CN205007977U - Reactor of phenyl -chloride silane is legally produced in pyrocondensation - Google Patents

Reactor of phenyl -chloride silane is legally produced in pyrocondensation Download PDF

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Publication number
CN205007977U
CN205007977U CN201520713319.9U CN201520713319U CN205007977U CN 205007977 U CN205007977 U CN 205007977U CN 201520713319 U CN201520713319 U CN 201520713319U CN 205007977 U CN205007977 U CN 205007977U
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China
Prior art keywords
reactor
conversion zone
boiler tube
comparison circuit
bypass
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CN201520713319.9U
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方卫民
范建平
徐慧芬
宋尚海
刘国晶
杨晓义
王德球
谭军
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ZHEJIANG FUSHITE GROUP CO Ltd
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ZHEJIANG FUSHITE GROUP CO Ltd
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Abstract

The utility model provides a reactor of phenyl -chloride silane is legally produced in pyrocondensation, include the raw materials economizer bank, have the conversion zone boiler tube, the radiant coil that press from both sides the cover, wherein the entry linkage is overlapped to pressing from both sides of export of raw materials economizer bank and conversion zone boiler tube, and the clamp cover of conversion zone boiler tube exports to enter the mouth with the radiant coil and is linked together, and the radiant coil exports and conversion zone boiler tube entry is linked together, be provided with reinforced bypass between the export of radiant coil and the conversion zone boiler tube entry. Control valve in the reinforced bypass receives comparison circuit's control. The utility model provides a reactor temperature controllability is good, and easy operation, but reactor continuous production improve production efficiency.

