CN102847490A - Organic silicon mechanical-free stirring continuous polymerization reactor - Google Patents
Organic silicon mechanical-free stirring continuous polymerization reactor Download PDFInfo
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- CN102847490A CN102847490A CN2012103243839A CN201210324383A CN102847490A CN 102847490 A CN102847490 A CN 102847490A CN 2012103243839 A CN2012103243839 A CN 2012103243839A CN 201210324383 A CN201210324383 A CN 201210324383A CN 102847490 A CN102847490 A CN 102847490A
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Abstract
The present invention discloses an organic silicon mechanical-free stirring continuous polymerization reactor. According to the organic silicon mechanical-free stirring continuous polymerization reactor, a liquid phase material inlet (7) and a solid phase material inlet (9) are symmetrically arranged on both sides of a gas phase outlet (8), wherein the gas phase outlet (8) is arranged on a middle position on the top of an upper cylinder (1) of a reactor body; a gas-liquid separator (10) arranged inside the upper cylinder (1) is opposite to the gas phase outlet (8); a side surface of the upper cylinder (1) is provided with an overflow port (6); the top of a diversion cylinder (2) arranged inside a lower cylinder (11) extends into the upper cylinder (1), and is communicated with the upper cylinder (1); the lower portion of the diversion cylinder (2) is internally communicated with the lower cylinder (11); a compressed gas inlet (4) is arranged on a middle position on the bottom of the lower cylinder (11); the compressed gas inlet (4) and the lower cylinder (11) are arranged on the same axis line; and a combination position of the compressed gas inlet (4) and the lower cylinder (11) is provided with a compressed gas distributor (5).
Description
Technical field
The present invention relates to a kind of organosilicon machinery-free and stir the serialization polymer reactor, especially a kind of continuous reaction device that is applicable to the solid-liquid phase reaction of organosilicon polymer in synthetic.
Background technology
Organosilicon material is the important component part of new chemical materials, and it is by the monomer of different degrees of functionality or intermediate, the combination of modification organic group, the polymer of making through polycondensation reaction.Its unique molecular structure is given the performance of its excellence, uniqueness.Along with the expansion of the human living space growth to the high performance material demand, the relation of organosilicon material and people's daily life, industrial and agricultural production and hi-tech development is further close, be widely used in nearly all industrial circle and high-technology fields such as Aero-Space, electric power electric, architectural engineering, textile garment, petrochemical industry, biological medicine, photovoltaic industry, agricultural, automobile, machinery, food, house ornamentation, daily use chemicals and personal care articles, become the indispensable high performance material of modern industry and daily life.At present, the production of domestic organopolysiloxane great majority adopt batch process, and the stage of reaction in the production process is usually in indirect tank reactor.Indirectly tank reactor mainly is comprised of the reactor kettle of jacketed and oar formula or gate stirrer.But adopt the diameter of agitator of this type all larger, so the rotating speed that obtains is all not too high, generally in 100r/min, material is in laminar condition usually, when especially producing silicone oil high viscosity product, so the relative motion between solid liquid phase is violent not, cause conversion rate of products low.When the product viscosity of producing is higher, the zone that the blade of agitator can not act under the effect of viscous force, forms the dead angle easily in reactor, if the too high easier formation channel of agitator speed.Because the structural limitations of indirect tank reactor, and organosilicon polymer is not the good conductor of heat, and material heat is that high-temperature medium by the reactor wall chuck provides in the reactor, therefore exist radial direction temperature difference large, cause reactor temperature inhomogeneous, too high near the still wall temperature, the local reaction aggravation makes the molecular weight distribution of product wide.Simultaneously, in indirect tank reactor, material is diametrically without relative speed, and the difficult exchange that energy and material occur just causes conducting heat in the reactor, mass transfer is inhomogeneous.Whipping process can produce the friction that produces between material and the reactor wall, falls low-energy utilization rate.And because adopt indirect tank reactor, so domestic organopolysiloxane product, especially there are the phenomenons such as unstable product quality in the silicone oil product.In addition, when organopolysiloxane is synthetic, be resin type catalyst at the synthetic normally used catalyst of silicone oil especially.When in indirect tank reactor, producing, whipping process also can increase the phase mutual friction between catalyst granules and the agitator, the small catalyst particles that generation is difficult to separate from product, and this parts of fine small catalyst particle not only increases the consumption of catalyst, production cost is increased, return the aspects such as product quality such as outward appearance, viscosity, dielectric properties and bring larger impact.
