阅读说明：本技术 一种抽滤系统及其抽滤方法 (Suction filtration system and suction filtration method thereof ) 是由 陈建立 王海 豆君 王永珊 肖莎莎 刘红斌 杨丹 左珊珊 于 2019-08-14 设计创作，主要内容包括：本发明提供了一种抽滤系统及其抽滤方法,其中该抽滤系统包括抽滤装置,所述抽滤装置包括用于在惰性气体保护下对待抽滤溶液进行固液分离的抽滤砂芯装置,和连通于所述抽滤砂芯装置并用于收集待抽滤溶液抽滤后的液体的抽滤收集装置；连通于所述抽滤收集装置并用于冷凝从抽滤收集装置中挥发的气体的冷凝装置；连通于所述冷凝装置的抽真空装置,所述抽真空装置用于调节抽滤装置和冷凝装置的压力状态；和管路系统,所述管路系统依次将所述抽滤装置、所述冷凝装置以及所述真空装置可控制地连接,从而避免待抽滤溶液在抽滤过程中和氧气和水发生反应,降低了对人体危害和设备腐蚀的风险。(The invention provides a suction filtration system and a suction filtration method thereof, wherein the suction filtration system comprises a suction filtration device, the suction filtration device comprises a suction filtration sand core device for carrying out solid-liquid separation on a solution to be subjected to suction filtration under the protection of inert gas, and a suction filtration collection device communicated with the suction filtration sand core device and used for collecting the liquid subjected to suction filtration of the solution to be subjected to suction filtration; the condensing device is communicated with the suction filtration and collection device and is used for condensing the gas volatilized from the suction filtration and collection device; the vacuumizing device is communicated with the condensing device and is used for adjusting the pressure states of the suction filtration device and the condensing device; and the pipeline system is used for sequentially connecting the suction filtration device, the condensing device and the vacuum device in a controllable manner, so that the reaction of the solution to be subjected to suction filtration with oxygen and water in the suction filtration process is avoided, and the risk of harm to human bodies and equipment corrosion is reduced.)

1. The utility model provides a suction filtration system for treating suction filtration solution carries out suction filtration, its characterized in that includes:

the suction filtration device comprises a suction filtration sand core device and a suction filtration collection device, wherein the suction filtration sand core device is used for carrying out solid-liquid separation on a solution to be subjected to suction filtration under the protection of inert gas, and the suction filtration collection device is communicated with the suction filtration sand core device and is used for collecting the liquid to be subjected to suction filtration of the solution to be subjected to suction filtration;

the condensing device is communicated with the suction filtration and collection device and is used for condensing the gas volatilized from the suction filtration and collection device;

the vacuumizing device is communicated with the condensing device and is used for adjusting the pressure states of the suction filtration device and the condensing device;

a piping system controllably connecting the suction filtration device, the condensing device, and the vacuum device in sequence.

2. The suction filtration system of claim 1,

the suction filtration sand core device comprises a sand core funnel and a displacement reagent container which is used for containing a displacement reagent and is communicated with the sand core funnel, wherein the sand core funnel comprises an inert gas inlet and a solution to be suction filtered, and one end of the displacement reagent container is communicated with the solution to be suction filtered;

the suction filtration collecting equipment comprises a suction filtration bottle and a solvent collector arranged in the suction filtration bottle, the sand core funnel is connected with the opening of the suction filtration bottle in a sealing mode, the lower end of the sand core funnel is inserted into the solvent collector, and the suction filtration bottle is communicated with the condensing device through the pipeline system.

3. The suction filtration system of claim 2,

the suction filtration sand core device further comprises a liquid seal part used for sealing the replacement reagent container, and the sand core funnel, the replacement reagent container and the liquid seal part are communicated through a pipeline system.

