CN115894174A - Preparation method of dialkoxy magnesium carrier for olefin polymerization catalyst - Google Patents
Preparation method of dialkoxy magnesium carrier for olefin polymerization catalyst Download PDFInfo
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- CN115894174A CN115894174A CN202211469203.6A CN202211469203A CN115894174A CN 115894174 A CN115894174 A CN 115894174A CN 202211469203 A CN202211469203 A CN 202211469203A CN 115894174 A CN115894174 A CN 115894174A
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- alcohol
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- magnesium powder
- dialkoxy magnesium
- carrier
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 22
- 239000011777 magnesium Substances 0.000 title claims abstract description 22
- 150000001336 alkenes Chemical class 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 239000002685 polymerization catalyst Substances 0.000 title claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- -1 amide compound Chemical class 0.000 claims abstract description 14
- 238000010992 reflux Methods 0.000 claims abstract description 13
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000001257 hydrogen Substances 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 239000011261 inert gas Substances 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 125000003118 aryl group Chemical group 0.000 claims description 4
- 125000000623 heterocyclic group Chemical group 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 229910052736 halogen Inorganic materials 0.000 claims description 3
- 150000002367 halogens Chemical group 0.000 claims description 3
- 229910052740 iodine Inorganic materials 0.000 claims description 3
- 239000011630 iodine Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 125000000547 substituted alkyl group Chemical group 0.000 claims description 2
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000003999 initiator Substances 0.000 abstract description 3
- 230000003321 amplification Effects 0.000 abstract description 2
- 238000011161 development Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- XDKQUSKHRIUJEO-UHFFFAOYSA-N magnesium;ethanolate Chemical compound [Mg+2].CC[O-].CC[O-] XDKQUSKHRIUJEO-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000036632 reaction speed Effects 0.000 description 3
- 238000001953 recrystallisation Methods 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- VBTQNRFWXBXZQR-UHFFFAOYSA-N n-bromoacetamide Chemical compound CC(=O)NBr VBTQNRFWXBXZQR-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 238000001226 reprecipitation Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000011954 Ziegler–Natta catalyst Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012662 bulk polymerization Methods 0.000 description 1
- 230000021523 carboxylation Effects 0.000 description 1
- 238000006473 carboxylation reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000010960 commercial process Methods 0.000 description 1
- 238000006114 decarboxylation reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000012685 gas phase polymerization Methods 0.000 description 1
- HONQAQNYJBKAMA-UHFFFAOYSA-L magnesium;ethyl carbonate Chemical compound [Mg+2].CCOC([O-])=O.CCOC([O-])=O HONQAQNYJBKAMA-UHFFFAOYSA-L 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
Abstract
The invention relates to a preparation method of a dialkoxy magnesium carrier for an olefin polymerization catalyst, belonging to the field of new material development. The method comprises the following steps: (1) Under the protection of inert gas, adding halogenated amide compound, metal magnesium powder and alcohol into a reactor, stirring, and heating for reflux reaction; (2) And after hydrogen is completely discharged, continuously preserving the heat, cooling, washing and drying to obtain the dialkoxy magnesium carrier. The preparation method has simple process, does not need complex operation, and is suitable for amplification and industrial production. The reaction condition is mild, the cost of raw materials is low, and the use of expensive initiators is avoided. The method can obtain uniform spherical dialkoxy magnesium carrier particles with controllable particle size.
Description
Technical Field
The invention relates to a preparation method of a dialkoxy magnesium carrier for an olefin polymerization catalyst, belonging to the field of new material development.
Background
Currently, magnesium chloride supported Ziegler-Natta catalysts are one of the most widely used catalysts for the polymerization of olefins such as polypropylene, polyethylene, etc. The Ziegler-Natta catalysts supported on magnesium chloride are generally solid catalysts of magnesium, titanium, halogen and consisting of organic compounds of the electron-donating type. When propylene is polymerized to produce polypropylene, the magnesium chloride-supported Ziegler-Natta catalyst may be used in a mixture with an organoaluminum compound as a cocatalyst and an organosilane compound as a stereoregulating agent in an appropriate ratio. The catalytic system is currently used in a variety of polymerization processes, particularly in a variety of commercial processes such as slurry polymerization, bulk polymerization, gas phase polymerization, and the like. Such catalytic systems, in addition to meeting the basic requirements of high catalytic activity and stereoregularity, also meet various requirements of particle morphology, such as suitable particle size and shape, uniform particle size distribution, minimal amounts of large or fine particles, and high apparent density.
