CN205347296U - Composite reaction ware that preparation low molecular weight polycarbonate used - Google Patents
Composite reaction ware that preparation low molecular weight polycarbonate used Download PDFInfo
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- CN205347296U CN205347296U CN201620020086.9U CN201620020086U CN205347296U CN 205347296 U CN205347296 U CN 205347296U CN 201620020086 U CN201620020086 U CN 201620020086U CN 205347296 U CN205347296 U CN 205347296U
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Abstract
The utility model discloses a composite reaction ware that preparation low molecular weight polycarbonate used, the vertical reactor of the two barrels component that the composite reaction ware cup jointed inside and outside being, the bottom and the interior barrel bottom of outer barrel are equipped with matter entrance and material export respectively, be equipped with the upper and lower vacuum of transesterification mouth on outer barrel and the interior barrel, interior barrel and outer barrel be double -layered shell type structure, the top of interior barrel is equipped with interior water conservancy diversion break plate, along the outside outer water conservancy diversion break plate that is equipped with with the internal wall connection of urceolus that extends in interior barrel top, barrel water conservancy diversion piece outside lieing in matter entrance the outer barrel cavity between the water conservancy diversion break plate is equipped with outside and barrel water conservancy diversion piece in being equipped with in the cavity of interior barrel. Realized not stirring the manufacturing equipment that can realize the material and fully react, satisfied the technological efficiency of polycarbonate production, had the simple and easy characteristics of manufacture.
Description
Technical field
This utility model is a kind of combined reactor preparing low-molecular polycarbonate, is specifically related in continuous production of polycarbonate by transesterification method flow process the reactor used in the ester exchange reaction stage, belongs to field of chemical equipment.
Background technology
Merlon is with excellent in cushion effect and famous, having prominent toughness, excellent electrical insulating property, broad use temperature range and dimensional stability, therefore Merlon and modified alloy are widely used in each industrial circles such as electric, electric tool, transportation, automobile, machinery, building, information storage, medical apparatus and instruments and defence and military.The industrial process of Merlon has light phosgenation and ester-interchange method in the world at present, and light phosgenation is that dihydroxy compounds carries out interfacial polycondensation with phosgene, and ester-interchange method is that dihydroxy compounds carries out body (melting) polycondensation with carbonic diester.Owing to the production process of ester-interchange method Merlon does not use phosgene, in recent years by more employing in newly-built process units.
In ester-interchange method Merlon course of reaction, having more than 95% byproduct of reaction (unit phenol) is produce in preliminary stage and the ester exchange reaction stage of reaction and extracted, and can this stage control be related to whole course of reaction and be normally carried out and the quality of final Merlon.The continuous production device of industrialization ester-interchange method Merlon is generally adopted the multiple reactors of series connection to complete ester exchange reaction.
State Intellectual Property Office authorizes a patent of invention CN101448872B at 2011.6.15, and name is called " method for continuous production of aromatic copolycarbonate and manufacture device ".The patent provides the method for continuous production of a kind of aromatic copolycarbonate and manufacture device.The apparatus for continuously production of the patent 2 series to having 3 vertical reactors being connected in series and 1 horizontal reactor is described, it is indicated that can use the reactor of the patterns such as stirring tank reactor, film reactor, centrifugal film evaporator for completing ester exchange stage vertical reactor.
State Intellectual Property Office authorizes a patent of invention CN102958976B at 2014.11.26, and name is called " method for continuous production of branched polycarbonate ".The patent provides the method for continuous production of a kind of branched polycarbonate, patent is pointed out in describing to adopt stirring tank reactor to complete ester exchange elementary reaction.
State Intellectual Property Office authorizes a patent of invention CN103314033B at 2015.05.27, and name is called " manufacture method of Merlon ".The patent provides a kind of present invention and high efficiency and the method stably manufacturing the excellent Merlon such as light resistance, the transparency, tone, thermostability, heat stability or mechanical strength can be provided.Patent middle finger adopts vertical mixing reactor in the ester exchange reaction stage.
