CN113698513B - Preparation method and application of catalyst - Google Patents
Preparation method and application of catalyst Download PDFInfo
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- CN113698513B CN113698513B CN202010437337.4A CN202010437337A CN113698513B CN 113698513 B CN113698513 B CN 113698513B CN 202010437337 A CN202010437337 A CN 202010437337A CN 113698513 B CN113698513 B CN 113698513B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F10/04—Monomers containing three or four carbon atoms
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The invention relates to the field of catalyst preparation, and discloses a preparation method and application of a catalyst. The method comprises the following steps: 1) After the main catalyst storage unit makes the main catalyst and the vaseline oil make first contact, a first mixture is obtained, and the first mixture is sent to the main catalyst preparation unit; 2) The vaseline fat is conveyed from the vaseline fat storage unit to the main catalyst preparation unit through the vaseline fat conveying unit; 3) Carrying out second contact on the first mixture and vaseline fat in a main catalyst preparation unit to obtain a second mixture; 4) And (3) feeding the second mixture into a catalyst pre-contact unit, and then carrying out third contact with a cocatalyst to obtain the catalyst. The method can solve the problem that the solid catalyst is attached to the container during feeding, reduces the waste of the catalyst, does not generate the container with the residual catalyst, is environment-friendly and economical, and is simple and convenient to operate.
Description
Technical Field
The invention relates to the field of catalyst preparation, in particular to a preparation method of a catalyst used in polypropylene production.
Background
In the current continuous polypropylene production process, either the SPHERIPOL process or the ST process is adopted, the catalyst is prepared by adding a solid catalyst into a mixture of vaseline oil and vaseline fat, or by adding the vaseline oil, the solid catalyst and the vaseline fat in sequence and then mixing. In actual industrial production, the solid catalyst is generally added by pouring the solid catalyst directly from its packaging container into a catalyst preparation tank.
Because the solid catalyst particles are smaller and are easy to absorb moisture and are in powder form, the solid catalyst particles can be partially adhered to the wall of a packaging container when being poured, and cannot be completely poured out, and even under the beating and vibration of an oscillator, a small amount of solid catalyst particles still remain adhered. Especially in wet summer, the solid catalyst sticking phenomenon is more serious. Therefore, not only is the waste of production raw materials caused, but also the treatment of the catalyst container makes the production enterprises face serious environmental protection pressure because the catalyst belongs to dangerous chemicals. In addition, when the catalyst is prepared by the method, even though the catalyst is stirred, the solid catalyst is difficult to be completely and uniformly dispersed in vaseline oil and vaseline grease, and part of the solid catalyst is not uniformly dispersed to cause agglomeration and caking, so that blocks with different sizes are formed, and the blocks also block a pipeline, so that the smooth production is influenced.
Disclosure of Invention
The invention aims to overcome the problems, and provides a preparation method of a catalyst, which can solve the problem that the catalyst is attached to a container when solid catalyst is fed, can reduce the waste of the catalyst, can not generate the container with the catalyst left, is environment-friendly and economical, and is simple and convenient to operate.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for preparing a catalyst, comprising the steps of:
1) After the main catalyst storage unit 100 makes the main catalyst and the vaseline oil make a first contact, a first mixture is obtained, and the first mixture is sent to the main catalyst preparation unit 300;
2) Transferring the petrolatum from the petrolatum storage unit 200 to the main catalyst formulation unit 300 through the petrolatum transfer unit;
3) The first mixture and petrolatum are subjected to a second contact in the main catalyst formulation unit 300 to obtain a second mixture;
4) After the second mixture is fed to the catalyst precontacting unit 400, it is subjected to a third contact with a cocatalyst to obtain a catalyst.
Preferably, in step 1), the main catalyst is a spherical polypropylene catalyst for loop processes.
Preferably, the main catalyst is a DQC401 catalyst and/or an HR catalyst; more preferably, the main catalyst is DQC401 catalyst.
Preferably, the mass-to-volume ratio of the main catalyst to the vaseline oil is 1:2.5-4kg/L, preferably 1:2.8-3.2kg/L, more preferably 1:3-3.2kg/L.
