CN103836330B - The device and method of storage of liquids, the device and method of transfer liquid - Google Patents

The device and method of storage of liquids, the device and method of transfer liquid Download PDF

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CN103836330B
CN103836330B CN201210483873.3A CN201210483873A CN103836330B CN 103836330 B CN103836330 B CN 103836330B CN 201210483873 A CN201210483873 A CN 201210483873A CN 103836330 B CN103836330 B CN 103836330B
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valve
pipeline
tank body
liquid
liquids
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CN103836330A (en
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吴景晖
姚力军
相原俊夫
潘杰
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Ningbo Chuangrun New Materials Co ltd
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Ningbo Chuangrun New Materials Co ltd
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Abstract

The device and method of storage of liquids, a device and method for transfer liquid, described liquid has corrosivity and composition easily and in air reacts, and the device of described storage of liquids comprises: the tank body of sealing, carrier pipe and pneumatic tube; Carrier pipe comprises material feeding mouth and discharge port, and discharge port is positioned at tank body, and material feeding mouth is positioned at outside tank body, the carrier pipe between material feeding mouth and tank body is provided with the first valve, and the first valve is for controlling conducting, the closedown of carrier pipe; Discharge port is less than the height of described air outlet to tank base to the height of tank base.To described storage device; in tank body, protection gas is filled with by carrier pipe; a seal protection compression ring border is created above the liquid of the storage in tank body; the composition contact in liquid-to-air is avoided to generate corrosivity aerosol; and; liquid is in seal protection compression ring border, can realize the long-term preservation of liquid.

Description

The device and method of storage of liquids, the device and method of transfer liquid
Technical field
The present invention relates to chemical industrial field, design device, the method for a kind of device of storage of liquids, method and transfer liquid especially, described liquid has corrosivity and the water vapour be easy in air reacts.
Background technique
Titanium tetrachloride (molecular formula TiCl 4), be the raw material of industry being usually used in producing titanium sponge and titanium dioxide.At room temperature, titanium tetrachloride remains colorless liquid, is easy to react with water vapour generate hydrochloric acid aerosol.Hydrochloric acid has aggressive, has great destruction to human body with the object contacted.Meanwhile, other resultants of reaction also have adverse effect to the quality control ensured in commercial Application process.And in the air of Workplace, be difficult to invariably there is water vapour.Therefore, in the storage and using process of titanium tetrachloride, the contact with air fully to be avoided.
But in the industry, existing titanium tetrachloride storage technology is directly inject and be stored in tank substantially, and is difficult to effectively avoid titanium tetrachloride to contact with air.And existing titanium tetrachloride transfer method is also is mostly open direct injections.Now, liquid titanium tetrachloride is reacted with the water vapour in air and is generated hydrochloric acid aerosol in the process being exposed to air, not only endangers site operation personnel's safety, is also unfavorable for the purity ensureing titanium tetrachloride.And in prior art, store and transfer titanium tetrachloride in the container of vacuum environment or protection hermetic seal environment, also there is no special device.
Summary of the invention
The problem that the present invention solves is sealed storage and the transfer that in prior art, titanium tetrachloride storage and transfer device cannot realize titanium tetrachloride, causes titanium tetrachloride to expose and produces hydrochloric acid aerosol in atmosphere.
For solving the problem, the invention provides a kind of device of storage of liquids, described liquid has corrosivity and composition easily and in air reacts, and comprising: the tank body of sealing, carrier pipe and pneumatic tube; Described carrier pipe comprises material feeding mouth and discharge port, described discharge port is positioned at described tank body, described material feeding mouth is positioned at outside described tank body, the carrier pipe between described material feeding mouth and tank body is provided with the first valve, and described first valve is for controlling conducting, the closedown of described carrier pipe; Described pneumatic tube comprises suction port and air outlet, described air outlet is positioned at described tank body, described suction port is positioned at outside described tank body, the pneumatic tube between described suction port and tank body is provided with the second valve, and described second valve is for controlling conducting, the closedown of described pneumatic tube; Described discharge port is less than the height of described air outlet to described tank base to the height of described tank base.
Optionally, described liquid is titanium tetrachloride.
Optionally, the pneumatic tube between described second valve and tank body is provided with the first barometer.
Optionally, the material of described carrier pipe and pneumatic tube is noncorroding metal, comprises stainless steel.
Optionally, described first valve is also for controlling the flow of liquid in described carrier pipe; Described second valve is also for controlling the flow of shielding gas in described pneumatic tube.
Optionally, described first valve and the second valve are ball valve.
Optionally, described discharge port is positioned at described tank base, and described air outlet is positioned at described tank body top.
Optionally, described tank body comprises: have the body of opening and seal the cap of described opening; The discharge port of described carrier pipe and the air outlet of described pneumatic tube all enter described tank interior by described cap.
Optionally, described tank body is double layer construction, the endothecium structure comprise layer structure, arranging within described layer structure.
Optionally, the material of described layer structure comprises stainless steel; The material of described endothecium structure comprises pure molybdenum or pure nickel.
Optionally, the composition in described air comprises water vapour.
For solving the problem, present invention also offers a kind of method using above-mentioned storage device storage of liquids, described liquid has corrosivity and water vapour easily and in air reacts, and comprising:
Open described first valve and the second valve, by described carrier pipe to input protection gas in described tank body, with the air in emptying tank body, described shielding gas is the inert gas that density is greater than air density;
After air in emptying described tank body, by described carrier pipe to infusion fluid in described tank body;
After the liquid in described tank body reaches prearranging quatity, close described first valve and the second valve.
Optionally, the pneumatic tube between described second valve and tank body is provided with the first barometer; After described first valve of closedown and the second valve, also comprise:
Open described second valve again, continue to pass into shielding gas in described tank body, monitored the pressure in described tank body by described first barometric reading;
When monitoring the pressure in described tank body and reaching slight positive pressure state, close described second valve.
Optionally, described shielding gas is argon gas.
For solving the problem, present invention also offers a kind of device of transfer liquid, described liquid has corrosivity and water vapour easily and in air reacts, and comprising: the pipeline of above-mentioned arbitrary storage device, reactor and the described storage device of connection and described reactor; Described pipeline head end is connected with described material feeding mouth; Described line end is connected with described reactor.
