CN214840087U - Chlorosilane filling system - Google Patents

Abstract

The utility model discloses a chlorosilane fills dress system, chlorosilane fill dress system including filling pipe, protection air supply, chlorosilane storage tank, gas-liquid separation device, vacuum pump and cooling device, fill the dress pipe and have protection gas port, chlorosilane import, evacuation mouth and fill the dress interface, protection air supply and protection gas port intercommunication, chlorosilane storage tank and chlorosilane import intercommunication, gas-liquid separation device are used for the separation to follow the chlorosilane import is supplied with liquid drop in the gaseous chlorosilane in the dress pipe, vacuum pump and evacuation mouth intercommunication, cooling device establish on filling the dress pipe and be located gas-liquid separation device and fill between the dress interface, and cooling device is arranged in cooling gaseous chlorosilane for liquid chlorosilane and separation and the noncondensable gas in the discharge chlorosilane. The utility model discloses a chlorosilane fills dress system has avoided impurity and the condition that the granularity exceeds standard in the chlorosilane, has promoted filling dress quality of chlorosilane.

Description

Chlorosilane filling system

Technical Field

The utility model relates to a chlorosilane fills dress technical field, specifically relates to a chlorosilane fills dress system.

Background

In the related art, chlorosilane such as dichlorosilane, trichlorosilane, silicon tetrachloride and monochlorotrihydrogensilicon is mostly filled by a gas cylinder, and the chlorosilane is introduced into the gas cylinder by using pressure difference, so that the filling is completed.

However, the above-described filling method has the following problems: firstly, when filling a single-port gas cylinder, the gas cylinder is provided with only one inlet and is not provided with an exhaust port, feeding can compress the space in the gas cylinder, the space in the gas cylinder is smaller and smaller along with the increase of feeding, the pressure difference between the feeding and the gas cylinder is reduced, the filling time is long, the filling process is easily influenced by the environment temperature, the pressure in the gas cylinder is increased due to the fact that the material is easily gasified at the high environment temperature, the raw material cannot be further filled into the gas cylinder, and the set weight cannot be effectively controlled; impurities such as trace water, hydrogen, metal, solid particles and the like exist in filling systems such as raw materials, filling pipelines and the like, so that the impurities in the chlorosilane exceed the standard easily, and the filling quality of the chlorosilane is influenced, but no further purification measures exist in the conventional scheme; and thirdly, aiming at the filling system with the filter partially added, although the filling quality is improved to a certain extent, the filter needs to be frequently replaced, and the filling cost is increased.

SUMMERY OF THE UTILITY MODEL

The present invention aims at solving at least one of the technical problems in the related art to a certain extent.

Therefore, the embodiment of the utility model provides a chlorosilane fills dress system, this chlorosilane fill dress system have avoided impurity and the condition that the granularity exceeds standard in the chlorosilane, have promoted filling of chlorosilane quality and filling dress efficiency.

According to the utility model discloses chlorosilane fills dress system includes: the charging pipe is provided with a protective gas port, a chlorosilane inlet, a vacuumizing port and a charging interface suitable for being connected with a chlorosilane gas cylinder; the protective gas source is communicated with the protective gas port and is used for supplying protective gas into the filling pipe to purge the filling pipe; the chlorosilane storage tank is communicated with the chlorosilane inlet and is used for storing and sub-boiling evaporating liquid chlorosilane so as to supply gaseous chlorosilane into the filling pipe; a gas-liquid separation device for separating liquid droplets in the gaseous chlorosilane supplied from the chlorosilane inlet into the filling pipe; the vacuum pump is communicated with the vacuumizing port and is used for vacuumizing the filling pipe and a chlorosilane gas cylinder connected with the filling interface; and the cooling device is arranged on the filling pipe and is positioned between the gas-liquid separation device and the filling interface, and the cooling device is used for cooling the gaseous chlorosilane into liquid chlorosilane and separating and discharging non-condensable gas in the chlorosilane.

According to the utility model discloses chlorosilane fills dress system has avoided impurity and the condition that the granularity exceeds standard in the chlorosilane, has promoted filling dress quality of chlorosilane and has filled dress efficiency.

In some embodiments, the cooling device is a chiller.

