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CN109250722B - Method for preparing monosilane by using organosilicon slag slurry - Google Patents

Method for preparing monosilane by using organosilicon slag slurry Download PDF

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Publication number
CN109250722B
CN109250722B CN201811087679.7A CN201811087679A CN109250722B CN 109250722 B CN109250722 B CN 109250722B CN 201811087679 A CN201811087679 A CN 201811087679A CN 109250722 B CN109250722 B CN 109250722B
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stirring
boiling
organic silicon
separation
liquid
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CN109250722A (en
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兰凤
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ZHEJIANG HUTU PHARMCHEM CO Ltd
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ZHEJIANG HUTU PHARMCHEM CO Ltd
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    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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    • C01B33/04Hydrides of silicon

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Abstract

The invention belongs to the technical field of monosilane preparation, and particularly relates to a method for preparing monosilane by using organosilicon slurry; the method comprises the following steps: firstly, the organic silicon slag slurry high-boiling-point substance separation and recovery equipment is improved, so that the organic silicon slag slurry high-boiling-point substance separation and recovery equipment is more convenient to use; mixing part of liquid nitrogen into a nitrogen storage container to keep the nitrogen in a low-temperature state; introducing low-temperature nitrogen into the improved organosilicon slurry high-boiling-point substance separation and recovery equipment, so that the organosilicon slurry high-boiling-point substance separation and recovery equipment is filled with the low-temperature nitrogen; putting the organic silicon slag slurry into improved organic silicon slag slurry high-boiling-point substance separation and recovery equipment, and separating the organic silicon slag slurry into waste slag and high-boiling-point substance liquid; high-boiling-point substance liquid is connected into a tower reactor, so that the high-boiling-point substance liquid is continuously pyrolyzed into monosilane at high temperature to complete monosilane preparation; the invention can effectively improve the efficiency of monosilane preparation and the safety of monosilane preparation process.

Description

Method for preparing monosilane by using organosilicon slag slurry
Technical Field
The invention belongs to the technical field of monosilane preparation, and particularly relates to a method for preparing monosilane by using organosilicon slurry.
Background
In recent years, the organosilicon industry has been rapidly developed in both application range and quantity, and simultaneously, a large amount of organosilicon waste is generated, so that the whole environment is greatly damaged. Thus, the organic silicon waste becomes the most important research object of many research institutions, and the research is carried out on how to treat and use the organic silicon waste. High-boiling residues accounting for 5 percent of the total amount of the monomers are generated in the synthetic process of producing the organic silicon mixed monomers. High boilers cannot be converted into useful siloxanes in a simple manner. In the past, the traditional method cannot be well utilized, and only can be used for simply hydrolyzing the traditional method to prepare acid, thereby causing public hazard; the long-term storage is harmful, and the corrosion to the storage tank is serious. Therefore, there are many technical methods for preparing monosilane by cracking high-boiling components, among which there is a thermal cracking method, and since the reaction temperature is high, the high-temperature cracking reactor is easily blocked by waste residues and carbon deposits, so that monosilane is difficult to prepare, the preparation efficiency is low, and the preparation effect is poor.
Disclosure of Invention
In order to make up for the defects of the prior art, the invention provides a method for preparing monosilane by using organosilicon slurry, and aims to improve the efficiency of monosilane preparation and the safety of monosilane preparation. According to the invention, the high-boiling-point substance separation and extraction is more convenient by improving the organic silicon slag slurry high-boiling-point substance separation and recovery equipment, and the monosilane preparation efficiency is improved; the nitrogen introduced into the organic silicon slag slurry high-boiling-point substance separation and recovery equipment is treated at low temperature in advance, so that the possibility of copper powder explosion is reduced, and the safety of the monosilane preparation process is effectively improved; the high-boiling residues are separately extracted from the organic silicon slag slurry, so that the high-temperature cracking reactor can be prevented from being blocked by waste residues, the preparation efficiency of monosilane is improved, and the conversion rate from the organic silicon slag slurry to monosilane is also improved.
The technical scheme adopted by the invention for solving the technical problems is as follows: the invention relates to a method for preparing monosilane by using organosilicon slurry, which comprises the following steps:
s1: before the organosilicon slurry high-boiling-point substance separation and recovery equipment is used, the organosilicon slurry high-boiling-point substance separation and recovery equipment is improved, a first vent pipe is externally connected to an elastic air bag, and a one-way air valve, a manual valve and a pipe joint are sequentially arranged on the first vent pipe, wherein the pipe joint is a free end, when a pneumatic opening and closing door needs to be closed, the pipe joint of the first vent pipe can be directly communicated with a second air pipe on the pneumatic opening and closing door, and the manual valve is opened, so that the elastic air bag can be used for conveying air for the pneumatic opening and closing door, and the requirement of additionally connecting a pipeline for conveying air is avoided, so that the organosilicon slurry high-boiling-point substance separation and recovery equipment is simpler and more convenient to use, and the improvement of the high-boiling-point;
s2: adding a vent pipe I into S1 organosilicon slag slurry high-boiling residue separation and recovery equipment for more convenient use, mixing a part of liquid nitrogen into a nitrogen storage container, keeping the nitrogen at a low temperature and keeping the temperature of the nitrogen below 5 ℃;
s3: the low-temperature nitrogen in the S2 is introduced into the hollow cavity in the organic silicon slag slurry high-boiling-point substance separation and recovery equipment through the external pipeline, and the organic silicon slag slurry high-boiling-point substance separation and recovery equipment is started to enable the motor to rotate, so that the organic silicon slag slurry high-boiling-point substance separation and recovery equipment is filled with the low-temperature nitrogen, copper powder in the organic silicon slag slurry is prevented from being exploded due to air under the condition that the high-boiling-point substances exist in the copper powder slurry, the air can be removed by the low-temperature nitrogen, the copper powder is at a low temperature, the possibility of copper powder explosion is reduced, and the safety of a user is effectively improved;
s4: after the air in the organic silicon slag slurry high-boiling-point substance separation and recovery equipment in the S3 is discharged by nitrogen, putting the organic silicon slag slurry into the organic silicon slag slurry high-boiling-point substance separation and recovery equipment, separating the organic silicon slag slurry into waste slag and high-boiling-point substance liquid, and simultaneously introducing gas generated in the organic silicon slag slurry high-boiling-point substance separation and recovery equipment into a sodium carbonate solution for neutralization reaction, so that the possibility that hydrogen chloride gas in the organic silicon slag slurry meets water in the air and becomes hydrochloric acid is avoided, and the possibility that the hydrogen chloride gas pollutes the environment is reduced;
s5: the liquid containing the high-boiling-point substances obtained in the step S4 is connected into a tower reactor, and the catalyst organic amine is sprayed in, fully stirred and mixed, and the high-boiling-point substances liquid is subjected to continuous high-temperature cracking at the temperature of 80-140 ℃ to break Si-Si bonds of the high-boiling-point substances, so that monosilane is obtained; because the waste residue is separated in S1, the waste residue can be prevented from blocking the high-temperature cracking reactor, and meanwhile, because the high-boiling-point substance enters the tower reactor in a liquid form, the carbon deposition is prevented from blocking the high-temperature cracking reactor, and the monosilane preparation efficiency is improved;