Optionally, for removably connecting between described pipeline head end and described material feeding mouth, described line end and described reactor are for removably connecting.
Optionally; described pipeline is provided with the 3rd valve on the position near pipeline head end; described pipeline is provided with the 4th valve on the position near line end; pipeline between described 3rd valve and the 4th valve is provided with the first protection gas supplying tube; described first protection gas supplying tube is provided with the 5th valve; described 3rd valve, the 4th valve are for controlling conducting, the closedown of described pipeline, and described 5th valve is for controlling conducting, the closedown of described first protection gas supplying tube.
Optionally, protect on gas supplying tube first between the protection gas inlet opening and described 5th valve of described first protection gas supplying tube and be provided with the second barometer.
Optionally, described pipeline is provided with the 6th valve on the position near line end, described 6th pipeline between valve and line end is provided with the 7th valve, pipeline between described 6th valve and the 7th valve is provided with the second protection gas supplying tube, described second protection gas supplying tube is provided with the 8th valve; Described 6th valve, the 7th valve are for controlling conducting, the closedown of described pipeline, and described 8th valve is for controlling conducting, the closedown of described second protection gas supplying tube.
Optionally, described tank base is provided with electronic scale, by the flow velocity of reading regulates liquid in pipeline of electronic scale.
For solving the problem, present invention also offers a kind of method using above-mentioned transfer device transfer liquid, described liquid has corrosivity and water vapour easily and in air reacts, and comprises step:
Open described first valve and the second valve, by described pneumatic tube to input protection gas in described tank body, flow in described reactor by described carrier pipe, pipeline to make the liquid in tank body under the pressure effect of shielding gas;
After the liquid in described reactor reaches prearranging quatity, close described first valve and the second valve.
Optionally, described shielding gas comprises argon gas.
Optionally, described pipeline is provided with the 3rd valve on the position near pipeline head end, described pipeline is provided with the 4th valve on the position near line end, pipeline between described 3rd valve and the 4th valve is provided with the first protection gas supplying tube, described first protection gas supplying tube is provided with the 5th valve;
Before by described pipeline access transfer device, also comprise step:
Open described 3rd valve, the 4th valve and the 5th valve, by the first protection gas supplying tube to input protection gas in described pipeline, with the air in emptying described pipeline;
After the air in described pipeline is emptying, close all valves in described pipeline, form the sealing pipeline being full of shielding gas;
Afterwards, by described sealing pipeline access reaction device;
In the transfer process of liquid, when opening the first valve, the second valve, also open the 3rd valve, the 4th valve close the 5th valve;
After the liquid in described reactor reaches prearranging quatity, when closing described first valve, the second valve, also close described 3rd valve and the 4th valve.
Optionally; described pipeline is provided with the 6th valve on the position near line end; described 6th pipeline between valve and line end is provided with the 7th valve; pipeline between described 6th valve and the 7th valve is provided with the second protection gas supplying tube; described second protection gas supplying tube is provided with the 8th valve, comprises step:
In the transfer process of liquid, when opening described first valve, the second valve, also open described 6th valve, the 7th valve and close described 8th valve;
After the liquid in described reactor reaches prearranging quatity, close described 6th valve, open described 7th valve, the 8th valve, the liquid of shielding gas to emptying described line end is passed into by described second protection gas supplying tube, close described 7th valve afterwards, open the 6th valve, and continue through the second protection gas supplying tube and pass into shielding gas to the liquid in emptying described pipeline; Or, open described 8th valve, the 6th valve, the 7th valve, passed into the liquid in shielding gas to emptying described pipeline by described second protection gas supplying tube;
Close all valves in described transfer device.
Optionally, described tank base is provided with electronic scale; In the transfer process of described liquid, monitor the reading of described electronic scale; According to the reading of described electronic scale, the flow velocity of regulates liquid in described pipeline.
Compared with prior art, the present invention has the following advantages:
The device of storage of liquids of the present invention, liquid is have corrosivity and composition easily and in air reacts.When using this device storage of liquids, before adding liquid in tank body, open the first valve and the second valve, in tank body, be filled with shielding gas by material feeding mouth, and shielding gas is the inert gas that density is greater than air density.Shielding gas forces the air in tank body to be discharged by air outlet, pneumatic tube; realize the effect of the air in emptying tank body; a dry protection hermetic seal environment is created to adding liquid in tank body for follow-up; avoid some composition in the air in liquid and tank body react and generate corrosivity aerosol, prevent aerosol from can work the mischief to environment with to the healthy safety of Field Force.Then; again by discharge port to adding liquid in tank body, in adding procedure, the pressure of liquid forces protection gas to be discharged from suction port; protection compression ring border makes liquid-to-air keep apart all the time, avoids the catalytic resultant of the composition in liquid-to-air to pollute the purity of liquid.Further, after the liquid in tank body reaches prearranging quatity, close the first valve and the second valve, be now protection hermetic seal environment above liquid, described sealed environment guarantees that liquid can not contact with air in storing process, realizes the longer-term storage of liquid.When liquid is titanium tetrachloride, the water vapour in titanium tetrachloride and air can be avoided to react and to generate corrosive hydrochloric acid aerosol, the long-term preservation of titanium tetrachloride can be realized.
The method of the above-mentioned storage device storage of liquids of use of the present invention; as mentioned previously; this storage device realizes in tank body, create a protection hermetic seal environment; and guarantee, being in the state with air exclusion completely to the process of adding liquid in the tank body of storage device, to avoid some composition reaction generation corrosivity aerosol in liquid-to-air.
The device comprising the transfer liquid of above-mentioned storage device of the present invention, has benefited from the good protection hermetic seal environment of this storage device, and the composition contact avoided in liquid-to-air generates corrosivity aerosol.On the other hand, protection hermetic seal environment guarantees that liquid has very high purity, realizes using the metal of this liquid production to have very high purity.
The method of the above-mentioned transfer device transfer liquid of use of the present invention; have benefited from the good protection hermetic seal environment of this transfer device; the transfer process of whole liquid is in complete sealing state; the composition contact avoided in liquid-to-air generates corrosivity aerosol, thus plays protection operator physical safety and the effect avoiding befouling environment.
