CN113845540B - System and method for synthesizing organic silicon monomer - Google Patents

System and method for synthesizing organic silicon monomer Download PDF

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Publication number
CN113845540B
CN113845540B CN202111281809.2A CN202111281809A CN113845540B CN 113845540 B CN113845540 B CN 113845540B CN 202111281809 A CN202111281809 A CN 202111281809A CN 113845540 B CN113845540 B CN 113845540B
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chloromethane
separation device
tank
tower
mixed monomer
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CN113845540A (en
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陈国辉
王三跃
后文杰
张�杰
杨银银
杜鹃
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Xinjiang Jingshuo New Material Co ltd
Xinte Energy Co Ltd
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Xinjiang Jingshuo New Material Co ltd
Xinte Energy Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02Silicon compounds
    • C07F7/08Compounds having one or more C—Si linkages
    • C07F7/12Organo silicon halides
    • C07F7/16Preparation thereof from silicon and halogenated hydrocarbons direct synthesis
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention provides a system and a method for synthesizing an organosilicon monomer, wherein the system comprises the following steps: the device comprises a synthesis device, a first separation device, a heat exchange device and a second separation device; the synthesizing apparatus includes: the device comprises a chloromethane air supply device, a charging tank, a fluidized bed, a first cyclone separation device, a second cyclone separation device, a third cyclone separation device and a first recovery device; the first separation device includes: the device comprises a washing tower, a lower reflux pump, a stripping tower, a second recovery device and a first condensing device; the heat exchange device includes: a heat exchanger, a first cooler and a chlorosilane tank; the second separation device includes: a chlorosilane mixed monomer tower, a reboiler and a chloromethane recovery device; according to the invention, the operation of operators is simplified, the labor cost and the machine material consumption are saved, the overhaul period is shortened, the process flow is shortened, the equipment investment is reduced, and the energy consumption is reduced.

Description

System and method for synthesizing organic silicon monomer
Technical Field
The invention relates to the technical field of organosilicon monomer synthesis processes, in particular to a system and a method for synthesizing organosilicon monomers.
Background
At present, the domestic industrial synthesis of methyl chlorosilane mainly adopts a direct method process route, namely silicon powder and methyl chloride are used as raw materials, copper powder is used as a catalyst, and gas-solid reaction is carried out in a fluidized bed reactor under specific conditions to generate a methyl chlorosilane mixture; washing methyl chlorosilane mixed monomers generated by the reaction to remove dust and high-boiling substances in synthesis gas, obtaining clean liquid-phase chlorosilane, separating unreacted chloromethane from the liquid-phase chlorosilane by a liquid-phase chlorosilane mixed monomer tower, recycling the unreacted chloromethane for synthesis reaction, and extracting methyl chlorosilane mixture generated by the reaction from the tower kettle and delivering the methyl chlorosilane mixture to a liquid-phase chlorosilane mixed monomer tank.
The direct method process route leads to complex production process, more product component types and great separation difficulty in the subsequent working section; the automation degree of individual systems of the production device is low, human participation factors are more, repeated labor of workers is more, production efficiency is low, and misoperation with a certain probability exists; and the monomer synthesis process route is inherited for years, and the defects of short process, more equipment, large device construction investment and the like exist.
Disclosure of Invention
The invention provides a system and a method for synthesizing an organic silicon monomer, which are used for solving the problems of complex production process, high separation difficulty in the subsequent working section and low automation degree in the prior art, and have misoperation with a certain probability; and the monomer synthesis process route has the problems of short flow, more equipment and large device construction investment.
In order to solve the above problems, the present invention is achieved as follows:
in a first aspect, the present invention provides a system for the synthesis of a silicone monomer, comprising:
the device comprises a synthesis device, a first separation device, a heat exchange device and a second separation device;
the synthesizing apparatus includes: the device comprises a chloromethane air supply device, a charging tank, a fluidized bed, a first cyclone separation device, a second cyclone separation device, a third cyclone separation device and a first recovery device; wherein the charging tank and the chloromethane air supply device are connected with the fluidized bed; the top of the fluidized bed is connected with the first cyclone separation device; the first cyclone separation device is connected with the second cyclone separation device; the second cyclone separation device is connected with the third cyclone separation device; the top of the third cyclone separation device is connected with the first separation device, and the bottom of the third cyclone separation device is connected with the first recovery device;
the first separation device includes: the device comprises a washing tower, a lower reflux pump, a stripping tower, a second recovery device and a first condensing device; wherein the first separation device is connected with the synthesis device through the washing tower; the lower end of the washing tower is connected with the stripping tower through a lower reflux pump; the top of the stripping tower is connected with the tower kettle of the washing tower; the bottom of the stripping tower is connected with the second recovery device; the top of the washing tower is connected with the first condensing device; the first condensing device is connected with the heat exchange device and the second separating device;
the heat exchange device includes: a heat exchanger, a first cooler and a chlorosilane tank; wherein the heat exchange device is connected with the first condensing device through the heat exchanger; the heat exchanger is connected with the first cooler and the second separation device; the first cooler is connected with the chlorosilane tank;
the second separation device includes: a chlorosilane mixed monomer tower, a reboiler and a chloromethane recovery device; the second separation device is connected with the first separation device through the chlorosilane mixed monomer tower; the chlorosilane mixed monomer tower is connected with the reboiler and the chloromethane recovery device; the second separation device is connected with the synthesis device through the chloromethane recovery device.
Optionally, the charging tank includes: silica powder charging jar and copper powder charging jar.
