CN204564159U - Siloxanes cracking integrated reaction system - Google Patents
Siloxanes cracking integrated reaction system Download PDFInfo
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- CN204564159U CN204564159U CN201520221865.0U CN201520221865U CN204564159U CN 204564159 U CN204564159 U CN 204564159U CN 201520221865 U CN201520221865 U CN 201520221865U CN 204564159 U CN204564159 U CN 204564159U
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- water conservancy
- conservancy diversion
- heat exchanger
- agitator
- siloxanes
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Abstract
The utility model discloses siloxanes cracking integrated reaction system, comprise columnar kettle, the central rotating shaft be connected with external motor is vertically arranged with in kettle, feature central rotating shaft is vertically arranged with three layers of agitator, the periphery of agitator is arranged with the circulation water conservancy diversion heat exchanger tube of upper and lower side opening, the upper end of circulation water conservancy diversion heat exchanger tube is provided with charging water conservancy diversion distributor, the inner wall even distribution of kettle has the full baffle plate of 4-6 sheet limit wall water conservancy diversion, the upper end of kettle is connected with rectifying column, three layers of agitator are upper strata turbine agitator, middle level turbine agitator and lower floor's propeller agitator, circulation water conservancy diversion heat exchanger tube is up-small and down-big taper type structure, the cylindrical shell of circulation water conservancy diversion heat exchanger tube surrounds annular enclosed structure by double-layer heat exchange plate, the outer surface of heat exchanger plates is provided with embossing, advantage is the three-step reaction effectively controlling cracking process, improve heat transfer effect, optimize cracking still flow field, reach and improve ring body yield, steady production, extend reaction time, improve the object of ring body quality.
Description
Technical field
The utility model relates to a kind of siloxanes cracking integrated reaction system.
Background technology
Siloxanes is the important intermediate that organosilicon is produced, and it is the base stock preparing the polysiloxane such as silicon rubber, silicone oil.The production process of current siloxanes is that hydrolyzing chlorosilane thing is carried out cracking rearrangement reaction under base catalyst condition, with the obtained lysate containing hexam ethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethyl five siloxanes etc.Then lysate obtains silicone products through refining spearation.
The cracking of siloxanes is normally carried out in the siloxanes cracking still with stirring.Under the catalytic action of alkaline hydrogen potassium oxide, there is three-step reaction in hydrolyzing chlorosilane thing: terminal hydroxy group displacement, condensation, Cheng Huan and open loop balanced reaction in cracking still.The reaction equation of three-step reaction is as follows:
End product could be generated due to above-mentioned three-step reaction will be there is in cracking process, therefore, how effectively controlling the generation of above-mentioned three-step reaction, improve response availability, is improve ring body yield, steady production, prolongation reaction time, improve the key of ring body quality.In order to effectively control cracking reaction, reach and improve ring body yield, steady production, prolongation reaction time, improve the object of ring body quality, in cracking still structure, heat exchange mode, stirring structure etc., a lot of research unit, manufacturing enterprise have all carried out large quantity research and improvement.
Patent CN03100035.5 discloses cracking and the rectification process of hydroxy-end capped dimethyl silicone polymer, the feature of the novel cracker adopted in this patent is: have employed hinged joint open turbine stirrer, make to be able to Homogeneous phase mixing between hydrolysate and catalyst, fully contact.Have employed the heating arrangement that chuck and coil pipe combine, substantially increase the heat transfer efficiency of cracking still.Patent CN200995138Y discloses a kind of cracking still, and it is the cracker cracking still in a kind of organosilicon industry in hydrolysate cracking process.It adopts S type half-pipe jacket or band spiral stream guidance template chuck, to improve heat transfer effect.Patent CN201210221210.4 discloses a kind of organosilicon cracking reaction still paddle structure, and its its shape of paddle is bottom consistent with arc still Bottom Shape.The material of reactor lower end can be made like this to be uniformly mixed fully under the effect of paddle, the reaction rate of its reaction rate and its remaining part of reactor is consistent.
Although above-mentioned disclosed patent and document have carried out a series of improvement to the equipment of Dimethyldichlorosilane hydrolysate cracking process and operating condition, its effect has not been significantly improved.Especially do not mention in the generation of the control cracking process three-step reaction to how effectively and improve.If can not from effectively control cracking process reaction, improve heat transfer effect, optimize cracking still flow field etc. thorough improvement is done to " transport " aspect that cracking process plays a crucial role, be just difficult to break existing technical merit.
