CN102212080A - Reaction device for preparing methyl chlorosilane and reaction system comprising same - Google Patents
Reaction device for preparing methyl chlorosilane and reaction system comprising same Download PDFInfo
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- CN102212080A CN102212080A CN2010101466693A CN201010146669A CN102212080A CN 102212080 A CN102212080 A CN 102212080A CN 2010101466693 A CN2010101466693 A CN 2010101466693A CN 201010146669 A CN201010146669 A CN 201010146669A CN 102212080 A CN102212080 A CN 102212080A
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Abstract
The invention relates to the field of preparation of methyl chlorosilane, in particular to a reaction device for preparing methyl chlorosilane and a reaction system comprising the same. The reaction device for preparing methyl chlorosilane comprises a cylindrical slurry bed reactor, wherein an inert medium is filled in the slurry bed reactor; a contact mass prepared from a catalyst and silica power suspends in the inert medium; and a built-in heat exchanger is arranged in the slurry bed reactor. In the reactor for preparing methyl chlorosilane, the cylindrical slurry bed reactor, the built-in heat exchanger of the reactor and/or an outer inert medium circulation device externally provided with a heat exchange device are adopted firstly; by adopting the cylindrical slurry bed reactor, the residence time of methane chloride in the reactor is prolonged, and the circulation amount of methane chloride is reduced; and by adopting the built-in heat exchanger and an external heat exchanger in the reactor, heat released by the reaction can be removed easily the temperature of a catalyst bed is easy to control, side reactions are reduced, and the selectivity of dimethyl dichlorosilane is increased.
Description
Technical field
The present invention relates to prepare the methyl chlorosilane field, particularly, relate to a kind of reactive system for preparing the reaction unit of methyl chlorosilane and comprise it.
Background technology
Organosilicon has the dual performance of inorganic materials and organic materials simultaneously, and high-low temperature resistant, electric insulation, excellent specific property such as weather-proof, corrosion-resistant, nonpoisonous and tasteless are widely used in fields such as electronics, automobile, oil, chemical industry, building, aerospace.In many leading-edge fields, organosilicon material has irreplaceable special role.Methyl chlorosilane is that preparing organosilicon material most important also is the organosilane monomer of consumption maximum, be the basis and the pillar of whole organosilicon industry, its production technology and technical study are the crucial problems of chemical field always, wherein with monochloro methane and silica flour under the effect of copper catalyst directly " direct method " of synthesizing methyl-chloro-silane become the focus of research.
In the reaction of above-mentioned " direct method " synthesizing methyl-chloro-silane, because the purposes of dimethyldichlorosilane(DMCS) is wide, consumption is big, becomes the major objective product of this reaction.Because this reaction is a very exothermic reaction, if the reactor local superheating can cause the generation of by products such as METHYL TRICHLORO SILANE, but under appropriate catalyst and operational condition, the selectivity of dimethyldichlorosilane(DMCS) is improved greatly.So for productive efficiency and the operating continuity that promotes the direct method reaction unit to greatest extent, the design that mode is shifted out in the heat release of reactor internal reaction is the core content of this Technology.
At present, commercial direct method synthesizing methyl-chloro-silane is based on the Technology of fluidized-bed reactor basically.With the fluidized-bed reaction technology of unstripped gas as the contact fluidizing medium, contact is uniformly dispersed, can improve heat transfer efficiency, help shifting out of heat of reaction.But there is the fluidisation dead angle in fluidized-bed, and raw material availability is low, causes the local superheating fever, cause the decomposition of raw material monochloro methane, generate some by products, and along with the carrying out that reacts, the particle diameter of contact is more and more littler, is taken out of reactor and becomes waste catalyst by air-flow easily.Patent CN2372052 discloses a kind of fluidized-bed of synthesizing methyl-chloro-silane, can destroy air pocket, reducing silica flour takes out of, prevent dust stratification caking, local superheating fever etc., this patent mainly is by the optimum combination internals, by the cylindrical shell center vertical pipes is set, and its periphery is provided with the pipe bundle heat exchanger that the two-layer vertical pipes that is circular layout is formed, and it is imposed radially and vertically fixing the fluidized-bed of a kind of synthesizing methyl-chloro-silane of designing with slip anchor, retaining plate and tube sheet.The feature of patent CN2923012 is, cylindrical shell side in thermal oil divider bottom is provided with a plurality of syngas outlet, in the cone side on gas distributor top a plurality of feed back charging openings are set, syngas outlet is 2-4, its angle is 180 degree-90 degree, the feed back charging opening is 1-4, and this improvement can reduce the fluidisation dead angle.Patent CN1382690 provides a kind of fine silicon grain and monochloro methane of making in fluidized-bed internal reaction and the continuous directly method of synthesizing methyl-chloro-silane.In the method, with gaseous silane, other gaseous reactants, unreacted monochloro methane and contain in the product logistics self-fluidized type bed of silica soot and emit, wherein, material to small part dust and liquid silane, other liquid reactant and composition thereof forms suspension, send into again in the fluidized-bed, circulate.In order to prolong the residence time of contact in reactor, patent CN101537329 has designed a kind of fluidized-bed reactor, specifically be between the bottom of fluidized-bed reactor grid distributor and cylindrical shell, to have set up air flow guiding device, this device comprises gas distribution tube, thrust-augmenting nozzle and gas distribution orchid, gas distribution tube is made up of 2 sections bend pipes at least, the bend pipe lower end is connected with thrust-augmenting nozzle, and every section bend pipe outer end middle portion is connected with gas feed, and the thrust-augmenting nozzle the other end is connected with the gas distribution flange.Increasing behind the guiding device can the by-passing portions unstripped gas and this portion gas tangentially entered fluidized-bed, tangential admission makes the interior gas of fluidized-bed add tangential velocity on original axial velocity basis that makes progress, the feed particles spiral that makes gas and carry secretly rises, the time lengthening that the rotational flow field of formation makes the reaction mass contact.
