CN108102013B - Composition of alkoxy magnesium particles and preparation method thereof - Google Patents
Composition of alkoxy magnesium particles and preparation method thereof Download PDFInfo
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- CN108102013B CN108102013B CN201810018036.0A CN201810018036A CN108102013B CN 108102013 B CN108102013 B CN 108102013B CN 201810018036 A CN201810018036 A CN 201810018036A CN 108102013 B CN108102013 B CN 108102013B
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- -1 alkoxy magnesium Chemical compound 0.000 title claims abstract description 73
- 239000002245 particle Substances 0.000 title claims abstract description 67
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 49
- 239000011777 magnesium Substances 0.000 title claims abstract description 49
- 239000000203 mixture Substances 0.000 title claims description 9
- 238000002360 preparation method Methods 0.000 title claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 64
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000126 substance Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 19
- 229920000136 polysorbate Polymers 0.000 claims abstract description 15
- 238000009826 distribution Methods 0.000 claims abstract description 9
- 150000001298 alcohols Chemical class 0.000 claims abstract description 7
- 235000019441 ethanol Nutrition 0.000 claims description 62
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 18
- 229910052740 iodine Inorganic materials 0.000 claims description 18
- 239000011630 iodine Substances 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 239000012265 solid product Substances 0.000 claims description 4
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims description 3
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 3
- 229920006395 saturated elastomer Polymers 0.000 claims description 3
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 1
- 150000001336 alkenes Chemical class 0.000 abstract description 4
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002685 polymerization catalyst Substances 0.000 abstract description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 15
- 239000003054 catalyst Substances 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 229920001214 Polysorbate 60 Polymers 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229920000098 polyolefin Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- MGWAVDBGNNKXQV-UHFFFAOYSA-N diisobutyl phthalate Chemical compound CC(C)COC(=O)C1=CC=CC=C1C(=O)OCC(C)C MGWAVDBGNNKXQV-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000009969 flowable effect Effects 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- XDKQUSKHRIUJEO-UHFFFAOYSA-N magnesium;ethanolate Chemical compound [Mg+2].CC[O-].CC[O-] XDKQUSKHRIUJEO-UHFFFAOYSA-N 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000011085 pressure filtration Methods 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000006114 decarboxylation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- AHUXYBVKTIBBJW-UHFFFAOYSA-N dimethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C1=CC=CC=C1 AHUXYBVKTIBBJW-UHFFFAOYSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000037048 polymerization activity Effects 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
- C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F110/04—Monomers containing three or four carbon atoms
- C08F110/06—Propene
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
Abstract
The invention discloses a component of spherical alkoxy magnesium particles and a method for preparing the spherical alkoxy magnesium particles. According to the invention, a certain amount of Tween substances are introduced into alcohol or mixed alcohol compounds, and contact reaction is carried out on the Tween substances and metal magnesium powder to prepare alkoxy magnesium; the obtained alkoxy magnesium particles have perfect shapes, high sphericity, higher stacking density and uniform and narrow particle size distribution. Meanwhile, the alkoxy magnesium particles can be used for preparing olefin polymerization catalysts.
Description
Technical Field
The invention relates to the field of preparation of alkoxy magnesium, in particular to a component of spherical alkoxy magnesium particles and a method for preparing the spherical alkoxy magnesium particles by using the component.
Background
As is well known, with the development of economy, the demand of polyolefin materials is higher and higher nowadays, and the high-efficiency polyolefin catalyst for producing polyolefin materials is widely applied in the field of polyolefin catalysts due to the well-controlled particle morphology and microstructure. The key role is the composition and microstructure of the carrier, and the carriers obtained by different methods correspondingly obtain catalysts with different structures and performances.