Summary of the invention
The invention provides a kind of organosilicon machinery-free and stir the serialization polymer reactor, it is not only easy for installation, and the organosilicon machinery-free of processing ease stirs polymer reactor.And utilize self special construction, need not mechanical agitation and can realize that liquid-liquid, solid-liquid phase component evenly mix, can reduce the wearing and tearing to solid component, realize the production technology long-period stable operation, by Compressed Gas the material in the reactor being carried out bubbling in addition in the process that mixes mixes, form the fluidized state of similar materials, finish mixing of materials, reach material steady heat transfer in the reactor, mass transport process.
The present invention has adopted following technical scheme: a kind of organosilicon machinery-free stirs the serialization polymer reactor, it comprises reactor body, the Compressed Gas distributor, gas-liquid separator and guide shell, described reactor body is by comprising successively upper shell and lower shell under upper, the centre position at the top of described upper shell is provided with gaseous phase outlet, bilateral symmetry at gaseous phase outlet is provided with liquid phase material entrance and solid-phase material entrance, in upper shell, be provided with gas-liquid separator, gas-liquid separator is relative with gaseous phase outlet, side at upper shell is provided with overfall, in lower shell, be provided with guide shell, the top of guide shell extend in the upper shell and is connected with upper shell, communicate in the bottom of guide shell and the lower shell, centre position, bottom at lower shell is provided with the Compressed Gas entrance, Compressed Gas entrance and lower shell are on same axis, the bottom sides of lower shell is provided with slag-drip opening, is provided with the Compressed Gas distributor at Compressed Gas entrance and lower shell junction.
The diameter of described upper shell is wider than the diameter of lower shell, and the length of upper shell is less than the length of lower shell.The diameter of described upper shell is 1.5～2.3 times of lower shell diameter, 0.4～0.7 times of the length of upper shell and the Length Ratio of lower shell.Be connected by the inversed taper platform transition between described upper shell and the lower shell, the drift angle of inversed taper platform is 70 °～100 °.Described Compressed Gas distributor is set to spherical distribution grid, and spherical distribution grid is 0.35～0.45 times of lower shell radius, is evenly distributed with through hole at spherical distribution grid, and the percent opening of spherical distribution grid is 0.15～0.3.Gas-liquid separator is installed under the reactor head gaseous phase outlet, and gas-liquid separator is set to taper shape, and the circular cone drift angle is 75 °～110 °, and the conical bottom radius surface is 0.5～0.8 times of upper shell radius.Described guide shell radius is 0.55～0.8 times of lower shell radius, and the length of guide shell is 1.1～1.3 times of lower shell length.