Although fluidized-bed process has comparative advantage in the industrial production of methyl chlorosilane at present, still there are every year some patents to make improvements and innovate, but fluidized bed reactor designs must become increasingly complex, more and more be difficult to operation, cost is also more and more higher, and can not fundamentally solve fluidized-bed and have the fluidisation dead angle and cause local superheating fever, and along with the carrying out of reaction, the particle diameter of contact is more and more littler, is taken out of some problems such as reactor easily by air-flow.
Slurry attitude bed process direct method synthesizing methyl-chloro-silane is suspended in contact in a kind of thermally-stabilised, liquid inert medium that boiling point is high exactly, and elevated temperature feeds the gaseous state monochloro methane and reacts, and obtains methyl chlorosilane.Slurry attitude bed process can make contact disperse evenly and significantly improve heat transfer efficiency, helps shifting out of heat of reaction, for the insoluble problem of above-mentioned fluidized-bed, is that the slurry attitude bed process technology of main characteristic can solve than being easier to slurry attitude bed.Patent US7153991 has reported the nanometer copper catalyst precursor body of use slurry attitude bed direct method synthesizing methyl-chloro-silane and the preparation method of nano assistant, and the paste state bed reactor that uses in reaction process has agitator.Patent US5728858 discloses organo-siloxane monomer synthetic slurry attitude bed process, the paste state bed reactor of this technology has stirring rake, alkyl alcohol gasification back and hydrogen enter slurry attitude bed from reactor bottom together, resultant and unreacted light constituent shift out with the gasiform form from the top of reactor, after condensation separation, unreacted light constituent carries out reuse.Above-mentioned patent is all used the non-long tube type slurry attitude bed that has agitator, make that like this residence time of gaseous state monochloro methane in reactor is shorter, strengthened the internal circulating load of monochloro methane, but agitator is poor for the mixing of materials effect of the paste state bed reactor of long cartridge type.Because the direct method synthesizing methyl-chloro-silane is a stronger exothermic process, the exothermic heat of reaction of above-mentioned slurry attitude bed process technology does not adopt the interchanger heat exchange, but the heat absorption of shifting out that depends on the product of unreacted unstripped gas and gasification comes balance, the appropriateness of this heat-obtaining mode and intensity are difficult to control, handiness is poor, the utilization again of taking out heat is needed further to adopt the interchanger exchange, do not have economy and universality.
Summary of the invention
Therefore, the purpose of this invention is to provide a kind of reaction unit for preparing methyl chlorosilane.
Another object of the present invention provides the system of the preparation methyl chlorosilane that comprises above-mentioned reaction unit.
Reaction unit according to preparation methyl chlorosilane of the present invention, wherein, described reaction unit comprises long cartridge type slurry reactor 1, its inside comprises unstripped gas sparger 2 and paste state bed reactor 3 from the bottom to top, in the described paste state bed reactor 3 inert media is housed, the contact that catalyzer and silica flour form is suspended in the inert media, be provided with embedded heat exchanger 6 in the described paste state bed reactor 3, built-in heat exchanger can be stablized control to temperature of reaction, and exothermic heat of reaction is converted into the superheated vapour recovery.