the organic silicon slag slurry high-boiling-point substance separation and recovery equipment in the S1 comprises a machine shell, a stirring and centrifuging integrated barrel, a stirring module, a pressurizing module, a centrifugal driving mechanism and a solid-liquid separation module, wherein the stirring and centrifuging integrated barrel is positioned at the middle upper part of the machine shell, the stirring and centrifuging integrated barrel is rotationally connected with the machine shell, the stirring and centrifuging integrated barrel is used for stirring and centrifuging organic silicon slag slurry, a feeding hole is formed in the upper part of the stirring and centrifuging integrated barrel, and a pneumatic opening and closing door is arranged at the bottom of the stirring and centrifuging integrated barrel; the stirring module is fixed at the upper end of the machine shell and is used for premixing the organic silicon slag slurry in the stirring and centrifuging integrated barrel; the pressurizing module is fixedly connected with the stirring module into a whole and is used for inputting inert gas into the stirring and centrifuging integrated barrel and pressurizing the inert gas to disperse oxygen in the stirring and centrifuging integrated barrel; the centrifugal driving mechanism is fixed on the side wall of the stirring module and is used for driving the stirring and centrifuging integrated barrel to centrifugally rotate so as to primarily separate the organic silicon slag slurry into filter residues and high-boiling-point substance liquid; the solid-liquid separation module is positioned at the lower part of the stirring and centrifuging integrated barrel and is used for extruding filter residues generated in the stirring and centrifuging integrated barrel so as to fully separate high-boiling-point substance liquid from the filter residues in the filter residues and realize the complete separation of the high-boiling-point substances; wherein,
the stirring and centrifuging integrated barrel comprises a barrel body, filter cloth, a cylindrical sealing cover and an automatic telescopic cylinder I, wherein the barrel body is rotatably connected with the shell through a bearing; the filter cloth is provided with a plurality of blocks, the filter cloth is uniformly embedded on the side wall of the barrel body, and the filter cloth can filter high-boiling-point substance liquid in the organic silicon residue slurry; the cylindrical sealing cover is sleeved outside the barrel body, and the end part of the cylindrical sealing cover is embedded with the barrel body to realize that the barrel body is sealed by the cylindrical sealing cover; the automatic telescopic cylinder I is positioned at the upper end of the barrel body and fixed on the shell and used for driving the cylindrical sealing cover to move up and down so as to enable the side wall of the barrel body to be closed or opened; be provided with drain pipe one on the casing, and drain pipe one is located the sealed cover side of cylindric, drain pipe one is used for discharging the high boiling thing liquid that flows out for the first time in the staving. When the device works, when the high-boiling-point substance separation and recovery equipment of the organic silicon slag slurry is used initially, nitrogen is introduced into the pressurizing module, and starting a motor I to drive a pressurizing module, leading the pressurizing module to introduce nitrogen into the stirring and centrifuging integrated barrel, after the nitrogen drives all oxygen in the organic silicon slag slurry high-boiling-point substance separation and recovery equipment out of the gas, starting the automatic telescopic cylinder to push the cylindrical sealing cover to move downwards to enable the side part of the barrel body to be in a sealing state, closing the pneumatic opening and closing door, simultaneously, adding the organosilicon slurry from the feed inlet, then closing the feed inlet, continuing to rotate the first motor, enabling the first motor to drive the stirring blade to rotate at a low speed to pre-mix and uniformly stir the organosilicon slurry in the stirring and centrifuging integrated barrel, wherein the uniformly mixing speed is not more than 100 revolutions per minute, the pressurizing module is used for continuously pressurizing the stirring and centrifuging integrated barrel in the process of uniformly mixing the organic silicon slag slurry, so that air at the position with poor air tightness is prevented from entering the stirring and centrifuging integrated barrel; after premixing and pressurization are completed, driving the first automatic telescopic cylinder to drive the cylindrical sealing cover to ascend, enabling the side wall of the barrel body to be in an open state, starting the centrifugal driving mechanism, enabling the centrifugal driving mechanism to drive the barrel body to rotate centrifugally, simultaneously increasing the rotating speed of the motor, enabling the stirring module to stir the organic silicon slag slurry more quickly, keeping the pressurization module to continuously introduce nitrogen into the stirring and centrifuging integrated barrel, stopping the rotation of the first motor when the gas pressure in the stirring and centrifuging integrated barrel is high enough, and keeping a certain liquid content in the organic silicon slag slurry after the barrel body rotates centrifugally to dry the organic silicon slag slurry in a preliminary centrifugal mode, so that air explosion caused by good activity of waste slag is avoided; after the organic silicon slag slurry is centrifuged, high-boiling-point substance liquid flows out through the liquid outlet pipe and is collected, and waste residues generated after the organic silicon slag slurry is centrifuged fall into the solid-liquid separation module through the opened pneumatic opening and closing door, so that the waste residues are further subjected to solid-liquid separation.
The stirring module comprises a motor I, a fixed seat, a stirring shaft, a helical blade and a stirring blade, wherein the fixed seat is used for fixing the motor I on the upper end of the casing, and the lower part of the fixed seat is provided with a hollow chamber; the stirring shaft is connected with the first motor; the helical blades and the stirring blades are alternately arranged on the stirring shaft, and the helical blades and the stirring blades are positioned in the stirring and centrifuging integrated barrel; the stirring shaft, the helical blade and the stirring blade are all made of Hastelloy materials or Monel materials, and the Hastelloy materials or the Monel materials have anti-corrosion characteristics, so that the service lives of the stirring shaft, the helical blade and the stirring blade can be prolonged. During operation, motor one rotates, and motor one passes through (mixing) shaft drive stirring vane and helical blade and rotates, and on the one hand, stirring vane can stir organosilicon sediment thick liquid, and on the other hand, helical blade can constantly be pressed close to the downward propelling movement of sediment thick liquid of (mixing) shaft, makes organosilicon sediment thick liquid can top-down flow down, is favorable to supplementary stirring vane stirring organosilicon sediment thick liquid of strengthening, improves organosilicon sediment thick liquid and mixes degree and centrifugal efficiency of stirring in advance.
The pressurizing module comprises a cam, an elastic air bag, an annular sealing part and a first air pipe, wherein the elastic air bag is fixed on the inner wall of the hollow chamber and is close to the cam; the cam is positioned in the hollow cavity, the cam is fixed on the stirring shaft, and the cam intermittently extrudes the elastic air bag along with the rotation of the stirring shaft; an annular groove is formed in the upper end of the barrel body, and a first through hole is formed in the annular groove; the annular sealing part is connected with the hollow cavity into a whole, the annular sealing part extends into the annular groove, and the annular sealing part is used for sealing the first through hole; the air pipe is communicated with the elastic air bag and the barrel body through the annular sealing part and the through hole I, and the air pipe I is provided with a one-way valve I. During operation, let in nitrogen gas in the cavity of hollowing, make nitrogen gas full of the cavity of hollowing, start motor one, motor one drive (mixing) shaft rotates and drives the cam and rotate, pivoted cam intermittent type formula extrusion elasticity gasbag, the continuous nitrogen gas with in the cavity of hollowing of elasticity gasbag inhales the interior transport of rethread trachea earlier on the staving, after the continuous nitrogen gas of carrying in to the staving of elasticity gasbag, be full of by nitrogen gas in the staving, afterwards, whole organosilicon sediment thick liquid high boiling substance separation recovery unit is full of by nitrogen gas, make the high air of boiling substance separation recovery unit of organosilicon sediment thick liquid be got rid of totally, inflammable and explosive thing and strong acid gas and air in the organosilicon sediment thick liquid have been avoided and have been produced harm.
The centrifugal driving mechanism comprises a second motor, a bevel gear and an annular bevel gear, the second motor is fixed on the side wall of the fixed seat, and the second motor is connected with the bevel gear; the annular bevel gear is fixed on the upper part of the barrel body, and the annular bevel gear is meshed with the bevel gear, so that the barrel body is driven by the motor II. During operation, the second motor rotates to drive the bevel gear to rotate, and the bevel gear is meshed with the annular bevel gear, so that the bevel gear drives the barrel body to rotate through the annular bevel gear, centrifugal rotation of the barrel body is achieved, and further the centrifugal function of the stirring and centrifuging integrated barrel is achieved.