Accompanying drawing explanation
Fig. 1 is the structural representation of the storage device of first embodiment of the invention;
Fig. 2 is the structural representation of the storage device of second embodiment of the invention;
Fig. 3 is the structural representation of the transfer device of first embodiment of the invention;
Fig. 4 is the structural representation of the transfer device of second embodiment of the invention;
Fig. 5 is the structural representation of the transfer device of third embodiment of the invention;
Fig. 6 is the structural representation of the transfer device of fourth embodiment of the invention.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention, but the present invention can implement to be much different from other modes described here.Based on the embodiment of the present invention, the every other embodiment that those skilled in the art obtain under not making creative work prerequisite, belongs to the scope of protection of the invention.
Secondly, the present invention utilizes schematic diagram to be described in detail, when describing the embodiment of the present invention in detail; for ease of explanation; the structural representation of indication equipment can be disobeyed general ratio and be made partial enlargement, and described schematic diagram is example, can not limit the scope of protection of the invention.
In a particular embodiment, the storage device of the present embodiment has corrosivity and the liquid that reacts as oxygen, nitrogen or water vapour of composition easily and in air for storing.Such as titanium tetrachloride very easily reacts with water vapour and generates hydrochloric acid aerosol, befouling environment the safety that is detrimental to health.The storage device of the present embodiment is particularly suitable for the storage of titanium tetrachloride liquid; but be not limited to titanium tetrachloride; with titanium tetrachloride, there is similar quality or some composition be easy in air reacts all applicable storage device of the present invention of liquid generating corrosivity aerosol, use the technique of storage device storage of liquids of the present invention all within protection scope of the present invention.
For ease of illustrating and understanding technical solution of the present invention, specific description of embodiments of the present invention will for titanium tetrachloride.
Fig. 1 ~ Fig. 2 is the structural representation of the storage device of the specific embodiment of the invention.
First embodiment
Fig. 1 is the structural representation of the storage device of first embodiment of the invention.
In a particular embodiment, with reference to Fig. 1, storage device comprises: the tank body 10 of sealing; Carrier pipe 12, comprise material feeding mouth 121 and discharge port 122, described material feeding mouth 121 is positioned at outside tank body 10, discharge port 122 is positioned at described tank body 10, carrier pipe 12 between described material feeding mouth 121 and tank body 10 is provided with the first valve 14, described first valve 14 is for controlling conducting, the closedown of carrier pipe 12; Pneumatic tube 13, comprise suction port 131 and air outlet 132, wherein, described suction port 131 is positioned at outside described tank body, air outlet 132 is positioned at tank body 10, pneumatic tube 13 between described suction port 131 and tank body 10 is provided with the second valve 15, described second valve 15 is for controlling conducting, the closedown of pneumatic tube 13.And the height bottom described discharge port 122 to tank body 10 is less than the height bottom described air outlet 132 to tank body 10.
In the present embodiment, in tank body 10, pass into the air in the emptying tank body 10 of shielding gas by carrier pipe 12, and the density of shielding gas is greater than air density, shielding gas can be deposited on the bottom of tank body 10.If the height bottom discharge port 122 to tank body 10 is more than or equal to the height bottom air outlet 132 to tank body 10; the shielding gas entering tank body 10 can directly be discharged by air outlet 132; and the most air in tank body 10 remain in the top of tank body 10, can not be discharged.So the height be less than bottom described air outlet 132 to tank body 10 of the height bottom discharge port 122 to tank body 10 can realize the effect of discharging air in tank body 10.As most preferred embodiment, air outlet 132 is positioned at the top of tank body 10.Because the density of shielding gas used in the present invention is large than air density, in emptying tank body 10 air process in, air can be gathered in the top of shielding gas.Air outlet 132 is arranged at top, impels air thoroughly, to be rapidly discharged, and realizes the air in whole emptying tank body 10.
In a particular embodiment; with reference to Fig. 1; pneumatic tube 13 between described second valve 15 and tank body 10 arranges the first barometer 16; determined the pressure of the gas in described tank body 10 by the reading of the first barometer 16, and regulate the first valve 14 to control to pass into the flow of shielding gas in tank body 10.The most important thing is, when in tank body 10 during storage of liquids, the reading according to the first barometer 16 regulates titanium tetrachloride (TiCl 4) pressure of protection gas of top, as titanium tetrachloride (TiCl 4) pressure of protection gas of top is slight positive pressure state, titanium tetrachloride can reach long-term best storage effect.
In a particular embodiment, the materials'use corrosion resistant material of described carrier pipe 12 and pneumatic tube 13, general selection corrosion resistance alloy, described corrosion resistance alloy selects stainless steel or Hastelloy.Hydrochloric acid aerosol is generated because titanium tetrachloride can react with water vapour, the selection of described corrosion resistance alloy realizes avoiding carrier pipe 12 and pneumatic tube 13 to suffer that hydrochloric acid aerosol corrodes substantially, extend the working life of carrier pipe 12 and pneumatic tube 13, also the reaction product of above-mentioned hydrochloric acid aerosol and carrier pipe 12 and pneumatic tube 13 can be avoided to pollute titanium tetrachloride liquid, guarantee that the Ti metal using titanium tetrachloride to prepare has high-purity.
On the other hand, described carrier pipe 12 is the circulation duct of titanium tetrachloride, if the internal diameter of carrier pipe 12 is excessive, the changes in flow rate amplitude of ducted titanium tetrachloride is bigger than normal, will the flow of more difficult control titanium tetrachloride; If the internal diameter of carrier pipe 12 is too small, then there is the possibility strengthening foreign matters from being blocked pipeline.So in a particular embodiment, the inside diameter ranges of carrier pipe 12 is: 5 ~ 15mm, as preferred embodiment, selection inside diameter ranges is: 8 ~ 15mm, can realize, to the accurate control of flow rate of liquid, also keeping higher manufacturing efficiency.