Optionally, the second cyclone separating apparatus comprises: a second cyclone separator and a venturi jet device; wherein the second cyclone separation device is connected with the first cyclone separation device through the second cyclone separator; the first end of the Venturi jetting device is connected with the bottom of the second cyclone separator; the first end of the venturi jet device is connected with the fluidized bed.
Optionally, the third cyclone separating apparatus comprises: the third cyclone separator, the receiving hopper and the discharging hopper; wherein one end of the receiving hopper is connected with the third cyclone separator; the other end of the receiving hopper is connected with one end of the discharging hopper; the other end of the discharge hopper is connected with the fluidized bed and the first recovery device.
Optionally, the first recovery device includes: the device comprises a contact body tank, a cloth bag filter, a solid waste treatment device and a tail gas washing device; wherein the fluidized bed and the third cyclone separation device are connected with the contact tank; the bottom of the touch body tank is connected with the solid waste treatment device, the top of the touch body tank is connected with one end of the cloth bag filter, and the other end of the cloth bag filter is connected with the tail gas washing device.
Optionally, the second recovery device includes: a sedimentation kettle, a sedimentation reflux pump and a slurry and slag treatment device; wherein the second recovery device is connected with the stripping tower through the precipitation kettle; the top and the bottom of the precipitation kettle are connected with the precipitation reflux pump; the sedimentation reflux pump is also connected with the slurry and slag treatment device.
Optionally, the first condensing device includes: the air cooler, the first condenser, the upper reflux pump and the chlorosilane mixed monomer intermediate tank; the first condensing device is connected with the washing tower, the first condenser and the chlorosilane mixed monomer intermediate tank through the air cooler; the first condenser is connected with the chlorosilane mixed monomer intermediate tank and the second separation device; and the chlorosilane mixed monomer intermediate tank is connected with the washing tower and the heat exchange device through the upper reflux pump.
Optionally, the methyl chloride recovery device includes: the device comprises a chloromethane compression device, a chloromethane heat exchanger, a chloromethane buffer tank, a condensation device, a chloromethane reflux tank and a chloromethane feed pump; wherein, the chloromethane compression device is connected with the chlorosilane mixed monomer synthesis tower; the chloromethane compression device is also connected with the chloromethane heat exchanger; the chloromethane heat exchanger and the chloromethane buffer tank form a communicating vessel structure, and the chloromethane heat exchanger is also connected with the condensing device; the condensing device is connected with the chloromethane reflux tank; the chloromethane reflux tank is connected with the chlorosilane mixed monomer separation tower and is connected with the chloromethane buffer tank through a chloromethane feed pump; the chloromethane buffer tank is connected with the chlorosilane mixed monomer synthesis tower.
Optionally, the method further comprises: and the quartz sand tank is connected with the fluidized bed.
In a second aspect, the present invention provides a method of organosilicon monomer synthesis, applied to the system of organosilicon monomer synthesis of any one of the first aspects, the method comprising: methyl chloride and silicon powder are sent into a synthesis device and sequentially pass through a first separation device, a heat exchange device and a second separation device to synthesize an organosilicon monomer;
conveying silicon powder and copper powder in a charging tank and chloromethane in a chloromethane gas supply device into a fluidized bed to generate a chlorosilane mixed monomer synthesis gas, wherein the chlorosilane mixed monomer synthesis gas enters a first cyclone separation device through a gas lifting pipe at the top of the fluidized bed; the chlorosilane mixed monomer synthesis gas comprises: methyl chloride, tetramethylsilane, trichlorosilane, dimethylmonohydrosilane, methyldichlorosilane, silicon tetrachloride, trimethylchlorosilane, methyltrichlorosilane, dimethyldichlorosilane, high boilers and fine silicon powder;
the first cyclone separation device performs primary separation on fine silicon powder in the chlorosilane mixed monomer synthesis gas by means of gravity; sending the separated chlorosilane mixed monomer synthesis gas into a second cyclone separation device; the second cyclone separation device performs secondary separation on the fine silicon powder in the chlorosilane mixed monomer synthesis gas by means of gravity, and sends the separated fine silicon powder into the fluidized bed through a venturi jet device; sending the separated chlorosilane mixed monomer synthesis gas into a third cyclone separation device; the third cyclone separation device performs three-stage separation on the fine silicon powder in the chlorosilane mixed monomer synthesis gas under the action of gravity, and sends the separated fine silicon powder into a contact tank through a receiving hopper and a discharge hopper; sending the separated chlorosilane mixed monomer synthesis gas into a washing tower, cooling and condensing the chlorosilane mixed monomer synthesis gas by the washing tower to form a liquid-phase chlorosilane mixed monomer, and rectifying the liquid-phase chlorosilane mixed monomer by the washing tower to form a gas-phase chlorosilane mixed monomer and a dust-containing high-boiling-point substance; the high-boiling-point substance containing dust is arranged at the bottom of the washing tower, the high-boiling-point substance containing dust is pumped into a stripping tower through a lower reflux pump, chloromethane in the high-boiling-point substance containing dust is sent into the washing tower through the stripping tower, the high-boiling-point substance containing dust in the bottom of the stripping tower is discharged into a precipitation kettle, and the precipitation kettle is used for carrying out precipitation reflux pumping to a slurry and slag treatment device;
the gas-phase chlorosilane mixed monomer enters an air cooler through the top of the washing tower to be condensed for the first time, and then is condensed for the second time through a condenser; the obtained liquid-phase chlorosilane mixed monomer is collected in a middle tank, the middle tank pumps the liquid-phase chlorosilane mixed monomer into a washing tower through an upper reflux pump part to serve as reflux liquid, and the other part is sent into a liquid-phase chlorosilane mixed monomer tower;
the liquid-phase chlorosilane mixed monomer tower separates out chloromethane from the tower top through rectification, and enters a chloromethane recovery device for recycling chloromethane; and the recovered chloromethane is led into the fluidized bed again.