Summary of the invention
Technical problem to be solved in the utility model be to provide a kind of effective control cracking process three-step reaction, improve heat transfer effect, optimize the siloxanes cracking integrated reaction system in cracking still flow field, this system reaches and improves ring body yield, steady production, prolongation reaction time, improves the object of ring body quality.
The utility model solves the problems of the technologies described above adopted technical scheme: a kind of siloxanes cracking integrated reaction system, comprise columnar kettle, described kettle is uprightly arranged, the central rotating shaft be connected with external motor is vertically arranged with in described kettle, described central rotating shaft is vertically arranged with three layers of agitator, described agitator periphery is arranged with the circulation water conservancy diversion heat exchanger tube of upper and lower side opening, the upper end of described circulation water conservancy diversion heat exchanger tube is provided with charging water conservancy diversion distributor, the inner wall even distribution of described kettle has the full baffle plate of 4-6 sheet limit wall water conservancy diversion, the upper end of described kettle is connected with rectifying column.
Agitator described in three layers is upper strata turbine agitator, middle level turbine agitator and lower floor's propeller agitator.Stirring blade adopts Combined stirring paddle, and upper strata and middle level are turbine type, and lower floor is pusher, effectively can control the flowing flow field of reactor inner fluid, and ensure that the time of staying that terminal hydroxy group displacement, condensation, Cheng Huan and ring-opening reaction are suitable.
Described circulation water conservancy diversion heat exchanger tube is up-small and down-big taper type structure.This version coordinates combined impeller, effectively can promote the fresh material entered in still and flow from top to bottom in cylinder, and then the material flowed out bottom heat exchanger tube is along the outside bottom-up flowing of heat exchanger tube.Up-small and down-big frustum structure is also that material circulation area in the process of the outer bottom-up flowing of cylinder progressively expands, thus adds disengagement area, thus product is steamed timely and effectively.By the guide functions of circulation water conservancy diversion heat exchanger tube, effectively extend material from entering reactor to the time of staying of flowing out reactor, thus reach the three-step reaction controlling cracking process, the displacement of main generation terminal hydroxy group, condensation reaction in circulation water conservancy diversion heat exchanger tube, and mainly become ring and open loop balanced reaction outward at circulation water conservancy diversion heat exchanger tube, thus reduce the generation of side reaction, finally improve the yield of reaction.Meanwhile, circulation water conservancy diversion heat exchanger tube internal and external flow field is subject to effective water conservancy diversion of cylinder, thus reduces flowing and the consumption of back-mixing momentum, because this reducing power of agitator.
The cylindrical shell of described circulation water conservancy diversion heat exchanger tube surrounds annular enclosed structure by double-layer heat exchange plate, and the outer surface of described heat exchanger plates is provided with embossing.Gap between two-layer heat exchanger plates is used for passing into cold and hot medium, and to play heat exchange effect, the heat exchanger plates of surface embossed effectively improves the turbulence of two side liquids, compared with simple heat exchanger tube, improves heat-transfer effect.
Described charging water conservancy diversion distributor is for annular and its annulus is provided with several Liquid inject distributor pipes, and described Liquid inject distributor pipe and horizontal direction are 15-60 ° of angle and towards interior below.Charging makes charging be uniformly distributed by charging water conservancy diversion distributor and optimizes flow field and the liquid that ejects of Liquid inject distributor pipe is consistent with the flow direction of liquid in reactor, thus decreases the friction loss of fluid flowing, and improves mixed effect.
The width of the described full baffle plate of limit wall water conservancy diversion is the 1/10-1/15 of kettle diameter, the top of the described full baffle plate of limit wall water conservancy diversion flushes with the upper end of described charging water conservancy diversion distributor, and the bottom of the described full baffle plate of limit wall water conservancy diversion flushes with the bottom of described circulation water conservancy diversion heat exchanger tube.
Described rectifying column adopts efficient random packing, and the upper end of described rectifying column is connected with overhead condenser.In order to improve the speed of cracking reaction, the product that reaction generates need steam in time, but because cracking reaction thing and product boiling point differ less, while steaming product, have a large amount of reactants to steam with product, therefore, rectifying column is set in the gas-phase product outlet of cracking still, plays the effect of purified product and recovery reactant simultaneously.Select efficient random packing in rectifying column, ensure separating effect, consider the easy bonding of material simultaneously, select random packing, easy cleaning.Overhead condenser and rectifying column integrated, decrease the resistance of ducting, pipeline can be reduced simultaneously and connect, reduce and take up an area.
The outer wall of described kettle is provided with heat exchange jacket.