In a particular embodiment, described first valve 14 also can be used for the flow controlling titanium tetrachloride in described carrier pipe 12; Second valve 15 is for controlling the flow of shielding gas in pneumatic tube 13.As preferred embodiment, the ball valve that the first valve 14 and the second valve 15 select sealing, anticorrosive property and operability combination property best.Described ball valve has throttling and controls the effect of flow.
In a particular embodiment, described discharge port 122 is positioned at described tank body 10 until the bottom of tank body 10, can realize the transfer completely of titanium tetrachloride in the tank body 10 in follow-up titanium tetrachloride transfer process, avoid the waste of material.
In a particular embodiment, with reference to Fig. 1, described tank body 10 comprises the body with opening and the cap 11 sealing described opening.It is inner that tank body 10 all can be inserted by described cap 11 in described discharge port 122 and air outlet 132.Cap 11 serves the seal action in titanium tetrachloride storing process.
Second embodiment
Fig. 2 is the structural representation of the storage device of second embodiment of the invention.
With reference to Fig. 2, described tank body 10 adopts double layer construction, and described double layer construction comprises layer structure 101 and endothecium structure 102.Other structures are identical with the first embodiment with position relationship, do not repeat them here.
In a first embodiment, when low to the purity requirement of titanium tetrachloride, described tank body 10 adopts single layer structure, and the material of described tank body 10 comprises stainless steel.But, as mentioned previously, in the longer-term storage process of titanium tetrachloride, alloying element in stainless steel, such as chromium, can with the hydrochloric acid generation chemical reaction that adulterates in titanium tetrachloride and production respective metal salt, and pollute titanium tetrachloride liquid, reduce the purity of titanium tetrachloride.So when higher to the purity requirement of titanium tetrachloride, the tank body 10 using the first single layer structure implemented obviously is inappropriate.In a second embodiment, with reference to Fig. 2, described tank body 10 uses double layer construction, arranges endothecium structure 102.Described layer structure 101 generally uses stainless steel material, and endothecium structure 102 uses corrosion resistant pure metal material, comprises pure molybdenum or pure nickel.Described endothecium structure 102 prevents titanium tetrachloride liquid from contacting with the layer structure 101 of described tank body 10, effectively avoids the metal reaction in the stainless steel of hydrochloric acid and layer structure, and avoids the layer structure 101 of described tank body 10 to be corroded.Further, ensure that the high-purity of titanium tetrachloride.So, to the double-deck selection of described tank body 10, achieve the long-term free of contamination storage to titanium tetrachloride.Certainly, in practical operation, whether adopt double layer construction, also will according to the holding time of titanium tetrachloride, or purity requirement need determine.
Based on the method for the storage titanium tetrachloride of the storage device of the first embodiment and the second embodiment, comprising:
First air emptying process is carried out to described tank body 10 inside: open described first valve 14 and the second valve 15, continue to be filled with shielding gas by material feeding mouth 121 in tank body 10.In a particular embodiment, described shielding gas is inert gas and density should be larger than air density, and shielding gas is deposited in the bottom of described tank body 10 gradually, and air place moves towards the top of tank body 10.Along with the volume of shielding gas increases, the air space in described tank body 10 gradually protected gas occupies, and the air in tank is discharged by described air outlet 132, pneumatic tube 13 and suction port 131.
In this process, guarantee that the height bottom described discharge port 122 to described tank body 10 is less than described suction port 132 to the height of described tank body 10, just can realize the air in emptying described tank body 10.According to describing above, shielding gas is gathered in the bottom of tank body 10, above-mentionedly arranges the effect that just can realize evacuation of air.As preferred embodiment, when described air outlet 132 is positioned at described tank body 10 top, air can be entered air outlet 132 more fast, the most up hill and dale and be discharged by suction port 131, that is realizes the effect of air in best emptying described tank body 10.
In a particular embodiment, described shielding gas selects argon gas.Because the density ratio air of argon gas is large, the character very torpescence of argon gas, can not burn can not be combustion-supporting, and argon gas itself there is no direct harm to human body.Therefore, argon gas can be used as a kind of desirable clean and seal protection gas.
Then, after the air in tank body 10 is drained, stops the injection of shielding gas, then in tank body 10, be filled with titanium tetrachloride liquid by described material feeding mouth 121.Because the density of titanium tetrachloride liquid is greater than argon gas, titanium tetrachloride is made to be deposited on the bottom of described tank body 10.Along with the increase of the amount of titanium tetrachloride, the shielding gas in described tank body 10 is subject to fluid pressure effect, and enters pneumatic tube 13 by described air outlet 132 and discharge through described suction port 131.Be filled with in process at titanium tetrachloride, shielding gas serves the buffer action of titanium tetrachloride and ambient air.The process that is filled with of titanium tetrachloride completely and external environment be isolated, the water vapour avoided in air contacts with titanium tetrachloride, can not produce hydrochloric acid aerosol and jeopardize the physical safety of staff, also ensure that the purity of titanium tetrachloride.
Finally; after the titanium tetrachloride liquid in tank body 10 reaches prearranging quatity, close the first valve 14 and the second valve 15, on the liquid level of titanium tetrachloride, form protection compression ring border; protection compression ring border is equivalent to a kind of sealing layer, guarantees that the titanium tetrachloride in storing process can not contact with air.As preferred embodiment; with reference to Fig. 1; first barometer 16 is set; according to the reading of the first barometer 16; accurately can judge and guarantee to reach slight positive pressure state between the protection compression ring border of described tank body 10 inside and ambient air, namely protecting gas ambient pressure higher than ambient air air pressure 200 ~ 400 Pascal.Under slight positive pressure state, because the pressure protecting compression ring border is a gentle air pressure, makes the air of external environment cannot overcome this pressure difference at all and enter in described tank body 10, also make described tank body 10 can not bear excessive pressure compression.Further, also can be judged the pressure of protection gas in tank body 10 in the process of follow-up transfer titanium tetrachloride by the reading change of the first barometer 16, then judge the speed of transfer titanium tetrachloride.
Fig. 3 ~ Fig. 6 is the structural representation of the transfer device of the titanium tetrachloride of the specific embodiment of the invention.
First embodiment
Fig. 3 is the structural representation of the transfer device of the first embodiment of the invention comprising Fig. 1.