Description

A kind of reactor of preparing phenyl chlorosilane by using thermal condensation method
Technical field
The utility model belongs to field of chemical equipment, is specifically related to a kind of reactor preparing phenyl chlorosilane.
Background technology
Phenyl chlorosilane comprises phenyl trichlorosilane and dichloromethyl phenylsilane etc., and be broad-spectrum organic silicon monomer, its consumption is only second to methylchlorosilane.Phenyl chlorosilane is a kind of purposes intermediate widely, can be used for the preparation coupling agent such as phenyltrimethoxysila,e, dimethoxydiphenylsilane and organosilicon polymer.Phenyl chlorosilane can improve the performance such as heat resistance, chemical stability, radioresistance of organosilicon product, makes organosilicon product more extensive in the application in the field such as Aero-Space, defence and military.The productivity ratio of current China phenyl chlorosilane monomer is lower, can not meet domestic demand.
The synthetic method of phenyl chlorosilane mainly comprises direct method, RMgBr method, condensation method etc.
(1) RMgBr method:
First chlorobenzene is prepared into tetraphenylphosphonium chloride magnesium solution, then generates phenyl chlorosilane and magnesium chloride with silicon tetrachloride reaction.The method selectivity of product is relatively good, but RMgBr activity is too strong, easy blast on fire, and a large amount of production and application Hazard ratio of industry are larger.
(2) direct method: by chlorobenzene and silicon under copper or silver powder catalyst 500 DEG C react,
Phenyl chlorosilane mixture is produced in reaction, through being separated obtained phenyl chlorosilane.The method raw material chlorobenzene and silica flour simple and easy to get, the conversion ratio of chlorobenzene is at about 30wt%, and major product phenyl trichlorosilane yield is at about 35wt%, but catalyst amount is 30 ~ 50wt% of silica flour consumption, and catalyst consumption amount is larger; And produce severe toxicity, carcinogenic Polychlorinated biphenyls accessory substance.
(3) condensation method:
Condensation method utilize the compound of silicon-hydrogen bond containing and aromatic series or aliphatic compound under catalyst about 600 DEG C carry out condensation reaction and generate organo-silicon compound.
HSiCl 3+C 6H 5Cl→C 6H 5SiCl 3+HCl
The production equipment of condensation method is based on tubular reactor, and equipment flowsheet is simple.The raw material of condensation method synthesis of phenyl chlorosilane is easy to get, object product yield is higher, and production cost is lower.But condensation method is very large by the impact of reaction temperature, after temperature is higher than 600 ~ 700 DEG C, the easy cracking of organic group in raw material and product, generates HSiCl 3, SiCl 4, H 2, CH 4boil accessory substance have carbon deposit generate low with HCl etc.; Material also easy disproportionation in this temperature range, the selectivity of product of generation is not high.
Authorization Notice No. is the reactor that the Chinese patent literature of CN102019155B discloses a kind of preparing phenyl chlorosilane by using thermal condensation method, comprise raw material preheating boiler tube, the conversion zone boiler tube of jacketed and radiant coil, wherein the outlet of raw material preheating pipe is connected with the JI of conversion zone boiler tube, the JO of conversion zone boiler tube is connected with radiant section furnace tube inlet, and radiant coil outlet is connected with conversion zone boiler tube entrance.Reaction mass by the chuck of raw material preheating boiler tube and conversion zone boiler tube to reaction mass preheating, after radiant coil heat temperature raising, enter conversion zone boiler tube again carry out condensation reaction, because material pipeline is longer in this reactor, each section of temperature is difficult to steady control, if the temperature of charge entering conversion zone boiler tube is too high, material thermal cracking situation is fierce, and easy coking blocking pipeline, makes product yield reduce.
Utility model content
The utility model, for addressing the deficiencies of the prior art, provides a kind of reaction temperature controllability good, preparing phenyl chlorosilane by using thermal condensation method reactor simple to operate.
The technical solution adopted in the utility model is as follows:
A reactor for preparing phenyl chlorosilane by using thermal condensation method, comprises raw material preheating pipe, conversion zone boiler tube, radiant coil and the burner for heating radiation section boiler tube with chuck; Wherein the outlet of raw material preheating pipe is connected with the JI of conversion zone boiler tube, the JO of conversion zone boiler tube is connected with radiant section furnace tube inlet, radiant coil outlet is connected with conversion zone boiler tube entrance, is provided with reinforced bypass between the outlet of described radiant coil and conversion zone boiler tube entrance.
The chuck of reaction mass through raw material preheating pipe, conversion zone boiler tube and the repeatedly heat exchange process of radiant coil, the temperature of material is higher, enters that the temperature of charge of conversion zone boiler tube is too high can affect product yield.Between radiant coil outlet and conversion zone boiler tube entrance, pipeline is provided with reinforced bypass, when the temperature of reaction system material exceeds the more suitable temperature range of condensation reaction, can through reinforced bypass in time to the material that reaction system provides temperature relatively low, the temperature of charge of timely regulation and control reaction system, ensures that material is produced under temperature range safely and efficiently.The material provided due to reinforced bypass is without raw material preheating pipe, the chuck of conversion zone boiler tube and the heat treatment process of radiant coil, therefore the temperature of material that reinforced bypass provides is than low through heat treated temperature of charge.Reinforced bypass is low larger with the temperature through heat treated material, and the regulating effect of bypass to temperature of charge during reaction might as well.
As preferably, temperature sensor is provided with in conversion zone boiler tube inlet location, described reactor is provided with for receiving temperature sensor signal and the first comparison circuit compared with first threshold, and described reinforced bypass is provided with the first control valve being controlled by the first comparison circuit output signal.
When the temperature of the material of temperature sensor measurement is greater than set first threshold, the first comparison circuit output signal the first control valve controlled in reinforced bypass regulates the mass flow of reinforced bypass.Controlled the first control valve in reinforced bypass by the first comparison circuit, more accurately and timely can regulate and control the temperature of reaction system material.
Further preferably, described reactor is provided with for receiving temperature sensor signal and the second comparison circuit compared with Second Threshold, and the fuel gas pipeline of described burner is provided with the second control valve being controlled by the second comparison circuit output signal.