The pneumatic opening and closing door comprises half doors, an elastic rope, a second air pipe and a controller, and sliding grooves matched with the two half doors are formed in the bottom of the barrel body; the half-split door is positioned in the sliding groove and is in sliding sealing fit with the sliding groove, and a rubber sealing sleeve is arranged at the end part of the half-split door; the rubber sealing sleeve is used for sealing the half-split door and the inner wall of the sliding chute, so that gas is prevented from overflowing from a gap between the half-split door and the inner wall of the sliding chute; one end of the second air pipe is positioned at the upper end of the barrel body, the other end of the second air pipe is communicated into the sliding chute, the second air pipe is used for introducing air into the sliding chute to close the two half doors, and a one-way valve II and an electromagnetic valve are arranged on the second air pipe; one end of the elastic rope is fixed at the end part of the sliding chute, the other end of the elastic rope is fixedly connected with the half-split door, and the elastic rope is used for returning the closed half-split door; the controller is arranged on the outer side wall of the shell and used for controlling the opening and closing of the electromagnetic valve; the electromagnetic valve is positioned in the barrel body and used for automatically releasing gas in the sliding chute to enable the half-divided door to return under the action of the elastic rope. During operation, connect the trachea through the external world and to two gas transmission of trachea, make the interior gas admission spouts of trachea two, will external world connect the trachea to remove after gas transmission finishes, will rise along with the atmospheric pressure in the spout, half minute door will be extruded, make two half minute doors draw close and closed, realize closing of pneumatic opening and shutting door, when pneumatic opening and shutting door need be opened, open through controller control solenoid valve, make the interior gas of spout released the barrel internal, under the effect of elasticity rope, half minute door returns, accomplish opening of pneumatic opening and shutting door.
The solid-liquid separation module comprises a separation chamber, an automatic reset cylinder, an extrusion block, a filter plate, a semi-automatic discharge channel, a second liquid outlet pipe and a gas outlet pipe, wherein the separation chamber is positioned at the lower end of the barrel body and is separated from the barrel body through a pneumatic opening and closing door; the filter plate divides the separation chamber into a liquid outlet chamber, and filter holes are formed in the filter plate; the automatic reset cylinder is positioned at the end part of the separation cavity and connected with the extrusion block, the automatic reset cylinder is used for pushing the extrusion block to move towards the filter plate so as to enable filter residues in the separation cavity to be filter-pressed, and the liquid state of the filter-pressed high-boiling residues flows out through the liquid outlet chamber and a second liquid outlet pipe at the lower end of the liquid outlet chamber; the length of the extrusion block is far longer than the opening width of the pneumatic opening and closing door, when the extrusion block extrudes the waste slag in the separation chamber, the upper end of the extrusion block can block the door opening of the pneumatic opening and closing door, and the waste slag is prevented from falling between the extrusion block and the automatic reset cylinder; the semi-automatic discharging channel is positioned beside the filter plate, and the semi-automatic discharging channel can automatically discharge the waste residues when the waste residues are sufficient. During operation, pneumatic opening and closing door is opened, in the separation cavity is fallen to the waste residue in the staving, start the automatic re-setting cylinder, the automatic re-setting cylinder is pushed the filter plate and is drawn close extrusion waste residue, under the continuous back and forth movement propelling movement of automatic re-setting cylinder, in the separation cavity is constantly fallen to the waste residue in the staving, the extrusion piece is extruded with the high thing liquid of boiling in the waste residue, high thing liquid that boils permeates the filter plate and gets into out the liquid room, and be collected from two flows of drain pipe, gas in the separation cavity is taken away from the outlet duct through air exhaust equipment, the waste residue falls down from semi-automatic discharging channel and is collected, residue and high thing liquid of boiling in the waste residue have been.
The semi-automatic discharging channel comprises a right-angle channel, a sealing plate, a strut, a spring and a supporting block, wherein one end of the strut is fixedly connected with the sealing plate, the other end of the strut is fixedly connected with the spring, the spring is positioned outside the right-angle channel, and the end part of the spring is abutted against the supporting block; the sealing plate is positioned in the right-angle channel and is in sliding connection with the right-angle channel, and the sealing plate is extruded by the waste residues and moves downwards until the sealing plate moves to the right angle of the right-angle channel, so that the waste residues overflow from the right angle of the right-angle channel, and the waste residues are discharged by the semi-automatic discharging channel; the supporting block is located on the shell, when the sealing plate is extruded by waste residues and moves downwards to be incapable of reaching the right angle of the right-angle channel, the supporting block can be taken out, and the sealing plate moves downwards by manually pulling the support downwards to enable the waste residues to fall out. When the waste residue separating device works, part of waste residue is extruded into the right-angle channel under the continuous extrusion of the extrusion block, along with the continuous falling of the waste residue in the barrel body and the continuous extrusion of the extrusion block, the waste residue in the separating chamber is gradually increased, the spring is compressed, the sealing plate is continuously moved downwards, the waste residue is enabled to obtain a temporary storage space, and when the sealing plate is pressed to the right angle of the right-angle channel, the waste residue is discharged from the right angle of the right-angle channel; when the sealing plate is extruded by the waste residues and moves downwards and cannot reach the right angle of the right-angle channel, the supporting block can be taken out, and the sealing plate moves downwards by manually pulling the support downwards so as to enable the waste residues to fall out.
The invention has the following beneficial effects:
1. according to the invention, the high-boiling-point substance separation and extraction is more convenient by improving the organic silicon slag slurry high-boiling-point substance separation and recovery equipment, and the monosilane preparation efficiency is improved; the nitrogen introduced into the organic silicon slag slurry high-boiling-point substance separation and recovery equipment is treated at low temperature in advance, so that the possibility of copper powder explosion is reduced, and the safety of the monosilane preparation process is effectively improved; the high-boiling residues are separately extracted from the organic silicon slag slurry, so that the blockage of a high-temperature cracking reactor by the waste residues can be avoided, and the efficiency of monosilane preparation is improved.
2. According to the invention, the organosilicon slurry is premixed by the stirring module, so that the organosilicon slurry is uniformly distributed, and lumpy waste residues are avoided, and a cushion is laid for subsequent centrifugal separation; make cam extrusion elasticity gasbag through motor drive cam, make the elasticity gasbag absorb the nitrogen gas in the hollow cavity and to letting in nitrogen gas and pressurization in the integrative bucket of stirring centrifugation, can drive the air in the high thing separation and recovery equipment that boils of organosilicon sediment thick liquid, avoid having the copper powder to meet the air and explode under the condition that the thing exists that boils, improved the security that the high thing that boils separated, and then effectively improve monosilane preparation process's security.
3. According to the invention, the organic silicon slag slurry is centrifuged and then is subjected to filter pressing again, so that high-boiling-point substances in the organic silicon slag slurry can be completely separated, and the separation effect of the high-boiling-point substances in the organic silicon slag slurry is effectively improved; meanwhile, the high-boiling-point substances in the organic silicon slag slurry are separated by adopting a centrifugal and filter pressing mode, and the efficiency is improved by one level compared with the organic silicon slag slurry treated by an evaporation mode; so that the preparation efficiency of monosilane is improved.
Drawings
FIG. 1 is a flow chart of a method of the present invention;
FIG. 2 is a schematic diagram of the hydrochloric acid storage tank of the present invention;
in the figure: the device comprises a machine shell 1, a feeding hole 11, a first liquid outlet pipe 12, a sliding groove 211, a stirring and centrifuging integrated barrel 2, a barrel body 21, a pneumatic opening and closing door 22, a half-dividing door 221, an elastic rope 222, a second gas pipe 223, filter cloth 23, a cylindrical sealing cover 24, a first automatic telescopic cylinder 25, a bearing 26, a stirring module 3, a first motor 31, a fixed seat 32, a hollow chamber 33, a spiral blade 34, a stirring blade 35, a pressurizing module 4, a cam 41, an elastic gas bag 42, an annular sealing part 43, a first gas pipe 44, a centrifugal driving mechanism 5, a second motor 51, a bevel gear 52, an annular bevel gear 53, a solid-liquid separation module 66, a separation chamber 61, an automatic resetting cylinder 62, a squeezing block 63, a filter plate 64, a semi-automatic discharging channel 65, a second liquid outlet pipe 66, a gas outlet pipe 67, a semi-automatic discharging channel 65, a right-.