State Intellectual Property Office authorizes a patent of invention CN1293118C at 2007.1.3, and name is called " method producing oligo-ester carbonate ".The patent provides a kind of continuation method adopting melt transesterification to produce oligo-ester carbonate, it is that reactant reacts in the presence of a catalyst, form flow path device continuously across by equipment such as perforated plate tower, centrifugal separator or baffle plate type separator and 2-6 the falling film evaporators with groove, prepare oligo-ester carbonate.The temperature of each equipment of reactant, catalyst and flow path device, pressure and the time of staying are controlled to be illustrated by patent, and the structure of the falling film evaporator with groove is described explanation.
State Intellectual Property Office authorizes a patent of invention CN101873891B at 2013.12.18, and name is called " method preparing Merlon in flash distillation deliming system ".The patent provides a set of reactor assembly preparing Merlon being made up of one or more reaction vessels, oligomerisation reactor, the first pressure control device, pre-heater, the second pressure control device, allotter and flash tank.The temperature of reactant, catalyst and reactor assembly and Stress control are illustrated by patent, but the structure of flash tank are not illustrated.
The continuous preparation method of Merlon and device thereof that above-mentioned patent describes all have a similarity, but are adopted combination and the structure thereof of the equipment being differently formed in flow process, form each different features.
Utility model content
The purpose of this utility model is in that to provide a kind of combined reactor preparing low-molecular polycarbonate, inside and outside cylinder structural design is adopted to form, outer flow guide distribution plate and outer cylinder body flow deflector it is provided with in outer cylinder body, inner barrel is provided with Inner guide distribution plate and guiding flow of inner cylinder body sheet, achieve to stir and can realize the process equipment that material fully reacts, meet the technological effect of polycarbonate production, there is manufacture and process easy feature.
This utility model is achieved through the following technical solutions: a kind of combined reactor preparing low-molecular polycarbonate, described combined reactor is the vertical reactor of two cylinder compositions of inside and outside socket, the bottom of outer cylinder body is provided with material inlet, and the bottom of inner barrel is provided with material outlet；Outer cylinder body is provided with vacuum port, and inner barrel is provided with lower vacuum port；Described inner barrel and outer cylinder body are jacket type structure, are provided with heating agent connector on described inner barrel and outer cylinder body；The top of described inner barrel is provided with Inner guide distribution plate；Stretch out along inner barrel top and be provided with the outer flow guide distribution plate being connected with outer cylinder body inwall；In the outer cylinder body cavity between material inlet and outer flow guide distribution plate, it is provided with outer cylinder body flow deflector, in the cavity of described inner barrel, is provided with guiding flow of inner cylinder body sheet.
The combined reactor of the present invention adopts the structure of inside and outside cylinder, and inside and outside cylinder is jacket type structure, adds the heating surface (area) (HS in unit volume, and chuck heating agent can use heat conduction wet goods, in order to quickly heats by the material of inside and outside cylinder.
Material carries out ester exchange reaction in outer cylinder body and inner barrel, after material sends into outer cylinder body from material inlet, under the effect of outer cylinder body flow deflector, on screw, horizontal sliding flows to outer flow guide distribution plate, and delivered to Inner guide distribution plate by outer flow guide distribution plate, after being then passed through guiding flow of inner cylinder body sheet, ester exchange reaction thing is sent from material outlet, and the phenol of generation is extracted from upper and lower vacuum port.
Described Inner guide distribution plate is the sieve-plate structure arranged along combined reactor horizontal line；For improving the material holdup time in inner barrel, described guiding flow of inner cylinder body sheet includes upper sieve plate and lower sieve plate, upper sieve plate and lower sieve plate are conical plate structure, the sieve aperture of upper sieve plate and lower sieve plate shifts to install, the vertex of a cone of upper sieve plate is down, and be provided with perforate at top, lower sieve plate be located at below upper sieve plate and the vertex of a cone upward.The setting of perforate is to ensure that upper sieve plate is without material dead angle, and material is not piled up at the upper sieve plate vertex of a cone.
The ratio of the sieve aperture gross area of described Inner guide distribution plate and the sieve aperture gross area of outer flow guide distribution plate is 1.1～1.5.In the present invention, the sieve aperture gross area of Inner guide distribution plate should be greater than the sieve aperture gross area of outer flow guide distribution plate, enters the load that the inlet amount of inner barrel can be born less than inner barrel, it is to avoid solid accumulation.