In some embodiments, the chlorosilane filling system further comprises a return pipe, wherein the return pipe is connected between the gas-liquid separation device and the chlorosilane storage tank and is used for returning the liquid drops to the chlorosilane storage tank.

In some embodiments, the chlorosilane filling system further comprises a weighing device and a first heating device, wherein the weighing device is used for weighing the chlorosilane gas cylinder, and the first heating device is used for heating the gas cylinder to heat part of liquid chlorosilane in the chlorosilane gas cylinder into gaseous chlorosilane.

In some embodiments, the chlorosilane filling system further comprises a detection device, and the detection device is detachably connected with the chlorosilane gas cylinder, so that part of liquid chlorosilane in the chlorosilane gas cylinder is heated into gaseous chlorosilane by the first heating device and enters the detection device for detection.

In some embodiments, the chlorosilane filling system further comprises a filling valve and a controller arranged at the filling interface, wherein the controller is connected with the weighing device and the filling valve to control the filling valve according to the weighing value of the weighing device.

In some embodiments, the chlorosilane filling system further comprises a filling panel, wherein the filling panel is internally provided with a filling channel, the filling channel is provided with an inlet communicated with the filling interface and a plurality of outlet ports, and the outlet ports are suitable for being detachably connected with a plurality of chlorosilane gas cylinders in a one-to-one correspondence manner.

In some embodiments, the chlorosilane filling system further comprises a second heating device, the second heating device is arranged on the chlorosilane storage tank and used for heating the surface of the chlorosilane in the chlorosilane storage tank through microwave or infrared radiation, a jacket is arranged on the periphery of the chlorosilane storage tank, the jacket is provided with a heating medium channel, and the heating medium channel is provided with a medium inlet used for introducing a heating medium to heat liquid chlorosilane in the chlorosilane storage tank and a medium outlet used for discharging the heating medium.

In some embodiments, a temperature sensor for detecting the temperature of liquid chlorosilane in the chlorosilane storage tank is arranged in the chlorosilane storage tank.

In some embodiments, the second heating device is provided in a plurality of layers in the up-down direction.

Drawings

Fig. 1 is an overall schematic diagram of chlorosilane fills dress system according to the embodiment of the utility model discloses.

Fig. 2 is a schematic view of the chlorosilane gas cylinder of fig. 1.

FIG. 3 is a schematic view of the chlorosilane storage tank of FIG. 1.

Fig. 4 is a schematic top view of the chlorosilane storage tank of fig. 3.

Reference numerals:

a filling tube 1; a protection gas port 11; a chlorosilane inlet 12; a vacuum-pumping port 13; a filling interface 14; a filling valve 15;

a protective gas source 2;

a chlorosilane storage tank 3; a liquid discharge port 31; a jacket 32; a medium outlet 33; a media inlet 34; a second heating device 35; a temperature sensor 36;

a gas-liquid separation device 4; a return pipe 41;

a cooling device 5; the noncondensable gas discharge port 51;

a vacuum pump 6;

a chlorosilane gas cylinder 7; a first heating device 71; a weighing device 72; a metal hose 73.

Detailed Description

Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings. The embodiments described below with reference to the drawings are exemplary and intended to be used for explaining the present invention, and should not be construed as limiting the present invention.

As shown in fig. 1 to 4, the chlorosilane filling system according to the embodiment of the present invention includes a filling pipe 1, a protective gas source 2, a chlorosilane storage tank 3, a gas-liquid separation device 4, a vacuum pump 6, and a cooling device 5.

The filling tube 1 has a protective gas port 11, a chlorosilane inlet 12, a vacuum port 13 and a filling connection 14 adapted to be connected to the chlorosilane gas cylinder 7.

As shown in fig. 1, the filling pipe 1 is a straight pipe, the filling pipe 1 extends along a direction from left to right, and the protective gas port 11, the chlorosilane inlet 12, the vacuum pumping port 13 and the filling interface 14 are sequentially arranged on the filling pipe 1 at intervals along the direction from left to right.

It will be appreciated that in other embodiments the filling tube 1 may also be a bent tube, a folded tube, a ring tube, etc. The protective gas port 11, the chlorosilane inlet 12, the vacuum-pumping port 13 and the filling interface 14 can also be arranged in other sequences, for example, the protective gas port 11 can be arranged between the chlorosilane inlet 12 and the vacuum-pumping port 13; the evacuation port 13 may also be provided to the left of the protection port 11 or to the right of the fill port 14.

