CN216972393U - Device for preparing olefin polymerization catalyst - Google Patents
Device for preparing olefin polymerization catalyst Download PDFInfo
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- CN216972393U CN216972393U CN202220473875.3U CN202220473875U CN216972393U CN 216972393 U CN216972393 U CN 216972393U CN 202220473875 U CN202220473875 U CN 202220473875U CN 216972393 U CN216972393 U CN 216972393U
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Abstract
The utility model provides a device for preparing an olefin polymerization catalyst, and relates to the field of catalyst preparation. The device comprises: the nitrogen supply device is connected with a first nitrogen pipeline and a second nitrogen pipeline; the double-row pipe is provided with a nitrogen filling pipe, a vacuum pipe and a branch pipe, the vacuum pipe is connected with a vacuum pump, one end of the nitrogen filling pipe is communicated with a first nitrogen pipeline, the other end of the nitrogen filling pipe is connected with a first oil bubbler, and an air outlet of the first oil bubbler is connected with a first glass valve; the first reaction device is used for loading and washing the active center of the catalyst, the first reaction device is communicated with the second nitrogen pipeline through a nitrogen pipeline three-way valve, the other interface of the nitrogen pipeline three-way valve is connected with a second oil bubbler, and the air outlet of the second oil bubbler is connected with a second glass valve. The preparation steps of the olefin polymerization catalyst are integrated in one device, and the operations of vacuumizing and filling nitrogen in all the steps are convenient, so that the preparation process is carried out under the protection of anhydrous, oxygen-free and nitrogen.
Description
Technical Field
The utility model relates to the field of catalyst preparation, in particular to a device for preparing an olefin polymerization catalyst.
Background
The preparation and storage of olefin polymerization (polyolefin) catalysts have extremely strict requirements on water and oxygen, and trace amounts of water and oxygen can cause permanent inactivation of the catalysts in the preparation and storage processes of the catalysts, so that the preparation of the olefin polymerization catalysts needs to be carried out under the protection of anhydrous, oxygen-free and nitrogen.
The preparation of Ziegler-Natta catalysts for olefin polymerization is generally divided into three stages: the method comprises the steps of mother liquor synthesis, active center loading and catalyst washing and drying, wherein the three steps are connected in a front-back and close manner, if the mother liquor of the catalyst needs to be transferred to a reactor loaded with the active center after being synthesized, the active center loading and the catalyst washing process are completed in the reactor, and the catalyst slurry is transferred to a drying bottle for vacuum drying after the washing is completed.
In the preparation process of the olefin polymerization catalyst in the prior art, each preparation step is carried out respectively, the steps are not effectively connected, in addition, each step needs to be carried out in a nitrogen atmosphere, and a temporary connecting pipeline is also needed for carrying out vacuum treatment, so the operation is troublesome. Therefore, there is a need in the art to design an apparatus for preparing olefin polymerization catalyst, which can integrate three steps into one apparatus, and the apparatus is convenient for vacuum-pumping and nitrogen-filling operations, so as to meet the stringent requirements of the preparation process for water and oxygen.
SUMMERY OF THE UTILITY MODEL
Therefore, the technical problem to be solved by the present invention is to provide an apparatus for preparing an olefin polymerization catalyst, which can integrate the preparation process of the catalyst in a set of apparatus, facilitate the operations of vacuum pumping and nitrogen filling in each step, and ensure that the preparation process is performed under the protection of anhydrous, oxygen-free and nitrogen.
Therefore, the utility model provides the following technical scheme:
the present invention provides an apparatus for preparing an olefin polymerization catalyst, comprising:
the nitrogen supply device is connected with a first nitrogen pipeline and a second nitrogen pipeline;
the double-row pipe is provided with a nitrogen filling pipe, a vacuum pipe and a branch pipe, the vacuum pipe is connected with a vacuum pump, one end of the nitrogen filling pipe is communicated with the first nitrogen pipeline, the other end of the nitrogen filling pipe is connected with a first oil bubble device, and an air outlet of the first oil bubble device is connected with a first glass valve;
the first reaction device is used for loading and washing the active center of the catalyst, the first reaction device is communicated with the second nitrogen pipeline through a nitrogen pipeline three-way valve, the other interface of the nitrogen pipeline three-way valve is connected with a second oil bubble device, and the gas outlet of the second oil bubble device is connected with a second glass valve.