According to the invention, the cyclone separation device is used for capturing fine powder and automatically returning to the bed, so that the operation of operators is simplified, the workload is lightened, and more time is provided for controlling system abnormality; and the high-boiling residues and the residual dust are completely removed, so that the chlorosilane mixed monomer sent to the chlorosilane tank does not contain the high-boiling residues, and a high-boiling residue removing tower is not required to be arranged for separating the high-boiling residues, thereby shortening the process flow, reducing the equipment investment and reducing the energy consumption.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to designate like parts throughout the figures. In the drawings:
fig. 1 is a schematic diagram of a system structure for synthesizing an organosilicon monomer according to an embodiment of the present invention.
Reference numerals:
a synthesis device 1, a first separation device 2 and a heat exchange device 3; a second separation device 4;
a chloromethane gas supply device 11; a charging tank 12; a fluidized bed 13; first cyclonic separating apparatus 14; a second cyclonic separating apparatus 15; a third cyclonic separating apparatus 16; a first recovery device 17; a washing tower 21; a lower return pump 22; a stripping column 23; a second recovery device 24; a first condensing device 25; a heat exchanger 31; a first cooler 32; a chlorosilane tank 33; a chlorosilane mixed monomer column 41; a reboiler 42; a chloromethane recovery device 43.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, an embodiment of the present invention provides a system for synthesizing an organosilicon monomer, including:
a synthesis device 1, a first separation device 2, a heat exchange device 3 and a second separation device 4;
the synthesizing apparatus 1 includes: a chloromethane gas supply device 11, a charging tank 12, a fluidized bed 13, a first cyclone separation device 14, a second cyclone separation device 15, a third cyclone separation device 16 and a first recovery device 17; wherein the charging tank 12 and the chloromethane gas supply device 11 are connected with the fluidized bed 13; the top of the fluidized bed 13 is connected with the first cyclone separation device 14; the first cyclone separating means 14 is connected to the second cyclone separating means 15; the second cyclonic separating apparatus 15 is connected to the third cyclonic separating apparatus 16; the top of the third cyclone separation device 16 is connected with the first separation device 2, and the bottom of the third cyclone separation device 16 is connected with the first recovery device 17;
the first separation device 2 includes: a washing tower 21, a lower reflux pump 22, a stripping tower 23, a second recovery device 24 and a first condensing device 25; wherein the first separation device 2 is connected with the synthesis device 1 through the washing tower 21; the lower end of the washing tower 21 is connected with the stripping tower 23 through a lower reflux pump 22; the top of the stripping tower 23 is connected with the tower kettle of the washing tower 21; the bottom of the stripping tower 23 is connected with the second recovery device 24; the top of the washing tower 21 is connected with the first condensing device 25; the first condensing device 25 is connected with the heat exchange device 3 and the second separating device 4;
the heat exchange device 3 includes: a heat exchanger 31, a first cooler 32, and a chlorosilane tank 33; wherein the heat exchange device 3 is connected with the first condensing device 25 through the heat exchanger 31; the heat exchanger 31 is connected with the first cooler 32 and the second separation device 4; the first cooler 32 is connected to the chlorosilane tank 33;
the second separation device 4 includes: a chlorosilane mixed monomer column 41, a reboiler 42 and a chloromethane recovery device 43; wherein the second separation device 4 is connected with the first separation device 2 through the chlorosilane mixed monomer column 41; the chlorosilane mixed monomer tower 41 is connected with the reboiler 42 and the chloromethane recovery device 43; the second separation device 4 is connected to the synthesis device 1 via the methyl chloride recovery device 43.
In the embodiment of the invention, the cyclone separation device captures the fine powder to automatically return to the bed, so that the operation of operators is simplified, the workload is lightened, and more time is provided for controlling the system abnormality; and the high-boiling residues and the residual dust are completely removed, so that the chlorosilane mixed monomer sent to the chlorosilane tank does not contain the high-boiling residues, and a high-boiling residue removing tower is not required to be arranged for separating the high-boiling residues, thereby shortening the process flow, reducing the equipment investment and reducing the energy consumption.
In an embodiment of the present invention, optionally, the charging tank includes: silica powder charging jar and copper powder charging jar.
In an embodiment of the present invention, optionally, the second cyclone separation device includes: a second cyclone separator and a venturi jet device; wherein the second cyclone separation device is connected with the first cyclone separation device through the second cyclone separator; the first end of the Venturi jetting device is connected with the bottom of the second cyclone separator; the first end of the venturi jet device is connected with the fluidized bed.
In an embodiment of the present invention, optionally, the third cyclone separation device includes: the third cyclone separator, the receiving hopper and the discharging hopper; wherein one end of the receiving hopper is connected with the third cyclone separator; the other end of the receiving hopper is connected with one end of the discharging hopper; the other end of the discharge hopper is connected with the fluidized bed and the first recovery device.
In an embodiment of the present invention, optionally, the first recovery device includes: the device comprises a contact body tank, a cloth bag filter, a solid waste treatment device and a tail gas washing device; wherein the fluidized bed and the third cyclone separation device are connected with the contact tank; the bottom of the touch body tank is connected with the solid waste treatment device, the top of the touch body tank is connected with one end of the cloth bag filter, and the other end of the cloth bag filter is connected with the tail gas washing device.