Preferably, the method further comprises: the step of mixing the first mixture is performed before the first mixture is fed to the main catalyst formulation unit 300.
Preferably, the mixing is performed by rotating the main catalyst storage unit 100 on the main catalyst tank drum 120.
Preferably, the time of the rotation is 8 to 48 hours, more preferably 16 to 48 hours, still more preferably 24 to 48 hours.
Preferably, the main catalyst storage unit 100 is a storage tank.
Preferably, the first mixture in the main catalyst storage unit 100 is fed to the main catalyst formulation unit 300 using an inert gas N.
Preferably, the inert gas N is N 2 CO and CO 2 One or more of (a), preferably N 2 。
Preferably, the inert gas N has a pressure of 0.2 to 0.6MPa, preferably 0.3 to 0.6MPa, more preferably 0.4 to 0.5MPa.
Preferably, in step 2), the petrolatum storage unit 200 is a storage tank.
Preferably, the petrolatum storage unit 200 has a stirrer 201 and a bubbler 202.
Preferably, in the petrolatum fat storage unit 200, the petrolatum is agitated in the presence of an inert gas N prior to delivery to the main catalyst formulation unit 300.
Preferably, the inert gas N is N 2 CO and CO 2 One or more of (a), preferably N 2 。
Preferably, the stirring temperature is 60-90 ℃ and the stirring time is 8-48h; more preferably, the stirring temperature is 70-90 ℃ and the stirring time is 16-48h; further preferably, the stirring temperature is 70-80 ℃ and the stirring time is 24-48h.
Preferably, in step 2), the petrolatum fat delivery unit includes a pipe connecting the petrolatum fat storage unit 200 with the main catalyst formulation unit 300, and a petrolatum fat delivery pump 210 and a petrolatum fat filter 220 provided on the pipe.
Preferably, the mass-to-volume ratio of the main catalyst to the petrolatum is 1:1.3-2kg/L, preferably 1:1.4-1.8kg/L, more preferably 1:1.5-1.7kg/L.
Preferably, in step 3), the main catalyst formulation unit 300 is a formulation tank.
Preferably, the main catalyst preparation unit 300 has a stirrer 301, and the main catalyst preparation unit 300 is vacuumized and stirred after the first mixture and the petrolatum are transferred to the main catalyst preparation unit 300.
Preferably, the degree of vacuum of the evacuation is 1 to 50mmHg, preferably 15 to 25mmHg.
Preferably, the temperature of the stirring is 60-80 ℃, and the stirring time is 4-96h.
Preferably, the method further comprises reducing the temperature of the second mixture to 8-12 ℃ before delivering the second mixture to the catalyst precontacting unit 400.
Preferably, the cocatalyst is triethylaluminium.
Preferably, the mass ratio of the main catalyst to the cocatalyst is 1:0.2-1, preferably 1:0.2-0.8; more preferably 1:0.3-0.5.
The second aspect of the invention provides the use of the above catalyst formulation method in the formulation of polypropylene catalysts.
Through the technical scheme, the main catalyst and the vaseline oil are mixed in the main catalyst storage unit in advance, and then the main catalyst preparation unit and the vaseline oil are introduced to be mixed, so that the problem that part of the main catalyst remains in the packaging container when the main catalyst is directly fed into the main catalyst preparation unit is solved. The invention can not only avoid the polypropylene manufacturer from processing the catalyst packaging container, but also improve the caking phenomenon generated in the catalyst preparation process and the production quality. In addition, the main catalyst storage device for mixing the main catalyst and the vaseline oil can be recycled after being cleaned, so that the resource waste is further reduced.
Drawings
FIG. 1 is a simplified schematic of the catalyst formulation process of the present invention.