A shielding gas source 2 communicates with the shielding gas port 11 for supplying shielding gas into the filling tube 1 to purge the filling tube 1. As shown in fig. 1, the shielding gas source 2 may be an inert gas, for example, the shielding gas source 2 may be nitrogen, argon, helium, or the like. The inert gas can be stored in a special storage container which communicates with a protective gas opening 11 in the filling pipe 1, through which protective gas opening 11 the filling pipe 1 can be filled with inert gas.

Before filling chlorosilane gas cylinder 7, can be with protection air supply 2 and fill filler pipe 1 switch-on, then utilize inert gas to sweep the replacement to fill filler pipe 1, from this, can replace the trace water, trace oxygen, impure gas etc. in filling filler pipe 1, play the effect that reduces impurity, be favorable to improving the filling quality of chlorosilane.

The chlorosilane storage tank 3 is communicated with the chlorosilane inlet 12, and the chlorosilane storage tank 3 is used for storing and sub-boiling evaporating liquid chlorosilane to supply gaseous chlorosilane into the filling pipe 1.

As shown in fig. 1, liquid chlorosilane is stored in the chlorosilane storage tank 3, and the liquid chlorosilane may be dichlorosilane, and may also be chlorosilane such as trichlorosilane, silicon tetrachloride, monochlorotrihydrogensilicon, and the like. The chlorosilane storage tank 3 is communicated with the chlorosilane inlet 12 on the filling pipe 1, the chlorosilane storage tank 3 has a heating function, so that liquid chlorosilane in the chlorosilane storage tank 3 can be sub-boiled and evaporated into gaseous chlorosilane, and the chlorosilane in the chlorosilane storage tank 3 can be supplied into the filling pipe 1 in a gaseous form. Therefore, metal ions, solid particles, siloxane compounds and the like in the chlorosilane storage tank 3 can be enriched in the chlorosilane storage tank 3, and cannot be supplied into the filling pipe 1 along with gaseous chlorosilane, so that the filling quality of the chlorosilane is improved.

The gas-liquid separation device 4 serves to separate liquid droplets from the gaseous chlorosilane which is fed from the chlorosilane inlet 12 into the filling pipe 1.

Specifically, the gas-liquid separation device 4 is arranged on the filling pipe 1, and the gas-liquid separation device 4 is positioned between the chlorosilane inlet 12 and the filling interface 14. The gas-liquid separation device 4 is a gas-liquid separator, the gas-liquid separation device 4 has a gas-liquid separation function, and in the chlorosilane filling process, the gas-liquid separation device 4 can filter liquid drops in the gaseous chlorosilane, so that the situation that metal ions, solid particles and siloxane compounds in the liquid drops enter the chlorosilane gas cylinder 7 is avoided, and the chlorosilane filling quality is further improved.

It is understood that in other embodiments, the gas-liquid separation device 4 may be provided on the pipeline between the charging pipe 1 and the chlorosilane storage tank 3.

The vacuum pump 6 is communicated with the vacuumizing port 13, and the vacuum pump 6 is used for vacuumizing the filling pipe 1 and the chlorosilane gas cylinder 7 connected with the filling interface 14.

As shown in fig. 1, the vacuum pump 6 communicates with the evacuation port 13 of the filling tube 1, and the vacuum pump 6 can generate a negative pressure, thereby performing a function of evacuating the filling tube 1. The contents of trace water, trace oxygen and impurity gas in the filling pipe 1 can be reduced by multiple times of vacuumizing of the vacuum pump 6 and multiple times of feeding inert gas into the protective gas source 2.

The cooling device 5 is arranged on the filling pipe 1 and is positioned between the gas-liquid separation device 4 and the filling interface 14, and the cooling device 5 is used for cooling the gaseous chlorosilane into liquid chlorosilane and separating and discharging non-condensable gas in the chlorosilane.