The use of magnesium alkoxides as supports for high performance catalysts is disclosed in a number of patent documents, and catalysts prepared with magnesium alkoxides supports have significantly higher activity, good hydrogen response and excellent copolymerisation performance. In recent years, there are various methods for preparing magnesium alkoxide reported in published technical literature, and the following methods are mainly used: one is a method in which magnesium metal is reacted with an alcohol in the presence of iodine to obtain spherical or ellipsoidal magnesium diethoxide as disclosed in Japanese patent laid-open Nos. 03-74341 and 04-368391, however, it is difficult to control the reaction rate appropriately, the obtained product is inevitably produced in the form of non-uniform large particles or fine powder, and the bulk density is generally low; another method is a spray drying process of diethoxymagnesium alcohol solution disclosed in Japanese patent laid-open No. 6-8733, which can prepare spherical particles and then perform decarboxylation treatment, and the process is complicated and expensive, and the obtained product is difficult to decarboxylate completely, and the product quality is difficult to meet the downstream use; in addition, there is a method in which magnesium metal is reacted with alcohol to obtain magnesium alkoxide, and then the magnesium alkoxide is mechanically ground to control the particle size, and this method has a problem in that the obtained product has non-uniform particle size, which seriously affects the use.
The invention aims to overcome the defects in the prior art and obtain regular spherical alkoxy magnesium particles with good morphology by adopting a simpler and more practical preparation method.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a component of spherical alkoxy magnesium particles, the spherical alkoxy magnesium particles prepared by the component have perfect shapes, high sphericity and higher bulk density, and the bulk density is more than or equal to 0.30 g/mL; the particles are uniform and have narrow particle size distribution, and the particle size distribution is less than or equal to 1.2; can be used as a carrier for preparing olefin polymerization catalysts. Another object of the present invention is to provide a method for preparing spherical magnesium alkoxide particles.
In order to achieve the purpose, the invention adopts the following technical scheme:
a composition of spherical magnesium alkoxide particles, the composition comprising the following components: metal magnesium powder, alcohol or mixed alcohol compounds, iodine simple substance and tween substances.
Further, the molar ratio of the alcohol or mixed alcohol compound to the metal magnesium powder is as follows: 2-40; the molar ratio of the iodine simple substance to the metal magnesium powder is as follows: 0.0001 to 0.2; the proportion of the tween substances added into the alcohol or the mixed alcohol compound is 0.001-500 g/L.
Further, the alcohol or mixed alcohol compound is shown as a general formula R1OH, wherein R is1Is C1～C20The hydrocarbon group of (b) may be a saturated or unsaturated linear, branched or cyclic chain.
Further, the alcohol or mixed alcohol compound includes, but is not limited to, a mixture of one or more of methanol, ethanol, isopropanol, n-butanol, n-hexanol, isooctanol, benzyl alcohol, and phenethyl alcohol.
Further, the molar ratio of the alcohol or mixed alcohol compound to the metal magnesium powder is as follows: 4 to 30.
Further, the molar ratio of the iodine simple substance to the metal magnesium powder is as follows: 0.001 to 0.1.
Further, the proportion of the tween substances added with the alcohol or the mixed alcohol compound is 0.01-200 g/L.
A method of making spherical magnesium alkoxide particles, the method comprising: under the protection of inert gas, dissolving the Tween substance in the alcohol or mixed alcohol compound, dissolving the iodine simple substance in the alcohol or mixed alcohol compound, adding the metal magnesium powder, and heating to the reflux temperature to maintain the reaction until no gas is generated; and washing and drying the solid product generated by the reaction to obtain the alkoxy magnesium particles.
Further, the spherical magnesium alkoxide particles prepared by the method have an average particle diameter of 15 to 120 microns and a particle size distribution Span ═ d90 to d10)/d50 of less than or equal to 1.2.
Further, the spherical magnesium alkoxide particles produced by the method have a bulk density greater than or equal to 0.30 g/mL.
The invention has the following beneficial technical effects:
1. the reaction material composition is simple, and the production cost is favorably reduced;
2. after the Tween substances are introduced, the obtained large particles and fine powder of the alkoxy magnesium particles are fewer, and the particle size distribution is narrower;
3. the alkoxy magnesium has perfect particle shape, good particle sphericity and suitable composition and structure for being used as a carrier of an olefin polymerization catalyst.