Detailed Description
A method for producing monosilane using the silicone slag slurry according to the present invention will be described below with reference to fig. 1 and 2.
As shown in fig. 1 and 2, the method for preparing monosilane by using the organosilicon slurry comprises the following steps:
s1: before the organosilicon slag slurry high-boiling-point substance separation and recovery equipment is used, the organosilicon slag slurry high-boiling-point substance separation and recovery equipment is improved, a first vent pipe is externally connected to an elastic air bag, and a one-way air valve, a manual valve and a pipe joint are sequentially arranged on the first vent pipe, wherein the pipe joint is a free end, when a pneumatic opening and closing door needs to be closed, the pipe joint of the first vent pipe can be directly communicated with a second air pipe on the pneumatic opening and closing door, and the manual valve is opened, so that the elastic air bag can be used for conveying air for the pneumatic opening and closing door, and the requirement of additionally connecting a pipeline for conveying air is avoided, so that the organosilicon slag slurry high-boiling-point substance separation and recovery equipment is simpler and more convenient to use, the improvement of the high-boiling-point substance separation efficiency in organosilicon slag slurry;
s2: adding a vent pipe I into S1 organosilicon slag slurry high-boiling residue separation and recovery equipment for more convenient use, mixing a part of liquid nitrogen into a nitrogen storage container, keeping the nitrogen at a low temperature and keeping the temperature of the nitrogen below 5 ℃;
s3: the low-temperature nitrogen in the S2 is introduced into the hollow cavity in the organic silicon slag slurry high-boiling-point substance separation and recovery equipment through the external pipeline, and the organic silicon slag slurry high-boiling-point substance separation and recovery equipment is started to enable the motor to rotate, so that the organic silicon slag slurry high-boiling-point substance separation and recovery equipment is filled with the low-temperature nitrogen, copper powder in the organic silicon slag slurry is prevented from being exploded due to air under the condition that the high-boiling-point substances exist in the copper powder slurry, the air can be removed by the low-temperature nitrogen, the copper powder is at a low temperature, the possibility of copper powder explosion is reduced, and the safety of a user is effectively improved;
s4: after the air in the organic silicon slag slurry high-boiling-point substance separation and recovery equipment in the S3 is discharged by nitrogen, putting the organic silicon slag slurry into the organic silicon slag slurry high-boiling-point substance separation and recovery equipment, separating the organic silicon slag slurry into waste slag and high-boiling-point substance liquid, and simultaneously introducing gas generated in the organic silicon slag slurry high-boiling-point substance separation and recovery equipment into a sodium carbonate solution for neutralization reaction, so that the possibility that hydrogen chloride gas in the organic silicon slag slurry meets water in the air and becomes hydrochloric acid is avoided, and the possibility that the hydrogen chloride gas pollutes the environment is reduced;
s5: the liquid containing the high-boiling-point substances obtained in the step S4 is connected into a tower reactor, and the catalyst organic amine is sprayed in, fully stirred and mixed, and the high-boiling-point substances liquid is subjected to continuous high-temperature cracking at the temperature of 80-140 ℃ to break Si-Si bonds of the high-boiling-point substances, so that monosilane is obtained; because the waste residue is separated in S1, the waste residue can be prevented from blocking the high-temperature cracking reactor, and meanwhile, because the high-boiling-point substance enters the tower reactor in a liquid form, the carbon deposition is prevented from blocking the high-temperature cracking reactor, and the monosilane preparation efficiency is improved;
the organic silicon slag slurry high-boiling-point substance separation and recovery equipment in the S1 comprises a machine shell 1, a stirring and centrifuging integrated barrel 2, a stirring module 3, a pressurizing module 4, a centrifugal driving mechanism 5 and a solid-liquid separation module 6, wherein the stirring and centrifuging integrated barrel 2 is positioned at the middle upper part of the machine shell 1, the stirring and centrifuging integrated barrel 2 is rotatably connected with the machine shell 1, the stirring and centrifuging integrated barrel 2 is used for stirring and centrifuging the organic silicon slag slurry, a feed inlet 11 is arranged at the upper part of the stirring and centrifuging integrated barrel 2, and a pneumatic opening and closing door 22 is arranged at the bottom of the stirring and centrifuging integrated barrel 2; the stirring module 3 is fixed at the upper end of the machine shell 1, and the stirring module 3 is used for premixing organic silicon slag slurry in the stirring and centrifuging integrated barrel 2; the pressurizing module 4 is fixedly connected with the stirring module 3 into a whole, and the pressurizing module 4 is used for inputting inert gas into the stirring and centrifuging integrated barrel 2 and pressurizing the inert gas to disperse oxygen in the stirring and centrifuging integrated barrel 2; the centrifugal driving mechanism 5 is fixed on the side wall of the stirring module 3, and the centrifugal driving mechanism 5 is used for driving the stirring and centrifuging integrated barrel 2 to centrifugally rotate so as to preliminarily separate the organic silicon slag slurry into filter residues and high-boiling-point substance liquid; the solid-liquid separation module 6 is positioned at the lower part of the stirring and centrifuging integrated barrel 2, and the solid-liquid separation module 6 is used for extruding filter residues generated in the stirring and centrifuging integrated barrel 2 so as to fully separate high-boiling-point substance liquid from the filter residues in the filter residues and realize the complete separation of the high-boiling-point substances; wherein,
as shown in fig. 2, the stirring and centrifuging integrated barrel 2 comprises a barrel body 21, filter cloth 23, a cylindrical sealing cover 24 and an automatic telescopic cylinder I25, wherein the barrel body 21 is rotatably connected with the machine shell 1 through a bearing 26; the filter cloth 23 is provided with a plurality of pieces, the filter cloth 23 is uniformly embedded on the side wall of the barrel body 21, and the filter cloth 23 can filter high-boiling-point substance liquid in the organic silicon residue slurry; the cylindrical sealing cover 24 is sleeved outside the barrel body 21, and the end part of the cylindrical sealing cover 24 is embedded with the barrel body 21 to realize that the barrel body 21 is sealed by the cylindrical sealing cover 24; the automatic telescopic cylinder I25 is positioned at the upper end of the barrel body 21, the automatic telescopic cylinder I25 is fixed on the machine shell 1, and the automatic telescopic cylinder I25 is used for driving the cylindrical sealing cover 24 to move up and down so as to enable the side wall of the barrel body 21 to be closed or opened; the machine shell 1 is provided with a first liquid outlet pipe 12, the first liquid outlet pipe 12 is located beside the cylindrical sealing cover 24, and the first liquid outlet pipe 12 is used for discharging high-boiling-point liquid flowing out of the barrel body 21 for the first time. When the device works, when the organic silicon slag slurry high-boiling-point substance separation and recovery device is initially used, nitrogen is introduced into the pressurizing module 4, the motor I31 is started, the motor I31 drives the pressurizing module 4, the pressurizing module 4 introduces nitrogen into the stirring and centrifuging integrated barrel 2, after the nitrogen drives all oxygen in the organic silicon slag slurry high-boiling-point substance separation and recovery device out of the air, the automatic telescopic cylinder I25 is started to push the cylindrical sealing cover 24 to move downwards so that the side part of the barrel body 21 is in a sealing state, the pneumatic opening and closing door 22 is closed, organic silicon slag slurry is added from the feeding hole 11, the feeding hole 11 is closed, the motor I31 is continuously rotated, the motor I31 drives the stirring blades 35 to rotate at a low speed so as to pre-mix the organic silicon slag slurry in the stirring and centrifuging integrated barrel 2, the uniform mixing speed is not more than 100 revolutions per minute, the pressurizing module 4 continuously pressurizes the stirring and centrifuging integrated barrel 2 in the organic silicon slag, air at the position with poor air tightness is prevented from entering the stirring and centrifuging integrated barrel 2; after premixing and pressurization are completed, driving an automatic telescopic cylinder I25 to drive a cylindrical sealing cover 24 to ascend, enabling the side wall of a barrel body 21 to be in an open state, starting a centrifugal driving mechanism 5, enabling the centrifugal driving mechanism 5 to drive the barrel body 21 to rotate centrifugally, simultaneously increasing the rotating speed of a motor I31, enabling a stirring module 3 to stir organic silicon slag slurry more quickly, keeping a pressurization module 4 to continuously introduce nitrogen into a stirring and centrifuging integrated barrel 2, stopping the rotation of the motor I31 when the gas pressure in the stirring and centrifuging integrated barrel 2 is high enough, and keeping a certain liquid content in the organic silicon slag slurry after the barrel body 21 rotates centrifugally to dry the organic silicon slag slurry preliminarily and centrifugally, so that air explosion caused by good activity of waste slag is avoided; after the organic silicon slag slurry is centrifuged, high-boiling-point substance liquid flows out through the first liquid outlet pipe 12 and is collected, and waste residues generated after the organic silicon slag slurry is centrifuged fall into the solid-liquid separation module 6 through the opened pneumatic opening and closing door 22, so that the waste residues are further subjected to solid-liquid separation.