Further, the apparatus for preparing an olefin polymerization catalyst further comprises:
the second reaction device is used for preparing catalyst mother liquor, and when a nitrogen atmosphere is provided for the second reaction device, the second reaction device is communicated with the branch pipes of the double-row pipes; when the catalyst mother liquor in the second reaction device is transferred into the first reaction device, the second reaction device is communicated with the first reaction device through a peristaltic pump.
Further, the apparatus for preparing an olefin polymerization catalyst further comprises:
a separation drying device including a separation container and a cooling device for separating and drying the catalyst, the separation container being communicated with the branch pipes of the double rows of pipes when a nitrogen atmosphere is supplied into the separation container; when the separation of the catalyst is carried out, the separation vessel is communicated with the first reaction device; when the solid in the separation container is dried in vacuum, the cooling device is respectively communicated with the separation container and the branch pipes of the double-row pipe.
Further, the first reaction device selects a jacketed five-mouth bottle, a stirrer is mounted on the jacketed five-mouth bottle, and the jacketed five-mouth bottle is connected with a program temperature controller.
Further, the nitrogen supply device selects a nitrogen cylinder.
Further, the second reaction device selects a three-mouth bottle.
Further, the separation vessel is a reaction tube; the cooling device selects a cold trap and a Dewar flask.
Furthermore, the first oil bubbler and the second oil bubbler are reverse suction prevention oil bubblers.
Further, the air outlets of the first oil bubbler and the second oil bubbler are connected with a waste gas recovery bottle.
Furthermore, a vacuum pipeline three-way valve and a vacuum pressure gauge are arranged between the vacuum pipe and the vacuum pump, and the other interface of the vacuum pipeline three-way valve is communicated with the atmosphere.
Further, a first stop valve is arranged on the first nitrogen pipeline and arranged between the nitrogen supply device and the double-row pipe.
Further, be provided with the second stop valve on the second nitrogen gas pipeline, the second stop valve sets up supply between nitrogen device and the nitrogen gas pipeline three-way valve.
The technical scheme of the utility model has the following advantages:
1. the device for preparing the olefin polymerization catalyst is provided with the double-row pipes which are respectively connected with the nitrogen pipeline and the vacuum pump, so that the operations of vacuumizing and filling nitrogen are convenient for various devices (such as a catalyst mother liquor preparation device and a catalyst separation and drying device) in the preparation process, and meanwhile, a reaction device for loading and washing the active center of the catalyst is positioned on the other nitrogen pipeline, so that the solution transfer operation between the reaction device and other devices provided with nitrogen protection by the double-row pipes under the protection of nitrogen is facilitated, and the solution transfer is realized by adjusting the pressure difference generated by the opening degree of a glass valve at the air outlet of a corresponding oil bubbler.
The utility model integrates the preparation steps of the olefin polymerization catalyst into one device, has simple device and reasonable layout, effectively associates each step, saves space, is convenient for personnel to operate, is convenient for the vacuumizing and nitrogen filling operation of each step, ensures that the preparation process is carried out under the protection of anhydrous, anaerobic and nitrogen, and avoids the adverse effect of water and oxygen in the air on other performances such as catalyst activity and the like.
2. The device for preparing the olefin polymerization catalyst, provided by the utility model, preferably adopts a separation drying device comprising a separation container and a cooling device, and can realize vacuum drying of the catalyst, for example, the cooling device selects a cold trap and a Dewar flask, so that the solvent can be cooled into the cold trap, and the influence of pumping residual organic solvent in the catalyst to a vacuum pump on the service life is avoided.