Description of the reference numerals
100: the main catalyst storage unit 120: main catalyst tank rotary drum
111. 112, 113: solenoid valve 200: vaseline grease storage unit
201. 301, 401: stirrer 202: bubbling device
210: petrolatum delivery pump 220: vaseline grease filter
300: main catalyst formulation unit 310: main catalyst filter
320: metering pump 400: catalyst precontacting unit
N: inert gas
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
FIG. 1 is a simplified schematic of the catalyst formulation process of the present invention. As shown in fig. 1, the preparation method of the catalyst provided by the invention comprises the following steps:
1) After the main catalyst storage unit 100 makes the main catalyst and the vaseline oil make a first contact, a first mixture is obtained, and the first mixture is sent to the main catalyst preparation unit 300;
2) Transferring the petrolatum from the petrolatum storage unit 200 to the main catalyst formulation unit 300 through the petrolatum transfer unit;
3) The first mixture and petrolatum are subjected to a second contact in the main catalyst formulation unit 300 to obtain a second mixture;
4) After the second mixture is fed to the catalyst precontacting unit 400, it is subjected to a third contact with a cocatalyst to obtain a catalyst.
The preparation method of the catalyst can be applied to the preparation of the catalyst used in the polypropylene production, in the current polypropylene production, polypropylene production enterprises purchase main catalysts from catalyst manufacturers and then prepare the main catalysts with vaseline grease and vaseline oil on production sites, and part of the main catalysts remain on the wall of a packaging container during the catalyst feeding process, so that the main catalysts are difficult to completely feed, not only can waste production raw materials be caused, but also the container with the main catalysts remains has the problem of difficult treatment.
In the invention, the main catalyst and vaseline oil are stored in the main catalyst storage tank in advance, the whole catalyst is transported to a polypropylene preparation manufacturer, and an empty tank for storing the main catalyst can be recovered, cleaned and reused after the catalyst preparation is completed. Therefore, the problems of catalyst residue and difficult treatment of the container with the catalyst residue in the prior art can be solved simultaneously, waste is reduced, and recycling of resources is realized.
According to the invention, in step 1), the main catalyst may be various spherical polypropylene catalysts for loop processes, for example, DQC401 catalyst and/or HR catalyst, preferably DQC401 catalyst.
According to the present invention, in step 1), the amounts of the procatalyst and the vaseline oil may vary within a wide range, so long as the procatalyst can be uniformly dispersed, without particular limitation. The amount of the vaseline oil can be determined according to the amount of the main catalyst, and preferably, the mass volume ratio of the main catalyst to the vaseline oil is 1:2.5-4kg/L, preferably 1:2.8-3.2kg/L, more preferably 1:3-3.2kg/L.
According to the present invention, in step 1), the main catalyst storage unit 100 may be various devices for storage in the art, so long as the purpose of storage and transportation can be satisfied, without particular limitation. Preferably, the main catalyst storage unit 100 is a storage tank.
In the present invention, in order to prevent the main catalyst from oxidative deterioration in contact with air, affecting the catalyst activity, the main catalyst storage unit 100 may introduce an inert gas so that the first contact is performed under the protection of the inert gas.
The inert gas introduced may be various gases which do not react with the main catalyst. The kind of the inert gas is not particularly limited, and may be, for example, N 2 CO and CO 2 One or more of (a), preferably N 2 。
In the present invention, the pressure of the inert gas filled in the main catalyst storage unit may be 0.01 to 0.06Mpa, preferably 0.03 to 0.05Mpa.
In the present invention, the main catalyst storage unit 100 may be rotated on the main catalyst tank drum 120, thereby mixing the first mixture in the main catalyst storage unit 100.
In the present invention, after the first contact is completed, the main catalyst storage unit 100 is preferably rotated on the main catalyst tank drum 120 for 8 to 48 hours before being fed into the main catalyst preparation unit 300 for main catalyst preparation; more preferably, the main catalyst storage unit 100 is rotated on the main catalyst tank drum 120 for 16 to 48 hours; it is further preferred that the main catalyst storage unit 100 is rotated on the main catalyst tank drum 120 for 24 to 48 hours. Through the rotation within the above time range, the first mixture in the main catalyst storage unit 100 can be uniformly mixed, which is not only advantageous for dispersion of the main catalyst, but also can prevent agglomeration of the main catalyst, prevent clogging of pipes during transfer, and facilitate subsequent preparation.