Preferably, can comprise feedstock heat exchanger 7 according to the reaction unit of preparation methyl chlorosilane of the present invention, described feedstock heat exchanger 7 is communicated with the bottom of described long cartridge type slurry reactor 1.Raw material monochloro methane and nitrogen heat up or do not carry out heat exchange and directly enter the long tube type paste state bed reactor through the reaction product heat exchange, the bottom of the slurry attitude bed that is formed by inert media and contact behind the gas distribution grid uniform distribution is up, and monochloro methane fully contacts with the contact surface and the homogeneous of bed temperature of reaction to satisfy.For guaranteeing the constant of reaction bed temperature, the heat that produces in the reaction is by built-in interchanger 6 heat-obtainings of reactor, and its heat transferring medium can be the industrial boiler feedwater, also can be that thermal oil or other are used for the medium of heat exchange.When adopting the oiler feed heat exchange, direct by-product superheated vapour.If adopt the thermal oil heat exchange, can be by the water cooling thermal oil by-product superheated vapour, the superheated vapour of two kinds of method outputs all can be used for outer for or use by oneself.The temperature of reaction of paste state bed reactor is 200～400 ℃, and reaction pressure is 0.1～1.0MPa, and the air speed of monochloro methane is 1000～15000h
-1, the air speed of nitrogen is 0～15000h
-1Described inert media is one or more in silicone oil, compound of silicate class, whiteruss, mineral oil, aromatic hydrocarbons and derivative thereof, the fused salt equal solvents such as methyl-silicone oil and phenyl silicone oil, and heat transferring medium is water or thermal oil.
Reaction unit according to preparation methyl chlorosilane of the present invention can also comprise long cartridge type slurry reactor 1, medium circulation volume pump 4 and external heat exchangers 5, wherein, described long cartridge type slurry reactor 1 inside comprises unstripped gas sparger 2 and paste state bed reactor 3 from the bottom to top, in the described paste state bed reactor 3 inert media is housed; One end of described medium circulation volume pump 4 is communicated with the side wall upper part of described paste state bed reactor 3, the other end is communicated with described external heat exchangers 5, the other end of described external heat exchangers 5 is communicated with the lower sidewall of described paste state bed reactor 3, under the effect of described medium circulation volume pump 4, inert media is transferred to the bottom of described paste state bed reactor 3 from the top of described paste state bed reactor 3.Therefore, medium circulation volume pump 4 and external heat exchangers 5 have constituted the external circulating device of inert media.Inert media is transferred to the bottom from reactor top by pump under the effect of external circulating device, strengthen mixing of materials, and external heat exchanger 5 can be stablized control to temperature of reaction, and exothermic heat of reaction is converted into the superheated vapour recovery.The contact that catalyzer and silica flour form is suspended in the inert media.
Preferably, the reaction unit of above-mentioned preparation methyl chlorosilane can comprise feedstock heat exchanger 7, and described feedstock heat exchanger 7 is communicated with the bottom of described long cartridge type slurry reactor 1.Raw material monochloro methane and nitrogen heat up or do not carry out heat exchange and directly enter the long tube type paste state bed reactor through the reaction product heat exchange, the bottom of the slurry attitude bed that is formed by inert media and contact behind the gas distribution grid uniform distribution is up, and monochloro methane fully contacts with the contact surface and the homogeneous of bed temperature of reaction to satisfy.For guaranteeing the constant of reaction bed temperature, the heat that produces in the reaction is by the inert media external circulating device heat-obtaining that has external heat-exchanger rig 5, and its heat transferring medium can be the industrial boiler feedwater, also can be that thermal oil or other are used for the medium of heat exchange.When adopting the oiler feed heat exchange, direct by-product superheated vapour.If adopt the thermal oil heat exchange, can be by the water cooling thermal oil by-product superheated vapour, the superheated vapour of two kinds of method outputs all can be used for outer for or use by oneself.
Preferably, the above-mentioned reaction unit according to the present invention, in the system of the inert media external circulating device that has heat-exchanger rig, can have liquid-solid separator 8, one end of described solid-liquid separator 8 is communicated with the side wall upper part of described paste state bed reactor 3, and the other end is communicated with described medium circulation volume pump 4.Can from reactive system, isolate waste catalyst and/or useless inert media according to reaction needed, replenish fresh inert media and contact simultaneously.
When using above-mentioned reaction unit to prepare methyl chlorosilane, the temperature of reaction of long cartridge type slurry reactor 1 is 200～400 ℃, and reaction pressure is 0.1～1.0MPa, and the air speed of monochloro methane is 1000～15000h
-1, the air speed of nitrogen is 0～15000h
-1Described inert media is one or more in silicone oil, compound of silicate class, whiteruss, mineral oil, aromatic hydrocarbons and derivative thereof, the fused salt equal solvents such as methyl-silicone oil and phenyl silicone oil, and heat transferring medium is water or thermal oil.