3. The device for preparing the olefin polymerization catalyst preferably adopts the anti-suck-back oil bubbler, so that the installation of a buffer bottle is omitted, unnecessary equipment is reduced, the space is saved, and meanwhile, the liquid paraffin in the anti-suck-back oil bubbler can isolate water vapor from entering a device system; the waste gas recovery bottle is additionally arranged at the gas outlet of the oil bubbler, because hydrogen chloride gas can be volatilized in the preparation process of the catalyst, the corrosion is strong, the equipment and the surrounding equipment environment are greatly influenced, and the waste gas overflow can be avoided by adopting the aqueous solution waste gas recovery bottle containing sodium hydroxide.
4. According to the device for preparing the olefin polymerization catalyst, the vacuum pipeline three-way valve and the vacuum pressure gauge are preferably arranged between the vacuum pipe and the vacuum pump, the other interface of the vacuum pipeline three-way valve is communicated with the atmosphere, so that the double-row pipe is convenient to carry out vacuum operation, and meanwhile, the vacuum pipeline three-way valve is adjusted before the vacuum pump is closed so that the vacuum pump is connected with the atmosphere, so that the oil suck-back of the vacuum pump can be avoided, and the effect of protecting the vacuum pump is achieved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic view showing the connection relationship between an apparatus for preparing an olefin polymerization catalyst according to an embodiment of the present invention in a case of performing step one;
FIG. 2 is a schematic view showing the connection relationship between the apparatus for preparing an olefin polymerization catalyst according to the embodiment of the present invention when step two is performed;
FIG. 3 is a schematic view showing the connection relationship between the apparatus for preparing an olefin polymerization catalyst according to the embodiment of the present invention when step three is performed;
FIG. 4 is a schematic diagram showing the connection relationship of the apparatus for preparing a catalyst for olefin polymerization according to the embodiment of the present invention when step four is performed.
Description of reference numerals:
1-a nitrogen supply means; 2-a first nitrogen line; 3-a second nitrogen line; 4-double row of tubes; 5-a vacuum pump; 6-a first oil bubbler; 7-a first glass valve; 8-a first reaction device; a 9-nitrogen pipeline three-way valve; 10-a second oil bubbler; 11-a second glass valve; 12-a first stop valve; 13-a second stop valve; 14-vacuum line three-way valve; 15-vacuum pressure gauge; 16-a stirrer; 17-program temperature controller; 18-a second reaction unit; 19-a peristaltic pump; 20-a separation vessel; 21-a cooling device; 22-a cold trap; 23-a dewar flask; 24-waste gas recovery bottle.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "left", "right", etc. indicate orientations or positional relationships based on those shown in the drawings only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" 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 otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
As shown in FIGS. 1 to 4, the present invention provides an apparatus for preparing an olefin polymerization catalyst, comprising:
a nitrogen supply device 1 connected with a first nitrogen pipeline 2 and a second nitrogen pipeline 3;
the double-row pipe 4 is provided with a nitrogen filling pipe, a vacuum pipe and a branch pipe, the vacuum pipe is connected with a vacuum pump 5, one end of the nitrogen filling pipe is communicated with the first nitrogen pipeline 2, the other end of the nitrogen filling pipe is connected with a first oil bubble device 6, and an air outlet of the first oil bubble device 6 is connected with a first glass valve 7;
the first reaction device 8 is used for loading and washing the active center of the catalyst, the first reaction device 8 is communicated with the second nitrogen pipeline 3 through a nitrogen pipeline three-way valve 9, the other interface of the nitrogen pipeline three-way valve 9 is connected with a second oil bubble device 10, and the air outlet of the second oil bubble device 10 is connected with a second glass valve 11.
The utility model integrates the preparation steps of the olefin polymerization catalyst into one device, has simple device and reasonable layout, effectively associates each step, saves space, is convenient for personnel to operate, is convenient for the vacuumizing and nitrogen filling operation of each step, ensures that the preparation process is carried out under the protection of anhydrous, anaerobic and nitrogen, and avoids the adverse effect of water and oxygen in the air on other performances such as catalyst activity and the like.
The nitrogen supply device 1 of the present invention is used for filling nitrogen into the whole preparation device system and providing a nitrogen protection environment, and all the devices capable of realizing the above functions are selected within the protection scope of the present invention, for example, a nitrogen bottle conventionally used in operation can be selected. To the nitrogen supply apparatus 1, a first nitrogen gas line 2 and a second nitrogen gas line 3 are connected.
