
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- CN1241969C CN1241969C CN 200410040329 CN200410040329A CN1241969C CN 1241969 C CN1241969 C CN 1241969C CN 200410040329 CN200410040329 CN 200410040329 CN 200410040329 A CN200410040329 A CN 200410040329A CN 1241969 C CN1241969 C CN 1241969C
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Abstract
The present invention discloses a miniature condensation polymerization and synthesis reaction device which comprises a reaction kettle, a heating and heat preserving system, a stirring system, a condensing, refluxing and fractionating system, a pressurizing system, a vacuum system, a testing and controlling system and a bracket (3), wherein the reaction kettle is hung on the fixed bracket (3); the heating and heat preserving system is coated on the outer side of the kettle body (1); the stirring system is arranged on the kettle cover (2); the condensing, refluxing and fractionating system is arranged on the upper part of one side of the reaction kettle, one end of the condensing, refluxing and fractionating system is fixed on the kettle cover (2) and communicated with an inner cavity of the kettle body (1), and the other end is connected with the vacuum system (59); the pressurizing system penetrates through from one side of the kettle cover (2) and is communicated with the inner cavity of the kettle body (1); the testing and controlling system is respectively connected with the heating and heat preserving system, the stirring system, the pressurizing system and the vacuum system. The present invention enables a plurality of technological steps of polyester synthesis to be carried out in one reaction kettle, which has the advantages of small occupation area, low investment, equipment simplification and more convenient operation. Thus, the miniature condensation polymerization reaction device is an ideal reaction device for condensation polymerization and synthesis in laboratories.
Description
One, technical field
The invention belongs to polycondensation synthetic reaction device technical field, be specifically related to a kind of miniature polycondensation synthetic reaction device.This device can satisfy high temperature resistant, the high pressure and the high vacuum condition of synthesizing polyester, polyamide-based superpolymer requirement simultaneously, is the ideal device that scientific research is carried out in the laboratory.
Two, background technology
Industrial polyester synthetic adopted ester-interchange method or direct high pressure acid system usually, and along with pure terephthalic acid's large-scale industrial production, it is more and more adopting direct high pressure acid system person at present.But adopt ester-interchange method no matter be, or direct high pressure acid system, because processing step just can be finished will pass through that all making beating, transesterify or esterification, precondensation, final minification gather etc., thereby industrial all be to adopt many stills proceed step by step, as lucky agate technology is 6 stills, the clock spinning process is 5 stills, and Yi Wenda technology is 6 stills, and E.I.Du Pont Company is 4 stills.Still is added corresponding support equipment, can make entire reaction plant area area big undoubtedly, and investment is many, and these are given no cause for much criticism for the suitability for industrialized production of polyester.But even it to be dwindled the laboratory lab scale research equipment of back as polyester modification or research and development polyester new variety, it is inapplicable then still to seem.This has hindered the development of polyester virtually.
Three, summary of the invention
The objective of the invention is to be difficult to be suitable for the defective of laboratory study, a kind of miniature polycondensation synthetic reaction device is provided at the many stills of polyester in industry substep production equipment.This device can all be placed on processing steps such as making beating, transesterify or the esterification of polyester synthetic reaction process, precondensation, final minification be poly-and carry out in the same reactor, can really realize the microminiaturization of polycondensation of polyester synthetic reaction device.