As shown in fig. 2, the stirring module 3 includes a first motor 31, a fixing seat 32, a stirring shaft, a helical blade 34 and a stirring blade 35, the fixing seat 32 is used for fixing the first motor 31 to the upper end of the casing 1, and a hollow chamber 33 is arranged at the lower part of the fixing seat 32; the stirring shaft is connected with a first motor 31; the helical blades 34 and the stirring blades 35 are alternately arranged on the stirring shaft, and the helical blades 34 and the stirring blades 35 are positioned in the stirring and centrifuging integrated barrel 2; the stirring shaft, the helical blade 34 and the stirring blade 35 are all made of hastelloy materials or Monel materials, and the hastelloy materials or the Monel materials have anti-corrosion characteristics, so that the service lives of the stirring shaft, the helical blade 34 and the stirring blade 35 can be prolonged. The during operation, a 31 rotations of motor, a 31 rotation of motor through (mixing) shaft drive stirring vane 35 and helical blade 34, and on the one hand, stirring vane 35 can stir organosilicon sediment thick liquid, and on the other hand, helical blade 34 can constantly be with pressing close to the downward propelling movement of sediment thick liquid of (mixing) shaft, makes the downward flow that organosilicon sediment thick liquid can top-down, is favorable to supplementary enhancement stirring vane 35 stirring organosilicon sediment thick liquid, improves organosilicon sediment thick liquid and mixes degree and centrifugal efficiency of stirring in advance.
As shown in fig. 2, the pressurizing module 4 comprises a cam 41, an elastic air bag 42, an annular sealing part 43 and a first air pipe 44, wherein the elastic air bag 42 is fixed on the inner wall of the hollow chamber 33, and the elastic air bag 42 is adjacent to the cam 41; the cam 41 is positioned in the hollow chamber 33, the cam 41 is fixed on the stirring shaft, and the cam 41 rotates along with the stirring shaft to intermittently extrude the elastic air bag 42; an annular groove is formed in the upper end of the barrel body 21, and a first through hole is formed in the annular groove; the annular sealing part 43 is connected with the hollow cavity 33 into a whole, the annular sealing part 43 extends into the annular groove, and the annular sealing part 43 is used for sealing the first through hole; the first air pipe 44 penetrates through the annular sealing part 43 and the first through hole to communicate the elastic air bag 42 with the barrel body 21, and a first check valve is arranged on the first air pipe 44. During operation, nitrogen is introduced into the hollow cavity 33, the hollow cavity 33 is filled with the nitrogen, the first motor 31 is started, the first motor 31 drives the stirring shaft to rotate to drive the cam 41 to rotate, the rotating cam 41 intermittently extrudes the elastic air bag 42, the elastic air bag 42 continuously sucks the nitrogen in the hollow cavity 33 and then conveys the nitrogen into the barrel body 21 through the first air pipe 44, after the elastic air bag 42 continuously conveys the nitrogen into the barrel body 21, the barrel body 21 is filled with the nitrogen, and then the whole organic silicon slag slurry high-boiling substance separation and recovery device is filled with the nitrogen, so that the air in the organic silicon slag slurry high-boiling substance separation and recovery device is completely discharged, and the harm caused by flammable and explosive substances in the organic silicon slag slurry and strong acid gas and air is avoided.
As shown in fig. 2, the centrifugal driving mechanism 5 includes a second motor 51, a bevel gear 52 and an annular bevel gear 53, the second motor 51 is fixed on the side wall of the fixed seat 32, and the second motor 51 is connected with the bevel gear 52; the annular bevel gear 53 is fixed to the upper portion of the tub 21, and the annular bevel gear 53 is engaged with the bevel gear 52 so that the tub 21 is driven by the second motor 51. During operation, the second motor 51 rotates to drive the bevel gear 52 to rotate, and the bevel gear 52 is meshed with the annular bevel gear 53, so that the bevel gear 52 drives the barrel body 21 to rotate through the annular bevel gear 53, the centrifugal rotation of the barrel body 21 is realized, and the centrifugal function of the stirring and centrifuging integrated barrel 2 is further realized.
As shown in fig. 2, the pneumatic opening and closing door 22 includes a half door 221, an elastic rope 222, a second air pipe 223 and a controller, and the bottom of the barrel 21 is provided with a chute 211 matched with the two half doors 221; the half-split door 221 is positioned in the sliding groove 211, the half-split door 221 is in sliding sealing fit with the sliding groove 211, and a rubber sealing sleeve is arranged at the end part of the half-split door 221; the rubber sealing sleeve is used for sealing the half-split door 221 and the inner wall of the sliding groove 211, so that gas is prevented from overflowing from a gap between the half-split door 221 and the inner wall of the sliding groove 211; one end of the second air pipe 223 is positioned at the upper end of the barrel body 21, the other end of the second air pipe 223 is communicated into the sliding groove 211, the second air pipe 223 is used for introducing air into the sliding groove 211 to close the two half doors 221, and a second check valve and an electromagnetic valve are arranged on the second air pipe 223; one end of the elastic rope 222 is fixed at the end of the sliding groove 211, the other end of the elastic rope 222 is fixedly connected with the half-split door 221, and the elastic rope 222 is used for returning the closed half-split door 221; the controller is arranged on the outer side wall of the shell and used for controlling the opening and closing of the electromagnetic valve; the electromagnetic valve is positioned in the barrel body 21 and used for automatically releasing air in the sliding groove 211 so that the half-divided door 221 returns under the action of the elastic rope 222. During operation, receive the trachea through the external world and transmit gas to trachea two 223, make the gas in the trachea two 223 get into in the spout 211, remove external world and receive the trachea after the gas transmission, will be along with the atmospheric pressure rise in the spout 211, half minute door 221 will be extrudeed, make two half minute doors 221 draw close and closed, realize closing of pneumatic door 22 that opens and shuts, when pneumatic door 22 that opens and shuts need open, open through controller control solenoid valve, make the gas in the spout 211 released in the staving 21, under the effect of elastic rope 222, half minute door 221 returns, accomplish opening of pneumatic door 22 that opens and shuts.