In an embodiment of the present invention, optionally, the second recovery device includes: a sedimentation kettle, a sedimentation reflux pump and a slurry and slag treatment device; wherein the second recovery device is connected with the stripping tower through the precipitation kettle; the top and the bottom of the precipitation kettle are connected with the precipitation reflux pump; the sedimentation reflux pump is also connected with the slurry and slag treatment device.
In an embodiment of the present invention, optionally, the first condensation device includes: the air cooler, the first condenser, the upper reflux pump and the chlorosilane mixed monomer intermediate tank; the first condensing device is connected with the washing tower, the first condenser and the chlorosilane mixed monomer intermediate tank through the air cooler; the first condenser is connected with the chlorosilane mixed monomer intermediate tank and the second separation device; and the chlorosilane mixed monomer intermediate tank is connected with the washing tower and the heat exchange device through the upper reflux pump.
In an embodiment of the present invention, optionally, the methyl chloride recovery device includes: the device comprises a chloromethane compression device, a chloromethane heat exchanger, a chloromethane buffer tank, a condensation device, a chloromethane reflux tank and a chloromethane feed pump; wherein, the chloromethane compression device is connected with the chlorosilane mixed monomer synthesis tower; the chloromethane compression device is also connected with the chloromethane heat exchanger; the chloromethane heat exchanger and the chloromethane buffer tank form a communicating vessel structure, and the chloromethane heat exchanger is also connected with the condensing device; the condensing device is connected with the chloromethane reflux tank; the chloromethane reflux tank is connected with the chlorosilane mixed monomer separation tower and is connected with the chloromethane buffer tank through a chloromethane feed pump; the chloromethane buffer tank is connected with the chlorosilane mixed monomer synthesis tower.
In the embodiment of the invention, the waste heat of the high-pressure and high-temperature chloromethane gas after the chloromethane compressor is utilized, the condensed chloromethane is utilized to obtain local materials, and the gasified chloromethane is used for a front system, so that the steam consumption of each heat exchanger in the front system is saved.
In an embodiment of the present invention, optionally, the method further includes: and the quartz sand tank is connected with the fluidized bed.
In the embodiment of the invention, the quartz sand tank is used for a quartz sand supplementing bed; after the quartz sand is fed into the bed, the quartz sand is fed into the bed by high-speed chloromethane gas flow, the height of the bed is within the range of 16-17.5 m, the range is determined according to the length of a U-shaped pipe in the bed, and the main heat exchange components in the bed are ensured to be sufficiently ground and cleaned; judging the height of the material surface of the bed layer through the pressure difference between the top and the bottom of the fluidized bed, when the pressure difference is smaller than a specific reference value, supplementing quartz sand into the fluidized bed, and when the pressure difference is higher than the specific reference value, stopping supplementing quartz sand into the fluidized bed, and repeating the steps until the total amount of the supplemented quartz sand is about 20 tons, wherein an electronic weighing instrument is arranged in a quartz sand tank, and the whole process takes about 3-4 hours from stopping the silicon powder supplementing bed to completing the quartz sand supplementing bed; after the supplementing amount of quartz sand into the fluidized bed is finished, switching nitrogen into the fluidized bed, stopping overheat chloromethane into the fluidized bed, stopping the reaction, closing a valve on a pipeline from the fluidized bed to a washing tower, and starting cooling of the reactor; when the reaction temperature is reduced to below 100 ℃, discharging the quartz sand-containing waste contact into a contact tank for protection and sealing by micro-positive pressure nitrogen; when the bed is removed on line next time, quartz sand contacts in the contact tank can be fully supplemented into the fluidized bed for reuse; after the online material returning is completed, the temperature of the fluidized bed is raised to 300 ℃, new silicon powder is pushed in again, a catalyst is added, and the device enters the next production operation period.
In the embodiment of the invention, the cyclone separation device captures the fine powder to automatically return to the bed, so that the operation of operators is simplified, the workload is lightened, and more time is provided for controlling the system abnormality; and the high-boiling residues and the residual dust are completely removed, so that the chlorosilane mixed monomer sent to the chlorosilane tank does not contain the high-boiling residues, and a high-boiling residue removing tower is not required to be arranged for separating the high-boiling residues, thereby shortening the process flow, reducing the equipment investment and reducing the energy consumption.