Miniature polycondensation synthetic reaction device provided by the invention comprises a reactor and supporting with it heat tracing system, stirring system, the condensing reflux fractionating system, compression system, vacuum system, test control system and support, reactor is unsettled to be fixed on the support, the heat tracing system is coated on the kettle outside, stirring system is installed on the kettle cover, the condensing reflux fractionating system is positioned at reactor one side top, the one end is fixed on the kettle cover and with the kettle inner chamber and communicates, the other end links to each other with vacuum system, compression system then passes with the kettle inner chamber from kettle cover one side wall surface and communicates, test control system respectively with the heat tracing system, stirring system, compression system links to each other with vacuum system, wherein
The kettle cover of reactor is to be fixed on the kettle by uniform trip bolt, the kettle cover middle part has the secondary ladder hole, so that stirring system to be installed, its outside, middle part has charging opening, gas via-hole and temperature test hole, discharge port is opened in the cylinder of autoclave body bottom central authorities and extension downwards, assigned an inverted T shape plug in it, discharge port cylinder outer wall has screw thread, mates fit sealing with the fastening swivel nut of spill with its tyre handle;
The heat tracing system is made up of resistance wire, electric furnace core, muff and thermometer, and the resistance wire string is around the electric furnace in-core, and muff is coated on outside the electric furnace core, and thermometer is inserted in the temperature test hole of reactor kettle cover;
Stirring system is made up of agitator arm, magnetic agitation mechanism, pulley belt and motor, motor links to each other with magnetic agitation mechanism by pulley belt, one end of magnetic agitation mechanism passes the ladder hole at reactor kettle cover middle part successively and links to each other with agitator arm with wherein seal washer, and be fixed on the kettle cover by the fastening external thread sleeve of T shape and kettle cover middle part ladder hole thread fit, the stirring end of agitator arm is the stirring-head of an anchor formula or oar formula;
The condensing reflux fractionating system is made up of Y shape pipe connecting, condensing reflux fractionation path, condensation pass and ball valve, the lower end of Y shape pipe connecting is fixed in the gas via-hole of reactor kettle cover, and its two upper end links to each other with condensing reflux fractionation path, condensation pass by ball valve respectively;
Compression system is by inertia source of the gas, inlet pipe, test tracheae, intake valve and weather gage are formed, inlet pipe one end and inertia source of the gas join, the other end passes with the kettle inner chamber from kettle cover one side wall surface and communicates, intake valve is installed on the inlet pipe that is positioned at reactor kettle cover side, weather gage then be installed in from another side wall of kettle cover pass and with test tracheae that the kettle inner chamber communicates on;
Test control system is made up of vacuum test instrument and integration test controller, the vacuum test instrument is connected in the vacuum passage, the integration test controller respectively with thermometer, the resistance wire of heat tracing system, the motor of stirring system, the test tracheae of compression system links to each other.
For the micromolecular compound that prevents to produce in the reaction process enters vacuum system, influence the works better of vacuum system, the present invention also is connected with one by stent support fixed cryo trapping between condensing reflux fractionating system and vacuum system, this cryo trapping can make the micromolecular compound condensation of coming from the condensing reflux fractionating system in the vacuum get rid of.Outer also available cryosel of this cryo trapping or cooled with liquid nitrogen.
Though miniature polycondensation synthetic reaction device provided by the invention has only a reactor; but dexterously the polyester synthetic is pulled an oar; transesterify or esterification; precondensation; the poly-needed heat tracing of processing step that waits of final minification; logical nitrogen protection; pressurization; the condensation fractionation; vacuumize; the designs of necessary auxiliary facility such as test control etc. and this still connect into for an integral body; not only make the making beating of polyester synthetic; transesterify or esterification; precondensation; the poly-processing step that waits of final minification can both carry out in same reactor; simplified equipment; and floor space is little; reduced investment; operating more conveniently, is a kind of ideal laboratory polycondensation synthetic reaction device.The present invention removes and can be used for direct high pressure acid system and ester-interchange method synthesizing polyester base polymer, also can be used for synthesizing polyamides class polycondensation polymerized thing.
Four, description of drawings
Fig. 1 is the structural representation of miniature polycondensation synthetic reaction device provided by the invention;
Fig. 2 is the plan structure synoptic diagram of reactor kettle cover of the present invention;
Fig. 3 is the sectional structure synoptic diagram of magnetic agitation of the present invention mechanism.
Five, embodiment
Provide embodiment and application examples below in conjunction with accompanying drawing, and the present invention is carried out concrete description.Be worth being pointed out that at this embodiment that provides only is used for that the invention will be further described; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field still belongs to protection scope of the present invention according to the invention described above content to some nonessential improvement and the adjustment that the present invention makes.
Embodiment
The miniature polycondensation synthetic reaction device that present embodiment provides as shown in Figure 1, it comprises a reactor, heat tracing system, stirring system, condensing reflux fractionating system, compression system, vacuum system, test control system, cryo trapping and support.