As shown in fig. 2, the solid-liquid separation module 6 includes a separation chamber 61, an automatic reset cylinder 62, an extrusion block 63, a filter plate 64, a semi-automatic discharge channel 65, a second liquid outlet pipe 66 and a gas outlet pipe 67, the separation chamber 61 is located at the lower end of the barrel 21, and the separation chamber 61 is separated from the barrel 21 by a pneumatic opening and closing door 22; the filter plate 64 divides the separation chamber 61 into a liquid outlet chamber, and filter holes are formed in the filter plate 64; the automatic reset cylinder 62 is positioned at the end part of the separation chamber 61, the automatic reset cylinder 62 is connected with the extrusion block 63, the automatic reset cylinder 62 is used for pushing the extrusion block 63 to move towards the filter plate 64 so as to enable filter residues in the separation chamber 61 to be filter-pressed, and the liquid state of the filter-pressed high-boiling residues flows out through the liquid outlet chamber and the liquid outlet pipe II 66 at the lower end of the liquid outlet chamber; the length of the extrusion block 63 is far longer than the opening width of the pneumatic opening and closing door 22, when the extrusion block 63 extrudes the waste slag in the separation chamber 61, the upper end of the extrusion block 63 can block the door opening of the pneumatic opening and closing door 22, and the waste slag is prevented from falling between the extrusion block 63 and the automatic reset cylinder 62; the semi-automatic discharging channel 65 is positioned beside the filter plate 64, and the semi-automatic discharging channel 65 can automatically drop waste residues when the waste residues are sufficient. During operation, pneumatic opening and closing door 22 is opened, the waste residue in the staving 21 falls into separation cavity 61, start automatic re-setting cylinder 62, automatic re-setting cylinder 62 pushes to filter plate 64 and draws close the extrusion waste residue, under the continuous back and forth movement propelling movement of automatic re-setting cylinder 62, the waste residue constantly falls into separation cavity 61 from the staving 21 in, the high boiling thing liquid in the waste residue is extruded to extrusion piece 63, high boiling thing liquid permeates filter plate 64 and gets into out the liquid room, and flow out from two 66 drain pipes and be collected, gas in the separation cavity 61 is taken away from outlet duct 67 through air extraction equipment, the waste residue falls from semi-automatic discharging channel 65 and is collected, the residue in the waste residue has been realized and high boiling thing liquid is separated once more.
As shown in fig. 2, the semi-automatic discharge channel 65 comprises a right-angled channel 651, a sealing plate 652, a post 653, a spring 654 and a support block 655, wherein one end of the post 653 is fixedly connected to the sealing plate 652, the other end of the post 653 is fixedly connected to the spring 654, the spring 654 is located outside the right-angled channel 651, and the end of the spring 654 abuts against the support block 655; the sealing plate 652 is positioned in the right-angle channel 651, the sealing plate 652 is in sliding connection with the right-angle channel 651, the sealing plate 652 is pressed by waste residues and moves downwards until the sealing plate 652 moves to the right angle of the right-angle channel 651, so that the waste residues overflow from the right angle of the right-angle channel 651, and the waste residues are discharged from the semi-automatic discharging channel 65; the support block 655 is located on the housing, and when the sealing plate 652 is pressed by the waste slag and moves downwards and cannot reach the right angle of the right-angle channel 651, the support block 655 can be taken out, and the sealing plate 652 is moved downwards by manually pulling the support 653 downwards, so that the waste slag falls out. During operation, part of the waste residues are extruded into the right-angle channel 651 under the continuous extrusion of the extrusion block 63, along with the continuous falling of the waste residues in the barrel body 21 and the continuous extrusion of the extrusion block 63, the waste residues in the separation chamber 61 are gradually increased, the spring 654 is compressed, the sealing plate 652 is continuously moved downwards, the waste residues obtain a temporary storage space, and when the sealing plate 652 is pressed to the right angle of the right-angle channel 651, the waste residues are discharged from the right angle of the right-angle channel 651; when the sealing plate 652 is pressed by the slag and moves downward and does not reach the right angle of the right angle channel 651, the support block 655 can be removed and the sealing plate 652 can be moved downward by manually pulling down the posts 653 to drop the slag.
The specific use flow is as follows:
when the device is used, when the device for separating and recovering the high-boiling-point substances of the organic silicon slag slurry is initially used, nitrogen is introduced into the hollow cavity 33, the hollow cavity 33 is filled with the nitrogen, the motor I31 is started, the stirring shaft is driven by the motor I31 to rotate to drive the cam 41 to rotate, the elastic air bag 42 is intermittently extruded by the rotating cam 41, the elastic air bag 42 continuously sucks the nitrogen in the hollow cavity 33 and then conveys the nitrogen into the barrel body 21 through the air pipe I44, after the elastic air bag 42 continuously conveys the nitrogen into the barrel body 21, the barrel body 21 is filled with the nitrogen, then, the whole device for separating and recovering the high-boiling-point substances of the organic silicon slag slurry is filled with the nitrogen, so that the air in the device for separating and recovering the high-boiling-point substances of the organic silicon slag slurry is completely discharged, the flammable and explosive substances in the organic silicon slag slurry and the strong acid gas are prevented from being harmful to the air, and, starting an automatic telescopic cylinder I25 to push a cylindrical sealing cover 24 to move downwards to enable the side part of a barrel body 21 to be in a sealing state, conveying gas to a gas pipe II 223 through an external gas receiving pipe, enabling the gas in the gas pipe II 223 to enter a sliding groove 211, removing the external gas receiving pipe after the gas conveying is finished, enabling a half door 221 to be extruded along with the increase of the air pressure in the sliding groove 211, enabling two half doors 221 to be closed and closed, closing a pneumatic opening and closing door 22, simultaneously adding organic silicon slurry from a feeding hole 11, then closing the feeding hole 11, continuously enabling a motor I31 to rotate, enabling the motor I31 to drive a stirring blade 35 to rotate at a low speed to stir and pre-mix the organic silicon slurry in a stirring and centrifuging integrated barrel 2, enabling the mixing speed to be not more than 100 revolutions per minute, on one hand, the stirring blade 35 can stir the organic silicon slurry, on the other hand, a spiral blade 34 can continuously push the slurry close to a, the organosilicon slurry can flow downwards from top to bottom, which is beneficial to the auxiliary reinforced stirring blade 35 to stir the organosilicon slurry and improves the premixing and uniform stirring degree and the centrifugation efficiency of the organosilicon slurry; in the process of uniformly mixing the organic silicon slag slurry, the first motor 31 drives the stirring shaft to rotate to drive the cam 41 to rotate, the rotating cam 41 intermittently extrudes the elastic air bag 42, the elastic air bag 42 continuously sucks nitrogen in the hollow cavity 33 and then conveys the nitrogen into the barrel body 21 through the first air pipe 44, after the elastic air bag 42 continuously conveys the nitrogen into the barrel body 21, the barrel body 21 is filled with the nitrogen, and then the whole organic silicon slag slurry high-boiling-point substance separation and recovery device is filled with the nitrogen, so that air in the organic silicon slag slurry high-boiling-point substance separation and recovery device is completely discharged, and flammable and explosive substances in the organic silicon slag slurry and strong acid gas and air are prevented from generating harm; after premixing and pressurization are completed, driving an automatic telescopic cylinder I25 to drive a cylindrical sealing cover 24 to ascend, enabling the side wall of a barrel body 21 to be in an open state, starting a centrifugal driving mechanism 5, enabling the centrifugal driving mechanism 5 to drive the barrel body 21 to rotate centrifugally, simultaneously increasing the rotating speed of a motor I31, enabling a stirring module 3 to stir organic silicon slag slurry more quickly, keeping a pressurization module 4 to continuously introduce nitrogen into a stirring and centrifuging integrated barrel 2, stopping the rotation of the motor I31 when the gas pressure in the stirring and centrifuging integrated barrel 2 is high enough, and keeping a certain liquid content in the organic silicon slag slurry after the barrel body 21 rotates centrifugally to dry the organic silicon slag slurry preliminarily and centrifugally, so that air explosion caused by good activity of waste slag is avoided; after the organosilicon slurry is centrifuged, high-boiling-point substance liquid flows out through the first liquid outlet pipe 12 and is collected, the electromagnetic valve is controlled by the controller to be opened, gas in the chute 211 is released into the barrel body 21, the half-door 221 returns under the action of the elastic rope 222, the pneumatic opening-closing door 22 is opened, waste residue generated after the organosilicon slurry is centrifuged falls into the separation chamber 61 through the opened pneumatic opening-closing door 22, the automatic reset cylinder 62 is started, the automatic reset cylinder 62 pushes the filter plate 64 to draw close and extrude the waste residue, the waste residue continuously falls into the separation chamber 61 from the barrel body 21 under the continuous back-and-forth movement pushing of the automatic reset cylinder 62, the high-boiling-point substance liquid in the waste residue is extruded by the extrusion block 63, the high-boiling-point substance liquid enters the liquid outlet chamber through the filter plate 64 and flows out from the second liquid outlet pipe 66 and is collected, the gas in the separation chamber 61 is pumped out from the gas outlet pipe 67 through, the waste residues fall from the semi-automatic discharging channel 65 and are collected, so that the residues in the waste residues and the high-boiling-point substance liquid are separated again;
in the process of separating residues in the waste residues from high-boiling-point substance liquid, part of the waste residues are extruded into the right-angle channel 651 under the continuous extrusion of the extrusion block 63, along with the continuous falling of the waste residues in the barrel body 21 and the continuous extrusion of the extrusion block 63, the waste residues in the separation chamber 61 are gradually increased, the spring 654 is compressed, the sealing plate 652 is continuously moved downwards, the waste residues are enabled to obtain a temporary storage space, and when the sealing plate 652 is pressed to the right angle of the right-angle channel 651, the waste residues are discharged from the right angle of the right-angle channel 651; when the sealing plate 652 is pressed by the slag and moves downward and does not reach the right angle of the right angle channel 651, the support block 655 can be removed and the sealing plate 652 can be moved downward by manually pulling down the posts 653 to drop the slag.