According to the present invention, the first mixture in the main catalyst storage unit 100 may be fed to the main catalyst preparation unit 300 through a main catalyst delivery unit including a pipe and solenoid valves 112, 113 provided on the pipe.
According to the present invention, the first mixture may be fed to the main catalyst formulation unit 300 using an inert gas N. The inert gas N is not particularly limited as long as it does not affect the activity of the catalyst. The inert gas N may be N 2 CO and CO 2 One or more of (a), preferably N 2 。
In the present invention, the pressure of the inert gas N is not particularly limited as long as the first mixture can be fed to the main catalyst preparation unit 300. Preferably, the inert gas N has a pressure of 0.2 to 0.6MPa, preferably 0.3 to 0.6MPa, more preferably 0.4 to 0.5MPa.
According to the present invention, in step 2), the petrolatum storage unit 200 may be various storage devices commonly used in the art, for example, may be a storage tank.
Preferably, the petrolatum storage unit 200 has a stirrer 201 and a bubbler 202.
According to the present invention, before the petrolatum is fed into the main catalyst preparing unit 300, the inert gas N may be blown into the petrolatum storage unit 200 by the bubbler 202, and the moisture in the petrolatum may be removed under the combined action of the blowing of the inert gas N and the stirring of the stirrer 201, so as to achieve the purpose of drying and dehydrating the petrolatum, and prevent the main catalyst from being adversely affected by the presence of the moisture in the subsequent steps.
According to the present invention, the inert gas N blown in by the bubbler is not particularly limited as long as it does not affect the catalyst activity, and may be, for example, N 2 CO and CO 2 One or more of (a), preferably N 2 。
According to the present invention, the amount of air taken in the bubbler can be varied within a wide range, and is not particularly limited, and may be, for example, 1 to 10Nm 3 Preferably 5-10Nm per hour 3 /h。
According to the present invention, in order to sufficiently dehydrate petrolatum, preferably, the stirring temperature is 60-90 ℃ and the stirring time is 8-48 hours; more preferably, the stirring temperature is 70-90 ℃ and the stirring time is 16-48h; further preferably, the stirring temperature is 70-80 ℃ and the stirring time is 24-48h.
According to the present invention, in step 2), the petrolatum lipid delivery unit comprises a pipe and a petrolatum lipid delivery pump 210 and a petrolatum lipid filter 220 mounted on the pipe. The petrolatum delivery pump 210 is configured to provide power and the petrolatum filter 220 is configured to filter the petrolatum to prevent the agglomerated petrolatum from clogging the tubing.
In the present invention, one end of the petrolatum fat delivery unit is connected to the petrolatum fat storage unit 200, and the other end is connected to the main catalyst formulation unit 300, so that petrolatum is fed from the petrolatum fat storage unit 200 to the main catalyst formulation unit 300.
In step 3) according to the present invention, the main catalyst formulation unit 300 may be various devices for performing catalyst formulation commonly used in the art, for example, a formulation tank. Preferably, the main catalyst formulation unit 300 has a stirrer 301, which can stir the contents of the formulation unit. Preferably, the main catalyst formulation unit 300 may regulate temperature.
In the present invention, the main catalyst preparation unit 300 may be preheated in advance, and then the first mixture and the petrolatum may be fed into the main catalyst preparation unit 300 to be mixed. This can shorten the preparation time of the catalyst.
According to the present invention, the amount of the petrolatum may vary widely, and is not particularly limited. The amount of petrolatum may be determined according to the amount of the main catalyst, preferably, the mass to volume ratio of the main catalyst to the petrolatum is 1:1.3-2kg/L, preferably 1:1.4-1.8kg/L, more preferably 1:1.5-1.7kg/L.
After the first mixture and petrolatum are fed into the main catalyst preparing unit 300, the main catalyst preparing unit 300 is vacuumized and stirred in order to prevent air from adversely affecting the main catalyst. Preferably, the vacuum degree of the vacuuming is 1-50mmHg, more preferably, the vacuum degree of the vacuuming is 15-25mmHg.
According to the present invention, in order to uniformly mix the first mixture and the petrolatum, preferably, the temperature of the stirring is 60 to 80 ℃, and the time of the stirring is 4 to 96 hours; more preferably, the temperature of the stirring is 65-75 ℃, and the stirring time is 48-72h.