Specifically, the cooling device 5 has a refrigeration effect, the cooling device 5 is arranged at the downstream of the gas-liquid separation device 4, and the gaseous chlorosilane filled in the filling pipe 1 can be condensed and cooled into the liquid chlorosilane by the cooling device 5, so that the pressure on the side of the filling interface 14 in the filling pipe 1 can be reduced, the generated pressure difference facilitates the filling of the chlorosilane into the chlorosilane gas cylinder 7, and the inert gas and other residual impurity gases (non-condensable gases) in the system in the filling pipe 1 can be mixed into the gaseous chlorosilane due to different dew points of different gases, the condensation and cooling of the cooling device 5 can liquefy the gaseous chlorosilane, and the non-condensable gases in the gaseous chlorosilane can keep a gaseous state, so that the separation of the non-condensable gases is realized, the impurities in the chlorosilane are further reduced, and the filling quality is improved.

As shown in fig. 1, the top of the cooling device 5 may be provided with a noncondensable gas discharge port 51, and the condensed and temperature-reduced separated noncondensable gas may be discharged through the noncondensable gas discharge port 51.

According to the utility model discloses chlorosilane fills dress system, protection air supply 2 and vacuum pump 6 can fill before chlorosilane gas cylinder 7 fills dress and sweep the replacement to filling dress pipe 1, and chlorosilane storage tank 3 can fill into filling pipe 1 with the form of gaseous state with chlorosilane through the mode of heating, and liquid drop in gaseous state chlorosilane can be separated out to gas-liquid separation device 4, and cooling device 5 can be through the noncondensable gas separation of condensing cooling with chlorosilane through the mode of cooling. The device has the advantages that the device can reduce impurities through arrangement and specific operation, the condition that the impurities in the chlorosilane exceed the standard is avoided, and the filling quality of the chlorosilane is improved.

In some embodiments, the cooling device 5 is a chiller. The deep cooler can reduce the temperature to minus 20 ℃ to minus 50 ℃, thereby fully meeting the requirement of condensation cooling.

In some embodiments, the chlorosilane filling system further comprises a return pipe 41, wherein the return pipe 41 is connected between the gas-liquid separation device 4 and the chlorosilane storage tank 3 and is used for returning liquid drops to the chlorosilane storage tank 3.

As shown in fig. 1, one end of the return pipe 41 is connected to the gas-liquid separation device 4, the other end of the return pipe 41 is connected to the chlorosilane storage tank 3, and liquid drops separated from gaseous chlorosilane by the gas-liquid separation device 4 can flow back to the chlorosilane storage tank 3 through the return pipe 41, so that the chlorosilane can be recovered, and waste is avoided.

In some embodiments, the chlorosilane filling system further comprises a weighing device 72 and a first heating device 71, wherein the weighing device 72 is used for weighing the chlorosilane gas cylinder 7, and the first heating device 71 is used for heating the chlorosilane gas cylinder to heat part of liquid chlorosilane in the chlorosilane gas cylinder 7 into gaseous chlorosilane.

As shown in fig. 2, the weighing device 72 may be a weighing sensor, and the weighing device 72 is disposed below the chlorosilane gas cylinder 7, so that the weight of the chlorosilane gas cylinder 7 can be weighed in real time, and the charging amount of chlorosilane in the chlorosilane gas cylinder 7 can be obtained.

The first heating device 71 can heat the chlorosilane gas cylinder 7, for example, the first heating device 71 can be a heating blanket or a heating belt wrapped on the outer periphery of the chlorosilane gas cylinder 7, and when the chlorosilane gas cylinder 7 is heated by the first heating device 71, chlorosilane in the chlorosilane gas cylinder 7 is heated and volatilized and flows out of the chlorosilane gas cylinder 7 in a gas form. Therefore, on one hand, when more chlorosilane is filled into the chlorosilane gas cylinder 7, more chlorosilane can be discharged in a heating mode, so that reasonable chlorosilane amount can be charged into the chlorosilane gas cylinder 7; on the other hand, the chlorosilane gas cylinder 7 can be communicated with detection equipment, and then chlorosilane in the chlorosilane gas cylinder 7 is volatilized to the detection equipment in a gas form in a heating mode, so that the detection is facilitated.

In some embodiments, the chlorosilane filling system further comprises a detection device, wherein the detection device is detachably connected with the chlorosilane gas cylinder 7, so that part of the liquid chlorosilane in the chlorosilane gas cylinder 7 is heated into gaseous chlorosilane by the first heating device 71 and enters the detection device for detection.