The first nitrogen pipeline 2 is connected with the double-row pipe 4 and is used for filling nitrogen into each device connected with the double-row pipe 4. The second nitrogen line 3 according to the present invention is connected to the first reaction unit 8 for loading and washing the active sites of the catalyst, for introducing nitrogen into the first reaction unit 8.
As an alternative embodiment of the present invention, the first nitrogen gas line 2 is provided with a first shutoff valve 12, the first shutoff valve 12 being provided between the nitrogen supply device 1 and the double-row pipe 4; and a second stop valve 13 is arranged on the second nitrogen pipeline 3, and the second stop valve 13 is arranged between the nitrogen supply device 1 and the nitrogen pipeline three-way valve 9. The first cutoff valve 12 and the second cutoff valve 13 are used to control the make-and-break of the first nitrogen line 2 and the second nitrogen line 3, respectively.
The double-row pipe 4 is provided with a nitrogen charging pipe, a vacuum pipe and a branch pipe, wherein the nitrogen charging pipe is parallel to the vacuum pipe, the left end and the right end of the nitrogen charging pipe are both open, one end of the vacuum pipe is closed, the other end of the vacuum pipe is open, the nitrogen charging pipe and the vacuum pipe are both communicated with the branch pipe, and the branch pipe, the nitrogen charging pipe and the vacuum pipe are controlled to be connected or disconnected through a piston. The open end of the vacuum tube is connected with a vacuum pump 5 for vacuumizing each device connected with the double-row tube 4. One end of the nitrogen filling pipe is communicated with the first nitrogen pipeline 2, the other end of the nitrogen filling pipe is connected with a first oil bubble device 6, and an air outlet of the first oil bubble device 6 is connected with a first glass valve 7. When the piston on the rotary branch pipe makes its and vacuum tube intercommunication, carry out evacuation work, when the piston on the rotary branch pipe makes its and nitrogen filling pipe intercommunication, carry out nitrogen filling work, the setting up of double row pipe 4 makes evacuation and nitrogen filling operation more convenient, more is favorable to providing anhydrous, anaerobic environment to the preparation system.
As an alternative embodiment of the present invention, a vacuum line three-way valve 14 and a vacuum pressure gauge 15 are disposed between the vacuum pipe and the vacuum pump 5, and another port of the vacuum line three-way valve 14 is communicated with the atmosphere. The arrangement facilitates vacuum operation of the double-row pipe 4, and simultaneously, the vacuum pipeline three-way valve 14 is adjusted before the vacuum pump 5 is closed so that the vacuum pump 5 is connected with the atmosphere, thereby preventing the vacuum pump 5 from sucking oil backwards and playing a role in protecting the vacuum pump 5.
The first reaction device 8 is used for loading and washing active centers of the catalyst. The first reaction device 8 can also realize the on-off of the second nitrogen pipeline 3 through the adjustment of the second stop valve 13 and the nitrogen pipeline three-way valve 9, when the first reaction device 8 needs to be vacuumized and replaced by nitrogen, the second nitrogen pipeline 3 is closed, meanwhile, the first reaction device 8 is connected with the double-row pipe 4, when the vacuumization and the replacement by nitrogen are completed, the connection of the first reaction device 8 and the double-row pipe 4 can be disconnected, the second stop valve 13 and the nitrogen pipeline three-way valve 9 are adjusted to be communicated with the second nitrogen pipeline 3, and at the moment, the second nitrogen pipeline 3 provides nitrogen protection. All devices capable of realizing the functions are selected within the protection scope claimed by the utility model, for example, the first reaction device 8 can select a jacketed five-mouth bottle, a stirrer 16 is installed on the jacketed five-mouth bottle, the jacketed five-mouth bottle is connected with a program temperature controller 17, reaction materials in the jacketed five-mouth bottle are uniformly mixed through the stirrer 16, and the reaction temperature in the jacketed five-mouth bottle is adjusted through the program temperature controller 17.