The olefin polymer catalyst preparation method is used for adjusting the particle size morphology of the carrier by a recrystallization and reprecipitation method, a spray drying method, an electrochemical method, or the like. Among them, recrystallization and reprecipitation methods have difficulty in adjusting the particle morphology and size of the carrier under the preparation conditions.
The method for preparing a catalyst using magnesium dialkyl obtained by reacting magnesium metal with alcohols as a carrier has recently become a research focus in the art because it can ensure a highly active catalyst and a polymer product having high stereoregularity. However, in the case of using dialkoxy magnesium as a support, since the morphology and size distribution of dialkoxy magnesium particles and the apparent density directly affect the particle characteristics of the catalyst and the polymerization product, it is necessary to prepare a dialkoxy magnesium support having a uniform size, a spherical shape, and a sufficiently high apparent density during the reaction of metallic magnesium with alcohols. In particular, a large amount of the large particle carrier causes deterioration of the flowability of the polymerization product, and it is difficult to meet the demand for industrial production.
Various methods for producing dialkoxy magnesium having a uniform shape have been disclosed in the prior art documents. US patent US5162277 discloses the following process: carboxylating amorphous diethoxymagnesium with carbon dioxide to obtain magnesium ethylcarbonate, followed by recrystallization using various different or mixed solvents in the presence of additives to obtain a carrier having a size of 5 to 10 μm. The same concept and method is used in US 5955396. Japanese patent laid-open No. H06-87773 adopts the following method: and (3) carrying out spray drying on the diethoxymagnesium alcohol solution after carbon dioxide carboxylation. Then, decarboxylation reaction is carried out to prepare spherical particles. However, these methods have disadvantages that the process is complicated, the kinds of raw materials used are large, and the particle size and morphology of the carrier cannot be appropriately provided as required.
Japanese patent laid-open Nos. H03-74341, 04-36891 and 08-73388 provide a method for synthesizing spherical or ellipsoidal diethoxymagnesium by reacting metallic magnesium with ethanol in the presence of iodine. However, in the production process, a large amount of reaction heat and hydrogen gas are generated, and since the reaction is rapid, it is not only difficult to control the reaction rate, but also there is a problem that the resultant diethoxymagnesium carrier contains a large amount of fine particles or irregularly shaped large particles formed by agglomeration of multiple particles. Thus, when a catalyst prepared according to the method is used for olefin polymerization, it causes excessive polymer particle size and the exothermic heat of polymerization generated during the polymerization destroys particle shape, causing serious adverse consequences in the process.
Disclosure of Invention
In order to solve the above-mentioned problems occurring in the prior art, the present invention provides a method for preparing a dialkoxy magnesium support for an olefin polymerization catalyst. The method takes halogenated amide compound as an initiator and takes metal magnesium powder and alcohol as reaction raw materials to prepare the dialkoxy magnesium carrier, thereby adjusting the particle size and the shape of the olefin polymerization catalyst.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for preparing a dialkoxymagnesium support for an olefin polymerization catalyst, the method comprising the steps of:
(1) Under the protection of inert gas, adding halogenated amide compound, metal magnesium powder and alcohol into a reactor, stirring, and heating for reflux reaction;
(2) And after hydrogen is completely discharged, continuously preserving the heat, cooling, washing and drying to obtain the dialkoxy magnesium carrier.
In the above technical solution, further, in the step (1), the halogenated amide compound is a compound having the following general formula:
wherein: r is alkyl, aryl, substituted alkyl, aryl, heterocycle or substituted heterocycle; x is halogen, including chlorine, bromine or iodine.
In the above-mentioned embodiment, in the step (1), the particle diameter of the magnesium metal powder is 10 to 500 μm, preferably 50 to 200 μm. If the average particle diameter of the metal magnesium is less than 10 μm, the average particle diameter of the carrier to be produced is too fine to be used; if it exceeds 500. Mu.m, the average particle size of the resulting carrier becomes too large, and the morphology of the carrier is difficult to form a uniform spherical shape.
In the above technical solution, in the step (1), the alcohol is one or more of C1 to C6 aliphatic alcohols and aromatic alcohols, preferably one or more of methanol, ethanol and propanol, and more preferably ethanol; the aliphatic alcohol comprises methanol, ethanol, n-propanol, isopropanol, n-butanol, and cyclohexanol.