The present invention has following beneficial effect: after having adopted above technical scheme, do not adopt the mechanical agitation mode during mixing of materials of the present invention, adopt Compressed Gas bubbling mode to the mixing of material, the wearing and tearing of mechanical agitation to solid constituent have been reduced, especially reduce solid catalyst because of the fine particle that wearing and tearing produce, make the separation of solid liquid phase easier to be simple.Reduce the wearing and tearing of solid catalyst, also reduced the consumption of catalyst simultaneously, more can arrive long period, the stable operation of device, the low cost of easier realization production technology, serialization.Gas-liquid separator of the present invention has adopted the spherical distribution grid with certain percent opening, it can play the effect of even distribution Compressed Gas, can form the bubble of stable and uniform, prevent the formation of air pocket, improve mixing, the convection current of material, impel polymerisation to carry out more fully, improve materials conversion rate and production efficiency.Mixing of materials and heat transfer mode have been optimized in the organic combination of gas-liquid separator of the present invention and guide shell, make the interior material of reactor and heat more can reach the state of homogeneous.Compressed Gas distributor of the present invention is installed in reactor bottom, the Compressed Gas distributor is the spherical distribution grid with certain percent opening, the radius of spherical distribution grid is 0.35～0.45 times of lower shell radius, percent opening is 0.15～0.3, after the even perforate of spherical distribution grid, help the distribution of Compressed Gas in reactor, promote that material mixes in reactor, make simultaneously material in reactor, produce circulation, improve the mass transfer mass-transfer efficiency.Organosilicon machinery-free of the present invention stirs in the serialization polymer reactor, gas-liquid separator is installed under the reactor head gaseous phase outlet, its profile is conical, the circular cone drift angle is 75 °～110 °, the conical bottom radius surface is 0.5～0.8 times of reacting cylinder body epimere, the solid that conical liquid-blocking cap is taken out of for separating of compressed gas, liquid components.The guide shell that the present invention has is installed in the lower shell, and the radius of guide shell is 0.55～0.8 times of lower shell radius, and the length of guide shell is 1.1～1.3 times of lower shell length.The gas of compressed gas distributor forms even bubble, again by overflowing behind the guide shell, in this process, form the state that is similar to boiling in the guide shell, " space " that boiling process produces filled up by the outer material of guide shell, the stable convection current of final formation guarantees the material in the reactor shell, the even transmission of heat.Compressed Gas entrance of the present invention and lower shell are on same axis, and Compressed Gas enters from reactor center like this, make the material of reactor both sides can participate in uniformly reaction, prevent the generation of bias current.
Description of drawings
Fig. 1 is the structural representation of the embodiment of the invention one.
Fig. 2 is the schematic top plan view of Compressed Gas distributor of the present invention.
Fig. 3 is Compressed Gas distributor assembling schematic diagram of the present invention.
Fig. 4 is that the A-A of Fig. 1 is to looking schematic diagram.
The specific embodiment
In Fig. 1, the invention provides a kind of organosilicon machinery-free and stir the serialization polymer reactor, it comprises reactor body, Compressed Gas distributor 5, gas-liquid separator 10 and guide shell 2, described reactor body is by comprising successively upper shell 1 and lower shell 11 under upper, be connected by inversed taper platform 12 transition between upper shell 1 and the lower shell 11, the drift angle of inversed taper platform 12 is 70 °～100 °, upper shell 1 and lower shell and inversed taper platform 12 can be welding, it also can be one-step casting moulding in the process, the diameter of upper shell 1 is wider than the diameter of lower shell 11, the length of upper shell 1 is less than the length of lower shell 11, the diameter of upper shell 1 is 1.5～2.3 times of lower shell 11 diameters, the diameter of present embodiment upper shell 1 is 2 times of lower shell 11 diameters, 0.4～0.7 times of the Length Ratio of the length of upper shell 1 and lower shell 11,0.5 times of the length of the upper shell 1 of present embodiment and the Length Ratio of lower shell 11, the centre position at the top of described upper shell 1 is provided with gaseous phase outlet 8, bilateral symmetry at gaseous phase outlet 8 is provided with liquid phase material entrance 7 and solid-phase