Specifically, the detection equipment can be chlorosilane concentration detection equipment, during the detection, with the bottleneck intercommunication of detection equipment and chlorosilane gas cylinder 7, then utilize first heating device 71 heating volatilization chlorosilane gas cylinder 7, the chlorosilane in the chlorosilane gas cylinder 7 can volatilize to the detection equipment in to accomplish the analysis and test.

In some embodiments, the chlorosilane filling system further comprises a filling valve 15 and a controller provided at the filling interface 14, the controller being connected to the weighing device 72 and the filling valve 15 for controlling the filling valve 15 in dependence on the weighing value of the weighing device 72.

As shown in fig. 1, the controller may be a PLC control system, and the filling valve 15 and the weighing device 72 are electrically connected to the controller. The charging amount of chlorosilane in the chlorosilane gas cylinder 7 can be controlled by the charging valve 15 and the weighing device 72, for example, a target value can be set to the weighing device 72, when the target value is lower, the charging valve 15 is kept in an open state, so that the chlorosilane gas cylinder 7 can be charged, and when the target value is higher, the controller can control the charging valve 15 to be closed, so that the charging amount of chlorosilane gas cylinder 7 can be controlled.

It will be appreciated that in other embodiments, the weighing device 72 may also be configured to have a threshold range, for example, the weighing device 72 may be configured to have a lower limit and an upper limit, and when the lower limit is lower, the filling valve 15 remains open to allow filling of the chlorosilane gas cylinder 7, and when the upper limit is higher, the controller controls the filling valve 15 to close.

Preferably, the difference between the upper limit value and the lower limit value is not more than 0.2 kg, namely the error range of chlorosilane filled in the chlorosilane gas cylinder 7 is kept within 0.2 kg.

In some embodiments, the chlorosilane filling system further comprises a filling panel having a filling passage therein, the filling passage having an inlet in communication with the filling interface 14 and a plurality of outlets adapted to be detachably connected to the plurality of chlorosilane gas cylinders 7 in a one-to-one correspondence.

As shown in fig. 1, the right end of the filling tube 1 is provided with a filling panel, a filling channel is arranged in the filling panel, the filling channel can be of a comb type, that is, the filling channel has an inlet and a plurality of outlets, the inlet of the filling channel is communicated with the filling tube 1, the plurality of outlets of the filling channel are detachably connected with the chlorosilane gas cylinder 7, and the outlet of the filling channel forms a filling interface 14.

Preferably, there are a plurality of filling valves 15, a plurality of filling valves 15 being provided on the filling panel, and a plurality of filling valves 15 controlling the opening and closing of the respective outlets of the filling channel in a one-to-one correspondence.

In some embodiments, the chlorosilane gas cylinder 7 is connected to the filling panel by a metal hose 73.

In some embodiments, the chlorosilane filling system further comprises a second heating device 35, the second heating device 35 is arranged on the chlorosilane storage tank 3 and used for heating the surface of the chlorosilane in the chlorosilane storage tank 3 through microwave or infrared radiation, the periphery of the chlorosilane storage tank 3 is provided with a jacket 32, the jacket 32 is provided with a heating medium channel, and the heating medium channel is provided with a medium inlet 34 for introducing a heating medium to heat the liquid chlorosilane in the chlorosilane storage tank 3 and a medium outlet 33 for discharging the heating medium.

As shown in fig. 3, a jacket 32 is arranged on the outer periphery of the chlorosilane storage tank 3, the jacket 32 is arranged on the middle lower part of the chlorosilane storage tank 3, a heating medium channel is arranged in the jacket 32, a heating medium can be filled into the jacket 32 through the heating medium channel, and the heating medium can exchange heat with liquid chlorosilane in the chlorosilane storage tank 3, so that heating of the liquid chlorosilane is realized.

The top of the chlorosilane storage tank 3 is also provided with a second heating device 35, the second heating device 35 is positioned above the jacket 32, the second heating device 35 can be an infrared heater, as shown in fig. 3, the infrared heater can be tubular, the infrared heater penetrates through the chlorosilane storage tank 3 in a sealing mode, and the infrared heater is horizontally arranged and at least partially positioned inside the chlorosilane storage tank 3. It will be appreciated that in other embodiments, the second heating device 35 may also be a microwave heating device.