The ratio of the sieve aperture gross area of described upper sieve plate and the cross-sectional area of inner barrel is 0.5～0.9, it is preferable that ratio is 0.6～0.8, select above-mentioned ratio data in order that guarantee that material is not piled up, the phenol of gasification can be extracted smoothly；The ratio of the sieve aperture gross area of described lower sieve plate and the cross-sectional area of inner barrel is 0.5～0.9, it is preferable that ratio is 0.6～0.8, select above-mentioned ratio data in order that guarantee that material is not piled up, the phenol of gasification can be extracted smoothly；The taper angle of described upper sieve plate is 120～170 °, and the taper angle of described lower sieve plate is 120～170 °, is conducive to increasing material time of staying in reactor.
In the present invention, it is contemplated that material total residence time and disengagement area, the length of described outer cylinder body and internal diameter ratio are 1.2～2.5, it is preferable that ratio is 1.5～2.0.The length of described inner barrel and internal diameter ratio are 2～5, it is preferable that ratio is 2.5～3.5, separately, for making inner barrel material pass through area by area >=outer cylinder body material, fully ensuring that the evaporation of phenol, the internal diameter ratio of described inner barrel and outer cylinder body is 0.7～0.9, it is preferable that ratio is 0.77～0.87.
For considering that material enters the pressure differential (outer cylinder body pressure >=inner barrel pressure) when inner barrel from outer cylinder body, material enters inner barrel momentary status for ejection, the distance at described inner barrel top to outer cylinder body top and outer cylinder body length ratio are 0.3～0.5, and the distance at inner barrel top to outer cylinder body top is vaporization chamber, it is simple to gas-liquid separation.
The quantity of described guiding flow of inner cylinder body sheet is more than one group, the guiding flow of inner cylinder body sheet of more than one group sets gradually along inner barrel top down, the total length of guiding flow of inner cylinder body sheet (total length of this guiding flow of inner cylinder body sheet be more than one group guiding flow of inner cylinder body sheet along cylinder top down arrange time total length) account for the 0.4～0.8 of inner barrel total length.Guiding flow of inner cylinder body sheet and the setting organizing guiding flow of inner cylinder body sheet in the present invention, it is possible to make reaction mass Homogeneous phase mixing in inner barrel, it is simple to the gas-liquid separation of material, and add the material time of staying at inner barrel more.
Described outer flow guide distribution plate is the ring-type sieve-plate structure arranged along outer cylinder body inwall, and the sieve aperture gross area of described outer flow guide distribution plate is 0.7～0.9 with the ratio of the cross-sectional area of material inlet.The control of this ratio can well realize the promotion of material, in conjunction with the setting of outer cylinder body flow deflector, makes material can be flowed by the horizontal sliding on screw after entering outer cylinder body, it is to avoid the use of the actuating units such as propeller, is conducive to the simplification of equipment.
Described outer flow guide distribution plate and the horizontal angle of combined reactor are 150～180 °, the present invention arranges the purpose of angle outside and is easy for the material flowing to inner barrel between flow guide distribution plate and combined reactor horizontal line, this angle is set to 150～180 °, allowing for material and enter the pressure differential (outer cylinder body pressure >=inner barrel pressure) when inner barrel from outer cylinder body, material enters inner barrel momentary status for ejection.
Described combined reactor is for the ester exchange reaction stage of polymerization technique flow process, and quantity is set to two or more, and plural combined reactor is sequentially connected in series use, and serial number is 2～5, it is preferred to 3～4.
This utility model compared with prior art, has the following advantages and beneficial effect:
(1) function combinations such as heating material intensification, mixing, flash distillation, gas-liquid separation and film forming are integrated by the combined reactor that this utility model relates to, and it is simple and easy to manufacture processing, it is not necessary to stirring, can realize material and fully react.
(2) combined reactor that this utility model relates to adopts the vertical response equipment with inside and outside tube structure, inside and outside barrel designs has the structures such as outer cylinder body flow deflector, outer flow guide distribution plate, guiding flow of inner cylinder body sheet, Inner guide distribution plate, and in conjunction with the rational proportion of the technological parameters such as its screening area, inside and outside cylinder dimensional structure, be conducive to the polymerization of Merlon to produce the technological effect reaching optimum.