With reference to Fig. 3, described transfer device comprises the storage device of reactor 30, first embodiment and the pipeline 20 being connected storage device and reactor 30.Wherein, pipeline head end is connected with described material feeding mouth; Line end is connected with described reactor 30.In a particular embodiment, described Placement can be selected to removably connect, and realizes the fractionation of pipeline, clean and cleaning.
Use the storage device of the first embodiment, as previously mentioned, described storage device has good sealing function, and not by the pollution of environment, keeps higher titanium tetrachloride purity.Carry out, in the process of titanium tetrachloride transfer, opening all valves at the described transfer device of use, storage device is now equivalent to the filling equipment of transfer device; In described tank body 10, shielding gas is passed into constantly by suction port 131, in tank body 10, the pressure of the shielding gas of top increases gradually, liquid titanium tetrachloride is subject to the effect protecting atmospheric pressure, enter described discharge port 122, enter pipeline head end by described carrier pipe 12, material feeding mouth, flow through pipeline 20 and arrive reactor 30 through described line end; After the titanium tetrachloride in described reactor 30 reaches prearranging quatity, close all valves.In a particular embodiment; have benefited from the excellent sealing effect protecting compression ring border above the titanium tetrachloride in described tank body 10; wholely to be in and air exclusion state toward the reinforced process in reactor; ensure that titanium tetrachloride can not contact with air and react with water vapour wherein and generate hydrochloric acid aerosol, avoid befouling environment and endanger the healthy and safe of operator.In a particular embodiment, the protection gas used selects argon gas.
Use the method for the transfer device transfer liquid of the first embodiment, comprise the following steps:
Open described first valve 14 and the second valve 15, continue to pass into shielding gas from described suction port 131, protection gas enters in tank body 10 by described second valve 15, pneumatic tube 13 and described air outlet 132;
Afterwards, the pressure of the shielding gas above tank body 10 increases gradually, forces the liquid in tank body 10 to enter discharge port 122, by carrier pipe 12, first valve 14 and pipeline 20, then enters described reactor 30 by line end;
After the liquid in described reactor 30 reaches prearranging quatity, stop passing into of described shielding gas, close the first valve 14 and the second valve 15 simultaneously.
In a particular embodiment, the carrier pipe 12 between described second valve 15 and tank body 10 is provided with the first barometer 16.Be transferred to after in described reactor 30 realizing tank body 10 titanium tetrachloride, also to continue to preserve the residue titanium tetrachloride in tank body 10, so after described first valve 14 of closedown and the second valve 15, also comprise: open described second valve 15 again, continue to pass into shielding gas in tank body 10, monitor the shielding gas pressure in described tank body 10 by the reading of the first barometer 16; When monitoring the pressure in described tank body 10 and reaching slight positive pressure state, close described second valve 15.As preferred steps, realize the longer-term storage of optimum residue titanium tetrachloride.
In a particular embodiment, described protection gas selects argon gas.
Second embodiment
With reference to figure 4; described pipeline 20 is provided with the 3rd valve 23 on the position near pipeline head end; described pipeline 20 is provided with the 4th valve 24 on the position near line end; pipeline 20 between the 3rd valve 23 and the 4th valve 24 is provided with the first protection gas supplying tube 40; described first protection gas supplying tube 40 is provided with the 5th valve 25; described 3rd valve 23, the 4th valve 24 are for controlling conducting, the closedown of described pipeline 20, and described 5th valve 25 is for controlling conducting, the closedown of described first protection gas supplying tube 40.First embodiment shown in other structure with position relationship with Fig. 3 of the present embodiment is identical, does not repeat them here.
Use the transfer device of the second embodiment; realize the process of carrying out evacuation of air before pipeline 20 is accessed transfer device: open all valves in pipeline; in pipeline 20, pass into shielding gas by the first protection gas supplying tube 40, the air comprising water vapour in pipeline 20 is discharged by pipeline head end and line end under the effect of shielding gas pressure.Then, all valves of blinding off a line in 20, form the sealing pipeline being full of protection gas.Afterwards sealing pipeline is accessed in transfer device, with reference to figure 4, be connected by slip-knot bolt 191 between pipeline head end and the material feeding mouth of carrier pipe 12, be connected by slip-knot bolt 192 between line end with reactor 30.
Further; when pipeline 20 is very short time; be transferred to after in reactor 30 at titanium tetrachloride; can by opening all valves in transfer device; and in pipeline, passing into shielding gas by the first protection gas supplying tube 40, the pressure of shielding gas forces titanium tetrachloride residual in pipeline to be noted respectively and gets back in tank body 10 and reactor 30.Therefore, this device also can realize the waste avoiding titanium tetrachloride, realizes material recycle.
In a particular embodiment, in conjunction with reference to figure 3 and Fig. 4, the first protection gas supplying tube 40 between described 5th valve 25 and the protection gas inlet opening of the first protection gas supplying tube 40 is provided with the second barometer 18.Described second barometer 18 can be used for measuring before opening described 5th valve 25; first protection gas supplying tube 40 is to the air pressure of input protection gas in described pipeline 20; and in conjunction with the reading of the first barometer 16: when the reading at described first barometer 16 place is less than the reading of the second barometer 18; namely the pressure in tank body 10 is at this moment less than the pressure of the protection gas inlet opening place protection gas of described first protection gas supplying tube 40, remaining titanium tetrachloride back-pressure can be returned tank body 10 after just guaranteeing to open described 5th valve 25.Arrange the second barometer 18 in the present embodiment can accurately control to protect gas supplying tube 40 to the opportunity of input protection gas in pipeline 20, with titanium tetrachloride residual in emptying pipeline 20 by described first.
Owing to accessing the first protection gas supplying tube 40 in described pipeline 20, can be implemented in before pipeline 20 accessed transfer device, air emptying process is carried out to described pipeline 20.And adding three valves compared to the first embodiment due to the transfer device of the second embodiment, in the process of the therefore transfer liquid of the second embodiment, the state of each valve has difference.