4. The suction filtration system of claim 3,

condensing equipment includes condensation collection device, condensation collection device is including the coolant container that is used for holding the liquid nitrogen and being used for the condensation to pass through the volatile gaseous condensation collector of suction filtration collection device, condensation collector place in coolant container, and pass through pipe-line system communicate in the buchner flask for collect volatile gas.

5. The suction filtration system of claim 4,

the condensing unit further comprises an absorption device positioned on one side of the condensing and collecting device, the absorption device comprises a liquid seal container used for containing deionized water and a vent arranged at the upper end of the liquid seal container, and the liquid seal container is communicated with the condensing and collecting device through a pipeline system.

6. Suction filtration system according to any one of claims 1 to 5,

the vacuumizing device comprises an oil-free vacuum pump communicated with the condensing device through a pipeline system and a pressure gauge arranged between the oil-free vacuum pump and the condensing device and located on the pipeline system.

7. The suction filtration system of claim 6,

the pipeline system comprises a glass tube and a control switch arranged on the glass tube, wherein the control switch comprises a silica gel hose and a hemostatic forceps which is used for opening or closing the silica gel hose by retracting and releasing the silica gel hose.

8. The suction filtration system of claim 2,

the suction filtration device also comprises a rubber plug, and the suction filtration bottle is hermetically connected with the sand core funnel through the rubber plug; or

The upper end opening of the filtration bottle is a frosted opening, and the filtration bottle is connected with the sand core funnel in a sealing mode through the frosted opening.

9. A suction filtration method using the suction filtration system according to any one of claims 1 to 9, comprising the steps of:

introducing inert gas into the suction filtration system through the suction filtration device, and keeping the suction filtration system in a negative pressure state through the vacuum pumping device after replacing air in the suction filtration system;

closing the vacuum pumping device to enable the inside of the suction filtration system to be in a positive pressure state, and adding a solution to be subjected to suction filtration into the suction filtration device under the protection of inert gas;

and opening a vacuumizing device to enable the suction filtration system to be in a negative pressure state, and performing suction filtration on the solution to be subjected to suction filtration in the suction filtration device until no liquid is dripped into the suction filtration collection device.

10. The suction filtration process according to claim 9,

opening evacuating device at the step and making suction filtration system be in the negative pressure state, be in suction filtration device wait that suction filtration solution is by the suction filtration, until there is not liquid to drip into behind the suction filtration collection device, still include the step:

and adding the replacement reagent in the replacement reagent container into the suction filtration sand core device of the suction filtration device for replacing the solution to be suction filtered remained in the suction filtration sand core device.

[ technical field ] A method for producing a semiconductor device

The invention relates to the field of anhydrous and anaerobic solvent treatment devices, in particular to a suction filtration system and a suction filtration method thereof.

[ background of the invention ]

Titanium tetrachloride (TiCl4) is an important intermediate for the production of metallic titanium and its compounds. In the preparation process of titanium tetrachloride, the solid content in the crude titanium tetrachloride needs to be analyzed and tested to adjust the chlorination reaction and the process conditions of the cyclone separator so as to keep the solid content below 1.5 percent. Therefore, it is necessary to suction-filter and dry the solid content in the crude titanium tetrachloride solution.

At room temperature, titanium tetrachloride is a colorless liquid and fuming in air produces a mixture of titanium dioxide solids and hydrochloric acid droplets. The hydrogen chloride (HCl) volatilized from the generated hydrochloric acid has suffocating smell, strong stimulation to the upper respiratory tract and corrosion to eyes, skin and mucous membrane. If the air leakage happens, the air leakage not only affects the atmosphere environment, but also brings certain risks to the life safety of the surroundings.

However, in the prior art, the crude titanium tetrachloride solution cannot be ensured not to be contacted with oxygen or water in the process of carrying out suction filtration on the crude titanium tetrachloride solution, and the risk of generating asphyxiating smell exists.