According to the present invention, in order to ensure that the temperature of the catalyst slurry is consistent with that of the propylene as a reaction raw material, to avoid breakage of the polymer produced by the prepolymerization, the second mixture is subjected to a temperature-reducing treatment before being fed to the catalyst precontacting unit 400. Preferably, the temperature of the second mixture is reduced to 8-12 ℃; more preferably, the temperature of the second mixture is reduced to 9-11 ℃.
According to the present invention, in step 4), the second mixture is fed to the catalyst precontacting unit 400 through a main catalyst transfer unit including a pipe and a filter 310 and a metering pump 320 provided on the pipe. The filter 310 is used to filter the second mixture to further prevent the catalyst from clogging the pipe. Metering pump 320 is used to meter the amount of the second mixture fed to catalyst precontacting unit 400 to calculate the amount of subsequent promoters.
In the present invention, in order to form the activation center of the main catalyst, for example, ti 4+ Reduction to Ti 3+ The present invention uses a cocatalyst which may be various cocatalysts used in the art to prepare polypropylene, for example, triethylaluminum.
According to the present invention, the second mixture is subjected to a third contact with the cocatalyst in the catalyst precontacting unit 400. The catalyst precontacting unit 400 may be a contact tank, and preferably, the catalyst precontacting unit 400 has a stirrer 401.
In the present invention, the amount of the cocatalyst may be determined according to the amount of the main catalyst, and preferably, the mass ratio of the main catalyst to the cocatalyst is 1:0.2-1, preferably 1:0.2-0.8; more preferably 1:0.3-0.5.
According to the present invention, in order to secure the stereospecificity of the polymer, an external electron DONOR, which may be various external electron DONORs commonly used in the art for preparing polypropylene, such as one or more of methylcyclohexyldimethoxy silane (C-DONOR), dicyclopentyl dimethoxy silane (D-DONOR), tetraethoxy silane (T-DONOR) and diisopropyldimethoxy silane (P-DONOR), may be further added in the third contact of the precontacting unit, in addition to the second mixture and the cocatalyst, and preferably, the electron DONOR is methylcyclohexyldimethoxy silane (C-DONOR).
In the present invention, the amount of the external electron donor may be determined according to the amount of the main catalyst, and preferably, the mass ratio of the main catalyst to the external electron donor is 1:0.01-0.15, preferably 1:0.01-0.1; more preferably 1:0.01-0.03.
According to the present invention, the second mixture, the cocatalyst and the external electron donor are sufficiently mixed after precontacting in the catalyst precontacting unit 400, and the mixing can be achieved by stirring with a stirrer 401. The stirring temperature is 8-12 ℃, the stirring time is 1-10min, preferably, the stirring temperature is 9-11 ℃, and the stirring time is 3-5min.
The second aspect of the invention provides an application of the preparation method of the catalyst in preparation of polypropylene catalysts.
The present invention will be described in detail with reference to examples, but the present invention is not limited to the examples. In the following examples, the reagents used were commercially available unless otherwise specified.
Example 1
1) 80kg of the main catalyst DQC401 and 248L of vaseline oil are put into a main catalyst storage tank with the volume of 460L to obtain a first mixture, and the main catalyst storage tank is filled with nitrogen until the pressure is 0.05Mpa and then is transported to a polypropylene manufacturer.
2) Before preparing the catalyst, the main catalyst storage tank is rotated on a catalyst tank rotary drum for 24 hours, and then the first mixture is sent into a main catalyst preparation tank preheated to 70 ℃ by nitrogen with the pressure of 0.5 Mpa;
3) After 124L of petrolatum was charged into the petrolatum storage tank, the bubbler was opened to introduce nitrogen while stirring, and the amount of nitrogen introduced into the bubbler was 5Nm 3 And/h, stirring at 70 ℃ for 24h. Filtering by a vaseline grease delivery pump through a vaseline grease filter, and delivering into a main catalyst preparation tank preheated to 70 ℃;
wherein step 2) and step 3) may be performed simultaneously.