Have for this, use the method for the transfer device transfer liquid of the second embodiment, comprise the following steps:
Before described pipeline 20 is accessed transfer device, comprising:
Open the 3rd valve 23 in pipeline 20, the 4th valve 24 and the 5th valve 25, by the first protection gas supplying tube 40 to input protection gas in pipeline 20, shielding gas spreads to the head and end of pipeline 20 gradually, and the pressure of shielding gas forces the air in pipeline 20 to be discharged by the head end of pipeline 20 and end;
After the air in pipeline 20 is emptying, stops the input of the shielding gas of the first protection gas supplying tube 40, and close the above-mentioned all valves opened, be then filled with shielding gas in pipeline 20 now, form the sealing pipeline 20 being full of shielding gas;
Afterwards, by being connected by slip-knot bolt 191 with the material feeding mouth of tank body 10 by the head end of described sealing pipeline 20, end is connected by slip-knot bolt 192 with reactor 30, makes pipeline 20 access in reaction device;
In the transfer process of liquid, also the 3rd valve 23, the 4th valve 24 keep the 5th valve 25 to close is opened when opening the first valve 14, the second valve 15, continue to pass into shielding gas in tank body 10 from described suction port 131, protection air pressure in tank body 10 above liquid increases gradually, forces liquid in tank body 10 by discharge port 122, carrier pipe 12, the 3rd valve 23, pipeline 20 and the 4th valve 24 inflow reactor 30;
After the liquid in reactor 30 reaches prearranging quatity, all valves in off-response device.
In a particular embodiment, can after the liquid in reactor 30 reach prearranging quatity, liquid residual in emptying pipeline 20.In a particular embodiment; the first protection gas supplying tube 40 between the 5th valve 25 and the protection gas inlet opening of the first protection gas supplying tube 40 is provided with the second barometer 18; then can judge open the opportunity that described 5th valve accurately controls to open the 5th valve 25 according to the reading of described first barometer 16 and the second barometer 18, to the determination on opportunity see the description in the second embodiment of transfer device of the present invention.
3rd embodiment
With reference to figure 5; when pipeline 20 is very long; described pipeline 20 is provided with the 6th valve 26 near line end place; pipeline 20 between the 6th valve 26 and line end is provided with the 7th valve 27; pipeline 20 on the 6th valve 26 and between the 7th valve 27 is provided with the second protection gas supplying tube 50, the second protection gas supplying tube 50 is provided with the 8th valve 28.Other structures of the present embodiment are identical with the first embodiment with position relationship, do not repeat them here.
In a particular embodiment; use the transfer device of the present embodiment; after being transferred to the titanium tetrachloride in reactor 30 and reaching prearranging quatity; close the 6th valve 26; and open the 7th valve 27 and the 8th valve 28; continue to pass into the titanium tetrachloride of shielding gas to emptying line end in pipeline 20 by the second protection gas supplying tube 50; close the 7th valve 27 afterwards; open the 6th valve 26, and continue through the second protection gas supplying tube 50 and pass into shielding gas to the titanium tetrachloride in emptying described pipeline 20.
And, before pipeline 20 is accessed transfer device, use the transfer device of the present embodiment, also can realize the effect of air in emptying pipeline 20.With reference to the transfer device of the second embodiment; open the 6th valve 26, the 7th valve 27 and the 8th valve 28; by the second protection gas supplying tube 50 input protection gas; with the air in emptying pipeline 20; then close the 6th valve 26, the 7th valve 27 and the 8th valve 28, form the sealing pipeline 20 being full of protection gas.
Compared to the transfer device of the first embodiment; the residual liquid of the object that the transfer device of the present embodiment increases by the second protection gas supplying tube 50 mainly in emptying pipeline 20; and add three valves compared to the first embodiment due to the transfer device of the 3rd embodiment; in the process of the therefore transfer liquid of the 3rd embodiment, the state of each valve has difference.So use the method for the transfer device transfer liquid of the 3rd embodiment, comprise the following steps:
In the transfer process of liquid, also open the 6th valve 26 and the 7th valve 27 when opening the first valve 14, the second valve 15 and close the 8th valve 28, continue to pass into shielding gas in tank body 10 by suction port 131, shielding gas pressure above tank body 10 increases gradually, forces the liquid in tank body 10 to enter carrier pipe 12, pipeline 20 be injected in reactor 30;
After the liquid in described reactor 30 reaches prearranging quatity, stop passing into of shielding gas, close the 6th valve 26, open the 7th valve 27, the 8th valve 28, the liquid of shielding gas to emptying described line end is passed into by the second protection gas supplying tube 50, close the 7th valve 27 afterwards, open the 6th valve 26, and continue through the second protection gas supplying tube 50 and pass into shielding gas to the liquid in emptying described pipeline 20; Or, open described 8th valve 28, the 6th valve 26, the 7th valve 27, passed into the liquid in shielding gas to emptying described pipeline 20 by described second protection gas supplying tube;
Close all valves in described transfer device.