[ summary of the invention ]

The invention aims to solve the technical problem of overcoming the defects of the prior art and provides a suction filtration device for crude titanium tetrachloride so as to avoid the harm to human bodies and the corrosion to equipment caused by gas formed by the reaction of a solution to be subjected to suction filtration in water and oxygen.

In order to solve the above problems, the present invention provides a suction filtration system for crude titanium tetrachloride, comprising:

the suction filtration device comprises a suction filtration sand core device and a suction filtration collection device, wherein the suction filtration sand core device is used for carrying out solid-liquid separation on a solution to be subjected to suction filtration under the protection of inert gas, and the suction filtration collection device is communicated with the suction filtration sand core device and is used for collecting the liquid to be subjected to suction filtration of the solution to be subjected to suction filtration;

the condensing device is communicated with the suction filtration and collection device and is used for condensing the gas volatilized from the suction filtration and collection device;

the vacuumizing device is communicated with the condensing device and is used for adjusting the pressure states of the suction filtration device and the condensing device; and

a piping system controllably connecting the suction filtration device, the condensing device, and the vacuum device in sequence.

In an embodiment of the invention, the suction filtration sand core device comprises a sand core funnel and a displacement reagent container which is used for containing a displacement reagent and is communicated with the sand core funnel, wherein the sand core funnel comprises an inert gas inlet positioned at the left end of a sand core funnel body and a solution to be suction filtered positioned at the upper end, and one end of the displacement reagent container is communicated with the solution to be suction filtered;

the suction filtration collection equipment comprises a suction filtration bottle and a solvent collector arranged in the suction filtration bottle, the sand core funnel is connected with the opening of the suction filtration bottle in a sealing manner, the lower end of the sand core funnel is inserted into the solvent collector, and the right end of the suction filtration bottle is communicated with the condensing device through the pipeline system.

In an embodiment of the present invention, the pumping filtration sand core device further includes a liquid seal portion for sealing the replacement reagent container and located on the right side of the replacement reagent container, and the sand core funnel, the replacement reagent container and the liquid seal portion are communicated through a pipeline system.

In an embodiment of the present invention, the condensing device includes a condensation collecting device, the condensation collecting device includes a cooling medium container for containing liquid nitrogen and a condensation collector for condensing the gas volatilized by the suction filtration collecting device, and the condensation collector is placed in the cooling medium container, is communicated with the suction filtration bottle through the pipeline system, and is used for collecting the volatilized gas.

In an embodiment of the present invention, the condensing device further includes an absorption device located at one side of the condensation collecting device, the absorption device includes a liquid seal container for containing deionized water and a vent arranged at an upper end of the liquid seal container, and the liquid seal container is communicated with the condensation collector through a pipeline system.

In an embodiment of the present invention, the vacuum pumping device includes an oil-free vacuum pump connected to the condensing device through a piping system, and a pressure gauge disposed between the oil-free vacuum pump and the condensing device and on the piping system.

In an embodiment of the invention, the pipeline system comprises a glass tube and a control switch installed on the glass tube, and the control switch comprises a silica gel hose and a hemostatic forceps which opens or closes the silica gel hose by retracting and releasing the hemostatic forceps.

In an embodiment of the present invention, the suction filtration collection apparatus further includes a base and a silica gel pad, and the suction filtration bottle is placed on the base and is isolated from the base by the silica gel pad.

In an embodiment of the invention, the suction filtration device further comprises a rubber plug, and the suction filtration bottle is hermetically connected with the sand core funnel through the rubber plug; or

The upper end opening of the filtration bottle is a frosted opening, and the filtration bottle is connected with the sand core funnel in a sealing mode through the frosted opening.