Reactor is fixed on the support 3 by unsettled the shelving in limit, upper edge that kettle 1 turns up, 2 of kettle covers are fixed on the kettle 1 by uniform trip bolt 4, kettle cover 2 middle parts have the secondary ladder hole 5 that stirring system is installed, this through hole outside has charging opening 6, gas via-hole 7 and temperature test hole 8, sees Fig. 2.Discharge port 9 is opened in the cylinder of kettle 1 bottom center and extension downwards, and its cylinder outer wall has screw thread, to mate fit sealings with the fastening swivel nut 10 of the spill of its tyre handle.Because the product viscosity of polycondensation is big and also will increase sharply with the reduction of temperature, especially after being lower than melting point polymer, temperature can condense into adamantine solid, be difficult to remove, so the present invention has also designed a T shape plug 11 that mates with discharge port, be inverted during use and assign in the discharge port 9, so not only can avoid product cold junction in discharge port to stop up, and good sealing effect, easy to operate.
The heat tracing system is coated on kettle 1 outside, is made up of resistance wire 12, electric furnace core 13, muff 14 and thermometer 15.Resistance wire 12 is wrapped in the electric furnace core 13, and muff 14 is coated on outside the electric furnace core 13.In order to make discharge port 9 keep certain temperature in Polycondensation Reactor and Esterification Reactor, be unlikely to influenced by ambient temperature and make temperature descend too fast and make discharging not smooth, the shell of muff 14 coats the top that thermal insulation layer continues to extend to vertically downward fastening swivel nut 10 handles of discharge port spill to the still bottom face.Thermometer 15 is inserted in the temperature test hole 8 of reactor kettle cover 2.Thermometer 15 is a thermocouple thermometer.
Stirring system is positioned on the reactor kettle cover 2, is made up of agitator arm 16, magnetic agitation mechanism, pulley belt 30 and motor 31.Magnetic agitation mechanism is made up of stir shaft 17, steel pipe socket 18, permanent magnet 19,20, permanent-magnet sealing cover 21, bearing 23, graphite annulus 24, seal head 25, sealing-ring 26, fastening external thread sleeve 27, sees Fig. 3.The bottom of steel pipe socket 18 be one turn up along the limit, during installation, this places kettle cover 2 middle part ladder holes 5 to lay on the first step step of seal washer 28 along the limit, and by fastening external thread sleeve of T shape 29 and thread fit on kettle cover 2 middle part ladder holes 5 second stage step walls it vertically is fixed on the kettle cover 2, steel pipe socket 18 middle part inwalls have one by different ring-shaped steps that form of internal diameter up and down.Stir shaft 17 front ends pass the ladder hole 5 at steel pipe socket 18, kettle cover middle part and the seal washer of wherein laying 28 is threaded with agitator arm 16, and the latter half of step that then relies on end outer wall evagination formation thereafter cooperates with steel pipe socket 18 middle part inwall ring-shaped steps is fixed in the steel pipe socket 18 it.The stirring end of agitator arm 16 is the stirring-head of an anchor formula or oar formula. Permanent magnet 19,20 has two, and one is cylindrical, and one is round shape.Columniform permanent magnet 19 is placed on the upper surface of stir shaft 17 in the steel pipe socket, and the pin tooth that passes through its lower surface evagination is connected with the cotter way coupling of stir shaft 17 upper surfaces, and being with a graphite annulus 24 on the step that upper end cylinder indent forms, this graphite annulus 24 coats columniform permanent magnet 19 upper ends wherein.20 of columnar permanent magnets are placed in the permanent-magnet sealing cover 21 that shape with it is complementary, and permanent-magnet sealing cover 21 is laid on steel pipe socket 18 outer walls at cylindrical magnet iron 19 positions within it by bearing 23 pivot bush units in its upper and lower two running-ons.Permanent-magnet sealing overlaps on the projection of 21 bottom outer walls and has a belt grooves 22, and pulley belt 30 is placed in wherein and links to each other with motor 31.Seal head 25 is the T-shaped cylinder in a cross section, is inverted the upper surface that is placed in graphite annulus 24 in the steel pipe socket, and the cylinder of the end that diameter is big has annular groove, wherein is placed with sealing-ring 26.Fastening external thread sleeve 27 is the T-shaped cylinder in a cross section, along cylinder axis to the through hole that has with the little newel post body coupling of seal head 25 diameters, during installation, be enclosed within on the little newel post's body of seal head 25 diameters, and the screw thread that has on the cylinder by the little end of its diameter, be connected with the internal thread coupling of steel pipe socket 18 ends, seal head 25 is fixing.When driving permanent-magnet sealing cover 21 by pulley belt 30, motor 31 rotates, the cylindrical permanent-magnet iron 20 that coats wherein will be along with rotation, and the magnetic force of its generation also just drives cylindrical magnet iron 19 that is positioned at steel pipe socket 18 and the stir shaft 17 that links to each other successively with it, agitator arm 16 also rotates together.Because the present invention has substituted the mechanical stirring of common employing with hermetically sealed magnetic agitation, thereby improved the stopping property that installs.In addition, make it demagnetization for fear of the temperatures involved permanent magnet of reactor, the present invention also is provided with a watercooling jacket 32 on 18 outer walls of the steel pipe socket between magnetic agitation mechanism and the kettle cover.