4th embodiment
With reference to figure 6, when pipeline 20 is very long, based on the transfer device of the 3rd embodiment, in pipeline 20, access the first protection gas supplying tube 40, can see the transfer device of the second embodiment to the setting of the first protection gas supplying tube 40.As preferred embodiment, described pipeline head end side also protect on the pipeline 20 of gas supplying tube 40 joint near pipeline 20 and first and is provided with the 9th valve 29, and the pipeline 20 of also close described joint, line end side is provided with the tenth valve 31.Use the transfer device of the present embodiment, segmentation can realize in the air emptying process before pipeline 20 accesses transfer device and the emptying pipeline 20 after shift titanium tetrachloride in reactor 30 residual titanium tetrachloride.To the air in the emptying pipeline 20 of segmentation, comprise: first, open the 5th valve 25, the 9th valve 29, the 3rd valve 23, close the tenth valve 31, by the first shielding gas supplying tube 40 input protection gas, shielding gas, to the diffusion of pipeline head end, forces the air of pipeline head end side to be drained, and closes the 9th valve 29, the 3rd valve 23 afterwards; Then, also guarantee the 6th valve 26 when opening the tenth valve 31, the 7th valve 27 is also on state, continue through the first protection gas supplying tube 40 input protection gas, shielding gas spreads to line end, force the air of line end side to be drained, close the 5th valve 25, the tenth valve 31, the 6th valve 26 and the 7th valve 27 afterwards; Further; can also, after the air of emptying line end side, the 7th valve 27 and the 8th valve 28 be only kept to keep on state, by the second protection gas supplying tube 50 input protection gas; shielding gas spreads to line end side, the residual air in thorough discharge conduit 20.The order of above-mentioned evacuation step is not inevitable; in a particular embodiment; can select only to carry out the first two step; or repeat certain step; or adjust the order of described three steps, or only by regulating respective valves and protecting the air in the emptying pipeline 20 of gas supplying tube 50 by second.Air in the emptying pipeline 20 of described segmentation, realizes the thorough evacuation of air compared with long pipe runs, the water vapour in discharge conduit.The step of the residual titanium tetrachloride in the emptying pipeline 20 after having shifted titanium tetrachloride, can see the air step in the emptying pipeline 20 of segmentation, and concrete steps and principle are all identical.Residual titanium tetrachloride in the emptying pipeline 20 of described segmentation, realize compared with the transfer completely of titanium tetrachloride residual in long pipe runs, recovery, avoid the waste of raw material, it also avoid titanium tetrachloride residual in pipeline and block pipeline, and affect the follow-up recycling to pipeline.Other structures of 4th embodiment are identical with the 3rd embodiment with position relationship, do not repeat them here.Use the transfer device of the present embodiment, the residual titanium tetrachloride in emptying pipeline 20 up hill and dale can be realized, avoid the waste of material, prevent titanium tetrachloride to be thrown into befouling environment in environment, especially realize compared with the emptying residual titanium tetrachloride of long pipe runs.
Certainly; 9th valve 29 and the tenth valve 31 of the present embodiment also may be used in the second enforcement; concrete link position can see the setting of the present embodiment; be placed in pipeline head end side and end side respectively and near the joint of described first protection gas supplying tube and pipeline, reach the effect of segmentation evacuation of air, residual titanium tetrachloride.
Compared to the transfer device of embodiment before, the structure of the transfer device of the 4th embodiment is different, therefore with reference to front piecewise analysis, and the method for transfer liquid in conjunction with aforementioned any embodiment, use the step of the method for the transfer device transfer liquid of the 4th embodiment to be summarized as follows:
Before pipeline 20 is accessed transfer device, carry out air emptying process to pipeline 20, concrete steps are see leading portion introduction;
In the process of transfer liquid, the first valve 14, second valve 15, the 3rd valve 24, the 9th valve 29, the tenth valve 31, the 6th valve 26 and the 7th valve 27 is kept to be on state, all the other valves are closed condition, in tank body 10, pass into shielding gas by material feeding mouth 121, the pressure of shielding gas forces the liquid in tank body 10 to enter in reactor 30 by carrier pipe 12, pipeline 20;
After the liquid in reactor 30 reaches prearranging quatity, shift further the residual liquid in pipeline 20, reclaim, concrete steps see describing above, can not repeat them here.
As preferred embodiment, with reference to Fig. 6, place an electronic scale 17 in the bottom of described tank body 10.In the transfer process of titanium tetrachloride; the flow velocity of titanium tetrachloride can be calculated according to the reading change of electronic scale 17; and the flow velocity by regulating the respective valves in the flow of the shielding gas of input in described pneumatic tube 13 and described transfer device to regulate titanium tetrachloride, realize the control to titanium tetrachloride transfer flow velocity.But this electronic scale 17 is not limited to the present embodiment, also may be used in the first embodiment, the second embodiment, the 3rd embodiment, for monitoring, calculating and the transfer velocity of regulates liquid.
Although the present invention with preferred embodiment openly as above; but it is not for limiting the present invention; any those skilled in the art without departing from the spirit and scope of the present invention; the Method and Technology content of above-mentioned announcement can be utilized to make possible variation and amendment to technical solution of the present invention; therefore; every content not departing from technical solution of the present invention; the any simple modification done above embodiment according to technical spirit of the present invention, equivalent variations and modification, all belong to the protection domain of technical solution of the present invention.

Claims (25)

1. a device for storage of liquids, described liquid has corrosivity and composition easily and in air reacts,
It is characterized in that, comprising: the tank body of sealing, carrier pipe and pneumatic tube;
Described carrier pipe comprises material feeding mouth and discharge port, described discharge port is positioned at described tank body, described material feeding mouth is positioned at outside described tank body, the carrier pipe between described material feeding mouth and tank body is provided with the first valve, and described first valve is for controlling conducting, the closedown of described carrier pipe;
Described pneumatic tube comprises suction port and air outlet, described air outlet is positioned at described tank body, described suction port is positioned at outside described tank body, the pneumatic tube between described suction port and tank body is provided with the second valve, and described second valve is for controlling conducting, the closedown of described pneumatic tube;
Described discharge port is less than the height of described air outlet to described tank base to the height of described tank base.
2. the device of storage of liquids as claimed in claim 1, it is characterized in that, described liquid is titanium tetrachloride.
3. the device of storage of liquids as claimed in claim 1, is characterized in that, the pneumatic tube between described second valve and tank body is provided with the first barometer.
4. the device of storage of liquids as claimed in claim 1, it is characterized in that, the material of described carrier pipe and pneumatic tube comprises stainless steel.
5. the device of storage of liquids as claimed in claim 1, it is characterized in that, described first valve is also for controlling the flow of liquid in described carrier pipe; Described second valve is also for controlling the flow of shielding gas in described pneumatic tube.
6. the device of storage of liquids as claimed in claim 5, it is characterized in that, described first valve and the second valve are ball valve.
7. the device of storage of liquids as claimed in claim 1, it is characterized in that, described discharge port is positioned at described tank base, and described air outlet is positioned at described tank body top.
8. the device of storage of liquids as claimed in claim 1, it is characterized in that, described tank body comprises: have the body of opening and seal the cap of described opening;
Described tank interior is all inserted by described cap in the discharge port of described carrier pipe and the air outlet of described pneumatic tube.
9. the device of storage of liquids as claimed in claim 1, it is characterized in that, described tank body is double layer construction, the endothecium structure comprise layer structure, arranging within described layer structure.