Reaction unit according to preparation methyl chlorosilane of the present invention can comprise long cartridge type slurry reactor 1, medium circulation volume pump 4 and external heat exchangers 5, wherein, comprise unstripped gas sparger 2 and paste state bed reactor 3 from the bottom to top in the described long cartridge type slurry reactor 1, in the described paste state bed reactor 3 inert media is housed, is provided with embedded heat exchanger 6 in the described paste state bed reactor 3; One end of described medium circulation volume pump 4 is communicated with the side wall upper part of described paste state bed reactor 3, the other end is communicated with described external heat exchangers 5, the other end of described external heat exchangers 5 is communicated with the lower sidewall of described paste state bed reactor 3, under the effect of described medium circulation volume pump 4, inert media is transferred to the bottom of described paste state bed reactor 3 from the top of described paste state bed reactor 3.
Reaction unit according to above-mentioned preparation methyl chlorosilane of the present invention, inert media is transferred to the bottom from reactor top by pump under the effect of external circulating device (medium circulation volume pump 4), strengthen mixing of materials, the built-in heat exchanger 6 and the external heat exchanger 5 of slurry attitude bed can be stablized control to temperature of reaction, and exothermic heat of reaction is converted into the superheated vapour recovery.
Preferably, according to the reaction unit of preparation methyl chlorosilane of the present invention, can comprise feedstock heat exchanger 7, described feedstock heat exchanger 7 is communicated with the bottom of described long cartridge type slurry reactor 1.The contact that catalyzer and silica flour form is suspended in the inert media, raw material monochloro methane and nitrogen heat up or do not carry out heat exchange and directly enter long tube type paste state bed reactor 3 through the reaction product heat exchange, the bottom of the slurry attitude bed that is formed by inert media and contact behind the gas distribution grid uniform distribution is up, and monochloro methane fully contacts with the contact surface and the homogeneous of bed temperature of reaction to satisfy.For guaranteeing the constant of reaction bed temperature, the heat that produces in the reaction is by reactor built-in interchanger 6 and the inert media external circulating device heat-obtaining that has external heat exchanger 5, its heat transferring medium can be industrial boiler feedwater, also can be that thermal oil or other are used for the medium of heat exchange.When adopting the oiler feed heat exchange, direct by-product superheated vapour.If adopt the thermal oil heat exchange, can be by the water cooling thermal oil by-product superheated vapour, the superheated vapour of two kinds of method outputs all can be used for outer for or use by oneself.
Preferably, reaction unit according to preparation methyl chlorosilane of the present invention, in the system of the inert media external circulating device that has heat-exchanger rig, have liquid-solid separator 8, can be according to reaction needed, from reactive system, isolate waste catalyst or useless inert media, replenish fresh inert media and contact simultaneously.The temperature of reaction of paste state bed reactor is 200～400 ℃, and reaction pressure is 0.1～1.0MPa, and the air speed of monochloro methane is 1000～15000h
-1, the air speed of nitrogen is 0～15000h
-1Described inert media is one or more in silicone oil, compound of silicate class, whiteruss, mineral oil, aromatic hydrocarbons and derivative thereof, the fused salt equal solvents such as methyl-silicone oil and phenyl silicone oil, and heat transferring medium is water or thermal oil.
Therefore, the present invention also provides a kind of system for preparing methyl chlorosilane, and it comprises the reaction unit of above-mentioned preparation methyl chlorosilane, also comprises heat exchanger 9 and 10, gas- liquid separator 11 and 12 and medium reuse volume pump 13;
Wherein,
Described reaction unit can comprise long cartridge type slurry reactor 1, its inside comprises unstripped gas sparger 2 and paste state bed reactor 3 from the bottom to top, in the described paste state bed reactor 3 inert media is housed, wherein, be provided with embedded heat exchanger 6 in the described paste state bed reactor 3
Perhaps, described reaction unit comprises long cartridge type slurry reactor 1, medium circulation volume pump 4 and external heat exchangers 5, in the described paste state bed reactor 3 inert media is housed, one end of described medium circulation volume pump 4 is communicated with the side wall upper part of described paste state bed reactor 3, the other end is communicated with described external heat exchangers 5, the other end of described external heat exchangers 5 is communicated with the lower sidewall of described paste state bed reactor 3, under the effect of described medium circulation volume pump 4, inert media is transferred to the bottom of described paste state bed reactor 3 from the top of described paste state bed reactor 3
Perhaps, described reaction unit comprises long cartridge type slurry reactor 1, medium circulation volume pump 4 and external heat exchangers 5, in the described paste state bed reactor 3 inert media is housed, be provided with embedded heat exchanger 6 in the described paste state bed reactor 3, one end of described medium circulation volume pump 4 is communicated with the side wall upper part of described paste state bed reactor 3, the other end is communicated with described external heat exchangers 5, the other end of described external heat exchangers 5 is communicated with the lower sidewall of described paste state bed reactor 3, under the effect of described medium circulation volume pump 4, inert media is transferred to the bottom of described paste state bed reactor 3 from the top of described paste state bed reactor 3
The top of described long cartridge type slurry reactor 1 is communicated with the top of described condenser 9, the top of described gas-liquid separator 11 is communicated with the bottom of described heat exchanger 9 and the top of described condenser 10 respectively, the bottom of described gas-liquid separator 11 is communicated with an end of described medium reuse volume pump 13, the other end of described medium reuse volume pump 13 is communicated with another opposing sidewalls bottom of paste state bed reactor 3, and the top of described gas-liquid separator 12 is communicated with the bottom of institute condenser 10 and the bottom of described long cartridge type slurry reactor 1 respectively.