The condensing reflux fractionating system is positioned at reactor one side top, is made up of Y shape pipe connecting 33, condensing reflux fractionation path, condensation pass and ball valve 40,41.For fear of leaning on too closely and the influence operation with the magnetic agitation mechanism of the reactor top that coexists, the bottom of the vertical part of Y shape pipe connecting 33 is fixed in the gas via-hole 7 of reactor kettle cover, rest part is bent into vertical again after kettle cover 2 outside oblique upper bendings, two upper ends of its bifurcated, one end is upright to link to each other with condensing reflux fractionation path by ball valve 40, the other end more from the center begins be oblique below bending after then oblique upper stretches out to the right, links to each other with condensation pass by ball valve 41 then.Condensing reflux fractionation path is connected and composed successively by filler fractional column 34, bridge piece 35, prolong 37, Y-tube 38, micrometering valve 39.Bridge piece 35 is one to be the L shaped bend pipe of acute angle, is connected with filler fractional column 34, prolong 37 respectively after being inverted 90 degree during installation, its bending place have one in pipe vertical built-in thermowell 36.After the vacant ports of Y-tube 38 connect stopping valve 45, be connected with pipe connecting 44 that communicate with cryo trapping 55 and that have an another stopping valve 46 again.Condensing reflux fractionation path is used for esterification or transesterify and precondensation stage, and wherein filler fractional column 34 is the reactants such as dibasic alcohol that are used for the condensation vaporization, water or other low molecular compound that the fractionation reaction produces; The thermowell 36 that is provided with on the bridge piece 35 is the temperature variation that are used to measure fractional column, surveys the fractionation situation of low molecular compound; Prolong 37 is low molecular compound condensations that reaction is produced, because it has constant slope, so before emitting without micrometering valve 39, the phlegma in the pipe can play the fluid-tight effect; Micrometering valve 39 is the pin type micrometering valve, is used to control the take-off rate of phlegma and regulates the still internal pressure.Condensation pass is made of prolong 42, and its other end directly with pipe connecting 44 that cryo trapping 55 communicates is connected by flange 43.
Compression system is made up of inertia source of the gas 47, inlet pipe 48, intake valve 49, test tracheae 50, weather gage 51 and overvoltage protection valve 52.Inlet pipe 48 1 ends and inertia source of the gas 47 join, and the other end passes with kettle 1 inner chamber from kettle cover 2 side walls and communicates, and intake valve 49 is installed on the inlet pipe 48 that is positioned at reactor kettle cover side.52 on weather gage 51 and overvoltage protection valve be installed in simultaneously from kettle cover 2 another side walls pass and with test tracheae 50 that kettle 1 inner chamber communicates on.Intake valve is a pin sealing micrometering valve.Weather gage is the positive/negative pressure table.The inertia source of the gas adopts high pure nitrogen.
Test control system is made up of vacuum test instrument 53 and integration test controller 54.Vacuum test instrument 52 is connected in the vacuum passage, and present embodiment specifically is connected on the vacuum passage pipe connecting 44 between cryo trapping 55 and the vacuum system 59.54 of integration test controllers by its test control contact respectively with thermometer 15, the resistance wire 12 of heat tracing system, the motor 31 of stirring system, the test tracheae 50 of compression system links to each other.Vacuum test instrument and integration test controller are the commercial goods.The ZDF-12/13 microcomputer type compound vacuum gauge that the vacuum test instrument adopts Chengdu Instruement Factory to produce.The WHF type reactor controller that the integration test controller adopts Weihai City, Shandong automatic control reactor company limited to produce.