Described Second Threshold is greater than first threshold, when the temperature of the material of temperature sensor measurement is greater than set Second Threshold, the second control valve on the fuel gas pipeline of the second comparison circuit output signal control combustion device, reduces the gas flow of burner by the second control valve thus reduces burner to the heating load of material.When the temperature of the material of temperature sensor measurement is less than set Second Threshold, do not produce the second comparison circuit signal, the second control valve does not limit the gas flow of burner.
Further preferred, described reactor is provided with for receiving temperature sensor signal and the 3rd comparison circuit compared with the 3rd threshold value, and is provided with the alarm being controlled by the 3rd comparison circuit output signal.
The 3rd described threshold value is greater than Second Threshold, and when the temperature of the material of temperature sensor measurement is greater than the 3rd set threshold value, the 3rd comparison circuit output signal triggered alarm is reported to the police.
In order to ensure that reinforced bypass material adds reaction system on suitable opportunity, as preferably, raw material preheating tube inlet and conversion zone coil outlet are in the homonymy of reactor, and described reinforced bypass is arranged on reactor opposite side.
Raw material preheating tube inlet and conversion zone coil outlet are in the top of reactor, and described reinforced bypass is arranged in the middle part of reactor.
Conversion zone coil outlet is reactant discharging opening, temperature is higher, conversion zone coil outlet and raw material preheating tube inlet are arranged on the top of homonymy and reactor, are conducive to the diffusion of conversion zone coil outlet place heat, increase raw material preheating pipe to the pre-heat effect of material.And reinforced bypass is arranged the opposite side at conversion zone coil outlet place and the middle part of reactor, make the distance of reinforced bypass and conversion zone coil outlet distant, reduce the heat exchange action of the material of reinforced bypass and the reactant of conversion zone coil outlet, make the temperature of the material of reinforced bypass and the Temperature Difference Ratio through heat treated material comparatively large, increase reinforced bypass material to the regulation and control efficiency of temperature of reaction system.
In sum, the temperature of reactor controllability of the condensation method synthesis of phenyl chlorosilane that the utility model provides is good, simple to operate, and reactor can continuous seepage, enhances productivity.
Accompanying drawing explanation
Fig. 1 is the structural representation of the reactor of the utility model preparing phenyl chlorosilane by using thermal condensation method;
Fig. 2 is the equipment schematic of the reactor of the utility model preparing phenyl chlorosilane by using thermal condensation method.
Detailed description of the invention
Below in conjunction with accompanying drawing, the reactor of the utility model preparing phenyl chlorosilane by using thermal condensation method is described in detail.
As shown in Figure 1, 2, the reactor of the utility model preparing phenyl chlorosilane by using thermal condensation method comprises housing, and the convective region 2 that case top is provided with chimney 3, housing central section is reactor, lower housing portion are the radiation area 1 of reactor.
Radiation area 1 is provided with radiant coil 8, be radiant coil 8 heat supply by burner, the burner that the utility model adopts is non-flaming combustion device 9, and non-flaming combustion device 9 is connected with combustion gas storage tank by pipeline, and the fuel gas supply conduit of non-flaming combustion device 9 is provided with the second control valve 17; The shell of radiation area 1 is also provided with the flame peephole 10 observing combustion case; The down either side of shell is also provided with nitrogen tube interface 12 and steam pipe interface 11.
Conversion zone boiler tube 7, the raw material preheating pipe 6 with chuck 13 is provided with in convective region 2; The entrance of raw material preheating pipe 6 and the exit of conversion zone boiler tube 7 are arranged on the same side of housing upper, and the outlet of conversion zone boiler tube 7 is discharging opening 5, and the entrance of raw material preheating pipe 6 is charging aperture 4.
Raw material preheating boiler tube 6 outlet is connected with the entrance of the chuck 13 of conversion zone boiler tube 7, the outlet of chuck 13 is connected with radiant coil 8 entrance, radiant coil 8 port of export is connected with conversion zone boiler tube 7 entrance by pipeline, conversion zone boiler tube 7 arrival end is provided with for detecting the temperature sensor 15 entering conversion zone boiler tube temperature of charge, radiant coil 8 exports on the pipeline that is connected with conversion zone boiler tube 7 entrance and is provided with reinforced bypass 14, feeds in raw material in bypass 14 and arrange the first control valve 16 in the middle part that reinforced bypass 14 is arranged on reactor reaction section boiler tube 7 exit opposite side.
The utility model reactor is also provided with alarm 18, wherein the first control valve 16, second control valve 17 and alarm 18 all accept and are controlled by the signal from temperature sensor 15, are also respectively equipped with the first comparison circuit, the second comparison circuit and the 3rd comparison circuit as to the process of signal.
The input of each comparison circuit all connects the signal output part of temperature sensor 15, wherein:
The output of the first comparison circuit connects the control end of the first control valve 16;
The output of the second comparison circuit connects the control end of the second control valve 17;
The output of the 3rd comparison circuit connects alarm 18.
When reactor of the present utility model uses, material enters reactor through charging aperture 4, react by entering conversion zone boiler tube 7 after the chuck 13 of raw material preheating pipe 6, conversion zone boiler tube 7 and radiant coil 8 pairs of heating materials, after reaction terminates, reactant discharges reactor by discharging opening 5.The temperature sensor 15 being arranged on the arrival end of conversion zone boiler tube 7 measures the temperature entering the material of conversion zone boiler tube 7, and signal is inputed to each comparison circuit respectively.
When the temperature of temperature sensor measurement is greater than set first threshold, the first comparison circuit exports road signal, opens the first control valve 16, adds cold material to reduce the temperature of the material entering conversion zone boiler tube by reinforced bypass.
When the temperature of temperature sensor measurement is greater than set Second Threshold, second comparison circuit output signal controls the second control valve 17 be arranged on the fuel gas pipeline of burner, reducing radiant coil to the heating load of material by reducing gas supply, reducing the temperature of the material through radiant coil.
When the temperature of temperature sensor is greater than the 3rd threshold value, the 3rd comparison output signal triggered alarm 18 is reported to the police.
According to technological requirement, it be first threshold is 650-700 DEG C that general each threshold value arranges scope, Second Threshold is 701-800 DEG C, the 3rd threshold value is 801-900 DEG C.In the present embodiment, first threshold is 680 DEG C, Second Threshold is 750 DEG C, the 3rd threshold value is 850 DEG C.
Reactor of the present utility model, by arranging reinforced bypass, can adjust temperature of charge in time, avoids material thermal cracking fierce, improves product yield.