Referring to fig. 1, the present invention provides a method for synthesizing an organosilicon monomer, which is applied to the system for synthesizing an organosilicon monomer according to any one of the first aspect, and the method includes: methyl chloride and silicon powder are sent into a synthesis device and sequentially pass through a first separation device, a heat exchange device and a second separation device to synthesize an organosilicon monomer;
conveying silicon powder and copper powder in a charging tank and chloromethane in a chloromethane gas supply device into a fluidized bed to generate a chlorosilane mixed monomer synthesis gas, wherein the chlorosilane mixed monomer synthesis gas enters a first cyclone separation device through a gas lifting pipe at the top of the fluidized bed; the chlorosilane mixed monomer synthesis gas comprises: methyl chloride, tetramethylsilane, trichlorosilane, dimethylmonohydrosilane, methyldichlorosilane, silicon tetrachloride, trimethylchlorosilane, methyltrichlorosilane, dimethyldichlorosilane, high boilers and fine silicon powder;
the first cyclone separation device performs primary separation on fine silicon powder in the chlorosilane mixed monomer synthesis gas by means of gravity; sending the separated chlorosilane mixed monomer synthesis gas into a second cyclone separation device; the second cyclone separation device performs secondary separation on the fine silicon powder in the chlorosilane mixed monomer synthesis gas by means of gravity, and sends the separated fine silicon powder into the fluidized bed through a venturi jet device; sending the separated chlorosilane mixed monomer synthesis gas into a third cyclone separation device; the third cyclone separation device performs three-stage separation on the fine silicon powder in the chlorosilane mixed monomer synthesis gas under the action of gravity, and sends the separated fine silicon powder into a contact tank through a receiving hopper and a discharge hopper; sending the separated chlorosilane mixed monomer synthesis gas into a washing tower, cooling and condensing the chlorosilane mixed monomer synthesis gas by the washing tower to form a liquid-phase chlorosilane mixed monomer, and rectifying the liquid-phase chlorosilane mixed monomer by the washing tower to form a gas-phase chlorosilane mixed monomer and a dust-containing high-boiling-point substance; the high-boiling-point substance containing dust is arranged at the bottom of the washing tower, the high-boiling-point substance containing dust is pumped into a stripping tower through a lower reflux pump, chloromethane in the high-boiling-point substance containing dust is sent into the washing tower through the stripping tower, the high-boiling-point substance containing dust in the bottom of the stripping tower is discharged into a precipitation kettle, and the precipitation kettle is used for carrying out precipitation reflux pumping to a slurry and slag treatment device;
the gas-phase chlorosilane mixed monomer enters an air cooler through the top of the washing tower to be condensed for the first time, and then is condensed for the second time through a condenser; the obtained liquid-phase chlorosilane mixed monomer is collected in a middle tank, the middle tank pumps the liquid-phase chlorosilane mixed monomer into a washing tower through an upper reflux pump part to serve as reflux liquid, and the other part is sent into a liquid-phase chlorosilane mixed monomer tower;
the liquid-phase chlorosilane mixed monomer tower separates out chloromethane from the tower top through rectification, and enters a chloromethane recovery device for recycling chloromethane; and the recovered chloromethane is led into the fluidized bed again.
In the embodiment of the invention, firstly, silicon powder and copper powder in a charging tank are conveyed into a fluidized bed by virtue of pneumatic force, and react with overheated chloromethane in the fluidized bed to generate chlorosilane mixed monomers, and a product enters a first cyclone separator from a gas phase synthesis gas through a gas-phase riser at the top of the fluidized bed; the main components of the chlorosilane mixed monomer synthesis gas are as follows: methyl chloride, tetramethylsilane, trichlorosilane, dimethylmonochlorosilane, methyldichlorosilane, silicon tetrachloride, trimethylchlorosilane, methyltrichlorosilane, dimethyldichlorosilane, high-boiling substances and a small amount of fine silicon powder; the chlorosilane mixed monomer synthesis gas enters a first cyclone separator, fine silicon powder is primarily separated, and captured fine powder is inserted into a material pipe in a fluidized bed through the first cyclone separator by means of gravity to complete automatic return; the synthetic gas from the first cyclone separator enters the second cyclone separator to continue to separate fine powder, the fine powder captured by the second cyclone separator enters the Venturi jetting device by gravity, and the automatic return of the fine powder is realized through the Venturi tube device; the synthetic gas from the second cyclone separator enters a third cyclone separator, silicon powder with finer granularity is continuously captured, the captured fine powder flow is subjected to a hopper and a discharge hopper, and finally discharged into a contact tank;
in the method, the contact body can be withdrawn on line before the shutdown and maintenance, when the contact body withdrawal flow is triggered, the system automatically stops supplementing silicon powder and copper powder to the fluidized bed, quartz sand is used for supplementing the bed, after the quartz sand is supplemented to the bed, the quartz sand is sent into the bed by high-speed chloromethane air flow to the height of the bed within the range of 16-17.5 meters, wherein the range is specifically determined according to the length of a U-shaped tube in the bed, and the main heat exchange components in the bed are fully ground and cleaned; judging the height of the material surface of the bed layer through the pressure difference between the top and the bottom of the fluidized bed, when the pressure difference is smaller than a specific reference value, supplementing quartz sand into the fluidized bed, and when the pressure difference is higher than the specific reference value, stopping supplementing quartz sand into the fluidized bed, and repeating the steps until the total amount of the supplemented quartz sand is about 20 tons, wherein the whole process takes about 3-4 hours from stopping the silicon powder supplementing bed to completing the quartz sand supplementing bed; after the supplementing amount of quartz sand into the fluidized bed is finished, switching nitrogen into the fluidized bed, stopping overheat chloromethane into the fluidized bed, stopping the reaction, closing a valve on a pipeline from the fluidized bed to a washing tower, and starting cooling of the reactor; when the reaction temperature is reduced to below 100 ℃, discharging the quartz sand-containing waste contact into a contact tank for protection and sealing by micro-positive pressure nitrogen; when the bed is removed on line next time, quartz sand contacts in the contact tank can be fully supplemented into the fluidized bed for reuse; after the online material returning is completed, the temperature of the fluidized bed is raised to 300 ℃, new silicon powder is pushed in again, a catalyst is added, and the device enters the next production operation period; the cyclone separation device captures the fine powder and automatically returns to the bed, so that the operation of operators is simplified, the workload is reduced, more time is allowed for controlling system abnormality, the frequency of detaching the fluidized bed during maintenance is reduced in the online bed returning process, the labor intensity of workers is reduced, the labor cost and the material consumption of machines are saved, the maintenance period is shortened, the fluidized bed is not required to be opened for cleaning during maintenance, the ignition combustion and environmental pollution accidents caused by maintenance are avoided, the cleanliness of a production site is greatly improved, and the safety maintenance is essentially realized; meanwhile, the sand-containing touch body in the touch body tank can be recycled, so that the production cost is reduced, and the comprehensive economic benefit is increased.