It should be noted that, when the chlorosilane storage tank 3 is used, the heating medium flowing into the jacket 32 can heat the liquid chlorosilane to a temperature close to the boiling point, the temperature of the heating medium is controlled, then the liquid chlorosilane close to the boiling point can be heated by the second heating device 35 and escapes from a gas-liquid interface in a molecular state, and the escaped gaseous chlorosilane flows into the subsequent gas-liquid separation device 4, so that the sub-boiling evaporation of the liquid chlorosilane in the chlorosilane storage tank 3 is realized, and the situations that a large amount of liquid drops are easily generated when the liquid chlorosilane boils and impurities such as metal ions and solid particles are carried by aerosol and enter the gas phase are avoided.

Preferably, the medium inlet 34 of the heating medium passage is provided at the bottom of the jacket 32, and the medium outlet 33 of the heating medium passage is provided at the top of the jacket 32. Therefore, the temperature of the liquid chlorosilane at the bottom of the chlorosilane storage tank 3 is slightly higher than that of the liquid chlorosilane at the top, so that the upper and lower convection circulation of the liquid chlorosilane is facilitated on one hand, and the slightly lower temperature of the top of the liquid chlorosilane is kept on the other hand, so that the sub-boiling evaporation of the chlorosilane storage tank 3 is facilitated to be guaranteed.

Preferably, the second heating device 35 is provided in plurality and layered in the up-down direction. As shown in fig. 1 and 2, the second heating devices 35 are infrared heating pipes, the number of the second heating devices 35 is four, two of the four second heating devices 35 are in a group, two groups of the second heating devices 35 are arranged at intervals in the up-down direction, two infrared heating pipes in a group below are arranged at intervals in parallel in the front-back direction, and two infrared heating pipes in a group above are arranged at intervals in parallel in the left-right direction. The layered arrangement is favorable for ensuring the uniform heating of the gas phase area at the top of the chlorosilane storage tank 3.

In some embodiments, a plurality of baffles are provided within jacket 32, which may serve to direct the flow of heating medium and slow the flow.

In some embodiments, a temperature sensor 36 for detecting the temperature of the liquid chlorosilane in the chlorosilane storage tank 3 is disposed in the chlorosilane storage tank 3. As shown in fig. 3, the temperature sensor 36 is disposed on the circumferential wall of the chlorosilane storage tank 3, and the temperature sensor 36 penetrates the jacket 32 and extends into the tank cavity of the chlorosilane storage tank 3 in a sealing manner. Can controller electric connection through temperature sensor 36, temperature sensor 36 can be with the temperature signal transmission of gathering for the controller, the controller can be to the temperature signal analysis of temperature sensor 36 gathering and according to the work of the joining of the interior heating medium of the result regulation and control of analysis in jacket 32 and second heating device 35, from this, can guarantee the invariant of the interior temperature of storage tank.

Preferably, the temperature sensor 36 is plural, and the plural temperature sensors 36 are arranged at intervals in the up-down direction. Therefore, the monitoring error of the single temperature sensor 36 can be reduced, and the accuracy of temperature signal acquisition is ensured.

In some embodiments, the bottom of the chlorosilane storage tank 3 is provided with a liquid outlet 31, and the residual liquid in the chlorosilane storage tank 3 can be discharged through the liquid outlet 31.

According to the utility model discloses chlorosilane fills dress method includes following step:

step 1: protective gas is supplied into the filling tube 1 to sweep the filling tube 1.

Specifically, inert gas is introduced into the filling pipe 1 through the protective gas source 2, and the introduced inert gas can perform purging replacement on the filling pipe 1. It should be noted that, when filling with the inert gas, a collecting container may be connected to one end of the filling pipe 1, and the introduced inert gas may be recycled by the collecting container.

Step 2: the filling tube 1 is evacuated.

And after the protective gas source 2 is filled for a period of time, stopping filling the inert gas into the filling pipe 1, cutting off the protective gas source 2 and the filling pipe 1, and then vacuumizing the filling pipe 1 by using the vacuum pump 6. It should be noted that, when the vacuum is drawn, the valves on the filling tube 1 need to be closed, so that the inside of the filling tube 1 is in a relatively sealed state.