Detailed Description
Hereinafter, embodiments of the present invention will be described in further detail with reference to examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The invention provides a component of spherical alkoxy magnesium particles, which comprises the following components: metal magnesium powder, alcohol or mixed alcohol compounds, iodine simple substance and tween substances; wherein, the mol ratio of the alcohol or the mixed alcohol compound to the metal magnesium powder is as follows: 2 to 40, preferably 4 to 30, when the amount of the alcohol or the mixed alcohol compound is too small, the viscosity of the reaction system is rapidly increased, and the reaction system cannot be effectively and uniformly dispersed, so that the generated particles are deteriorated, and when the amount of the alcohol or the mixed alcohol compound is too large, the stacking density of the generated magnesium alkoxide particles is generally low, the strength of the particles is also poor, and the performance improvement of a subsequent catalyst is not facilitated. The molar ratio of the iodine simple substance to the metal magnesium powder is as follows: 0.0001 to 0.2, preferably 0.001 to 0.1, to control a suitable initial reaction rate. The adding proportion of the tween substances to the alcohol or the mixed alcohol compound is 0.001-500 g/L, and the preferable adding proportion is 0.01-200 g/L.
In the method for preparing the magnesium alkoxide particles, the shape of the used magnesium metal powder particles is not strictly limited, but the powder with the average particle size of 5-350 microns, preferably 20-200 microns is required, so that the average particle size of the generated magnesium alkoxide particles is controlled to be 15-120 microns, the reactivity of the particles can be ensured to be relatively uniform, and the particle shape of the magnesium alkoxide particles is relatively perfect and uniform.
The alcohol or mixed alcohol compound of the invention is shown as the general formula R1OH, wherein R is1Is C1～C20The hydrocarbon group of (b) may be a saturated or unsaturated linear, branched or cyclic chain; the alcohol or mixed alcohol compound includes but is not limited to one or more of methanol, ethanol, isopropanol, n-butanol, n-hexanol, isooctanol, benzyl alcohol, and phenethyl alcohol; ethanol is preferred. In order to ensure the excellent performance of the prepared alkoxy magnesium, the water content in the alcohol is preferably as low as possible, generally controlled to be less than 1000ppm, preferably less than 200 ppm.
The adding sequence of the reaction raw materials in the method for preparing the spherical alkoxy magnesium particles is not strictly specified, and can be determined according to requirements. The magnesium powder can be added at one time or added in batches, the reaction rate can be controlled well by adding in batches, the reaction can be carried out at 0-100 ℃, generally, the reaction rate is faster when the temperature is higher, and the reaction is better controlled at the reflux temperature. The reaction time is generally 1 to 20 hours, preferably 2 to 10 hours, until no gas is generated. The solid product after the reaction may be washed several times with a mixed alcohol before the reaction or ordinary ethanol (water content less than 200ppm), or may be washed with an inert organic solvent such as hexane, toluene, etc., and then dried to obtain magnesium alkoxide particles. The whole process is completed under the protection of inert gas, wherein the inert gas is helium, argon or nitrogen, and the nitrogen is preferably used in the invention.
The invention will be further illustrated with reference to specific examples:
example 1
Fully replacing a reactor with high-purity nitrogen, sequentially adding 0.1 g of Tween-60, 20 ml of absolute ethyl alcohol and 0.1 g of iodine under the protection of nitrogen, stirring to dissolve, heating, adding 1.0 g of 80-150-mesh magnesium powder and 10 ml of absolute ethyl alcohol, maintaining reflux reaction, adding 1.0 g of 80-150-mesh magnesium powder and 10 ml of absolute ethyl alcohol again at intervals of 20 minutes, adding 4.0 g of magnesium powder and 55 ml of absolute ethyl alcohol in 4 times, maintaining reflux reaction for 4 hours after adding materials, washing twice with absolute ethyl alcohol, wherein the amount of absolute ethyl alcohol is 80 ml each time, washing twice with hexane, the amount of hexane is 100 ml each time, and drying to obtain off-white solid flowable powder after washing is finished, wherein specific results are shown in table 1.