Compared with prior art, the utility model has the advantage of:
1, circulation water conservancy diversion heat exchanger tube is set.Circulation water conservancy diversion heat exchanger tube is up-small and down-big taper type structure.Its effect one optimizes the flow field of still inner fluid flowing, effectively controls the three-step reaction of cracking process, reduces the generation of side reaction.Reduce flowing and the consumption of back-mixing momentum, reduce power of agitator.Two is that circulation water conservancy diversion heat exchanger tube is also for high efficient heat exchanging inner member.Circulation water conservancy diversion heat exchanger tube surrounds annular enclosed structure by the double-layer heat exchange plate of surface embossed.Gap between two-layer heat exchanger plates is used for passing into cold and hot medium, and to play heat exchange effect, the heat exchanger plates of surface embossed effectively improves the turbulence of two side liquids, compared with simple heat exchanger tube, improves heat-transfer effect.In addition, in order to increase heat transfer effect, except circulation water conservancy diversion heat exchanger tube, the outer wall of cracking still is also provided with heating (cooling) chuck, for heating (cooling).
2, charging is made charging be uniformly distributed by charging water conservancy diversion distributor and is optimized flow field.Charging water conservancy diversion distributor is positioned at the upper end of circulation water conservancy diversion heat exchanger tube, and described charging is uniformly distributed as annular and its annulus is provided with several Liquid inject distributor pipes, and Liquid inject distributor pipe and horizontal direction are 15-60 ° of angle and towards interior below.Divide charging flow-guiding cloth device to ensure being evenly distributed of charging, and the injection direction of Liquid inject distributor pipe down, the liquid ejected is consistent with the flow direction of liquid, thus decreases the friction loss of fluid flowing, and improves mixed effect.
3, stirring blade adopts Combined stirring paddle.Upper strata and middle level are turbine type, and lower floor is pusher, effectively can control the flowing flow field of reactor inner fluid, and ensure that the time of staying that terminal hydroxy group displacement, condensation, Cheng Huan and ring-opening reaction are suitable.
4, integrated equipment, reduces and takes up an area, and reduces and consumes.In order to improve the speed of cracking reaction, reaction generate product need steam in time, but due to cracking reaction thing and product boiling point difference less, while steaming product, have a large amount of reactants to steam with product, therefore, rectifying column is set in the gas-phase product outlet of cracking still.Play the effect of purified product and recovery reactant simultaneously.Rectifying column internals select efficient random packing, ensure separating effect, consider the easy bonding of material simultaneously, select random packing easy cleaning.Overhead condenser and rectifying column integrated, decrease the resistance of ducting, pipeline can be reduced simultaneously and connect, reduce and take up an area.
Accompanying drawing explanation
Fig. 1 is the structural representation of the utility model siloxanes cracking integrated reaction system;
Fig. 2 is the structural representation one of the utility model circulation water conservancy diversion heat exchanger tube;
Fig. 3 is the structural representation two of the utility model circulation water conservancy diversion heat exchanger tube;
Fig. 4 is charging water conservancy diversion structure of distributor schematic diagram of the present utility model.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, the utility model is described in further detail.
Specific embodiment
Siloxanes cracking integrated reaction system, as shown in Figure 1, comprise columnar kettle 1, kettle 1 is uprightly arranged, and is vertically arranged with the central rotating shaft 3 be connected with external motor 2 in kettle 1, central rotating shaft 3 is vertically arranged with three layers of agitator, agitator periphery is arranged with the circulation water conservancy diversion heat exchanger tube 4 of upper and lower side opening, the upper end of circulation water conservancy diversion heat exchanger tube 4 is provided with charging water conservancy diversion distributor 5, and the inner wall even distribution of kettle 1 has the full baffle plate 6 of 4-6 sheet limit wall water conservancy diversion, and the upper end of kettle 1 is connected with rectifying column 7.
In this particular embodiment, as shown in Figure 1, three layers of agitator are upper strata turbine agitator 8, middle level turbine agitator 9 and lower floor's propeller agitator 10.As shown in Figures 2 and 3, circulation water conservancy diversion heat exchanger tube 4 is up-small and down-big taper type structure, and the cylindrical shell of circulation water conservancy diversion heat exchanger tube 4 surrounds annular enclosed structure by double-layer heat exchange plate 11, and the outer surface of heat exchanger plates 11 is provided with embossing.As shown in Figure 4, charging water conservancy diversion distributor 5 is for annular and its annulus is provided with several Liquid inject distributor pipes 12, and Liquid inject distributor pipe 12 and horizontal direction are 15-60 ° of angle and towards interior below.The width of the full baffle plate 6 of limit wall water conservancy diversion is the 1/10-1/15 of kettle 1 diameter, and the top of the full baffle plate 6 of limit wall water conservancy diversion flushes with the upper end of charging water conservancy diversion distributor 5, and the bottom of the full baffle plate 6 of limit wall water conservancy diversion flushes with the bottom of circulation water conservancy diversion heat exchanger tube 4.Rectifying column 7 adopts efficient random packing 13, and the upper end of rectifying column 7 is connected with overhead condenser 14, and the outer wall of kettle 1 is provided with heat exchange jacket 15.