In the above technical solution, further, in the step (1), the mass ratio of the halogenated amide compound to the metal magnesium powder is 0.001 to 0.2:1. if it is less than 0.001:1, the reaction speed is slow, such as more than 0.2:1, the resulting particles are oversized or produce a large amount of fines.
In the above technical solution, further, the usage ratio of the metal magnesium powder to the alcohol is: the mass of the metal magnesium powder is that the volume of the alcohol is =1g (5-50) ml, and preferably 1g (7-20) ml. If the using amount of the alcohol is too small, the alcohol is difficult to stir uniformly; if the amount of the alcohol is too large, the surface of the particles becomes rough because the apparent density of the carrier of the product to be produced decreases.
In the above technical solution, in the step (1), the stirring speed is 50 to 300rpm/min, preferably 70 to 250rpm/min. If the stirring speed is out of this range, the particles will be non-uniform.
In the above technical solution, further, in the step (1), the reflux reaction temperature is 60 to 90 ℃, and the reflux reaction time is 0.5 to 10 hours, preferably 1 to 5 hours. When the temperature is lower than 60 ℃, the reaction speed is too slow; when the temperature is higher than 90 ℃, the reaction speed is too fast, the amount of fine particles increases, and a coagulation and agglomeration phenomenon occurs, and a uniform spherical carrier of a desired size cannot be obtained.
In the above technical scheme, further, in the step (2), the heat preservation time is 0.5-10 h, and then the temperature is reduced to 10-50 ℃.
In the above technical solution, further, in the step (2), one or more of hydrocarbons and ethers are used for the washing.
In the above technical solution, further, in the step (2), the drying is performed for 0.5 to 10 hours under nitrogen.
In the above technical solution, further, the dialkoxy magnesium carrier is spherical, and the particle size is 10 to 80 μm.
Compared with the prior art, the invention has the following beneficial effects:
1. the preparation method has simple process, does not need complex operation, and is suitable for amplification and industrial production.
2. The reaction condition is mild, the cost of raw materials is low, and the use of expensive initiator is avoided.
3. The invention can obtain uniform spherical dialkoxy magnesium carrier particles with controllable particle size.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the invention to these specific embodiments. It will be appreciated by those skilled in the art that the present invention encompasses all alternatives, modifications and equivalents as may be included within the scope of the claims.
Example 1
After a sufficient replacement with nitrogen gas was performed in a 5L glass reaction flask equipped with a stirrer, a heating jacket, and a reflux condenser, 2g N-bromoacetamide, 60g of magnesium metal (powder having an average particle size of 100 μm), 800mL of anhydrous ethanol were charged, and stirred at a stirring speed of 240rpm/min, and the reaction flask was heated to 78 ℃ to maintain ethanol reflux. After 5min of reaction, hydrogen was generated indicating initiation of the reaction. After all hydrogen is discharged, the reflux reaction is continued for 2h, the temperature is reduced to 50 ℃, and the mixture is washed for 3 times by using 2000mL of normal hexane. The washed product was dried under nitrogen for 24h to give 270g (95% yield) of a white powdery solid with good fluidity.
The dried product was suspended in n-hexane and subjected to particle size measurement by a laser particle sizer by a light transmission method, resulting in an average particle diameter of 17 μm.
Example 2
After a sufficient replacement with nitrogen gas was performed in a 5L glass reaction flask equipped with a stirrer, a heating jacket, and a reflux condenser, 3g N-bromoacetamide, 60g of magnesium metal (powder having an average particle size of 100 μm), 800mL of anhydrous ethanol were charged, and stirred at a stirring speed of 240rpm/min, and the reaction flask was heated to 78 ℃ to maintain ethanol reflux. After 5min of reaction, hydrogen was generated indicating initiation of the reaction. After all hydrogen is discharged, the reflux reaction is continued for 2h, the temperature is reduced to 50 ℃, and the mixture is washed for 3 times by using 2000mL of normal hexane. The washed product was dried under nitrogen for 24h to give 265g (94% yield) of a white powdery solid with good flowability.
The dried product was suspended in n-hexane and subjected to particle size measurement by a laser particle sizer by a light transmission method, resulting in an average particle diameter of 30 μm.
The above examples are intended to be illustrative of the present invention and are not intended to limit the invention to these particular embodiments. Other variations and modifications within the spirit and scope of the invention and the appended claims will occur to persons skilled in the art and are intended to be covered by the invention.