In order to solve the above problems, the present invention also provides a suction filtration method using the suction filtration system for crude titanium tetrachloride as described above, comprising the steps of:

installing the suction filtration system;

introducing inert gas into the suction filtration system through the suction filtration device, displacing air in the suction filtration system, and keeping the suction filtration system in a negative pressure state through the vacuum pumping device;

closing the vacuum pumping device to enable the inside of the suction filtration system to be in a positive pressure state, and adding a solution to be subjected to suction filtration into the suction filtration device under the protection of inert gas;

and opening a vacuumizing device to enable the suction filtration system to be in a negative pressure state, and performing suction filtration on the solution to be subjected to suction filtration in the suction filtration device until no liquid is dripped into the suction filtration collection device.

In an embodiment of the present invention, after the step of turning on the vacuum pumping device to make the suction filtration system in a negative pressure state, and suction filtering the solution to be suction filtered in the suction filtration device until no liquid drops into the suction filtration collection device, the method further includes the steps of:

adding a replacement reagent in a replacement reagent container into the suction filtration sand core device of the suction filtration device for replacing the solution to be suction filtered remained in the suction filtration sand core device

Compared with the prior art, the invention has the advantages that:

1. the suction filtration device of the suction filtration system is in the protective atmosphere of inert gas when the solution to be treated is subjected to suction filtration, and the vacuum pumping device enables the suction filtration system to be in a negative pressure state in the suction filtration process of the solution to be treated, so that the solution to be treated can be prevented from being contacted by outside air and moisture, and harmful gases such as smoke and fog are prevented from being generated;

2. according to the suction filtration system, the silica gel pad is arranged between the suction filtration bottle and the base of the suction filtration device, so that after the suction filtration operation of the suction filtration system is completed, the sealing of the whole suction filtration system can be ensured, the suction filtration bottle can be rapidly disassembled, and the test efficiency is improved;

3. the condensing device of the suction filtration system adopts the matching use of the liquid nitrogen and the cold trap, so that the volatilized solvent can be quickly solidified, and the volatile components are prevented from entering the vacuum-pumping device, thereby avoiding the damage of equipment.

[ description of the drawings ]

Fig. 1 is a schematic structural view of a suction filtration system for crude titanium tetrachloride according to an embodiment of the present invention.

Fig. 2 is a schematic structural diagram of a pipeline system of the suction filtration system for crude titanium tetrachloride according to the above embodiment of the present invention.

FIG. 3 is a schematic flow chart of the suction filtration method of the suction filtration system for crude titanium tetrachloride according to the above embodiment of the present invention.

In the drawings:

10. a suction filtration device; 11. a suction filtration sand core device; 111. a sand core funnel; 112. a replacement reagent container; 113. a liquid seal section; 114. an inert gas outlet; 115. a solution to be filtered is imported; 12. a suction filtration and collection device; 121. a suction flask; 122. a solvent collector; 123. a base; 124. a silica gel pad; 125. a rubber plug; 20. a condensing unit; 21. a condensing and collecting device; 211. a cooling medium container; 212. a condensation collector; 22. an absorption device; 221. a liquid-sealed container; 222. a vent port; 30. a vacuum pumping device; 31. an oil-free vacuum pump; 32. a pressure gauge; 40. a piping system; 41. a glass tube; 42. a rubber hose; 43 hemostatic forceps.

[ detailed description ] embodiments

The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art. The basic principles of the invention, as defined in the following description, may be applied to other embodiments, variations, modifications, equivalents, and other technical solutions without departing from the spirit and scope of the invention.

In the description of the present invention, it is to be understood that the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. In the description of the present invention, it should be noted that, unless explicitly stated or limited otherwise, the terms "connected" and "connected" are to be interpreted broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.

As shown in fig. 1 to fig. 2, the present invention is a specific illustration of a suction filtration system for crude titanium tetrachloride, wherein the suction filtration system is used for suction filtration of a solution to be suction filtered, so as to perform solid-liquid separation of the solution to be suction filtered under the protection of an inert gas, and avoid the solution to be suction filtered from contacting moisture and oxygen. It will be understood by those skilled in the relevant art that the solution to be suction filtered is preferably embodied as a solution that is readily reactive to water and oxygen, and specifically, in the present invention, the solution to be suction filtered may be embodied as a crude titanium tetrachloride solution.