In the embodiment of the invention, dust is removed by the cyclone separation device; the chlorosilane mixed monomer synthesis gas enters a washing tower, the synthesis gas is cooled and condensed in the tower to form liquid-phase chlorosilane, and high-boiling residues containing residual dust are enriched in the tower kettle under the rectification action of the tower; the high-boiling substances containing dust are pumped into a stripping tower through a lower reflux pump part, the light components are stripped and then enter a washing tower again, and the high-boiling substances containing dust at the bottom of the stripping tower are discharged into a precipitation kettle again; the high-boiling substances entering the precipitation kettle have larger dust content and black slag-like appearance; the precipitation kettle uses heat conduction oil as a heat medium, high-boiling substances with more dust in the precipitation kettle are distilled and concentrated, and then the high-boiling substances are pumped into a slurry residue treatment section by a precipitation reflux pump; after the working procedures of liquefying, rectifying, stripping and precipitating the chlorosilane mixed monomer synthesis gas in the washing tower, the dust-containing high-boiling substances and the residual fine powder are completely removed; the gas-phase chlorosilane from which high boiling and fine powder is removed enters an air cooler from the top of a washing tower to be condensed, then the gas-phase chlorosilane is subjected to deep cooling through a condenser, and liquid-phase chlorosilane mixed monomers after the twice condensation are collected in a middle tank; the chlorosilane mixed monomer is partially pumped into a washing tower through an upper reflux pump to be used as reflux liquid, and the other part is sent into a chlorosilane mixed monomer tower; the high-boiling-point substances and residual dust in the chlorosilane mixed monomer are removed, so that a high-boiling-point substance removing tower is not required to be arranged for separating the high-boiling-point substances when the chlorosilane mixed monomer is separated by the chlorosilane mixed monomer tower, the process flow is shortened, the equipment investment is reduced, and the energy consumption is reduced.
In the embodiment of the invention, two flows of materials enter the chlorosilane mixed monomer tower, one flow is non-condensable gas after condensation of a condenser, the other flow is chlorosilane mixed monomer, after the two flows of materials enter the chlorosilane mixed monomer tower, the two flows of materials are rectified, and light components of the main component of the chloromethane are separated out from the top of the tower and enter a buffer tank at the inlet of a compressor, and then are sucked and pressurized by a chloromethane compressor to be discharged; the high-pressure gas-phase chloromethane at the outlet of the chloromethane compressor enters the shell side of a chloromethane heat exchanger, exchanges heat with the liquid-phase chloromethane in the tube side, sequentially passes through two condensers, and finally is condensed into liquid-phase chloromethane to flow into a chloromethane reflux tank; the high-temperature gas-phase chloromethane entering the shell pass of the chloromethane heat exchanger exchanges heat and then is cooled, part of the chloromethane is condensed into a liquid phase and then flows into a chloromethane reflux tank, and then is pumped into a chloromethane buffer tank by a chloromethane feed pump; the chloromethane buffer tank is communicated with the chloromethane heat exchanger to form a communicating vessel; the liquid-phase chloromethane in the chloromethane buffer tank is connected in series with the tube side of the chloromethane heat exchanger, and is subjected to heat transfer with the high-temperature gas-phase chloromethane from the compressor through the heat exchange tube, and the liquid-phase chloromethane is vaporized and then enters the chloromethane buffer tank and then enters the superheater; the liquid-phase chloromethane entering the tube side of the chloromethane heat exchanger, wherein the heavier components which are not vaporized and contain chlorosilane are gradually enriched at the lower end socket of the heat exchanger, and the heavier components can be discharged into the chloromethane reflux tank continuously in a small amount through a blow-down pipeline at the bottom of the chloromethane heat exchanger; the low-temperature liquid-phase chloromethane containing heavier components in the chloromethane reflux tank can be sent into the chlorosilane mixed monomer tower again for rectification through pressure, and the heavy components finally flow to the chlorosilane mixed monomer tank from the tower bottom of the chlorosilane mixed monomer tower; realizes the separation of light and heavy components in the low-temperature liquid-phase chloromethane and achieves the aim of purifying and recycling the chloromethane.
In the embodiment of the invention, the cyclone separation device captures the fine powder to automatically return to the bed, so that the operation of operators is simplified, the workload is lightened, and more time is provided for controlling the system abnormality; and the high-boiling residues and the residual dust are completely removed, so that the chlorosilane mixed monomer sent to the chlorosilane tank does not contain the high-boiling residues, and a high-boiling residue removing tower is not required to be arranged for separating the high-boiling residues, thereby shortening the process flow, reducing the equipment investment and reducing the energy consumption.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The embodiments of the present invention have been described above with reference to the accompanying drawings, but the present invention is not limited to the above-described embodiments, which are merely illustrative and not restrictive, and many forms may be made by those having ordinary skill in the art without departing from the spirit of the present invention and the scope of the claims, which are to be protected by the present invention.