(3) this utility model designs outer cylinder body flow deflector in outer cylinder body, structural design and the outer flow guide distribution screen hole gross area in conjunction with outer flow guide distribution plate meet the proportionate relationship of 0.7～0.9 with material inlet cross-sectional area, on the one hand, can realize being flowed by the horizontal sliding on screw after material enters outer cylinder body, avoid the use of the actuating units such as propeller, be conducive to the simplification of equipment；On the other hand, can make there is pressure differential between material inlet and outer flow guide distribution plate, be conducive to the ejection of material, make material form good gas-liquid separation effect at outer cylinder body top, improve the technological effect that polycarbonate polymerization produces.
(4) this utility model is designed with chuck for inside and outside cylinder, not only increases the heating surface (area) (HS of material in unit volume, it is also possible to quickly heated by the material of inside and outside cylinder by chuck heating agent (such as conduction oil, steam etc.), shortens the response time.
(5) this utility model be located at the Inner guide distribution plate at inner barrel top and internal many groups guiding flow of inner cylinder body sheet with the use of, meet sieve aperture to shift to install, the ratio of the sieve aperture gross area of each upper and lower sieve plate and the cross-sectional area of inner barrel meets 0.5～0.9 etc., material can be made to be sufficiently complete gas-liquid separation in inner barrel, and add the material time of staying in inner chamber body.
(6) guiding flow of inner cylinder body sheet described in the utility model sets gradually along inner barrel top down, and the total length of guiding flow of inner cylinder body sheet accounts for the 0.4～0.8 of inner barrel total length, in actual mechanical process, can according to the liquid level needing adjustment material of technique, thus being controlled adjusting to material time of staying in reactor, it is simple to technological operation and control.
Accompanying drawing explanation
Fig. 1 is the structural representation of combined reactor described in the utility model.
Fig. 2 is the top view of outer flow guide distribution plate described in the utility model.
Fig. 3 is the top view of Inner guide distribution plate described in the utility model.
Fig. 4 is the sectional view of upper sieve plate described in the utility model.
Fig. 5 is the top view of upper sieve plate described in the utility model.
Fig. 6 is the sectional view of lower sieve plate described in the utility model.
Fig. 7 is the top view of lower sieve plate described in the utility model.
Wherein, 1 outer cylinder body, 2 material inlets, 3 inner barrels, 4 material outlets, vacuum port on 5,6 times vacuum ports, 7 heating agent connectors, 8 Inner guide distribution plates, 9 outer flow guide distribution plates, 10 outer cylinder body flow deflectors, 11 guiding flow of inner cylinder body sheets, 1101 upper sieve plates, 1102 times sieve plates, 1103 perforates.
Detailed description of the invention
Below in conjunction with embodiment, this utility model is described in further detail, but embodiment of the present utility model is not limited to this.
Embodiment 1:
A kind of combined reactor preparing low-molecular polycarbonate, as shown in Figure 1, this combined reactor is the vertical reactor of two cylinder compositions of inside and outside socket, and design has the structures such as material gateway, upper and lower vacuum port, chuck heating agent, inside and outside flow guide distribution plate, is specifically summarized as follows:
(1) bottom of outer cylinder body 1 is provided with material inlet 2, and the bottom of inner barrel 3 is provided with material outlet 4.
(2) outer cylinder body 1 is provided with vacuum port 5, and inner barrel 3 is provided with lower vacuum port 6, as it is shown in figure 1, vacuum is provided at the top of outer cylinder body 1 in the ester exchange reaction in the present embodiment；Lower vacuum port 6 is provided at the lower half of inner barrel 3.
(3) inner barrel 3 and outer cylinder body 1 are jacket type structure, are provided with heating agent connector 7 on inner barrel 3 and outer cylinder body 1.
(4) stretch out along inner barrel 3 top and be provided with the outer flow guide distribution plate 9 being connected with outer cylinder body 1 inwall, as shown in Figure 2, this outer flow guide distribution plate 9 ring-type sieve-plate structure for arranging along outer cylinder body 1 inwall, in the present embodiment, outer flow guide distribution plate 9 and the horizontal angle of combined reactor (α) are 150 °, the ratio (S of the sieve aperture gross area of outer flow guide distribution plate 9 and the cross-sectional area of material inlet 2Outer sieve/SImport) it is 0.7.