4) Vacuumizing the main catalyst preparation tank and stirring the second mixture, wherein the vacuum degree is 20mmHg, the stirring temperature is 70 ℃, and the stirring time is 48 hours; after stirring, the temperature of the second mixture in the main catalyst formulation tank was reduced to 10 ℃.
5) The second mixture obtained in step 4) was fed to a catalyst precontacting tank via a main catalyst filter and a metering pump, mixed with 24kg of triethylaluminum and 0.8kg of methylcyclohexyldimethoxy silane (C-DONOR) in the precontacting tank, and stirred at 10℃for 4 minutes to obtain a catalyst.
Example 2
The procedure of example 1 was followed, except that the amount of the main catalyst was 80kg, the amount of vaseline oil was 240L, the amount of vaseline oil was 120L, the amount of the cocatalyst was 40kg, and the amount of the external electron donor was 2.4kg.
Example 3
The procedure of example 1 was followed, except that the amount of the main catalyst was 80kg, the amount of vaseline oil was 256L, the amount of vaseline oil was 136L, the amount of the cocatalyst was 32kg, and the amount of the external electron donor was 1.6kg.
According to the technical scheme, the main catalyst and the vaseline oil are mixed in the main catalyst storage tank (main catalyst storage unit) in advance, and then the main catalyst preparation tank (main catalyst preparation unit) and the vaseline oil are introduced to be mixed again, so that the problem that part of the main catalyst remains in the packaging container when the main catalyst is directly fed into the main catalyst preparation tank is solved. In addition, the main catalyst storage tank for mixing the main catalyst and the vaseline oil can be cleaned and then recycled, so that the resource waste is further reduced.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner without contradiction. The various possible combinations of the invention are not described in detail in order to avoid unnecessary repetition.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (33)
1. A method of preparing a catalyst, comprising the steps of:
1) After the main catalyst storage unit (100) makes the main catalyst and the vaseline oil make a first contact, a first mixture is obtained, and the first mixture is sent to the main catalyst preparation unit (300);
2) Transferring petrolatum from a petrolatum storage unit (200) to a main catalyst formulation unit (300) through a petrolatum delivery unit, the petrolatum storage unit (200) having an agitator (201) and a bubbler (202);
3) Carrying out second contact on the first mixture and vaseline fat in a main catalyst preparation unit (300) to obtain a second mixture;
4) The second mixture is fed into a catalyst pre-contact unit (400) and then is subjected to third contact with a cocatalyst to obtain a catalyst,
wherein the method further comprises: a step of mixing the first mixture before feeding it to the main catalyst formulation unit (300), said mixing being carried out by rotating the main catalyst storage unit (100) on the main catalyst tank drum (120);
the main catalyst is a spherical polypropylene catalyst for a loop process;
the first mixture in the main catalyst storage unit (100) is sent to the main catalyst preparation unit (300) by using inert gas;
in a petrolatum fat storage unit (200), stirring the petrolatum fat in the presence of inert gas before delivering the petrolatum fat to a main catalyst preparation unit (300), wherein the stirring temperature is 60-90 ℃ and the stirring time is 8-48h;
before the vaseline fat is sent to the main catalyst preparation unit (300), inert gas is blown into the vaseline fat storage unit (200) by using a bubbler (202), and the air inflow of the bubbler is 1-10Nm 3 /h。
2. The method for preparing a catalyst according to claim 1, wherein the main catalyst is DQC401 catalyst and/or HR catalyst.
3. The method for preparing a catalyst according to claim 2, wherein the main catalyst is DQC401 catalyst.
4. The method for preparing the catalyst according to claim 1, wherein the mass-to-volume ratio of the main catalyst to the vaseline oil is 1:2.5-4kg/L.
5. The method for preparing the catalyst according to claim 4, wherein the mass-to-volume ratio of the main catalyst to the vaseline oil is 1:2.8-3.2kg/L.
6. The method for preparing the catalyst according to claim 5, wherein the mass-to-volume ratio of the main catalyst to the vaseline oil is 1:3-3.2kg/L.