material entrance 9, in upper shell 1, be provided with gas-liquid separator 10, gas-liquid separator 10 is relative with gaseous phase outlet 8, gas-liquid separator 10 is installed under the reactor head gaseous phase outlet 8, gas-liquid separator 10 is set to taper shape, the circular cone drift angle is 75 °～110 °, the circular cone drift angle of present embodiment is 75 °, the conical bottom radius surface is 0.5～0.8 times of upper shell 1 radius, present embodiment conical bottom radius surface is 0.6 times of upper shell 1 radius, be provided with overfall 6 in the side of upper shell 1, in Fig. 4, in lower shell 11, be provided with guide shell 2, the top of guide shell 2 extend in the upper shell 1 and is connected with upper shell 1, communicate in the bottom of guide shell 2 and the lower shell 11, guide shell 2 radiuses are 0.55～0.8 times of lower shell 11 radiuses, present embodiment guide shell 2 radiuses are 0.6 times of lower shell 11 radiuses, the length of guide shell 2 is 1.1～1.3 times of lower shell 11 length, the length of present embodiment guide shell 2 is 1.2 times of lower shell 11 length, centre position, bottom at lower shell 11 is provided with Compressed Gas entrance 4, Compressed Gas entrance 4 and lower shell 11 are on same axis, the bottom sides of lower shell 11 is provided with slag-drip opening 3, slag-drip opening 3 can regularly be got rid of dead catalyst, also comprise liquid phase material entrance 7 and solid-phase material entrance 9 in reactor head, be provided with overfall 6 in the side of upper shell 1, by the material mouth of pipe can be continuous to the reactor convey materials, material after the reaction then enters subsequent processing by overfall, reach the purpose of continuous process, in Fig. 2 and Fig. 3, be provided with Compressed Gas distributor 5 in Compressed Gas entrance 4 and lower shell 11 junctions, Compressed Gas distributor 5 is set to spherical distribution grid, spherical distribution grid is 0.35～0.45 times of lower shell radius, the spherical distribution grid of present embodiment is 0.4 times of lower shell radius, be evenly distributed with through hole 13 at spherical distribution grid, the percent opening of spherical distribution grid is 0.15～0.3, and the percent opening of the spherical distribution grid of present embodiment is 0.2.
The course of work of the present invention is: liquid phase reacting material enters reactor body by liquid phase material entrance 7 after mixing, the solid phase reaction material enters upper shell 1 by solid-phase material entrance 9 after mixing, Compressed Gas enters by forming uniform bubble after 5 distributions of overcompression gas distributor from Compressed Gas entrance 4, gas through Compressed Gas distributor 5 enters guide shell 2, under the effect of Compressed Gas, gas in the guide shell 2, liquid and solid phase also flow up, volume of material in the guide shell 2 expands, and guide shell 2 outer liquid phase and solid phases enter in the guide shell 2, form stable circulation, thereby reach material axially and transmission radially, make material fully contact and react at guide shell 2 interior exterior domains; Compressed Gas is carried a small amount of liquid phase, solid-phase material secretly under the effect of gas-liquid separator 10 in up process, liquid phase, solid-phase material are got back in the reactor body, and gas phase component is discharged from gaseous phase outlet 8; Material through fully reaction enters subsequent processing by overfall 6.Dead catalyst or other waste residues are discharged reaction system by slag-drip opening 3.
Claims (7)
1. an organosilicon machinery-free stirs the serialization polymer reactor, it is characterized in that it comprises reactor body, Compressed Gas distributor (5), gas-liquid separator (10) and guide shell (2), described reactor body is by comprising successively upper shell (1) and lower shell (11) under upper, the centre position at the top of described upper shell (1) is provided with gaseous phase outlet (8), bilateral symmetry at gaseous phase outlet (8) is provided with liquid phase material entrance (7) and solid-phase material entrance (9), in upper shell (1), be provided with gas-liquid separator (10), gas-liquid separator (10) is relative with gaseous phase outlet (8), be provided with overfall (6) in the side of upper shell (1), in lower shell (11), be provided with guide shell (2), the top of guide shell (2) extend in the upper shell (1) and is connected with upper shell (1), communicate in the bottom of guide shell (2) and the lower shell (11), be provided with Compressed Gas entrance (4) in the centre position, bottom of lower shell (11), Compressed Gas entrance (4) and lower shell (11) are on same axis, the bottom sides of lower shell (11) is provided with slag-drip opening (3), is provided with Compressed Gas distributor (5) in Compressed Gas entrance (4) and lower shell (11) junction.