(A) In the above embodiment, nitrogen gas is introduced into the stirring and centrifuging integrated tank, but the present invention is not limited thereto, and a rare gas that does not react with the silicone slurry may be introduced.
While one embodiment of the present invention has been described above, the present invention is not limited to the above embodiment, and various modifications can be made without departing from the scope of the present invention.
Industrial applicability
According to the invention, the high-boiling-point substance separation and extraction is more convenient by improving the organic silicon slag slurry high-boiling-point substance separation and recovery equipment, and the monosilane preparation efficiency is improved; the nitrogen introduced into the organic silicon slag slurry high-boiling-point substance separation and recovery equipment is treated at low temperature in advance, so that the possibility of copper powder explosion is reduced, and the safety of the monosilane preparation process is effectively improved; the high-boiling-point substances are separately extracted from the organic silicon slag slurry, so that the blockage of a high-temperature cracking reactor by waste residues can be avoided, the efficiency of monosilane preparation is improved, and the conversion rate of the high-boiling-point substances to monosilane is improved; therefore, the organic silicon slag slurry high-boiling residue separation and recovery equipment is useful in the technical field of monosilane preparation.

Claims (7)

1. A method for preparing monosilane by using organosilicon slurry is characterized in that; the method comprises the following steps:
s1: before the organic silicon slag slurry high-boiling-point substance separation and recovery equipment is used, the organic silicon slag slurry high-boiling-point substance separation and recovery equipment is improved, a first vent pipe is externally connected to an elastic air bag, and a one-way air valve, a manual valve and a pipe joint are sequentially arranged on the first vent pipe, wherein the pipe joint is a free end, when a pneumatic opening and closing door needs to be closed, the pipe joint of the first vent pipe can be directly communicated with a second air pipe on the pneumatic opening and closing door, and the air can be conveyed by the elastic air bag for the pneumatic opening and closing door after the manual valve is opened;
s2: adding a vent pipe I into S1 organosilicon slag slurry high-boiling residue separation and recovery equipment for more convenient use, mixing a part of liquid nitrogen into a nitrogen storage container, keeping the nitrogen at a low temperature and keeping the temperature of the nitrogen below 5 ℃;
s3: introducing the low-temperature nitrogen in the S2 into a hollow cavity in the organic silicon slag slurry high-boiling-point substance separation and recovery equipment through an external pipeline, starting the organic silicon slag slurry high-boiling-point substance separation and recovery equipment, and rotating a motor to ensure that the interior of the organic silicon slag slurry high-boiling-point substance separation and recovery equipment is filled with the low-temperature nitrogen;
s4: after the air in the organic silicon slag slurry high-boiling-point substance separation and recovery equipment in the S3 is discharged by nitrogen, putting the organic silicon slag slurry into the organic silicon slag slurry high-boiling-point substance separation and recovery equipment, and separating the organic silicon slag slurry into waste slag and high-boiling-point substance liquid;
s5: the liquid containing the high-boiling-point substances obtained in the step S4 is connected into a tower reactor, and the catalyst organic amine is sprayed in, fully stirred and mixed, and the high-boiling-point substances liquid is subjected to continuous high-temperature cracking at the temperature of 80-140 ℃ to break Si-Si bonds of the high-boiling-point substances, so that monosilane is obtained;
the organic silicon slag slurry high-boiling-point substance separation and recovery equipment in the S1 comprises a machine shell (1), a stirring and centrifuging integrated barrel (2), a stirring module (3), a pressurizing module (4), a centrifugal driving mechanism (5) and a solid-liquid separation module (6), wherein the stirring and centrifuging integrated barrel (2) is positioned at the middle upper part of the machine shell (1), the stirring and centrifuging integrated barrel (2) is rotatably connected with the machine shell (1), the stirring and centrifuging integrated barrel (2) is used for stirring and centrifuging the organic silicon slag slurry, a feeding hole (11) is formed in the upper part of the stirring and centrifuging integrated barrel (2), and a pneumatic opening and closing door (22) is formed in the bottom of the stirring and centrifuging integrated barrel (2); the stirring module (3) is fixed at the upper end of the machine shell (1), and the stirring module (3) is used for premixing organic silicon slag slurry in the stirring and centrifuging integrated barrel (2); the pressurizing module (4) is fixedly connected with the stirring module (3) into a whole, and the pressurizing module (4) is used for inputting inert gas into the stirring and centrifuging integrated barrel (2) and pressurizing to disperse oxygen in the stirring and centrifuging integrated barrel (2); the centrifugal driving mechanism (5) is fixed on the side wall of the stirring module (3), and the centrifugal driving mechanism (5) is used for driving the stirring and centrifuging integrated barrel (2) to centrifugally rotate so as to primarily separate the organic silicon slag slurry into filter residues and high-boiling-point liquid; the solid-liquid separation module (6) is positioned at the lower part of the stirring and centrifuging integrated barrel (2), and the solid-liquid separation module (6) is used for extruding filter residues generated in the stirring and centrifuging integrated barrel (2) so as to fully separate high-boiling-point substance liquid from the filter residues in the filter residues and realize the complete separation of the high-boiling-point substances; wherein,
the stirring and centrifuging integrated barrel (2) comprises a barrel body (21), filter cloth (23), a cylindrical sealing cover (24) and an automatic telescopic cylinder I (25), wherein the barrel body (21) is rotatably connected with the machine shell (1) through an arranged bearing (26); the filter cloth (23) is provided with a plurality of pieces, the filter cloth (23) is uniformly embedded on the side wall of the barrel body (21), and the filter cloth (23) can filter high-boiling-point substance liquid in the organosilicon slurry; the cylindrical sealing cover (24) is sleeved outside the barrel body (21), and the end part of the cylindrical sealing cover (24) is embedded with the barrel body (21) to realize that the barrel body (21) is sealed by the cylindrical sealing cover (24); the automatic telescopic cylinder I (25) is positioned at the upper end of the barrel body (21), the automatic telescopic cylinder I (25) is fixed on the shell (1), and the automatic telescopic cylinder I (25) is used for driving the cylindrical sealing cover (24) to move up and down to enable the side wall of the barrel body (21) to be closed or opened; be provided with drain pipe (12) on casing (1), and drain pipe (12) are located cylindric sealed cowling (24) side, and drain pipe (12) are used for discharging the high boiling thing liquid of initial outflow in staving (21).