Preferably, reaction unit according to preparation methyl chlorosilane of the present invention, in the system of the inert media external circulating device that has heat-exchanger rig, have liquid-solid separator 8, can be according to reaction needed, from reactive system, isolate waste catalyst or useless inert media, replenish fresh inert media and contact simultaneously.
The temperature of reaction of described paste state bed reactor 3 is 200～400 ℃, and reaction pressure is 0.1～1.0MPa, and the air speed of monochloro methane is 1000～15000h
-1, the air speed of nitrogen is 0～15000h
-1By above-mentioned reactive system, after unreacted monochloro methane and resultant shift out from the paste state bed reactor upper end with the gasiform form, through once cooling (condenser 9), the control air outlet temperature is 120～200 ℃, isolate some inert medias of carrying secretly and carry out reuse by medium reuse volume pump 13, after institute's condenser 10 secondaries cooling, the control air outlet temperature is 10～30 ℃, the liquid product that obtains is transported to the product purification unit, obtains unreacted monochloro methane gas and is transported to long cartridge type slurry reactor 1 and carries out reuse.Described inert media is one or more in silicone oil, compound of silicate class, whiteruss, mineral oil, aromatic hydrocarbons and derivative thereof, the fused salt equal solvents such as methyl-silicone oil and phenyl silicone oil, and heat transferring medium is water or thermal oil.
The invention has the advantages that:
1, the present invention's reactor of preparing methyl chlorosilane has at first adopted a kind of long tube type paste state bed reactor, its built-in heat exchanger and/or have the inert media external circulating device of heat-exchanger rig outward, long tube type slurry attitude bed has increased the residence time of monochloro methane in reactor, reduced the internal circulating load of monochloro methane, the exothermic heat of reaction that all can make built-in heat exchanger in the reactor and external heat exchanger shifts out easily with reaction bed temperature and is easier to control, be beneficial to the generation that reduces side reaction, improve the selectivity of dimethyldichlorosilane(DMCS).
2, the external circulating device that has an inert media replaces the mixing of materials that built-in agitator is strengthened the paste state bed reactor of long cartridge type, has solved agitator and has been unfavorable for the mixing of materials of long cartridge type paste state bed reactor and the problems such as installation that built-in heat exchanger is unfavorable for agitator.
3, in the system of inert media external circulating device, have liquid-solid separator, can in time from reactive system, isolate waste catalyst and/or useless inert media, replenish the slurry of fresh inert media and contact simultaneously according to reaction needed.
4, in the built-in heat-exchange system of paste state bed reactor and external heat-exchange system, single-stage or multi-stage heat-exchanger have been installed, to prepare methyl chlorosilane reaction liberated heat and be used to produce superheated vapour and enriching and recovering, and react the heat that self produces and be easier to recycling.
5, long tube type paste state bed reactor built-in and the external heat exchanger formula can be stablized reaction bed temperature in the control reaction process, and also being suitable for other is the gas-solid reaction of feature with the thermopositive reaction.
Description of drawings
Fig. 1 is the system according to the preparation methyl chlorosilane of embodiments of the invention 1.
Fig. 2 is the system according to the preparation methyl chlorosilane of embodiments of the invention 2.
Fig. 3 is the system according to the preparation methyl chlorosilane of embodiments of the invention 3.
Description of drawings:
1: long cartridge type slurry reactor 2: unstripped gas sparger
3: paste state bed reactor 4: the medium circulation volume pump
5: external heat exchangers 6: embedded heat exchanger
7: feedstock heat exchanger 8: liquid-solid separator
9: condenser 10: condenser
11: gas-liquid separator 12: gas-liquid separator
13: medium reuse volume pump
Embodiment
Below further specify the concrete implementation step of processing method of the present invention by accompanying drawing 1, accompanying drawing 2 and accompanying drawing 3.