As shown in fig. 1, the suction filtration system includes a suction filtration device 10, a condensation device 20, a vacuum device 30, and a piping system 40, wherein the piping system 40 controllably connects the suction filtration device 10, the condensation device 20, and the vacuum device 30 in sequence. Here, the controlled connection means that the suction filter device 10, the condenser device 20 and the vacuum pump device 30 can be connected or disconnected by controlling the pipe system 40. The suction filtration device 10 comprises a suction filtration sand core device 11 for carrying out solid-liquid separation on a solution to be subjected to suction filtration under the protection of inert gas and a suction filtration collection device 12 which is communicated with the suction filtration sand core device 11 and is used for collecting the liquid to be subjected to suction filtration of the solution to be subjected to suction filtration; the condensing device 20 is communicated with the suction filtration and collection device 12 and is used for condensing and collecting the gas volatilized from the suction filtration and collection device 12; the vacuum pumping device 30 is communicated with the condensing device 20 and is used for adjusting the pressure states of the suction filtration device 10 and the condensing device 20. Here, the pressure state includes a positive pressure state greater than the atmospheric pressure or a negative pressure state less than the atmospheric pressure.

As shown in fig. 1, the sand core filtering device 11 comprises a sand core funnel 111 and a displacing agent container 112 which is used for containing a displacing agent and communicated with the sand core funnel 111, wherein the sand core funnel 111 is provided with an inert gas inlet 114 which is arranged at the left end of the body of the sand core funnel 111 so as to allow an inert body to enter the sand core funnel 111 and a solution to be filtered and filtered 115 which is arranged at the upper end so as to allow the solution to be filtered and filtered to enter the sand core funnel 111, one end of the displacing agent container 112 is communicated with the solution to be filtered and filtered 115 so as to displace the titanium tetrachloride solution which may be remained in a filter cake through the displacing agent in the displacing agent container 112 after the filtering process. It is worth mentioning that in the embodiment of the present invention, dichloromethane is usually contained in the transpose reagent container 112 to ensure that the amount of water contained in the transpose reagent itself is low. In addition, in the embodiment of the present invention, the inert gas may be implemented as nitrogen, and the nitrogen is continuously filled into the suction filtration device 10 during the suction filtration process to protect the suction filtration solution from contacting water or oxygen, so as to prevent the solvent of the solution to be suction filtered from reacting with water or oxygen to generate smoke and fog, which affect the safety of human body or radiate the vacuum-pumping device 30.

The suction filtration collection device 12 comprises a filter flask 121 and a solvent collector 122 arranged in the filter flask 121, the sand core funnel 111 is connected to the opening of the filter flask 121 in a sealing manner, the lower end of the sand core funnel 111 is inserted into the solvent collector 122, so that when a solution to be suction filtered is suction filtered in the sand core funnel 111, the solid content in the solution to be suction filtered is collected in the sand core funnel 111 and forms a filter cake, liquid (solvent) in the solution to be suction filtered flows into the solvent collector 122 through the lower end opening of the sand core funnel 111, and the right end of the filter flask 121 is communicated with the condensing device 20 through the pipeline system 40.

As shown in fig. 1, the suction filtration collection device 12 further includes a base 123 and a silica gel pad 124, the suction filtration bottle 121 is placed on the base 123, and the silica gel pad 124 isolates the suction filtration bottle 121 from the base 123, so that the suction filtration system can be kept sealed, the suction filtration bottle 121 can be rapidly detached from the suction filtration system, and the test efficiency can be improved. In order to better detach the suction bottle 121 from the suction filtration system, grease can be applied to the silicone pad 124 when the silicone pad is used, so that the sealing effect and the detachment convenience are improved.