2. The method for preparing monosilane by using the organosilicon slurry according to claim 1, wherein: the stirring module (3) comprises a first motor (31), a fixed seat (32), a stirring shaft, a spiral blade (34) and a stirring blade (35), wherein the fixed seat (32) is used for fixing the first motor (31) at the upper end of the machine shell (1), and a hollow cavity (33) is arranged at the lower part of the fixed seat (32); the stirring shaft is connected with a first motor (31); the spiral blades (34) and the stirring blades (35) are alternately arranged on the stirring shaft, and the spiral blades (34) and the stirring blades (35) are positioned in the stirring and centrifuging integrated barrel (2).
3. The method for preparing monosilane by using the organosilicon slurry according to claim 2, wherein: the pressurizing module (4) comprises a cam (41), an elastic air bag (42), an annular sealing part (43) and a first air pipe (44), wherein the elastic air bag (42) is fixed on the inner wall of the hollow chamber (33), and the elastic air bag (42) is close to the cam (41); the cam (41) is positioned in the hollow cavity (33), the cam (41) is fixed on the stirring shaft, and the cam (41) intermittently extrudes the elastic air bag (42) along with the rotation of the stirring shaft; an annular groove is formed in the upper end of the barrel body (21), and a first through hole is formed in the annular groove; the annular sealing part (43) is connected with the hollow cavity (33) into a whole, the annular sealing part (43) extends into the annular groove, and the annular sealing part (43) is used for sealing the first through hole; the first air pipe (44) penetrates through the annular sealing part (43) and the first through hole to communicate the elastic air bag (42) with the barrel body (21), and a first check valve is arranged on the first air pipe (44).
4. The method for preparing monosilane by using the organosilicon slurry according to claim 2, wherein: the centrifugal driving mechanism (5) comprises a second motor (51), a bevel gear (52) and an annular bevel gear (53), the second motor (51) is fixed on the side wall of the fixed seat (32), and the second motor (51) is connected with the bevel gear (52); the annular bevel gear (53) is fixed at the upper part of the barrel body (21), and the annular bevel gear (53) is meshed with the bevel gear (52) so that the barrel body (21) is driven by the second motor (51).
5. The method for preparing monosilane by using the organosilicon slurry according to claim 1, wherein: the pneumatic opening and closing door (22) comprises a half door (221), an elastic rope (222), a second air pipe (223) and a controller, and a sliding groove (211) matched with the two half doors (221) is formed in the bottom of the barrel body (21); the half-split door (221) is positioned in the sliding groove (211), the half-split door (221) is in sliding sealing fit with the sliding groove (211), and a rubber sealing sleeve is arranged at the end part of the half-split door (221); the rubber sealing sleeve is used for sealing the half-split door (221) and the inner wall of the sliding groove (211) to prevent gas from overflowing from a gap between the half-split door (221) and the inner wall of the sliding groove (211); one end of the second air pipe (223) is located at the upper end of the barrel body (21), the other end of the second air pipe (223) is communicated into the sliding groove (211), the second air pipe (223) is used for introducing air into the sliding groove (211) to close the two half doors (221), and a second check valve and an electromagnetic valve are arranged on the second air pipe (223); one end of the elastic rope (222) is fixed at the end of the sliding groove (211), the other end of the elastic rope (222) is fixedly connected with the half-split door (221), and the elastic rope (222) is used for returning the closed half-split door (221); the controller is arranged on the outer side wall of the shell and used for controlling the opening and closing of the electromagnetic valve; the electromagnetic valve is positioned in the barrel body (21) and used for automatically releasing gas in the sliding groove (211) to enable the half-divided door (221) to return under the action of the elastic rope (222).
6. The method for preparing monosilane by using the organosilicon slurry according to claim 1, wherein: the solid-liquid separation module (6) comprises a separation chamber (61), an automatic reset cylinder (62), an extrusion block (63), a filter plate (64), a semi-automatic discharge channel (65), a second liquid outlet pipe (66) and a gas outlet pipe (67), the separation chamber (61) is positioned at the lower end of the barrel body (21), and the separation chamber (61) is separated from the barrel body (21) through a pneumatic opening and closing door (22); the filter plate (64) divides the separation chamber (61) into a liquid outlet chamber, and filter holes are formed in the filter plate (64); the automatic reset cylinder (62) is positioned at the end part of the separation cavity (61), the automatic reset cylinder (62) is connected with the extrusion block (63), the automatic reset cylinder (62) is used for pushing the extrusion block (63) to move towards the filter plate (64) so that filter residues in the separation cavity (61) are subjected to filter pressing, and the liquid state of the filter-pressed high-boiling-point substance flows out through the liquid outlet chamber and a second liquid outlet pipe (66) at the lower end of the liquid outlet chamber; the semi-automatic discharging channel (65) is positioned beside the filter plate (64), and the semi-automatic discharging channel (65) can automatically drop waste residues when the waste residues are sufficient.
7. The method for preparing monosilane by using the organosilicon slurry according to claim 6, wherein: the semi-automatic discharging channel (65) comprises a right-angle channel (651), a sealing plate (652), a support post (653), a spring (654) and a supporting block (655), one end of the support post (653) is fixedly connected with the sealing plate (652), the other end of the support post (653) is fixedly connected with the spring (654), the spring (654) is positioned outside the right-angle channel (651), and the end part of the spring (654) is abutted against the supporting block (655); the sealing plate (652) is positioned in the right-angle channel (651), the sealing plate (652) is in sliding connection with the right-angle channel (651), the sealing plate (652) is extruded by waste residues and moves downwards until the sealing plate (652) moves to the right-angle position of the right-angle channel (651), so that the waste residues overflow from the right-angle position of the right-angle channel (651), and the waste residues are discharged from the semi-automatic discharging channel (65); the supporting block (655) is positioned on the shell, when the sealing plate (652) is extruded by waste slag and moves downwards and cannot reach the right angle of the right-angle channel (651), the supporting block (655) can be taken out, and the sealing plate (652) moves downwards by manually pulling the support (653) downwards, so that the waste slag falls out.
CN201811087679.7A 2018-09-18 2018-09-18 Method for preparing monosilane by using organosilicon slag slurry Expired - Fee Related CN109250722B (en)

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CN109897058A (en) * 2019-02-28 2019-06-18 天津大学 An organosilicon slurry slag treatment system and treatment process
CN111791528A (en) * 2020-07-24 2020-10-20 张建华 A silicone extrusion device

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2174950C1 (en) * 2000-08-15 2001-10-20 Общество с ограниченной ответственностью "Ц.Е.С. - Украина" Method of preparing silane
WO2006041272A1 (en) * 2004-10-12 2006-04-20 The Ministry Of Education And Sciences Of Republic Kazakhstan Republican State Enterprise 'center Of Chemical-Technological Researches' Method of silane production
CN101386626A (en) * 2008-10-31 2009-03-18 江苏宏达新材料股份有限公司 Organosilicon slag slurry treatment method and apparatus thereof
CN105037414A (en) * 2015-07-29 2015-11-11 湖北兴瑞化工有限公司 Method and device for recovering efficient high-boiling substance from organic silicon residue slurry

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2174950C1 (en) * 2000-08-15 2001-10-20 Общество с ограниченной ответственностью "Ц.Е.С. - Украина" Method of preparing silane
WO2006041272A1 (en) * 2004-10-12 2006-04-20 The Ministry Of Education And Sciences Of Republic Kazakhstan Republican State Enterprise 'center Of Chemical-Technological Researches' Method of silane production
CN101386626A (en) * 2008-10-31 2009-03-18 江苏宏达新材料股份有限公司 Organosilicon slag slurry treatment method and apparatus thereof
CN105037414A (en) * 2015-07-29 2015-11-11 湖北兴瑞化工有限公司 Method and device for recovering efficient high-boiling substance from organic silicon residue slurry

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