Claims (7)

1. A method for synthesizing an organosilicon monomer is characterized by being applied to a device for synthesizing the organosilicon monomer,
the device for synthesizing the organosilicon monomer comprises:
the device comprises a synthesis device, a first separation device, a heat exchange device and a second separation device;
the synthesizing apparatus includes: the device comprises a chloromethane air supply device, a charging tank, a fluidized bed, a first cyclone separation device, a second cyclone separation device, a third cyclone separation device and a first recovery device; wherein the charging tank and the chloromethane air supply device are connected with the fluidized bed; the top of the fluidized bed is connected with the first cyclone separation device; the first cyclone separation device is connected with the second cyclone separation device; the second cyclone separation device is connected with the third cyclone separation device; the top of the third cyclone separation device is connected with the first separation device, and the bottom of the third cyclone separation device is connected with the first recovery device; the first recovery device includes: the device comprises a contact body tank, a cloth bag filter, a solid waste treatment device and a tail gas washing device; wherein the fluidized bed and the third cyclone separation device are connected with the contact tank; the bottom of the touch body tank is connected with a solid waste treatment device, the top of the touch body tank is connected with one end of the cloth bag filter, and the other end of the cloth bag filter is connected with the tail gas washing device;
the first separation device includes: the device comprises a washing tower, a lower reflux pump, a stripping tower, a second recovery device and a first condensing device; wherein the first separation device is connected with the synthesis device through the washing tower; the lower end of the washing tower is connected with the stripping tower through a lower reflux pump; the top of the stripping tower is connected with the tower kettle of the washing tower; the bottom of the stripping tower is connected with the second recovery device; the top of the washing tower is connected with the first condensing device; the first condensing device is connected with the heat exchange device and the second separating device;
the heat exchange device includes: a heat exchanger, a first cooler and a chlorosilane tank; wherein the heat exchange device is connected with the first condensing device through the heat exchanger; the heat exchanger is connected with the first cooler and the second separation device; the first cooler is connected with the chlorosilane tank;
the second separation device includes: a chlorosilane mixed monomer tower, a reboiler and a chloromethane recovery device; the second separation device is connected with the first separation device through the chlorosilane mixed monomer tower; the chlorosilane mixed monomer tower is connected with the reboiler and the chloromethane recovery device; the second separation device is connected with the synthesis device through the chloromethane recovery device;
the second cyclonic separating apparatus comprises: a second cyclone separator and a venturi jet device; wherein the second cyclone separation device is connected with the first cyclone separation device through the second cyclone separator; the first end of the Venturi jetting device is connected with the bottom of the second cyclone separator; the first end of the venturi jet device is connected with the fluidized bed;
further comprises: the quartz sand tank is connected with the fluidized bed;
the method comprises the following steps: methyl chloride and silicon powder are sent into a synthesis device and sequentially pass through a first separation device, a heat exchange device and a second separation device to synthesize an organosilicon monomer;
conveying silicon powder and copper powder in a charging tank and chloromethane in a chloromethane gas supply device into a fluidized bed to generate a chlorosilane mixed monomer synthesis gas, wherein the chlorosilane mixed monomer synthesis gas enters a first cyclone separation device through a gas lifting pipe at the top of the fluidized bed; the chlorosilane mixed monomer synthesis gas comprises: methyl chloride, tetramethylsilane, trichlorosilane, dimethylmonohydrosilane, methyldichlorosilane, silicon tetrachloride, trimethylchlorosilane, methyltrichlorosilane, dimethyldichlorosilane, high boilers and fine silicon powder;
the first cyclone separation device performs primary separation on fine silicon powder in the chlorosilane mixed monomer synthesis gas by means of gravity; sending the separated chlorosilane mixed monomer synthesis gas into a second cyclone separation device; the second cyclone separation device performs secondary separation on the fine silicon powder in the chlorosilane mixed monomer synthesis gas by means of gravity, and sends the separated fine silicon powder into the fluidized bed through a venturi jet device; sending the separated chlorosilane mixed monomer synthesis gas into a third cyclone separation device; the third cyclone separation device performs three-stage separation on the fine silicon powder in the chlorosilane mixed monomer synthesis gas under the action of gravity, and sends the separated fine silicon powder into a contact tank through a receiving hopper and a discharge hopper; sending the separated chlorosilane mixed monomer synthesis gas into a washing tower, cooling and condensing the chlorosilane mixed monomer synthesis gas by the washing tower to form a liquid-phase chlorosilane mixed monomer, and rectifying the liquid-phase chlorosilane mixed monomer by the washing tower to form a gas-phase chlorosilane mixed monomer and a dust-containing high-boiling-point substance; the high-boiling-point substance containing dust is arranged at the bottom of the washing tower, the high-boiling-point substance containing dust is pumped into a stripping tower through a lower reflux pump, chloromethane in the high-boiling-point substance containing dust is sent into the washing tower through the stripping tower, the high-boiling-point substance containing dust in the bottom of the stripping tower is discharged into a precipitation kettle, and the precipitation kettle is used for carrying out precipitation reflux pumping to a slurry and slag treatment device;
the gas-phase chlorosilane mixed monomer enters an air cooler through the top of the washing tower to be condensed for the first time, and then is condensed for the second time through a condenser; the obtained liquid-phase chlorosilane mixed monomer is collected in a middle tank, the middle tank pumps the liquid-phase chlorosilane mixed monomer into a washing tower through an upper reflux pump part to serve as reflux liquid, and the other part is sent into a liquid-phase chlorosilane mixed monomer tower;
the liquid-phase chlorosilane mixed monomer tower separates out chloromethane from the tower top through rectification, and enters a chloromethane recovery device for recycling chloromethane; and introducing the recovered chloromethane into the fluidized bed again;
wherein the quartz sand tank is used for a quartz sand supplementing bed; after the quartz sand is fed into the bed, the quartz sand is fed into the bed by high-speed chloromethane gas flow, and the height of the bed is within the range of 16-17.5 m; judging the height of the bed material level through the pressure difference between the top and the bottom of the fluidized bed, supplementing quartz sand into the fluidized bed when the pressure difference is smaller than a specific reference value, stopping supplementing quartz sand into the fluidized bed when the pressure difference is higher than the specific reference value, and repeating the steps until the total amount of the supplemented quartz sand is about 20 tons, wherein an electronic weighing instrument is arranged in the quartz sand tank; after the supplementing amount of quartz sand into the fluidized bed is finished, switching nitrogen into the fluidized bed, stopping overheat chloromethane into the fluidized bed, stopping the reaction, closing a valve on a pipeline from the fluidized bed to a washing tower, and starting cooling of the reactor; when the reaction temperature is reduced to below 100 ℃, discharging the quartz sand-containing waste contact into a contact tank for protection and sealing by micro-positive pressure nitrogen; when the bed is removed on line next time, quartz sand contacts in the contact tank can be fully supplemented into the fluidized bed for reuse; after the online material returning is completed, the temperature of the fluidized bed is raised to 300 ℃, new silicon powder is pushed in again, a catalyst is added, and the device enters the next production operation period.