(5) top of inner barrel 3 is provided with Inner guide distribution plate 8, outer cylinder body 1 is connected with inner barrel 3 by Inner guide distribution plate 8, as shown in Figure 3, Inner guide distribution plate 8 is the sieve-plate structure arranged along combined reactor horizontal line, the ratio (S of the sieve aperture gross area of Inner guide distribution plate 8 and the sieve aperture gross area of outer flow guide distribution plate 9Interior sieve/SOuter sieve) it is 1.1.
(6) as it is shown in figure 1, be provided with outer cylinder body flow deflector 10 in outer cylinder body 1 cavity between material inlet 2 and outer flow guide distribution plate 9.
(7) in the cavity of inner barrel 3, guiding flow of inner cylinder body sheet 11 it is provided with, as also shown in e.g. figs. 4-7, including upper sieve plate 1101 and lower sieve plate 1102, upper sieve plate 1101 and lower sieve plate 1102 are conical plate structure, the sieve aperture of upper sieve plate 1101 and lower sieve plate 1102 shifts to install, the vertex of a cone of upper sieve plate 1101 down, and is provided with perforate 1103 at top, lower sieve plate 1102 be located at below upper sieve plate 1101 and the vertex of a cone upward.In the present embodiment, the ratio (S of the sieve aperture gross area of upper sieve plate 1101 and the cross-sectional area of inner barrel 3Top sieve/SInner core) it is 0.5；Ratio (the S of the sieve aperture gross area of lower sieve plate 1102 and the cross-sectional area of inner barrel 3Lower sieve/SInner core) it is 0.5.The taper angle (β) of upper sieve plate 1101 is 120 °, and the taper angle (γ) of lower sieve plate 1102 is 120 °.As in figure 2 it is shown, the quantity of the guiding flow of inner cylinder body sheet 11 of the present embodiment is three groups, three groups of guiding flow of inner cylinder body sheets 11 set gradually along inner barrel 3 top down, and the total length of guiding flow of inner cylinder body sheet 11 accounts for the 0.4(L of inner barrel 3 total length4/L2).
In the present embodiment, the length of outer cylinder body 1 and internal diameter ratio (L1/D1) it is 1.2, the length of inner barrel 3 and internal diameter are than being (L2/D2) 2, the internal diameter ratio (D of inner barrel 3 and outer cylinder body 12: D1) it is 0.8, the distance at inner barrel 3 top to outer cylinder body 1 top and outer cylinder body 1 length ratio (L3/L1) it is 0.3.
Embodiment 2:
A kind of polymerization technique flow process preparing low-molecular polycarbonate, in this technological process, the ester exchange reaction stage adopts the difference of the mode that three combined reactors are sequentially connected in series, the combined reactor that the present embodiment relates to and embodiment 1 such as shown in table 1,2.
The structural parameters table of table 1 combined reactor
The process control parameter table of table 2 combined reactor
Embodiment 3:
A kind of polymerization technique flow process preparing low-molecular polycarbonate, the mode that in this technological process, four combined reactors of ester exchange reaction stage employing are sequentially connected in series, the difference of the combined reactor that the present embodiment relates to and embodiment 1 is as shown in Table 3, 4.
The structural parameters table of table 3 combined reactor
The process control parameter table of table 4 combined reactor
Embodiment 4:
A kind of polymerization technique flow process preparing low-molecular polycarbonate, the mode that in this technological process, four combined reactors of ester exchange reaction stage employing are sequentially connected in series, the difference of the combined reactor that the present embodiment relates to and embodiment 1 is as shown in Table 5,6.
The structural parameters table of table 5 combined reactor
The process control parameter table of table 6 combined reactor
The above; it it is only preferred embodiment of the present utility model; not this utility model is done any pro forma restriction, every according to technical spirit of the present utility model, above example is made any simple modification, equivalent variations, each fall within protection domain of the present utility model.