As shown in fig. 1, in order to ensure that the connection between the filtration bottle 121 and the sand core funnel 111 is kept sealed, the filtration device 10 further comprises a rubber plug 125, and the filtration bottle 121 and the sand core funnel 111 are hermetically connected through the rubber plug 125; or the upper end opening of the filter flask 121 is a frosted opening, and the filter flask 121 and the sand core funnel 111 are connected in a sealing manner through the frosted opening.

As shown in fig. 1, the pumping filtration core apparatus 11 further comprises a liquid seal 113 for sealing the displaceable reagent container 112 and located at the right side of the displaceable reagent container 112, and the sand core funnel 111, the displaceable reagent container 112 and the liquid seal 113 are communicated through a piping system 40. Further, the liquid seal portion 113 includes a liquid seal and a housing chamber for housing the liquid seal, and an air outlet is provided at a rear end of the housing chamber. The liquid seal 113 is used to isolate the external air from entering the transposing reagent container 112 through the containing cavity, wherein the liquid seal can be implemented by, but not limited to, liquid paraffin, and can also be implemented as a non-volatile liquid reagent.

In order to prevent the solvent from evaporating from the filter flask 121 through the line system 40 into the evacuation device 30 and thus from corroding the evacuation device 30, a condensation device 20 is provided between the evacuation device 30 and the filter apparatus 10. As shown in fig. 1, the condensing device 20 includes a condensing and collecting device 21, the condensing and collecting device 21 includes a cooling medium container 211 for containing a cooling medium and a condensing and collecting device 212 for condensing the gas volatilized by the suction filtration and collecting device 12, and the condensing and collecting device 212 is disposed in the cooling medium container 211 and is communicated with the suction filtration bottle 121 through the pipeline system 40 for condensing and collecting the volatilized gas. It is worth mentioning that in the condensation and collection device 21, the cooling medium in the cooling medium container 211 is liquid nitrogen, and the condensation and collection device 212 is implemented as a cold trap, so that the volatilized solvent can be rapidly solidified, and the volatilization into the vacuum extractor 30 can be prevented, thereby avoiding the damage of the equipment.

In order to further absorb or collect the volatilized gas, as shown in fig. 1, the condensing device 20 further includes an absorption device 22 located at the right side of the condensation collecting device 21, the absorption device 22 includes a liquid seal container 221 for containing liquid and a vent 222 disposed at the upper end of the liquid seal container 221, and the liquid seal container 221 is communicated with the condensation collector 212 through a pipeline system 40. The liquid in the liquid-tight container 221 is preferably deionized water, wherein the glass tube 41 or the flexible tube in the piping system 40 is directly inserted into the deionized water, so as to further remove the volatile gas. The vent 222 prevents suck back of the vacuum 30.

In an embodiment of the present invention, as shown in fig. 1, the vacuum pumping device 30 includes an oil-free vacuum pump 31 communicated with the condensing device 20 through a piping system 40, and a pressure gauge 32 disposed between the oil-free vacuum pump 31 and the condensing device 20 and on the piping system 40. The pipeline system 40 comprises glass tubes 41 and a control switch arranged between the two glass tubes 41 and used for controlling the conduction of the glass tubes 41, wherein the control switch comprises a silica gel hose 42 and a hemostatic forceps 43 which opens or closes the silica gel hose 42 by retracting and releasing. According to the invention, the hemostatic forceps 43 are adopted to be matched with the silica gel hose 42 in a retractable manner to realize the rapid switching of the control switch, so that the operation is convenient and the efficiency is high.

In addition, the embodiment of the invention provides a replacement mode of the cold trap of the condensation collection device 21. The control switch at the inert gas inlet is firstly turned on to adjust the air inflow of the inert gas so that the inside of the suction filtration system is in a positive pressure state, and meanwhile, the system cannot be damaged due to overhigh pressure due to the protection of the liquid seal part 113. The control switch between the oil-free vacuum pump 32 and the absorption device 22 is gradually closed and the control switch on the vent 222 is opened in order to prevent the liquid in the absorption device 22 from being sucked back into the cold trap, and at the same time, the control switch between the suction filtration collection device 12 and the condensation collection device 21 is closed by the hemostatic forceps 43 to strip the cold trap out of the suction filtration system for replacement of the cold trap.