Example 2
This example differs from example 1 only in that: "0.1 g of Tween-60" in example 1 was adjusted to "0.5 g of Tween-60".
Example 3
This example differs from example 1 only in that: the "0.1 g of iodine" in example 1 was adjusted to "0.4 g of iodine".
Example 4
This example differs from example 1 only in that: the "20 ml of absolute ethanol" in example 1 was adjusted to "50 ml of absolute ethanol".
Example 5
This example differs from example 1 only in that: "0.1 g of Tween-60" in example 1 was adjusted to "2.0 g of Tween-60".
Comparative example 1
Fully replacing a reactor with high-purity nitrogen, sequentially adding 15 ml of absolute ethyl alcohol and 0.15 g of iodine under the protection of nitrogen, stirring to dissolve, heating, adding 1.0 g of 80-150-mesh magnesium powder and 10 ml of absolute ethyl alcohol, maintaining a reflux reaction, adding 1.0 g of 80-150-mesh magnesium powder and 10 ml of absolute ethyl alcohol again at intervals of 20 minutes, adding 4.0 g of magnesium powder and 55 ml of absolute ethyl alcohol in 4 times in total, maintaining the reflux reaction for 4 hours after adding materials, washing twice with absolute ethyl alcohol, wherein the amount of absolute ethyl alcohol in each time is 80 ml, washing twice with hexane, the amount of hexane in each time is 100 ml, and drying to obtain off-white solid flowable powder after washing is finished, wherein specific results are shown in table 1.
Example 6
The magnesium alkoxide particles prepared by the invention can be used for synthesizing catalyst components for olefin polymerization: adding 50 ml of titanium tetrachloride into a reactor repeatedly replaced by high-purity nitrogen, cooling to 0 ℃, adding 5g of alkoxy magnesium particles obtained in example 1, slowly heating to 80 ℃, adding 1.5 ml of DIBP (diisobutyl phthalate), continuously heating to 110, maintaining the reaction for 2 hours, then performing pressure filtration on the liquid to be clean, adding 50 ml of titanium tetrachloride again, heating to 110, maintaining the reaction for 2 hours, performing pressure filtration on the liquid to be clean, repeating the process again, washing the obtained solid for 3 times at 50 ℃ by using 100 ml of hexane, and finally drying to obtain solid catalyst powder.
Polymerization of propylene: after the reactor was purged with high-purity nitrogen gas by full displacement, 1.5mmol of triethylaluminum and 0.1mmol of diphenyldimethoxysilane were added, 10mg of the above catalyst was further added, 2.5L of liquid propylene and 1L of hydrogen (under a standard condition) were added under stirring, and the reaction was maintained at 70 ℃ for 1 hour to obtain 586 g of a polymer having a bulk density of 0.41g/ml and a melt index of 3.75g/10 min.
TABLE 1
As shown in Table 1, the magnesium alkoxide prepared in examples 1 to 5 had a good particle morphology, a high bulk density and a narrow particle distribution, compared to the comparative example. Meanwhile, from the results of example 6, the catalyst prepared by using the magnesium alkoxide particles has high propylene polymerization activity and high bulk density, and is suitable for the production of polypropylene.
The test method involved in the invention is as follows:
1. particle size and distribution of support and catalyst: the MASTERSIZE particle size distribution instrument uses n-hexane as a dispersing agent, and the measuring range is 0.02-2000 mu m. span ═ D (D)90-D10)/D50。
2. Determination of bulk density: DIN-53194.
3. The sphericity of the particles is determined using the CAMSIZER apparatus standard from Retsch, Germany.
The above description is only for the purpose of illustrating the present invention, and it should be understood that the present invention is not limited to the above embodiments, and various modifications conforming to the spirit of the present invention are within the scope of the present invention.