Claims (9)
1. A method for preparing a dialkoxymagnesium support for an olefin polymerization catalyst, characterized by comprising the steps of:
(1) Under the protection of inert gas, adding halogenated amide compound, metal magnesium powder and alcohol into a reactor, stirring, and heating for reflux reaction;
(2) And after hydrogen is completely discharged, continuously preserving the heat, cooling, washing and drying to obtain the dialkoxy magnesium carrier.
2. The process according to claim 1, wherein in the step (1), the halogenated amide compound is a compound having the following general formula:
wherein: r is alkyl, aryl, substituted alkyl, aryl, heterocycle or substituted heterocycle; x is halogen, including chlorine, bromine or iodine;
the particle size of the metal magnesium powder is 10-500 mu m;
the alcohol is one or more of C1-C6 aliphatic alcohol and aromatic alcohol; the aliphatic alcohol comprises methanol, ethanol, n-propanol, isopropanol, n-butanol, and cyclohexanol.
3. The production method according to claim 1, wherein in the step (1), the mass ratio of the halogenated amide compound to the metallic magnesium powder is 0.001 to 0.2:1;
the dosage ratio of the metal magnesium powder to the alcohol is as follows: the mass of the metal magnesium powder is that the volume of the alcohol is =1g, (5-50) ml.
4. The production method according to claim 1, wherein in the step (1), the stirring speed is 50 to 300rpm/min.
5. The preparation method according to claim 1, wherein in the step (1), the reflux reaction temperature is 60-90 ℃ and the reflux reaction time is 0.5-10 h.
6. The preparation method according to claim 1, wherein in the step (2), the heat preservation time is 0.5-10 h, and then the temperature is reduced to 10-50 ℃.
7. The method according to claim 1, wherein in step (2), the washing is carried out using one or more of hydrocarbons and ethers.
8. The method according to claim 1, wherein in the step (2), the drying is performed under nitrogen for 0.5 to 10 hours.
9. The method according to claim 1, wherein the dialkoxymagnesium support has a spherical shape with a particle diameter of 10 to 80 μm.
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| CN202211469203.6A CN115894174A (en) | 2022-11-22 | 2022-11-22 | Preparation method of dialkoxy magnesium carrier for olefin polymerization catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134789A (en) * | 2006-08-30 | 2008-03-05 | 三星Total株式会社 | Method for preparation of spherical support for olefin polymerization catalyst |
| JP2009102478A (en) * | 2007-10-22 | 2009-05-14 | Toho Titanium Co Ltd | Method for synthesizing alkoxy magnesium, method for manufacturing solid catalyst component for polymerizing olefins and catalyst therefor |
| CN101802023A (en) * | 2007-12-12 | 2010-08-11 | 三星Total株式会社 | Method of preparation of spherical support for olefin polymerization catalyst |
| CN102089078A (en) * | 2008-07-11 | 2011-06-08 | 三星Total株式会社 | Method for controlling size of spherical carrier for olefin polymerization catalyst |
| CN105777490A (en) * | 2016-04-18 | 2016-07-20 | 德州元光工贸有限公司 | Preparation method of large-particle size magnesium ethylate |
| CN105801352A (en) * | 2016-04-18 | 2016-07-27 | 德州元光工贸有限公司 | Preparation method of spherical magnesium ethylate |
-
2022
- 2022-11-22 CN CN202211469203.6A patent/CN115894174A/en active Pending
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| CN101134789A (en) * | 2006-08-30 | 2008-03-05 | 三星Total株式会社 | Method for preparation of spherical support for olefin polymerization catalyst |
| JP2009102478A (en) * | 2007-10-22 | 2009-05-14 | Toho Titanium Co Ltd | Method for synthesizing alkoxy magnesium, method for manufacturing solid catalyst component for polymerizing olefins and catalyst therefor |
| CN101802023A (en) * | 2007-12-12 | 2010-08-11 | 三星Total株式会社 | Method of preparation of spherical support for olefin polymerization catalyst |
| CN102089078A (en) * | 2008-07-11 | 2011-06-08 | 三星Total株式会社 | Method for controlling size of spherical carrier for olefin polymerization catalyst |
| CN105777490A (en) * | 2016-04-18 | 2016-07-20 | 德州元光工贸有限公司 | Preparation method of large-particle size magnesium ethylate |
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