As an alternative embodiment of the present invention, the apparatus for preparing an olefin polymerization catalyst further comprises: a second reaction device 18 for preparing a catalyst mother liquor, wherein when a nitrogen atmosphere is provided in the second reaction device 18, the second reaction device 18 is communicated with the branch pipes of the double row of pipes 4; when the catalyst mother liquor in the second reaction device 18 is transferred to the first reaction device 8, the second reaction device 18 is communicated with the first reaction device 8 through a peristaltic pump 19. Therefore, the preparation of the catalyst mother liquor can be carried out in the nitrogen atmosphere, and the prepared catalyst mother liquor is transferred to the first reaction device 8 under the protection of nitrogen for the next step. All options for a device capable of performing the above-described functions are within the scope of the claimed invention, for example, the second reaction device 18 may be a three-necked flask.
As an alternative embodiment of the present invention, the apparatus for preparing an olefin polymerization catalyst further comprises: a separation drying means including a separation vessel 20 and a cooling means 21 for separating and drying the catalyst, the separation vessel 20 communicating with the branch pipes of the double row pipes 4 when a nitrogen atmosphere is supplied into the separation vessel 20; when the separation of the catalyst is performed, the separation vessel 20 is communicated with the first reaction device 8; when the solids in the separation vessel 20 are vacuum dried, the cooling device 21 is connected to the separation vessel 20 and the branch pipes of the double row pipe 4, respectively. All the devices capable of realizing the functions are selected within the protection scope claimed by the utility model, for example, the separation container 20 is selected as a reaction tube, the cooling device 21 is selected as a cold trap 22 and a dewar 23, so that the vacuum drying of the catalyst can be realized, and the cold trap and the dewar 23 can cool the solvent into the cold trap, so as to prevent the residual organic solvent in the catalyst from being pumped to the vacuum pump 5 to affect the service life.
The first oil bubbler 6 and the second oil bubbler 10 are used for displaying gas flow rate, and the first glass valve 7 or the second glass valve 11 connected with the gas outlet of the first oil bubbler is used for regulating and controlling the gas outlet flow rate, so that the gas pressure of the first nitrogen pipeline 2 or the second nitrogen pipeline 3 is regulated, the gas pressure in a device connected with the first glass valve is changed, and the transfer of a catalyst or a solvent is realized. For example, when the catalyst is separated, the separation vessel 20 is connected to the first reaction apparatus 8, the separation vessel 20 is connected to the double row pipe 4, the second glass valve 11 is adjusted so that the pressure in the first reaction apparatus 8 is higher than that in the separation vessel 20, the catalyst slurry is transferred from the first reaction apparatus 8 to the separation vessel 20 to be allowed to stand and delaminated, then the first glass valve 7 is adjusted so that the pressure in the separation vessel 20 is higher than that in the first reaction apparatus 8, and the solvent in the upper layer of the separation vessel 20 is transferred to the first reaction apparatus 8, thereby performing solid-liquid separation.
As an alternative embodiment of the present invention, the first oil bubbler 6 and the second oil bubbler 10 are both suck-back-preventing oil bubblers; the air outlets of the first oil bubbler 6 and the second oil bubbler 10 are both connected with a waste gas recovery bottle 24. The anti-suck-back oil bubbler is adopted, so that the installation of a buffer bottle is omitted, unnecessary equipment is reduced, the space is saved, and meanwhile, the liquid paraffin in the anti-suck-back oil bubbler can isolate water vapor from entering a device system; the waste gas recovery bottle 24 is additionally arranged at the gas outlet of the oil bubbler, because hydrogen chloride gas can be volatilized in the preparation process of the catalyst, the catalyst is strong in corrosivity and has great influence on equipment and the environment of peripheral equipment, and the waste gas can be prevented from overflowing by adopting the aqueous solution waste gas recovery bottle 24 containing sodium hydroxide.
The apparatus provided by the present invention and the method for preparing olefin polymerization catalyst using the apparatus will be further described with reference to the following specific examples.