Cryo trapping 55 is to place cross-sectional shape vertically to be oblong container, by support 56 support fixation, be connected between condensing reflux fractionating system and the vacuum system 59, on the condensate outlet pipe 57 of its bottom center ball valve 58 is installed, top has can insert in the container and the through hole of the pipe connecting 44 that communicates with condensing reflux fractionation path, condensation pass and the vacuum system 59 of condensing reflux fractionating system respectively.
Application examples 1
Should use-case be direct high pressure acid system synthesizing polyester.
Raw material is joined in the kettle from the charging opening 6 on the reactor kettle cover 2, seals the back and operate accordingly by following operation:
1, closeall valve behind the beater addition, open motor 31 stirring to pulps after 1 hour, beginning heating gradually is raised to about 180 ℃ temperature in the kettle, and Open valve 40,39,49 then, in still, feed high pure nitrogen by valve 49, it is got rid of air from valve 39.Logical nitrogen after 10 minutes valve-off 39,49 make the still internal pressure rise to 2～3kg.f/cm
2Power continues heated and stirred.
When 2, esterification treated that temperature in the kettle rises to 230 ℃ of left and right sides, regulated valve 49 made the still internal pressure remain on 2～3kg.f/cm
2About power.After treating that filler fractional column 34 column top temperatures begin to rise to 120～140 ℃, electric valve 39 regulates the still internal pressure and water distillates speed, keeps still internal pressure and temperature.When esterification finishes, filler fractional column 34 column top temperatures begin to descend, and the still internal pressure is also along with decline, and when no longer including water and distillating, open valve 39, emit all water of condensation in the prolong 37, make it to communicate with atmosphere, make the still internal pressure reduce to 0 after, reacted again 10～30 minutes.
3, precondensation: open valve 45,46, valve-off 39 begins to vacuumize, and carries out prepolymerization reaction, by vacuum tightness in the valve 39 fine setting stills, makes it to reach 10～50mmHg, and keeps about 2 hours of 230～250 ℃ of reactions of temperature in the kettle.
4, final minification is poly-: open valve 41, and valve-off 40,45,46, vacuum tightness reaches 0.1～0.5mmHg in the still Yi Bian continue to be evacuated to, and reaches 280～285 ℃ Yi Bian continue to be heated to temperature in the kettle, and keeps this temperature and vacuum tightness to react about 3 hours.Along with the carrying out of reaction, the electric current of motor 31 increases to about 1A, and rotating speed is about 20r/min, reaches reaction end, and the polyester intrinsic viscosity that obtain this moment is about 0.8.
5, reacted after, valve-off 41 stops to vacuumize, and feeds a small amount of high pure nitrogen by valve 49, makes the still internal pressure reach 0.1～1kg.f/cm
2Power is opened fastening swivel nut 10 then while hot, extracts T shape plug 11 and allows product flow into cooling trough, traction, pelletizing.The take-off rate of material is regulated still internal pressure size by valve 49 and is controlled.
Application examples 2
Should use-case be the ester-interchange method synthesizing polyester.
Raw material is joined in the kettle from the charging opening 6 on the reactor kettle cover 2, seals the back and operate accordingly by following operation:
1, making beating: open valve 40,39 after reinforced, close all the other valves, open agitator motor 31, about 1 hour of stirring to pulp, then under agitation gradually heating make temperature in the kettle be elevated to 120～140 ℃.
2, transesterify: when treating that temperature in the kettle rises to 160～180 ℃, valve 39 outlet has methyl alcohol to distillate, and continues to heat up and keeps 180～200 ℃ of temperature till the no methyl alcohol outflow of valve 39 outlets.
3, precondensation: open valve 45,46, valve-off 39 begins to vacuumize, and carries out prepolymerization reaction, by vacuum tightness in the valve 39 fine setting stills, makes it to reach 10～50mmHg, keeps about 2 hours of 230～250 ℃ of reactions of temperature in the kettle simultaneously.
4, final minification is poly-: open valve 41, and valve-off 40,45,46, vacuum tightness reaches 0.1～0.5mmHg in the still Yi Bian continue to be evacuated to, and reaches 280～285 ℃ Yi Bian continue to be heated to temperature in the kettle, and keeps this temperature and vacuum tightness to react about 3 hours.Along with the carrying out of reaction, the electric current of motor 31 increases to about 1A, and rotating speed is about 20r/min, reaches reaction end, and the polyester intrinsic viscosity that obtain this moment is about 0.8.