7. The method for preparing a catalyst according to claim 1, wherein the time of rotation is 8 to 48 hours.
8. The method for preparing a catalyst according to claim 7, wherein the time of rotation is 16-48 hours.
9. The method for preparing a catalyst according to claim 8, wherein the time of rotation is 24 to 48 hours.
10. The method for preparing a catalyst according to claim 1, wherein the main catalyst storage unit (100) is a storage tank.
11. The method for preparing a catalyst according to any one of claims 1 to 10, wherein the inert gas is N 2 And/or CO 2 。
12. The method for preparing a catalyst according to claim 11, wherein the inert gas is N 2 。
13. The method for preparing a catalyst according to any one of claims 1 to 10, wherein the inert gas has a pressure of 0.2 to 0.6MPa.
14. The method for preparing a catalyst according to claim 13, wherein the inert gas has a pressure of 0.3 to 0.6MPa.
15. The method for preparing a catalyst according to claim 14, wherein the inert gas has a pressure of 0.4 to 0.5MPa.
16. The method of preparing a catalyst according to any one of claims 1 to 10, wherein in step 2), the petrolatum lipid storage unit (200) is a storage tank.
17. The method for preparing a catalyst according to any one of claims 1 to 10, wherein the stirring temperature is 70 to 90 ℃ and the stirring time is 16 to 48 hours.
18. The method for preparing a catalyst according to claim 17, wherein the stirring temperature is 70-80 ℃ and the stirring time is 24-48 hours.
19. The method of preparing a catalyst according to any one of claims 1 to 10, wherein in step 2), the petrolatum fat delivery unit comprises a pipe connecting a petrolatum fat storage unit (200) with a main catalyst preparation unit (300), and a petrolatum fat delivery pump (210) and a petrolatum fat filter (220) provided on the pipe.
20. The method for preparing a catalyst according to any one of claims 1 to 10, wherein the mass to volume ratio of the main catalyst to the petrolatum is 1:1.3-2kg/L.
21. The method for preparing the catalyst according to claim 20, wherein the mass-to-volume ratio of the main catalyst to the petrolatum is 1:1.4-1.8kg/L.
22. The method for preparing the catalyst according to claim 21, wherein the mass-to-volume ratio of the main catalyst to the petrolatum is 1:1.5-1.7kg/L.
23. The catalyst preparation method according to any one of claims 1 to 10, wherein in step 3), the main catalyst preparation unit (300) is a preparation tank.
24. The method of preparing a catalyst according to claim 23, wherein the main catalyst preparing unit (300) has a stirrer (301), and the main catalyst preparing unit (300) is evacuated and stirred after the first mixture and the petrolatum are transferred to the main catalyst preparing unit (300).
25. The method for preparing a catalyst according to claim 24, wherein the degree of vacuum of the vacuum is 1 to 50mmHg.
26. The method for preparing a catalyst according to claim 25, wherein the degree of vacuum of the vacuum is 15 to 25mmHg.
27. The method for preparing a catalyst according to claim 24, wherein the temperature of stirring is 60-80 ℃ and the time of stirring is 4-96 hours.
28. The method of formulating a catalyst according to any one of claims 1-10, wherein the method further comprises reducing the temperature of the second mixture to 8-12 ℃ prior to delivering the second mixture to the catalyst precontacting unit (400).
29. The method of preparing a catalyst according to any one of claims 1 to 10, wherein the cocatalyst is triethylaluminum.
30. The method for preparing a catalyst according to any one of claims 1 to 10, wherein the mass ratio of the main catalyst to the cocatalyst is 1:0.2-1.
31. The method for preparing a catalyst according to claim 30, wherein the mass ratio of the main catalyst to the cocatalyst is 1:0.2-0.8.
32. The method for preparing a catalyst according to claim 31, wherein the mass ratio of the main catalyst to the cocatalyst is 1:0.3-0.5.
33. Use of the method of formulating a catalyst according to any one of claims 1 to 32 in the formulation of a polypropylene catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010437337.4A CN113698513B (en) | 2020-05-21 | 2020-05-21 | Preparation method and application of catalyst |
Applications Claiming Priority (1)
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