Examples
This example provides an apparatus for preparing an olefin polymerization catalyst, comprising a nitrogen supply apparatus 1 to which a first nitrogen line 2 and a second nitrogen line 3 are connected:
the first nitrogen pipeline 2 is sequentially connected with a first stop valve 12, a double-row pipe 4 and a first oil bubbler 6, wherein the nitrogen pipe of the double-row pipe 4 is communicated with the first nitrogen pipeline 2, a vacuum pipe of the double-row pipe 4 is sequentially connected with a vacuum pipeline three-way valve 14, a vacuum pressure gauge 15 and a vacuum pump 5, and the other interface of the vacuum pipeline three-way valve 14 is communicated with the atmosphere; the first oil bubbler 6 selects an anti-suck-back oil bubbler, the air outlet of the first oil bubbler is connected with a first glass valve 7, and finally a waste gas recovery bottle 24 is introduced;
a second stop valve 13 and a nitrogen pipeline three-way valve 9 are sequentially connected to the second nitrogen pipeline 3, the nitrogen pipeline three-way valve 9 is respectively connected with a second oil bubbler 10 and a first reaction device 8, the second oil bubbler 10 selects an anti-suck-back oil bubbler, an air outlet of the second oil bubbler is connected with a second glass valve 11, and finally a waste gas recovery bottle 24 is introduced, the first reaction device 8 is used for loading and washing an active center of a catalyst, a jacketed five-mouth bottle is selected, a stirrer 16 is installed on the jacketed five-mouth bottle, and the jacketed five-mouth bottle is connected with a program temperature controller 17;
the device also comprises a second reaction device 18 for preparing catalyst mother liquor, a separation container 20 for separating and drying the catalyst and a cooling device 21, wherein the second reaction device 18 selects a three-mouth bottle; the separation container 20 selects a reaction tube; the cooling device 21 selects a cold trap 22 and a dewar 23.
As shown in FIGS. 1 to 4, the steps of preparing the olefin polymerization catalyst by using the apparatus provided in the above embodiment are as follows:
the method comprises the following steps: as shown in fig. 1, the second reaction device 18 is subjected to vacuum nitrogen gas replacement through the double row of tubes 4; when the second stop valve 13 is in a closed state, the nitrogen pipeline three-way valve 9 is adjusted, the second nitrogen pipeline 3 is communicated with the first reaction device 8, the connection between the second nitrogen pipeline 3 and the second oil bubbler 10 is disconnected, the first reaction device 8 and the double-row pipe 4 are connected, and the first reaction device 8 is subjected to vacuum nitrogen replacement through the double-row pipe 4; after the replacement is finished, under the nitrogen protection state, a second stop valve 13 is opened, a nitrogen pipeline three-way valve 9 is adjusted to a three-way pipeline full-connection state, a pipeline connecting the first reaction device 8 and the double-row pipe 4 is removed, and the nitrogen protection of the first reaction device 8 is provided by a second nitrogen pipeline 3; the operation of preparing the catalyst mother liquor is carried out in the second reaction device 18;
step two: as shown in fig. 2, the second reaction device 18 is connected with the first reaction device 8 through a peristaltic pump 19 under the protection of nitrogen, and the prepared catalyst mother liquor in the second reaction device 18 is transferred into the first reaction device 8; removing the second reaction device 18 and the peristaltic pump 19; the operations of loading and washing the active sites of the catalyst are carried out in the first reaction device 8;
step three: as shown in fig. 3, after the loading and washing of the catalyst active center in the first reactor 8 are completed, the separator 20 is connected to the branch pipes of the double row pipe 4 and the first reactor 8, and the double row pipe 4 provides nitrogen protection to the separator 20; adjusting the opening degree of the second glass valve 11 to make the air pressure in the first reaction device 8 higher than that in the separation container 20 under the stirring state of the catalyst, so that the catalyst slurry in the first reaction device 8 is transferred to the separation container 20; after the catalyst slurry is settled in the separation container 20 to separate the catalyst solid from the solvent liquid, the opening degree of the first glass valve 7 is adjusted to make the air pressure in the separation container 20 higher than that in the first reaction device 8, so that the upper layer of the solvent is transferred to the first reaction device 8; the operation is repeated for a plurality of times to completely transfer the catalyst slurry into the separation container 20 and remove redundant solvent in the catalyst, thereby facilitating the drying operation;
step four: as shown in fig. 4, the separation container 20 is disconnected from the branch pipes of the double row pipe 4, the cooling device 21 is connected with the separation container 20, specifically, the cold trap 22 is respectively connected with the double row pipe 4 and the separation container 20, the cold trap is cooled by a dewar 23 filled with liquid nitrogen, and then the drying of the solid in the separation container 20 is completed by a vacuum drying method, and finally the powdery catalyst is obtained.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the utility model.