As shown in Figure 1, unstripped gas monochloro methane and nitrogen at first are warmed up to 250 ℃ by feedstock heat exchanger 7 before entering reactor, enter the paste state bed reactor 3 that inert media is housed through unstripped gas sparger 2 then, in temperature of reaction is 300 ℃, reaction pressure is to react under the 0.3MPa, and the reaction velocity of adjusting the unstripped gas monochloro methane is 8000h
-1, the air speed of nitrogen is 10000h
-1Constant in order to ensure reactor batch temperature, the built-in heat exchanger 6 timely heat-obtainings of heat by fluidized-bed reactor are emitted in reaction, and the superheated vapour more than the by-product 1.5MPa.After in paste state bed reactor 3, finishing the product of reaction and unreacted monochloro methane and shifting out from paste state bed reactor 3 upper ends with the gasiform form, after condenser 9 once cools off, through gas-liquid separator 11, the control air outlet temperature is 160 ℃, the inert media of liquid for being entrained with carries out reuse through volume pump 13.The gas that comes out through gas-liquid separator 11, after the cooling of condenser 10 secondaries, through gas-liquid separator 12, the control air outlet temperature is 20 ℃, gas is unreacted monochloro methane, carries out reuse through reuse feedstock heat exchanger 7, and liquid also is product, be transported to the product purification unit, the selectivity that obtains dimethyldichlorosilane(DMCS) reaches 84%.
Embodiment 2
As shown in Figure 2, unstripped gas monochloro methane and nitrogen at first are warmed up to 250 ℃ by feedstock heat exchanger 7 before entering reactor, enter the paste state bed reactor 3 that inert media is housed through unstripped gas sparger 2 then, in temperature of reaction is 300 ℃, reaction pressure is to react under the 0.3MPa, and the reaction velocity of adjusting the unstripped gas monochloro methane is 8000h
-1, the air speed of nitrogen is 10000h
-1Constant in order to ensure reactor batch temperature, the external heat exchanger 5 timely heat-obtainings of heat by fluidized-bed reactor are emitted in reaction, and the superheated vapour more than the by-product 1.5MPa.By regulating medium circulation volume pump 4, make inert media under the effect of external circulating device, transfer to the bottom by pump from reactor top, strengthen mixing of materials.In the system of the inert media external circulating device that has heat-exchanger rig, have liquid-solid separator 8, can from reactive system, isolate waste catalyst or useless inert media according to reaction needed, replenish the slurry of fresh inert media and contact simultaneously.After in paste state bed reactor 3, finishing the product of reaction and unreacted monochloro methane and shifting out from paste state bed reactor 3 upper ends with the gasiform form, after condenser 9 once cools off, through gas-liquid separator 11, the control air outlet temperature is 160 ℃, the inert media of liquid for being entrained with carries out reuse through volume pump 13.The gas that comes out through gas-liquid separator 11, after the cooling of condenser 10 secondaries, through gas-liquid separator 12, the control air outlet temperature is 20 ℃, gas is unreacted monochloro methane, carries out reuse through reuse feedstock heat exchanger 7, and liquid also is product, be transported to the product purification unit, the selectivity that obtains dimethyldichlorosilane(DMCS) reaches 89%.
Embodiment 3
As shown in Figure 3, unstripped gas monochloro methane and nitrogen at first are warmed up to 250 ℃ by feedstock heat exchanger 7 before entering reactor, enter the paste state bed reactor 3 that inert media is housed through unstripped gas sparger 2 then, in temperature of reaction is 300 ℃, reaction pressure is to react under the 0.3MPa, and the reaction velocity of adjusting the unstripped gas monochloro methane is 8000h
-1, the air speed of nitrogen is 10000h
-1Constant in order to ensure reactor batch temperature, built-in heat exchanger 6 and the external heat exchanger 5 timely heat-obtainings of heat by fluidized-bed reactor are emitted in reaction, and the superheated vapour more than the by-product 1.5MPa.By regulating medium circulation volume pump 4, make inert media under the effect of external circulating device, transfer to the bottom by pump from reactor top, strengthen mixing of materials.In the system of the inert media external circulating device that has heat-exchanger rig, have liquid-solid separator 8, can from reactive system, isolate waste catalyst or useless inert media according to reaction needed, replenish fresh inert media and contact simultaneously.After in paste state bed reactor 3, finishing the product of reaction and unreacted monochloro methane and shifting out from paste state bed reactor 3 upper ends with the gasiform form, after condenser 9 once cools off, through gas-liquid separator 11, the control air outlet temperature is 160 ℃, the inert media of liquid for being entrained with carries out reuse through volume pump 13.The gas that comes out through gas-liquid separator 11, after the cooling of condenser 10 secondaries, through gas-liquid separator 12, the control air outlet temperature is 20 ℃, gas is unreacted monochloro methane, carries out reuse through reuse feedstock heat exchanger 7, and liquid also is product, be transported to the product purification unit, the selectivity that obtains dimethyldichlorosilane(DMCS) reaches 92%.