Similarly, an alternative to the solvent trap 15 is provided in embodiments of the present invention. Firstly, a control switch at an inert gas inlet is turned on to adjust the air input of the inert gas so that the inside of the suction filtration system is in a positive pressure state, and meanwhile, the control switch between the suction filtration collection device 12 and the condensation collection device 2 is turned off. Then, the filtration bottle 121 is opened slowly, the silicone rubber gasket 124 is separated from the base 123 under a positive pressure, and the silicone rubber hose 42 or the glass tube 41 located at the front end of the control switch between the filtration collection device 12 and the condensation collection device 2 is inserted into the solvent collection bottle 122. And then a control switch between the suction filtration collection device 12 and the condensation collection device 2 is opened, and the liquid in the solvent collection bottle 122 enters the condensation collector 212 under the combined action of the negative pressure and the inert gas, so that the volatilization of the solvent of the solution to be suction filtered is avoided. For example, when the solution to be filtered is a crude titanium tetrachloride solution, volatilization of titanium tetrachloride can be avoided.

As shown in fig. 3, the present invention also provides a suction filtration method using the suction filtration system for crude titanium tetrachloride, comprising the steps of:

s100, introducing inert gas into a suction filtration system through a suction filtration device 10, displacing the gas in the suction filtration system, and keeping the suction filtration system in a negative pressure state through a vacuumizing device 30;

s200, closing the vacuumizing device 30 to enable the inside of the suction filtration system to be in a positive pressure state, and adding a solution to be subjected to suction filtration into the suction filtration device 10 under the protection of inert gas;

s300, opening the vacuumizing device 30 to enable the suction filtration system to be in a negative pressure state, and carrying out suction filtration on the solution to be subjected to suction filtration in the suction filtration device 10 until no liquid is dripped into the suction filtration and collection device 12.

Specifically, in step S100, an inert gas is introduced into the suction filtration system through the suction filtration device 10 so as to displace air remaining in the suction filtration system, and further, the air is continuously pumped out of the suction filtration system through the vacuum pumping device 30 to perform suction filtration until the pressure in the suction filtration system is negative pressure.

Before step S200, the method further includes the steps of: adding a displacing reagent into the displacing reagent bottle. Here, the substitution reagent is preferably embodied as dichloromethane to reduce moisture in the substitution reagent. In step S3, the solution to be suction filtered is added to the suction filter core apparatus 11, and further, to two thirds of the volume of the core funnel 111 in the suction filter core.

In step S300, the solution to be filtered is rapidly filtered in the filtering apparatus 10 under negative pressure until no liquid is dropped from the filtering sand core apparatus 11 to the filtering and collecting apparatus 12, at which time the filtering is completed. In the suction filtration process, be provided with condensing equipment 20 between evacuating device 30 and suction filtration device 10, can prevent that the liquid that collects in suction filtration collection device 12 of suction filtration device 10 from volatilizing the direct contact in evacuating device 30, and then corroding evacuating device 30.

After step S300, further comprising the steps of: and adding the replacement reagent in the replacement reagent container 112 into the suction filtration sand core device 11 of the suction filtration device 10 for replacing the solution to be suction filtered remained in the suction filtration sand core device 11. Preferably, at least 3 substitutions are made during this step to ensure that no titanium tetrachloride remains in the filter cake.