Claims (10)
1. An apparatus for preparing an olefin polymerization catalyst, comprising:
the nitrogen supply device is connected with a first nitrogen pipeline and a second nitrogen pipeline;
the double-row pipe is provided with a nitrogen filling pipe, a vacuum pipe and a branch pipe, the vacuum pipe is connected with a vacuum pump, one end of the nitrogen filling pipe is communicated with the first nitrogen pipeline, the other end of the nitrogen filling pipe is connected with a first oil bubble device, and an air outlet of the first oil bubble device is connected with a first glass valve;
the first reaction device is used for loading and washing the active center of the catalyst, the first reaction device is communicated with the second nitrogen pipeline through a nitrogen pipeline three-way valve, the other interface of the nitrogen pipeline three-way valve is connected with a second oil bubble device, and the gas outlet of the second oil bubble device is connected with a second glass valve.
2. The apparatus for preparing an olefin polymerization catalyst according to claim 1, further comprising:
the second reaction device is used for preparing catalyst mother liquor, is communicated with the branch pipes of the double-row pipes and is used for providing a nitrogen atmosphere into the second reaction device; the second reaction device is communicated with the first reaction device through a peristaltic pump and is used for transferring the catalyst mother liquor in the second reaction device to the first reaction device.
3. The apparatus for preparing an olefin polymerization catalyst according to claim 1, further comprising:
the separation drying device comprises a separation container and a cooling device and is used for separating and drying the catalyst, and the separation container is communicated with the branch pipes of the double-row pipes and is used for providing a nitrogen atmosphere into the separation container; the separation container is communicated with the first reaction device and is used for separating the catalyst; and the cooling device is respectively communicated with the separation container and the branch pipes of the double-row pipes and is used for carrying out vacuum drying on the solid in the separation container.
4. The apparatus for preparing olefin polymerization catalyst according to claim 1, wherein the first reaction device is a jacketed five-neck flask, a stirrer is installed on the jacketed five-neck flask, and the jacketed five-neck flask is connected with a program temperature controller; the nitrogen supply device is a nitrogen cylinder.
5. The apparatus for preparing olefin polymerization catalyst according to claim 2, wherein the second reaction unit is a three-necked flask.
6. The apparatus for preparing an olefin polymerization catalyst according to claim 3, wherein the separation vessel is selected from a reaction tube; the cooling device selects a cold trap and a Dewar flask.
7. The apparatus for preparing olefin polymerization catalyst according to claim 1, wherein the first oil bubbler and the second oil bubbler are reverse suction oil bubblers.
8. The apparatus for preparing olefin polymerization catalyst according to claim 7, wherein the gas outlets of the first and second oil bubblers are connected with a waste gas recovery bottle.
9. The apparatus for preparing olefin polymerization catalyst according to claim 1, wherein a vacuum line three-way valve and a vacuum pressure gauge are disposed between the vacuum pipe and the vacuum pump, and another port of the vacuum line three-way valve is connected to the atmosphere.
10. The apparatus for preparing an olefin polymerization catalyst according to claim 1,
a first stop valve is arranged on the first nitrogen pipeline and is arranged between the nitrogen supply device and the double-row pipe;
and a second stop valve is arranged on the second nitrogen pipeline, and the second stop valve is arranged between the nitrogen supply device and the nitrogen pipeline three-way valve.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202220473875.3U CN216972393U (en) | 2022-03-03 | 2022-03-03 | Device for preparing olefin polymerization catalyst |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202220473875.3U CN216972393U (en) | 2022-03-03 | 2022-03-03 | Device for preparing olefin polymerization catalyst |
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