Claims (9)
1. the combined reactor preparing low-molecular polycarbonate, it is characterized in that: described combined reactor is the vertical reactor of two cylinder compositions of inside and outside socket, the bottom of outer cylinder body (1) is provided with material inlet (2), and the bottom of inner barrel (3) is provided with material outlet (4)；Outer cylinder body (1) is provided with vacuum port (5), and inner barrel (3) is provided with lower vacuum port (6)；Described inner barrel (3) and outer cylinder body (1) are jacket type structure, are provided with heating agent connector (7) on described inner barrel (3) and outer cylinder body (1)；The top of described inner barrel (3) is provided with Inner guide distribution plate (8)；Stretch out along inner barrel (3) top and be provided with the outer flow guide distribution plate (9) being connected with outer cylinder body (1) inwall；It is provided with outer cylinder body flow deflector (10) at outer cylinder body (1) cavity being positioned between material inlet (2) and outer flow guide distribution plate (9), in the cavity of described inner barrel (3), is provided with guiding flow of inner cylinder body sheet (11).
2. a kind of combined reactor preparing low-molecular polycarbonate according to claim 1, it is characterised in that: described Inner guide distribution plate (8) is the sieve-plate structure arranged along combined reactor horizontal line；Described guiding flow of inner cylinder body sheet (11) includes upper sieve plate (1101) and lower sieve plate (1102), upper sieve plate (1101) and lower sieve plate (1102) are conical plate structure, the sieve aperture of upper sieve plate (1101) and lower sieve plate (1102) shifts to install, the vertex of a cone of upper sieve plate (1101) is down, and be provided with perforate (1103) at top, lower sieve plate (1102) be located at upper sieve plate (1101) lower section and the vertex of a cone upward.
3. a kind of combined reactor preparing low-molecular polycarbonate according to claim 2, it is characterized in that: the ratio of the sieve aperture gross area of the sieve aperture gross area of described Inner guide distribution plate (8) and outer flow guide distribution plate (9) is 1.1～1.5, the ratio of the sieve aperture gross area of described Inner guide distribution plate (8) and the cross-sectional area of inner barrel (3) is 0.7～0.8.
4. a kind of combined reactor preparing low-molecular polycarbonate according to claim 3, it is characterised in that: the ratio of the cross-sectional area of the sieve aperture gross area of described upper sieve plate (1101) and inner barrel (3) is 0.5～0.9；The ratio of the sieve aperture gross area of described lower sieve plate (1102) and the cross-sectional area of inner barrel (3) is 0.5～0.9；The taper angle of described upper sieve plate (1101) is 120～170 °, and the taper angle of described lower sieve plate (1102) is 120～170 °.
5. a kind of combined reactor preparing low-molecular polycarbonate according to claim 4, it is characterized in that: length and the internal diameter ratio of described outer cylinder body (1) are 1.2～2.5, length and the internal diameter ratio of described inner barrel (3) are 2～5, and the internal diameter ratio of described inner barrel (3) and outer cylinder body (1) is 0.7～0.9.
6. a kind of combined reactor preparing low-molecular polycarbonate according to claim 5, it is characterised in that: the distance at described inner barrel (3) top to outer cylinder body (1) top and outer cylinder body (1) length ratio are 0.3～0.5.
7. a kind of combined reactor preparing low-molecular polycarbonate according to any one of claim 1～6, it is characterized in that: the quantity of described guiding flow of inner cylinder body sheet (11) is more than one group, the guiding flow of inner cylinder body sheet (11) of more than one group sets gradually along inner barrel (3) top down, and the total length of guiding flow of inner cylinder body sheet (11) accounts for the 0.4～0.8 of inner barrel (3) total length.
8. a kind of combined reactor preparing low-molecular polycarbonate according to claim 7, it is characterized in that: the described outer flow guide distribution plate (9) the ring-type sieve-plate structure for arranging along outer cylinder body (1) inwall, the ratio of the sieve aperture gross area of described outer flow guide distribution plate (9) and the cross-sectional area of material inlet (2) is 0.7～0.9.
9. a kind of combined reactor preparing low-molecular polycarbonate according to claim 8, it is characterised in that: described outer flow guide distribution plate (9) and the horizontal angle of combined reactor are 150～180 °.
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| CN201620020086.9U CN205347296U (en) | 2016-01-11 | 2016-01-11 | Composite reaction ware that preparation low molecular weight polycarbonate used |
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