Claims (6)

1. a reactor for preparing phenyl chlorosilane by using thermal condensation method, comprises raw material preheating pipe, conversion zone boiler tube, radiant coil and the burner for heating radiation section boiler tube with chuck; Wherein the outlet of raw material preheating pipe is connected with the JI of conversion zone boiler tube, the JO of conversion zone boiler tube is connected with radiant section furnace tube inlet, radiant coil outlet is connected with conversion zone boiler tube entrance, it is characterized in that, between the outlet of described radiant coil and conversion zone boiler tube entrance, be provided with reinforced bypass.
2. the reactor of preparing phenyl chlorosilane by using thermal condensation method as claimed in claim 1, it is characterized in that, temperature sensor is provided with in conversion zone boiler tube inlet location, described reactor is provided with for receiving temperature sensor signal and the first comparison circuit compared with first threshold, and described reinforced bypass is provided with the first control valve being controlled by the first comparison circuit output signal.
3. the reactor of preparing phenyl chlorosilane by using thermal condensation method as claimed in claim 2, it is characterized in that, described reactor is provided with for receiving temperature sensor signal and the second comparison circuit compared with Second Threshold, and the fuel gas pipeline of described burner is provided with the second control valve being controlled by the second comparison circuit output signal.
4. the reactor of preparing phenyl chlorosilane by using thermal condensation method as claimed in claim 3, it is characterized in that, described reactor is provided with for receiving temperature sensor signal and the 3rd comparison circuit compared with the 3rd threshold value, and is provided with the alarm being controlled by the 3rd comparison circuit output signal.
5. the reactor of preparing phenyl chlorosilane by using thermal condensation method as claimed in claim 1, it is characterized in that, raw material preheating tube inlet and conversion zone coil outlet are in the homonymy of reactor, and described reinforced bypass is arranged on reactor opposite side.
6. the reactor of preparing phenyl chlorosilane by using thermal condensation method as claimed in claim 1, it is characterized in that, raw material preheating tube inlet and conversion zone coil outlet are in the top of reactor, and described reinforced bypass is arranged in the middle part of reactor.
CN201520713319.9U 2015-09-15 2015-09-15 Reactor of phenyl -chloride silane is legally produced in pyrocondensation Active CN205007977U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201520713319.9U CN205007977U (en) 2015-09-15 2015-09-15 Reactor of phenyl -chloride silane is legally produced in pyrocondensation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201520713319.9U CN205007977U (en) 2015-09-15 2015-09-15 Reactor of phenyl -chloride silane is legally produced in pyrocondensation

Publications (1)

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CN205007977U true CN205007977U (en) 2016-02-03

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111659329A (en) * 2019-03-07 2020-09-15 江西福特化工新材料有限公司 Condensation reaction device

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111659329A (en) * 2019-03-07 2020-09-15 江西福特化工新材料有限公司 Condensation reaction device
CN111659329B (en) * 2019-03-07 2022-05-24 江西福特化工新材料有限公司 Condensation reaction device

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