5, reacted after, valve-off 41 stops to vacuumize, and feeds a small amount of high pure nitrogen by valve 49, makes the still internal pressure reach 0.1～1kg.f/cm
2Power is opened fastening swivel nut 10 then while hot, extracts T shape plug 11 and allows product flow into cooling trough, traction, pelletizing.The take-off rate of material is regulated still internal pressure size by valve 49 and is controlled.
Application examples 3
Should use-case be the melt phase polycondensation synthesizing polyamides.
Raw material is joined in the kettle from the charging opening 6 on the reactor kettle cover 2, seals the back and operate accordingly by following operation:
1, batch mixing: open valve 40,39 after reinforced, close all the other valves, open agitator motor 31, stir about 1 hour, then under agitation gradually heating make and be elevated to temperature requiredly in the still, and feed inert protective gas by valve 49.
2, precondensation: open valve 45,46, valve-off 39 begins to vacuumize, and carries out prepolymerization reaction, by vacuum tightness in the valve 39 fine setting stills, makes it to reach 10～50mmHg, and reacts about 2 hours down at 200～220 ℃.
3, final minification is poly-: treat that mixing speed reduces gradually, when motor 31 electric currents begin to increase, open valve 41, valve-off 40,45,46, continue to be evacuated to the interior vacuum tightness of still on one side and reach 0.1～0.5mmHg, continuing to be heated to temperature in the kettle reaches 260～280 ℃ on one side, and keeps this temperature and vacuum tightness reaction to reach terminal point in about 3 hours.
4, reacted after, valve-off 41 stops to vacuumize, and feeds a small amount of high pure nitrogen by valve 49, makes the still internal pressure reach 0.1～1kg.f/cm
2Power is opened fastening swivel nut 10 then while hot, extracts T shape plug 11 and allows product flow into cooling trough, traction, pelletizing.The take-off rate of material is regulated still internal pressure size by valve 49 and is controlled.
Claims (10)
1, a kind of miniature polycondensation synthetic reaction device, this device comprises a reactor, the heat tracing system, stirring system, the condensing reflux fractionating system, compression system, vacuum system, test control system and support (3), reactor is unsettled to be fixed on the support (3), the heat tracing system is coated on kettle (1) outside, stirring system is installed on the kettle cover (2), the condensing reflux fractionating system is positioned at reactor one side top, the one end is fixed in kettle cover (2) and upward and with kettle (1) inner chamber communicates, the other end links to each other with vacuum system (59), compression system then passes with kettle (1) inner chamber from kettle cover (2) one side wall surfaces and communicates, test control system respectively with the heat tracing system, stirring system, compression system links to each other with vacuum system, wherein
The kettle cover of reactor (2) is to be fixed on the kettle (1) by uniform trip bolt (4), kettle cover (2) middle part has secondary ladder hole (5), so that stirring system to be installed, its outside, middle part has charging opening (6), gas via-hole (7) and temperature test hole (8), discharge port (9) is opened in the cylinder of kettle (1) bottom center and extension downwards, assigned an inverted T shape plug (11) in it, discharge port (9) cylinder outer wall has screw thread, mates fit sealing with the fastening swivel nut of spill (10) with its tyre handle;
The heat tracing system is made up of resistance wire (12), electric furnace core (13), muff (14) and thermometer (15), resistance wire (12) string is in electric furnace core (13), muff (14) is coated on outside the electric furnace core (13), and thermometer (15) is inserted in the temperature test hole (8) of reactor kettle cover;
Stirring system is made up of agitator arm (16), magnetic agitation mechanism, pulley belt (30) and motor (31), motor (31) links to each other with magnetic agitation mechanism by pulley belt (30), the secondary ladder hole (5) that one end of magnetic agitation mechanism passes reactor kettle cover middle part successively links to each other with agitator arm (16) with the seal washer of wherein laying (28), and be fixed on the kettle cover (2) by the fastening external thread sleeve of T shape (29) and kettle cover middle part ladder hole (5) thread fit, the stirring end of agitator arm (16) is the stirring-head of an anchor formula or oar formula;
The condensing reflux fractionating system is made up of Y shape pipe connecting (33), condensing reflux fractionation path, condensation pass and ball valve (40,41), the lower end of Y shape pipe connecting (33) is fixed in the gas via-hole (7) of reactor kettle cover, and its two upper end links to each other with condensing reflux fractionation path, condensation pass by ball valve (40,41) respectively;
Compression system is by inertia source of the gas (47), inlet pipe (48), intake valve (49), test tracheae (50) and weather gage (51) are formed, inlet pipe (48) one ends and inertia source of the gas (47) join, the other end passes with kettle (1) inner chamber from kettle cover (2) one side wall surfaces and communicates, intake valve (49) is installed on the inlet pipe (48) that is positioned at reactor kettle cover side, weather gage (51) then be installed in from another side wall of kettle cover (2) pass and with test tracheae (50) that kettle (1) inner chamber communicates on;
Test control system is made up of vacuum test instrument (53) and integration test controller (54), vacuum test instrument (53) is connected in the vacuum passage, integration test controller (54) respectively with thermometer (15), the resistance wire (12) of heat tracing system, the motor of stirring system (31), the test tracheae (50) of compression system links to each other.