2. An apparatus for the synthesis of a silicone monomer as set forth in claim 1, characterized in that it comprises:
the device comprises a synthesis device, a first separation device, a heat exchange device and a second separation device;
the synthesizing apparatus includes: the device comprises a chloromethane air supply device, a charging tank, a fluidized bed, a first cyclone separation device, a second cyclone separation device, a third cyclone separation device and a first recovery device; wherein the charging tank and the chloromethane air supply device are connected with the fluidized bed; the top of the fluidized bed is connected with the first cyclone separation device; the first cyclone separation device is connected with the second cyclone separation device; the second cyclone separation device is connected with the third cyclone separation device; the top of the third cyclone separation device is connected with the first separation device, and the bottom of the third cyclone separation device is connected with the first recovery device; the first recovery device includes: the device comprises a contact body tank, a cloth bag filter, a solid waste treatment device and a tail gas washing device; wherein the fluidized bed and the third cyclone separation device are connected with the contact tank; the bottom of the touch body tank is connected with a solid waste treatment device, the top of the touch body tank is connected with one end of the cloth bag filter, and the other end of the cloth bag filter is connected with the tail gas washing device;
the first separation device includes: the device comprises a washing tower, a lower reflux pump, a stripping tower, a second recovery device and a first condensing device; wherein the first separation device is connected with the synthesis device through the washing tower; the lower end of the washing tower is connected with the stripping tower through a lower reflux pump; the top of the stripping tower is connected with the tower kettle of the washing tower; the bottom of the stripping tower is connected with the second recovery device; the top of the washing tower is connected with the first condensing device; the first condensing device is connected with the heat exchange device and the second separating device;
the heat exchange device includes: a heat exchanger, a first cooler and a chlorosilane tank; wherein the heat exchange device is connected with the first condensing device through the heat exchanger; the heat exchanger is connected with the first cooler and the second separation device; the first cooler is connected with the chlorosilane tank;
the second separation device includes: a chlorosilane mixed monomer tower, a reboiler and a chloromethane recovery device; the second separation device is connected with the first separation device through the chlorosilane mixed monomer tower; the chlorosilane mixed monomer tower is connected with the reboiler and the chloromethane recovery device; the second separation device is connected with the synthesis device through the chloromethane recovery device;
the second cyclonic separating apparatus comprises: a second cyclone separator and a venturi jet device; wherein the second cyclone separation device is connected with the first cyclone separation device through the second cyclone separator; the first end of the Venturi jetting device is connected with the bottom of the second cyclone separator; the first end of the venturi jet device is connected with the fluidized bed;
further comprises: and the quartz sand tank is connected with the fluidized bed.
3. The apparatus for synthesizing a silicone monomer according to claim 2, wherein,
the feed tank includes: silica powder charging jar and copper powder charging jar.
4. The apparatus for synthesizing a silicone monomer according to claim 2, wherein,
the third cyclonic separating apparatus comprises: the third cyclone separator, the receiving hopper and the discharging hopper; wherein one end of the receiving hopper is connected with the third cyclone separator; the other end of the receiving hopper is connected with one end of the discharging hopper; the other end of the discharge hopper is connected with the fluidized bed and the first recovery device.
5. The apparatus for synthesizing a silicone monomer according to claim 2, wherein,
the second recovery device includes: a sedimentation kettle, a sedimentation reflux pump and a slurry and slag treatment device; wherein the second recovery device is connected with the stripping tower through the precipitation kettle; the top and the bottom of the precipitation kettle are connected with the precipitation reflux pump; the sedimentation reflux pump is also connected with the slurry and slag treatment device.
6. The apparatus for synthesizing a silicone monomer according to claim 2, wherein,
the first condensing unit includes: the air cooler, the first condenser, the upper reflux pump and the chlorosilane mixed monomer intermediate tank; the first condensing device is connected with the washing tower, the first condenser and the chlorosilane mixed monomer intermediate tank through the air cooler; the first condenser is connected with the chlorosilane mixed monomer intermediate tank and the second separation device; and the chlorosilane mixed monomer intermediate tank is connected with the washing tower and the heat exchange device through the upper reflux pump.
7. The apparatus for synthesizing a silicone monomer according to claim 2, wherein,
the chloromethane recovery device comprises: the device comprises a chloromethane compression device, a chloromethane heat exchanger, a chloromethane buffer tank, a condensation device, a chloromethane reflux tank and a chloromethane feed pump; wherein, the chloromethane compression device is connected with the chlorosilane mixed monomer synthesis tower; the chloromethane compression device is also connected with the chloromethane heat exchanger; the chloromethane heat exchanger and the chloromethane buffer tank form a communicating vessel structure, and the chloromethane heat exchanger is also connected with the condensing device; the condensing device is connected with the chloromethane reflux tank; the chloromethane reflux tank is connected with the chlorosilane mixed monomer separation tower and is connected with the chloromethane buffer tank through a chloromethane feed pump; the chloromethane buffer tank is connected with the chlorosilane mixed monomer synthesis tower.
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