Therefore, as shown in fig. 1 to 2, the suction filtration principle of a suction filtration system of the present invention is as follows: here, the suction filtration principle of the suction filtration system will be described by taking a crude titanium tetrachloride solution as an example, the suction filtration system is connected in the arrangement shown in fig. 1, and liquid-sealed paraffin oil, liquid nitrogen and deionized water are respectively filled into the liquid-sealed portion 113, the cooling medium container 211 and the liquid-sealed container 221. And (3) opening all the control switches, introducing inert gas (nitrogen) into the suction filtration system through the inert gas inlet 114, gradually closing the control switch at the position of the solution inlet 115 to be subjected to suction filtration, the control switch at the upper end of the displacement reagent container 112 and the control switch between the absorption device 22 and the vacuumizing device 30, and performing inert gas (nitrogen) displacement on the suction filtration system for 30 minutes. And (3) starting the oil-free vacuum pump 31, starting a control switch between the absorption device 22 and the vacuumizing device 30, closing a control switch on the vent port 222, closing a control switch between the displacement reagent container 112 and the sand core funnel 111 and a control switch at the position of the inert gas inlet 114, and performing suction filtration on the suction filtration system until the pressure gauge 32 displays a negative pressure state. Then the oil-free vacuum pump 31 is turned off, the control switch between the absorption device 22 and the vacuumizing device 30 is turned off, the control switch between the inert gas inlet 115 and the sand core funnel 111 is turned on until the pressure gauge 32 shows a positive pressure state, then the control switch between the inert gas inlet 114 and the liquid seal part 113, the control switch between the absorption device 22 and the vacuumizing device 30 and the control switch between the vent 222 are gradually turned on, the switching is repeated for 3 times, the bolster suction filtration system is in the positive pressure state, at this time, the control switch on the solution inlet 115 to be subjected to suction filtration, the control switch of the replacement reagent container and the control switch between the absorption device 22 and the vacuumizing device 30 are all in the off state, and the rest control switches are all turned on. The control switch for controlling the opening of the substitution reagent container 112 is then closed after the control switch for controlling the upper end of the substitution reagent container 112 is opened and the control switch for controlling the lower end of the substitution reagent container 112 is closed, and the substitution reagent (here, methylene chloride is used as an example) is added to the substitution reagent container 112 through the opening of the substitution reagent container 112, and the liquid level of the added substitution reagent is set to 2/3 of the volume of the substitution reagent container 112. And (3) starting a control switch for controlling the inlet 115 of the solution to be filtered, enabling the uniformly shaken crude titanium tetrachloride solution to flow into the sand core funnel 111 through the inlet 115 of the solution to be filtered under the protection of nitrogen, enabling the liquid level of the crude titanium tetrachloride solution to reach 2/3, and then closing the control switch for controlling the inlet 115 of the solution to be filtered. And (3) closing a control switch on the control vent 222, opening the oil-free vacuum pump 31, starting a control switch between the absorption device 22 and the vacuumizing device 30, and adjusting the control switch for controlling the air inflow of the inert gas inlet 114 to enable the system to be in a negative pressure state, so that the crude titanium tetrachloride solution in the sand core funnel 111 is rapidly filtered in the negative pressure state until no liquid is dripped into the solvent collector 15. The control switch between the displacement agent container 112 and the sand core funnel 111 is opened to allow the displacement agent (methylene chloride solution) to enter the sand core funnel 111 and the titanium tetrachloride in the filter cake is displaced by the methylene chloride solution, preferably at least 3 times, to ensure that no more titanium tetrachloride remains in the filter cake. And then switching the suction filtration system to a positive pressure state, taking out the filter cake, and carrying out further analysis and test. The process can avoid the harm to human body and the corrosion to equipment caused by the gas formed by the reaction of the solution of titanium tetrachloride in water and oxygen.

It will be appreciated by persons skilled in the art that the embodiments of the invention described above and shown in the drawings are given by way of example only and are not limiting of the invention. The objects of the invention have been fully and effectively accomplished. The functional and structural principles of the present invention have been shown and described in the examples, and any variations or modifications of the embodiments of the present invention may be made without departing from the principles.