2, miniature polycondensation synthetic reaction device according to claim 1, it is characterized in that between the condensing reflux fractionating system of this device and vacuum system (59), also being connected with a cryo trapping (55) by support (56) support fixation, this cryo trapping (55) is to place cross-sectional shape vertically to be oblong container, on the condensate outlet pipe (57) of its bottom center ball valve (58) is installed, top have can insert in the container and respectively with the condensing reflux fractionation path of condensing reflux fractionating system, the through hole of the pipe connecting (44) that condensation pass and vacuum system (59) communicate, with the pipe connecting (44) of condensing reflux fractionation path on also be equipped with two stopping valve (45,46).
3, miniature polycondensation synthetic reaction device according to claim 1 and 2, it is characterized in that magnetic agitation mechanism is by stir shaft (17), steel pipe socket (18), permanent magnet (19,20), permanent-magnet sealing cover (21), bearing (23), graphite annulus (24), seal head (25), sealing-ring (26), fastening external thread sleeve (27) is formed, the bottom of steel pipe socket (18) be one turn up along the limit, during installation, this is positioned on the seal washer (28) that kettle cover (2) middle part ladder hole (5) step lays along the limit, and it vertically is fixed on the kettle cover (2) by the fastening external thread sleeve of T shape (29) and kettle cover middle part ladder hole (5) thread fit, steel pipe socket (18) middle part inwall has a ring-shaped step, stir shaft (17) front end passes steel pipe socket (18), kettle cover (2) is threaded with agitator arm (16), latter half ofly then relies in the middle part of step that end outer wall evagination thereafter forms and the steel pipe socket (18) the inwall ring-shaped step to cooperate it is fixed in wherein; Permanent magnet (19,20) there are two, one is cylindrical, one is round shape, columniform permanent magnet (19) is placed on the interior stir shaft (17) of steel pipe socket (18), and the pin tooth that passes through its lower surface evagination is connected with the cotter way coupling of stir shaft (17) upper surface, and be with a graphite annulus (24) on the step that upper end cylinder indent forms, this graphite annulus (24) coats columniform permanent magnet (19) upper end wherein, columnar permanent magnet (20) then is placed in the permanent-magnet sealing cover (21) that shape is complementary with it, permanent-magnet sealing cover (21) is by on it, bearing (23) pivot bush unit in two running-ons is laid on steel pipe socket (18) outer wall at cylindrical magnet iron (19) position within it down, has a belt grooves (22) on the projection of permanent-magnet sealing cover (21) bottom outer wall; Seal head (25) is the T-shaped cylinder in a cross section, is inverted on the graphite annulus (24) that is placed in the steel pipe socket (18), and sealing-ring (26) is arranged in the cylinder annular groove of the end that diameter is big; Fastening external thread sleeve (27) also is the T-shaped cylinder in a cross section, axially have through hole with the little newel post body coupling of seal head diameter, during installation, be enclosed within on the little newel post's body of seal head (25) diameter, and the screw thread that has on the cylinder by the little end of its diameter, be connected with the internal thread coupling of steel pipe socket (18) end, seal head (25) is fixing.