Claims (10)
1. reaction unit for preparing methyl chlorosilane, it is characterized in that, described reaction unit comprises long cartridge type slurry reactor (1), its inside comprises unstripped gas sparger (2) and paste state bed reactor (3) from the bottom to top, described paste state bed reactor is equipped with inert media in (3), is provided with embedded heat exchanger (6) in the described paste state bed reactor (3).
2. the reaction unit of preparation methyl chlorosilane according to claim 1 is characterized in that, described device also comprises feedstock heat exchanger (7), and described feedstock heat exchanger (7) is communicated with the bottom of described long cartridge type slurry reactor (1).
3. a reaction unit for preparing methyl chlorosilane is characterized in that, described reaction unit comprises long cartridge type slurry reactor (1), medium circulation volume pump (4) and external heat exchangers (5),
Wherein,
Described long cartridge type slurry reactor (1) inside comprises unstripped gas sparger (2) and paste state bed reactor (3) from the bottom to top, and described paste state bed reactor is equipped with inert media in (3);
One end of described medium circulation volume pump (4) is communicated with the side wall upper part of described paste state bed reactor (3), the other end is communicated with described external heat exchangers (5), the other end of described external heat exchangers (5) is communicated with the lower sidewall of described paste state bed reactor (3), under the effect of described medium circulation volume pump (4), inert media is transferred to the bottom of described paste state bed reactor (3) by described medium circulation volume pump (4) from the top of described paste state bed reactor (3).
4. the reaction unit of preparation methyl chlorosilane according to claim 3, it is characterized in that, described reaction unit also comprises solid-liquid separator (8), one end of described solid-liquid separator (8) is communicated with the side wall upper part of described paste state bed reactor (3), and the other end is communicated with described outer medium circulation volume pump (4).
5. the reaction unit of preparation methyl chlorosilane according to claim 3 is characterized in that, described device also comprises feedstock heat exchanger (7), and described feedstock heat exchanger (7) is communicated with the bottom of described long cartridge type slurry reactor (1).
6. a reaction unit for preparing methyl chlorosilane is characterized in that, described reaction unit comprises long cartridge type slurry reactor (1), medium circulation volume pump (4) and external heat exchangers (5),
Wherein,
Comprise unstripped gas sparger (2) and paste state bed reactor (3) in the described long cartridge type slurry reactor (1) from the bottom to top, be provided with embedded heat exchanger (6) in the described paste state bed reactor (3), and in the described paste state bed reactor (3) inert media is housed;
One end of described medium circulation volume pump (4) is communicated with the side wall upper part of described paste state bed reactor (3), the other end is communicated with described external heat exchangers (5), the other end of described heat exchanger (5) is communicated with the lower sidewall of described paste state bed reactor (3), under the effect of described medium circulation volume pump (4), inert media is transferred to the bottom of described paste state bed reactor (3) from the top of described paste state bed reactor (3).
7. the reaction unit of preparation methyl chlorosilane according to claim 6, it is characterized in that, described reaction unit also comprises solid-liquid separator (8), one end of described solid-liquid separator (8) is communicated with the side wall upper part of described paste state bed reactor (3), and the other end is communicated with described medium circulation volume pump (4).
8. the reaction unit of preparation methyl chlorosilane according to claim 6 is characterized in that, described device also comprises feedstock heat exchanger (7), and described feedstock heat exchanger (7) is communicated with the bottom of described long cartridge type slurry reactor (1).
9. a system for preparing methyl chlorosilane is characterized in that, described system comprises reaction unit, condenser (9) and (10), gas-liquid separator (11) and (12) and the medium reuse volume pump (13) for preparing methyl chlorosilane;
Wherein,
Described reaction unit comprises long cartridge type slurry reactor (1), its inside comprises unstripped gas sparger (2) and paste state bed reactor (3) from the bottom to top, described paste state bed reactor is equipped with inert media in (3), wherein, be provided with embedded heat exchanger (6) in the described paste state bed reactor (3), and/or, described reaction unit also comprises medium circulation volume pump (4) and external heat exchangers (5), one end of described medium circulation volume pump (4) is communicated with by the side wall upper part of described solid-liquid separator (8) with described paste state bed reactor (3), the other end is communicated with described external heat exchangers (5), the other end of described external heat exchangers (5) is communicated with the lower sidewall of described paste state bed reactor (3), under the effect of described medium circulation volume pump (4), inert media is transferred to the bottom of described paste state bed reactor (3) from the top of described paste state bed reactor (3)
The top of described long cartridge type slurry reactor (1) is communicated with the top of described condenser (9), the top of described gas-liquid separator (11) is communicated with the bottom of described condenser (9) and the top of described condenser (10) respectively, the bottom of described gas-liquid separator (11) is communicated with an end of described medium reuse volume pump (13), the other end of described medium reuse volume pump (13) is communicated with another opposing sidewalls bottom of paste state bed reactor (3), and the top of described gas-liquid separator (12) is communicated with the bottom of described heat exchanger (10) and the bottom of described long cartridge type slurry reactor (1) respectively.