Application Example
Above-mentioned specific embodiment siloxanes cracking integrated reaction system is adopted to carry out cracking reaction to Dimethyldichlorosilane hydrolysate.The parameter of cracking still: kettle 1 internal diameter 1200mm, through 600mm in circulation water conservancy diversion heat exchanger tube 4, the mass flow sending into siloxanes cracking integrated reaction system is: 3751kg/h, composition: ring body 66 wt%, thread 33wt%, other 1 wt%.Catalyst for cracking adopts potassium hydroxide, and catalyst charge is 190kg/h.Siloxanes cracking integrated reaction operating pressure is :-0. 095MPaG, and cracking reaction temperature is 150 DEG C.All middle pressure steam is passed in circulation water conservancy diversion heat exchanger tube 4 and heat exchange jacket 14.After the reaction of this cracking system, outlets products composition (wt%) is: disiloxane (D2): 0.32%, trisiloxanes (D3): 7.72%, tetrasiloxane (D4): 76.22%, tetrasiloxane (D5): 13.60%, six siloxanes (D6): 1.85%, seven siloxanes (D7): 0.3%.
Above-described embodiment further illustrates of the present utility model, but protection domain of the present utility model is as the criterion with claims.
Claims (8)
1. a siloxanes cracking integrated reaction system, comprise columnar kettle, described kettle is uprightly arranged, the central rotating shaft be connected with external motor is vertically arranged with in described kettle, it is characterized in that: described central rotating shaft is vertically arranged with three layers of agitator, described agitator periphery is arranged with the circulation water conservancy diversion heat exchanger tube of upper and lower side opening, the upper end of described circulation water conservancy diversion heat exchanger tube is provided with charging water conservancy diversion distributor, the inner wall even distribution of described kettle has the full baffle plate of 4-6 sheet limit wall water conservancy diversion, and the upper end of described kettle is connected with rectifying column.
2. siloxanes cracking integrated reaction system according to claim 1, is characterized in that: the agitator described in three layers is upper strata turbine agitator, middle level turbine agitator and lower floor's propeller agitator.
3. siloxanes cracking integrated reaction system according to claim 1, is characterized in that: described circulation water conservancy diversion heat exchanger tube is up-small and down-big taper type structure.
4. siloxanes cracking integrated reaction system according to claim 3, is characterized in that: the cylindrical shell of described circulation water conservancy diversion heat exchanger tube surrounds annular enclosed structure by double-layer heat exchange plate, and the outer surface of described heat exchanger plates is provided with embossing.
5. siloxanes cracking integrated reaction system according to claim 1, it is characterized in that: described charging water conservancy diversion distributor is for annular and its annulus is provided with several Liquid inject distributor pipes, described Liquid inject distributor pipe and horizontal direction are 15-60 ° of angle and towards interior below.
6. siloxanes cracking integrated reaction system according to claim 1, it is characterized in that: the width of the described full baffle plate of limit wall water conservancy diversion is the 1/10-1/15 of kettle diameter, the top of the described full baffle plate of limit wall water conservancy diversion flushes with the upper end of described charging water conservancy diversion distributor, and the bottom of the described full baffle plate of limit wall water conservancy diversion flushes with the bottom of described circulation water conservancy diversion heat exchanger tube.
7. siloxanes cracking integrated reaction system according to claim 1, it is characterized in that: described rectifying column adopts efficient random packing, the upper end of described rectifying column is connected with overhead condenser.
8. the siloxanes cracking integrated reaction system according to any one of claim 1-7, is characterized in that: the outer wall of described kettle is provided with heat exchange jacket.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104815605A (en) * | 2015-04-14 | 2015-08-05 | 中国化学赛鼎宁波工程有限公司 | Siloxane pyrolysis integrated reaction system |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN104815605A (en) * | 2015-04-14 | 2015-08-05 | 中国化学赛鼎宁波工程有限公司 | Siloxane pyrolysis integrated reaction system |
CN104815605B (en) * | 2015-04-14 | 2016-06-29 | 中国化学赛鼎宁波工程有限公司 | Siloxanes cracking integrated reaction system |
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C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150819 Termination date: 20180414 |