And step 3: repeating the step 1 and the step 2 for a predetermined number of times.

After the vacuum pump 6 is pumped for a period of time, the vacuum pump 6 is closed, then the inert gas is introduced into the filling pipe 1 again by using the protective gas source 2 for purging and replacement, and the operation is repeated for many times. And impurities such as trace water, trace oxygen and the like in the filling pipe 1 can be diluted through repeated vacuumizing and repeated sweeping and replacement.

Preferably, the predetermined number of times is 40, i.e., at least 40 vacuums and 40 purge replacements are required.

And 4, step 4: connecting the chlorosilane gas cylinder 7 with a filling interface 14 of the filling pipe 1, and vacuumizing the chlorosilane gas cylinder 7.

Specifically, the chlorosilane gas cylinder 7 can be connected with the filling interface 14 on the filling pipe 1 by using the metal hose 73, after the connection is finished, the valve on the chlorosilane gas cylinder 7 and the corresponding filling valve 15 on the filling pipe 1 are opened, so that the chlorosilane gas cylinder 7 can be communicated with the filling pipe 1, and then the filling pipe 1 and the chlorosilane gas cylinder 7 are vacuumized by using the vacuum pump 6. The chlorosilane gas cylinder 7 is vacuumized, so that impurities in the chlorosilane gas cylinder 7 can be diluted, and the filling quality can be ensured.

Preferably, an absolute pressure of 10Pa is maintained while evacuating the chlorosilane gas cylinder 7.

And 5: the chlorosilane storage tank 3 is heated to sub-boil the liquid chlorosilane in the chlorosilane storage tank 3 into gaseous chlorosilane to supply the gaseous chlorosilane into the filling pipe 1.

After the chlorosilane gas cylinder 7 is vacuumized, the jacket 32 of the chlorosilane storage tank 3 and the second heating device 35 are used for heating the liquid chlorosilane in the chlorosilane storage tank 3, and the liquid chlorosilane in the chlorosilane storage tank 3 flows into the filling pipe 1 in the form of gaseous chlorosilane.

Step 6: and (3) carrying out vapor-liquid separation on the gaseous chlorosilane supplied into the filling pipe 1 by using a ground gas-liquid separation device 4 arranged on the filling pipe 1.

Specifically, the gaseous chlorosilane flowing out of the chlorosilane storage tank 3 flows into the gas-liquid separation device 4, and the gas-liquid separation device 4 separates liquid droplets in the gaseous chlorosilane and discharges the liquid droplets back into the chlorosilane storage tank 3 through the return pipe 41.

And 7: and cooling the gaseous chlorosilane separated from the vapor and the liquid into liquid chlorosilane by using a cooling device 5 arranged on the filling pipe 1, and separating and discharging noncondensable gas in the liquid chlorosilane.

Gaseous chlorosilane treated by the gas-liquid separation device 4 flows through the cooling device 5, and the cooling device 5 can condense and cool the gaseous chlorosilane, so that the gaseous chlorosilane can be condensed into liquid chlorosilane. The non-condensable gas in the condensation cooling can be discharged or collected through a non-condensable gas discharge port 51 at the top of the cooling device 5.

And 8: liquid chlorosilane is filled into the chlorosilane gas cylinder 7 through the filling pipe 1, and the step 1 and the step 2 are executed for a preset number of times after filling is finished.

Specifically, liquid chlorosilane generated by condensation of the cooling device 5 is filled into the chlorosilane gas cylinder 7 under the action of pressure difference, and after a set amount of liquid chlorosilane is filled into the chlorosilane gas cylinder 7, a valve on the chlorosilane gas cylinder 7 is closed.

And finally, purging and replacing the filling pipe 1 for multiple times through the protective gas source 2, and vacuumizing the filling pipe 1 for multiple times through the vacuum pump 6, so that the effect of diluting chlorosilane in the filling pipe 1 can be achieved, and after dilution is completed, the gas cylinder is detached from the filling interface 14, so that chlorosilane filling is completed.