10. the system of preparation methyl chlorosilane according to claim 9, it is characterized in that, described device also comprises feedstock heat exchanger (7), one end of described feedstock heat exchanger (7) is communicated with the bottom of described long cartridge type slurry reactor (1), and the other end is communicated with the top of described gas-liquid separator (12).
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172072A (en) * | 2011-12-20 | 2013-06-26 | 储晞 | Reactor and method for realizing synthesis of chlorosilane |
| CN105296956A (en) * | 2015-11-20 | 2016-02-03 | 沈阳黎明航空发动机(集团)有限责任公司 | Aluminizing process method for inner cavity and outer surface of cobalt-base alloy blade |
| CN106749380A (en) * | 2017-02-23 | 2017-05-31 | 镇江江南化工有限公司 | A kind of methyl chlorosilane monomer synthesizes circulating reaction system |
| CN109821483A (en) * | 2019-03-28 | 2019-05-31 | 合盛硅业股份有限公司 | The automatic continuous adding method of catalyst and device |
| CN113200834A (en) * | 2021-05-15 | 2021-08-03 | 公主岭市恒昌科技有限公司 | Method for preparing hydroxypivalaldehyde |
| CN114130328A (en) * | 2021-11-10 | 2022-03-04 | 北京中教金源科技有限公司 | Photo-thermal synergistic continuous phase catalytic system |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5728858A (en) * | 1996-10-10 | 1998-03-17 | Osi Specialties, Inc. | Activation of copper-silicon slurries for the direct synthesis of trialkoxysilanes |
| CN2372052Y (en) * | 1997-07-07 | 2000-04-05 | 吉林化学工业股份有限公司电石厂 | Phi 1.2 meter fluidized bed for synthesizing methylchlorosilane |
| CN1483037A (en) * | 2000-12-01 | 2004-03-17 | ��³�նٹ�˾ | Rochow-muller direct synthesis using nanosized copper catalyst precursors |
| CN101456877A (en) * | 2008-12-08 | 2009-06-17 | 江苏宏达新材料股份有限公司 | Contact masses processing method during methylchlorosilane synthesis |
| CN101480595A (en) * | 2009-01-08 | 2009-07-15 | 浙江大学 | Slurry bubble column reactor with needle type fin column tube bundle |
-
2010
- 2010-04-12 CN CN2010101466693A patent/CN102212080A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5728858A (en) * | 1996-10-10 | 1998-03-17 | Osi Specialties, Inc. | Activation of copper-silicon slurries for the direct synthesis of trialkoxysilanes |
| CN2372052Y (en) * | 1997-07-07 | 2000-04-05 | 吉林化学工业股份有限公司电石厂 | Phi 1.2 meter fluidized bed for synthesizing methylchlorosilane |
| CN1483037A (en) * | 2000-12-01 | 2004-03-17 | ��³�նٹ�˾ | Rochow-muller direct synthesis using nanosized copper catalyst precursors |
| CN101456877A (en) * | 2008-12-08 | 2009-06-17 | 江苏宏达新材料股份有限公司 | Contact masses processing method during methylchlorosilane synthesis |
| CN101480595A (en) * | 2009-01-08 | 2009-07-15 | 浙江大学 | Slurry bubble column reactor with needle type fin column tube bundle |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103172072A (en) * | 2011-12-20 | 2013-06-26 | 储晞 | Reactor and method for realizing synthesis of chlorosilane |
| CN103172072B (en) * | 2011-12-20 | 2016-08-17 | 储晞 | Realize reactor and the method for chlorosilane synthesis |
| CN105296956A (en) * | 2015-11-20 | 2016-02-03 | 沈阳黎明航空发动机(集团)有限责任公司 | Aluminizing process method for inner cavity and outer surface of cobalt-base alloy blade |
| CN106749380A (en) * | 2017-02-23 | 2017-05-31 | 镇江江南化工有限公司 | A kind of methyl chlorosilane monomer synthesizes circulating reaction system |
| CN106749380B (en) * | 2017-02-23 | 2020-04-07 | 镇江江南化工有限公司 | Methyl chlorosilane monomer synthesis circulation reaction system |
| CN109821483A (en) * | 2019-03-28 | 2019-05-31 | 合盛硅业股份有限公司 | The automatic continuous adding method of catalyst and device |
| CN113200834A (en) * | 2021-05-15 | 2021-08-03 | 公主岭市恒昌科技有限公司 | Method for preparing hydroxypivalaldehyde |
| CN114130328A (en) * | 2021-11-10 | 2022-03-04 | 北京中教金源科技有限公司 | Photo-thermal synergistic continuous phase catalytic system |
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