Claims (8)
1. Spherical alkoxy magnesium particles are characterized by being prepared from the following components: metal magnesium powder, alcohol or mixed alcohol compounds, iodine simple substance and tween substances; the molar ratio of the alcohol or mixed alcohol compound to the metal magnesium powder is 2-40: 1; the molar ratio of the iodine simple substance to the metal magnesium powder is 0.0001-0.2: 1; the proportion of adding alcohol or mixed alcohol compounds into the Tween substances is 0.01-200 g/L; under the protection of inert gas, dissolving the Tween substance in the alcohol or mixed alcohol compound, dissolving the iodine simple substance in the alcohol or mixed alcohol compound, adding the metal magnesium powder, and heating to the reflux temperature to maintain the reaction until no gas is generated; and washing and drying the solid product generated by the reaction to obtain the alkoxy magnesium particles.
2. The spherical magnesium alkoxide particles of claim 1, wherein the alcohol or mixed alcohol compound is of formula R1OH, wherein R is1Is C1～C20The hydrocarbon group of (b) is a saturated or unsaturated linear, branched or cyclic chain.
3. The spherical magnesium alkoxide particles according to claim 1, wherein the alcohol or mixed alcohol compound comprises a mixture of one or more of methanol, ethanol, isopropanol, n-butanol, n-hexanol, isooctanol, benzyl alcohol, phenethyl alcohol.
4. The spherical alkoxy magnesium particles according to claim 1, wherein the molar ratio of the alcohol or mixed alcohol compound to the metal magnesium powder is 4 to 30: 1.
5. the spherical alkoxy magnesium particle according to claim 1, wherein the molar ratio of the elemental iodine to the magnesium metal powder is 0.001-0.1: 1.
6. the preparation method of the spherical alkoxy magnesium particles is characterized in that the spherical alkoxy magnesium particles are prepared from the following components: metal magnesium powder, alcohol or mixed alcohol compounds, iodine simple substance and tween substances; the molar ratio of the alcohol or mixed alcohol compound to the metal magnesium powder is 2-40: 1; the molar ratio of the iodine simple substance to the metal magnesium powder is 0.0001-0.2: 1; the proportion of adding alcohol or mixed alcohol compounds into the Tween substances is 0.01-200 g/L; the method comprises the following steps: under the protection of inert gas, dissolving the Tween substance in the alcohol or mixed alcohol compound, dissolving the iodine simple substance in the alcohol or mixed alcohol compound, adding the metal magnesium powder, and heating to the reflux temperature to maintain the reaction until no gas is generated; and washing and drying the solid product generated by the reaction to obtain the alkoxy magnesium particles.
7. The method according to claim 6, wherein the spherical magnesium alkoxide particles produced by the method have an average particle diameter of 15 to 120 μm and a particle diameter distribution Span = (d90-d10)/d50 of 1.2 or less.
8. The method of claim 6, wherein the spherical magnesium alkoxide particles produced by the method have a bulk density of 0.30g/mL or greater.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2004269467A (en) * | 2003-03-12 | 2004-09-30 | Toho Catalyst Co Ltd | Production method for dialkoxy magnesium, and solid catalyst component and catalyst for polymerization of olefins |
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| JPS59133209A (en) * | 1983-01-20 | 1984-07-31 | Chisso Corp | Support for olefin polymerization catalyst |
| CN1034736C (en) * | 1994-04-08 | 1997-04-30 | 中国科学院化学研究所 | Olefinic polymeric carrier catalyst system and preparation method thereof |
| CN101906017A (en) * | 2009-06-04 | 2010-12-08 | 中国石油化工股份有限公司 | Method for preparing alkoxyl magnesium solid particles |
| CN102453127B (en) * | 2010-10-19 | 2013-06-05 | 中国石油化工股份有限公司 | Spherical carrier for olefin polymerization catalyst and preparation method thereof |
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| JP2004269467A (en) * | 2003-03-12 | 2004-09-30 | Toho Catalyst Co Ltd | Production method for dialkoxy magnesium, and solid catalyst component and catalyst for polymerization of olefins |
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