2. organosilicon machinery-free according to claim 1 stirs the serialization polymer reactor, it is characterized in that the diameter of described upper shell (1) is wider than the diameter of lower shell (11), and the length of upper shell (1) is less than the length of lower shell (11).
3. organosilicon machinery-free according to claim 2 stirs the serialization polymer reactor, the diameter that it is characterized in that described upper shell (1) is 1.5～2.3 times of lower shell (11) diameter, 0.4～0.7 times of the Length Ratio of the length of upper shell (1) and lower shell (11).
4. organosilicon machinery-free according to claim 1 stirs the serialization polymer reactor, it is characterized in that being connected by inversed taper platform (12) transition between described upper shell (1) and the lower shell (11), and the drift angle of inversed taper platform (12) is 70 °～100 °.
5. organosilicon machinery-free according to claim 1 stirs the serialization polymer reactor, it is characterized in that described Compressed Gas distributor (5) is set to spherical distribution grid, spherical distribution grid is 0.35～0.45 times of lower shell radius, be evenly distributed with through hole (13) at spherical distribution grid, the percent opening of spherical distribution grid is 0.15～0.3.
6. organosilicon machinery-free according to claim 1 stirs the serialization polymer reactor, it is characterized in that gas-liquid separator (10) is installed under the reactor head gaseous phase outlet (8), gas-liquid separator (10) is set to taper shape, the circular cone drift angle is 75 °～110 °, and the conical bottom radius surface is 0.5～0.8 times of upper shell (1) radius.
7. organosilicon machinery-free according to claim 1 stirs the serialization polymer reactor, it is characterized in that described guide shell (2) radius is 0.55～0.8 times of lower shell (11) radius, the length of guide shell (2) is 1.1～1.3 times of lower shell (11) length.
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| CN201210324383.9A CN102847490B (en) | 2012-09-05 | 2012-09-05 | Organic silicon mechanical-free stirring continuous polymerization reactor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111054278A (en) * | 2019-12-02 | 2020-04-24 | 河南金鹏化工有限公司 | Continuous production process and device for thiodicarb synthesis reaction |
| CN113231065A (en) * | 2021-05-31 | 2021-08-10 | 珠海格力电器股份有限公司 | Co/AC filter material and preparation method and application thereof |
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| CN101274245A (en) * | 2007-03-28 | 2008-10-01 | 中国石油大学(北京) | Annular space air-lift gas-solid loop flow reactor |
| CN201969548U (en) * | 2011-01-24 | 2011-09-14 | 中国石油化工股份有限公司 | Internal circulating-flow slurry bed reactor |
| CN202860505U (en) * | 2012-09-05 | 2013-04-10 | 江苏梅兰化工有限公司 | Continuous polymerization reactor without mechanical stirring for organic silicon |
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2012
- 2012-09-05 CN CN201210324383.9A patent/CN102847490B/en active Active
Patent Citations (6)
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| US4035152A (en) * | 1976-05-24 | 1977-07-12 | The United States Of America As Represented By The United States Energy Research And Development Administration | Distribution plate for recirculating fluidized bed |
| US20070145610A1 (en) * | 2004-01-15 | 2007-06-28 | Rasmus Breivik | Vapour-liquid distribution tray |
| CN1994546A (en) * | 2006-11-24 | 2007-07-11 | 哈尔滨工业大学 | Three-phase circulating fluidized bed photochemical reactor with a plurality of light sources and Fe/inorganic carrier catalyst preparation and method for processing waste water thereby |
| CN101274245A (en) * | 2007-03-28 | 2008-10-01 | 中国石油大学(北京) | Annular space air-lift gas-solid loop flow reactor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111054278A (en) * | 2019-12-02 | 2020-04-24 | 河南金鹏化工有限公司 | Continuous production process and device for thiodicarb synthesis reaction |
| CN113231065A (en) * | 2021-05-31 | 2021-08-10 | 珠海格力电器股份有限公司 | Co/AC filter material and preparation method and application thereof |
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