4, miniature polycondensation synthetic reaction device according to claim 3 is characterized in that also being provided with a watercooling jacket (32) on steel pipe socket (18) outer wall between magnetic agitation mechanism and the kettle cover (2).
5, miniature polycondensation synthetic reaction device according to claim 1 and 2, the condensing reflux fractionation path that it is characterized in that the condensing reflux fractionating system is by filler fractional column (34), bridge piece (35), prolong (37), Y-tube (38), micrometering valve (39) connects and composes successively, bridge piece (35) is one to be the L shaped bend pipe of acute angle, be inverted during installation behind 90 degree respectively and filler fractional column (34), prolong (37) connects, its bending place have one in pipe vertical built-in thermowell (36), after the vacant port of Y-tube (38) connects stopping valve (45), be connected again with cryo trapping (55) pipe connecting that communicate and that have another stopping valve (46) (44); Condensation pass is made of prolong (42), and an end of the Y shape pipe connecting (33) that is attached thereto by ball valve (41) begins to be oblique below and bends from the middle part.
6, miniature polycondensation synthetic reaction device according to claim 4, the condensing reflux fractionation path that it is characterized in that the condensing reflux fractionating system is by filler fractional column (34), bridge piece (35), prolong (37), Y-tube (38), micrometering valve (39) connects and composes successively, bridge piece (35) is one to be the L shaped bend pipe of acute angle, be inverted during installation behind 90 degree respectively and filler fractional column (34), prolong (37) connects, its bending place have one in pipe vertical built-in thermowell (36), after the vacant port of Y-tube (38) connects stopping valve (45), be connected again with cryo trapping (55) pipe connecting that communicate and that have another stopping valve (46) (44); Condensation pass is made of prolong (42), and an end of the Y shape pipe connecting (33) that is attached thereto by ball valve (41) begins to be oblique below and bends from the middle part.
7, miniature polycondensation synthetic reaction device according to claim 1 and 2 is characterized in that testing also being connected to an overvoltage protection valve (52) on the tracheae (50).
8, miniature polycondensation synthetic reaction device according to claim 3 is characterized in that testing also being connected to an overvoltage protection valve (52) on the tracheae (50).
9, miniature polycondensation synthetic reaction device according to claim 5 is characterized in that testing also being connected to an overvoltage protection valve (52) on the tracheae (50).
10, miniature polycondensation synthetic reaction device according to claim 6 is characterized in that testing also being connected to an overvoltage protection valve (52) on the tracheae (50).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410040329 CN1241969C (en) | 2004-07-29 | 2004-07-29 | Miniature condensation polymerization synthesis reaction device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410040329 CN1241969C (en) | 2004-07-29 | 2004-07-29 | Miniature condensation polymerization synthesis reaction device |
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| CN1597730A CN1597730A (en) | 2005-03-23 |
| CN1241969C true CN1241969C (en) | 2006-02-15 |
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| CN 200410040329 Expired - Fee Related CN1241969C (en) | 2004-07-29 | 2004-07-29 | Miniature condensation polymerization synthesis reaction device |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101220140B (en) * | 2007-12-24 | 2010-08-25 | 中昊晨光化工研究院 | Reaction device for interesterification and polycondensation reaction |
| CN103657572A (en) * | 2012-09-25 | 2014-03-26 | 昆山尚达智机械有限公司 | Novel chemical reaction tank |
| CN103381352B (en) * | 2013-07-25 | 2015-03-25 | 无锡意凯自动化技术有限公司 | Nitrogen pressurization device for parallel reactor |
| CN104892931B (en) * | 2015-06-25 | 2017-03-15 | 安庆市虹泰新材料有限责任公司 | A kind of polyamide processing unit (plant) |
| CN105536652B (en) * | 2016-02-27 | 2017-10-31 | 杭州若水化学科技有限公司 | It is a kind of to remove the stress reaction device and method of the water produced in course of reaction |
| CN110003431B (en) * | 2019-04-16 | 2021-07-20 | 浙江新诺高分子材料有限公司 | Preparation method of dispersion emulsion of high-alkali-resistance aqueous polyurethane |
| CN111729627A (en) * | 2020-06-28 | 2020-10-02 | 苏州东子云工业技术科技有限公司 | Experimental reation kettle of new material |
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