In some embodiments, in step 2 and step 8, the vacuum pump 6 may be used to perform a negative pressure holding test on the filling pipe 1, and the protection gas source 2 may be used to perform a positive pressure holding test on the filling pipe 1.

In some embodiments, in step 8, the detection device may be communicated with the filled chlorosilane gas cylinder 7, and then the chlorosilane in the chlorosilane gas cylinder 7 is heated by the first heating device 71 and is introduced into the detection device in a gaseous state.

In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", and the like, indicate the orientation or positional relationship indicated based on the drawings, and are only for convenience of description and simplicity of description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be construed as limiting the present invention.

Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless expressly specified otherwise.

In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," and "fixed" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally formed; may be mechanically coupled, may be electrically coupled or may be in communication with each other; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.

In the present application, unless expressly stated or limited otherwise, the first feature may be directly on or directly under the second feature or indirectly via intermediate members. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.

In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.

Although embodiments of the present invention have been shown and described, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art without departing from the scope of the present invention.

Claims (10)

1. A chlorosilane filling system, comprising:

the charging pipe is provided with a protective gas port, a chlorosilane inlet, a vacuumizing port and a charging interface suitable for being connected with a chlorosilane gas cylinder;

the protective gas source is communicated with the protective gas port and is used for supplying protective gas into the filling pipe to purge the filling pipe;

the chlorosilane storage tank is communicated with the chlorosilane inlet and is used for storing and sub-boiling evaporating liquid chlorosilane so as to supply gaseous chlorosilane into the filling pipe;

a gas-liquid separation device for separating liquid droplets in the gaseous chlorosilane supplied from the chlorosilane inlet into the filling pipe;

the vacuum pump is communicated with the vacuumizing port and is used for vacuumizing the filling pipe and a chlorosilane gas cylinder connected with the filling interface;

and the cooling device is arranged on the filling pipe and is positioned between the gas-liquid separation device and the filling interface, and the cooling device is used for cooling the gaseous chlorosilane into liquid chlorosilane and separating and discharging non-condensable gas in the chlorosilane.

2. The chlorosilane filling system of claim 1, wherein the cooling device is a chiller.

3. The chlorosilane filling system according to claim 1, further comprising a return pipe connected between the gas-liquid separation device and the chlorosilane storage tank for returning the liquid droplets to the chlorosilane storage tank.

4. The chlorosilane filling system according to claim 1, further comprising a weighing device and a first heating device, wherein the weighing device is used for weighing the chlorosilane gas cylinder, and the first heating device is used for heating the gas cylinder to heat part of liquid chlorosilane in the chlorosilane gas cylinder into gaseous chlorosilane.

5. The chlorosilane filling system according to claim 4, further comprising a detection device, wherein the detection device is detachably connected with the chlorosilane gas cylinder, so that part of the liquid chlorosilane in the chlorosilane gas cylinder is heated into the gaseous chlorosilane by the first heating device and enters the detection device for detection.

6. The chlorosilane filling system of claim 4, further comprising a filling valve and a controller arranged at the filling interface, wherein the controller is connected with the weighing device and the filling valve to control the filling valve according to a weighing value of the weighing device.

7. The chlorosilane filling system of claim 1, further comprising a filling panel having a filling channel therein, the filling channel having an inlet in communication with the filling interface and a plurality of outlets, the plurality of outlets adapted to be removably connected to a plurality of chlorosilane gas cylinders in a one-to-one correspondence.

8. The chlorosilane filling system according to any one of claims 1 to 7, further comprising a second heating device, wherein the second heating device is arranged on the chlorosilane storage tank and used for heating the level of the chlorosilane in the chlorosilane storage tank by microwave or infrared radiation, a jacket is arranged on the periphery of the chlorosilane storage tank, the jacket is provided with a heating medium channel, and the heating medium channel is provided with a medium inlet used for introducing a heating medium to heat liquid chlorosilane in the chlorosilane storage tank and a medium outlet used for discharging the heating medium.

9. The chlorosilane filling system according to claim 8, wherein a temperature sensor for detecting the temperature of the liquid chlorosilane in the chlorosilane storage tank is arranged in the chlorosilane storage tank.

10. The chlorosilane filling system according to claim 8, wherein the second heating device is provided in a plurality of layers in the vertical direction.

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