10. the device of storage of liquids as claimed in claim 9, it is characterized in that, the material of described layer structure comprises stainless steel; The material of described endothecium structure comprises pure molybdenum or pure nickel.
The device of 11. storage of liquids as claimed in claim 1, it is characterized in that, the composition in described air comprises water vapour.
12. 1 kinds of methods using the device storage of liquids of claim 1, storage of liquids described in any one of 3-11, described liquid has corrosivity and water vapour easily and in air reacts, it is characterized in that, comprise: open described first valve and the second valve, by described carrier pipe to input protection gas in described tank body, with the air in emptying tank body, described shielding gas is the inert gas that density is greater than air density; After air in emptying described tank body, by described carrier pipe to infusion fluid in described tank body;
After the liquid in described tank body reaches prearranging quatity, close described first valve and the second valve.
The method of 13. storage of liquids as claimed in claim 12, is characterized in that, the pneumatic tube between described second valve and tank body is provided with the first barometer;
After described first valve of closedown and the second valve, also comprise: open described second valve again, continue to pass into shielding gas in described tank body, monitored the pressure in described tank body by described first barometric reading;
When monitoring the pressure in described tank body and reaching slight positive pressure state, close described second valve.
The method of 14. storage of liquids as claimed in claim 12, it is characterized in that, described shielding gas is argon gas.
The device of 15. 1 kinds of transfer liquids, described liquid has corrosivity and water vapour easily and in air reacts, it is characterized in that, comprise the device of the described storage of liquids of the device of the storage of liquids described in any one of claim 1-11, reactor and connection and the pipeline of described reactor;
Described pipeline head end is connected with described material feeding mouth; Described line end is connected with described reactor.
The device of 16. transfer liquids as claimed in claim 15, is characterized in that, for removably connecting between described pipeline head end and described material feeding mouth, described line end and described reactor are for removably connecting.
The device of 17. transfer liquids as claimed in claim 15; it is characterized in that; described pipeline is provided with the 3rd valve on the position near pipeline head end; described pipeline is provided with the 4th valve on the position near line end; pipeline between described 3rd valve and the 4th valve is provided with the first protection gas supplying tube; described first protection gas supplying tube is provided with the 5th valve; described 3rd valve, the 4th valve are for controlling conducting, the closedown of described pipeline, and described 5th valve is for controlling conducting, the closedown of described first protection gas supplying tube.
The device of 18. transfer liquids as claimed in claim 17, is characterized in that, protects between the protection gas inlet opening of gas supplying tube and described 5th valve first to protect on gas supplying tube be provided with the second barometer described first.
The device of 19. transfer liquids as claimed in claim 15, it is characterized in that, described pipeline is provided with the 6th valve on the position near line end, described 6th pipeline between valve and line end is provided with the 7th valve, pipeline between described 6th valve and the 7th valve is provided with the second protection gas supplying tube, described second protection gas supplying tube is provided with the 8th valve; Described 6th valve, the 7th valve are for controlling conducting, the closedown of described pipeline, and described 8th valve is for controlling conducting, the closedown of described second protection gas supplying tube.
The device of 20. transfer liquids as claimed in claim 15, is characterized in that, described tank base is provided with electronic scale, by the flow velocity of reading regulates liquid in pipeline of electronic scale.
21. 1 kinds of methods using the device transfer liquid of the transfer liquid of claim 15, described liquid has corrosivity and water vapour easily and in air reacts, and it is characterized in that, comprise step:
Open described first valve and the second valve, by described pneumatic tube to input protection gas in described tank body, flow in described reactor by described carrier pipe, pipeline to make the liquid in tank body under the pressure effect of shielding gas;
After the liquid in described reactor reaches prearranging quatity, close described first valve and the second valve.
The method of 22. transfer liquids as claimed in claim 21, it is characterized in that, described shielding gas comprises argon gas.
The method of 23. transfer liquids as claimed in claim 21, it is characterized in that, described pipeline is provided with the 3rd valve on the position near pipeline head end, described pipeline is provided with the 4th valve on the position near line end, pipeline between described 3rd valve and the 4th valve is provided with the first protection gas supplying tube, described first protection gas supplying tube is provided with the 5th valve;
Before by the device of described pipeline access transfer liquid, also comprise step:
Open described 3rd valve, the 4th valve and the 5th valve, by the first protection gas supplying tube to input protection gas in described pipeline, with the air in emptying described pipeline;
After the air in described pipeline is emptying, close all valves in described pipeline, form the sealing pipeline being full of shielding gas;
Afterwards, by described sealing pipeline access reaction device;
In the transfer process of liquid, when opening the first valve, the second valve, also open the 3rd valve, the 4th valve close the 5th valve;
After the liquid in described reactor reaches prearranging quatity, when closing described first valve, the second valve, also close described 3rd valve and the 4th valve.
The method of 24. transfer liquids as claimed in claim 21; it is characterized in that; described pipeline is provided with the 6th valve on the position near line end; described 6th pipeline between valve and line end is provided with the 7th valve; pipeline between described 6th valve and the 7th valve is provided with the second protection gas supplying tube; described second protection gas supplying tube is provided with the 8th valve, comprises step:
In the transfer process of liquid, when opening described first valve, the second valve, also open described 6th valve, the 7th valve and close described 8th valve;
After the liquid in described reactor reaches prearranging quatity, close described 6th valve, open described 7th valve, the 8th valve, the liquid of shielding gas to emptying described line end is passed into by described second protection gas supplying tube, close described 7th valve afterwards, open the 6th valve, and continue through the second protection gas supplying tube and pass into shielding gas to the liquid in emptying described pipeline; Or, open described 8th valve, the 6th valve, the 7th valve, passed into the liquid in shielding gas to emptying described pipeline by described second protection gas supplying tube;
Close all valves in the device of described transfer liquid.
The method of 25. transfer liquids as claimed in claim 21, it is characterized in that, described tank base is provided with electronic scale;
In the transfer process of described liquid, monitor the reading of described electronic scale;
According to the reading of described electronic scale, the flow velocity of regulates liquid in described pipeline.
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CN106145013B (en) 2016-06-28 2019-01-22 京东方科技集团股份有限公司 A kind of liquid transfer device and its control method
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